GB1565144A - Creation of Inventions and Patents with Artificial Intelligence

GB1565144A – Carbon black process and apparatus for the production thereof
– Google Patents

GB1565144A – Carbon black process and apparatus for the production thereof
– Google Patents
Carbon black process and apparatus for the production thereof

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Publication number
GB1565144A

GB1565144A
GB18061/77A
GB1806177A
GB1565144A
GB 1565144 A
GB1565144 A
GB 1565144A
GB 18061/77 A
GB18061/77 A
GB 18061/77A
GB 1806177 A
GB1806177 A
GB 1806177A
GB 1565144 A
GB1565144 A
GB 1565144A
Authority
GB
United Kingdom
Prior art keywords
reaction section
carbon black
inches
reactor
rubber
Prior art date
1976-04-30
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)

Expired

Application number
GB18061/77A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

Phillips Petroleum Co

Original Assignee
Phillips Petroleum Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
1976-04-30
Filing date
1977-04-29
Publication date
1980-04-16

1977-04-29
Application filed by Phillips Petroleum Co
filed
Critical
Phillips Petroleum Co

1980-04-16
Publication of GB1565144A
publication
Critical
patent/GB1565144A/en

Status
Expired
legal-status
Critical
Current

Links

Espacenet

Global Dossier

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carbon black
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-1
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antioxidant agent
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methane
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C
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ethoxyquin
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n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine
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diphenylamine
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octadecanoic acid
Chemical compound

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stearic acid
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2,2,4-trimethyl-1h-quinoline
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dimethylcarbamothioyl n,n-dimethylcarbamodithioate
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Carbon
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Classifications

C—CHEMISTRY; METALLURGY

C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR

C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS

C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black

C09C1/44—Carbon

C09C1/48—Carbon black

C09C1/50—Furnace black ; Preparation thereof

C—CHEMISTRY; METALLURGY

C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON

C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients

C08K3/00—Use of inorganic substances as compounding ingredients

C08K3/02—Elements

C08K3/04—Carbon

C—CHEMISTRY; METALLURGY

C01—INORGANIC CHEMISTRY

C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

C01P2006/00—Physical properties of inorganic compounds

C01P2006/10—Solid density

C—CHEMISTRY; METALLURGY

C01—INORGANIC CHEMISTRY

C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

C01P2006/00—Physical properties of inorganic compounds

C01P2006/12—Surface area

C—CHEMISTRY; METALLURGY

C01—INORGANIC CHEMISTRY

C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

C01P2006/00—Physical properties of inorganic compounds

C01P2006/19—Oil-absorption capacity, e.g. DBP values

Description

PATENT SPECIFICATION ( 11) 1 565 144
( 21) Application No 18061/77 ( 22) Filed 29 Apr 1977 ( 19) N ( 31) Convention Application No 681977 ( 32) Filed 30 Apr 1976 in At ( 33) United States of America (US)
At ( 44) Complete Specification Published 16 Apr 1980
V) ( 51) INT CL 3 CO 9 C 1/48 C 08 K 3/04 ( 52) Index at Acceptance C 1 A J 1 J 201 J 243 J 246 J 300 J 302 J 685 J 701 J 703 J 712 J 714 J 717 J 719 J 721 J 722 J 724 J 731 J 732 J 734 J 741 J 743 J 744 J 755 J 761 J 765 J 766 C 3 K 100 400 MA ( 54) CARBON BLACK, PROCESS AND APPARATUS FOR THE PRODUCTION THEREOF ( 71) We, PHILLIPS PETROLEUM COMPANY, a corporation organised and existing under the laws of the State of Delaware, United States of America, of Bartlesville, Oklahoma, United States of America, do hereby declare the invention for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:-
This invention relates to carbon black In a more specific aspect, this invention relates to rubber compositions contaning carbon black Furthermore, the invention relates to carbon black reactors in which carbon blacks can be made.
A broad variety of carbon blacks have been disclosed in the art These blacks differ in many properties from each other and are made by different procedures The main field of 10 use of the blacks depends upon their properties Since the carbon black as such cannot be sufficiently characterized by its chemical composition or by its ingredients, it has become widely accepted to characterize the carbon black by the properties it exhibits Thus the carbon black can, e g, be characterized by its surface area which is, as usually, an inverse measurement of the nodule size Another important characteristic of the carbon black is its 15 structure, which is a measure of the complexity of the individual carbon black aggregates or of the number of nodules “fused” together in one carbon black aggregate.
Great efforts have been made in the industry to correlate properties of rubbers incorporating carbon black and properties of carbon black Unfortunately, there is not one single property of carbon black that, if made high or low enough, results in an ideal rubber 20 composition Certain properties of carbon black are related to abrasion of the rubber composition; others are related to the tensile strength; others are related to the heat buildup.
Efforts have been made to correlate the tint or tinting strength of carbon black to the abrasion resistance of rubbers In this connection the statement has been made that 25 high-tint carbon black incorporated in rubber results in highly abrasionresistance rubber compositions As will be shown, no such correlation exists.
High abrasion resistance of a carbon black/rubber composition is one desirable property of such a composition Another desirable property is low heat buildup or low hysteresis.
The heat buildup is a measurement of how much of the elastic deformation energy put into 30 a carbon black/rubber composition remains in his composition as heat after the deformation forces have been released The hysteresis, or heat buildup, is measured by measuring the temperature of a sample subjected to deformations This property, hysteresis, of carbon black/rubber compositions is very important particularly for tires made with such a composition The higher the heat buildup, the greater the chances are that tires made from 35 such rubbers are destroyed or even begin to burn Serious accidents have been attributed to the failure of tires made from such high heat buildup rubber compositions It would, therefore, be very desirable to reduce the heat buildup of rubber/carbon black compositions.
In accordance with this invention we have discovered a novel carbon black which, when 40 1 565 144 incorporated in rubber, results in a rubber composition having both a low heat buildup and a high abrasion resistance This novel carbon black is characterized by having a tint residual of -6 or less and a tint of from 70-100 As used herein, the tint residual of carbon black is a property defined by the following formula: 5 TR = T l 56 0 + 1 057 (CTAB) 0 002745 (CTAE)2 0 2596 (DBP) 0.201 (N 2 SA CTAB)l, where TR is the tint residual; CTAB is the surface area of the carbon black measured 10 as described by J Janzen and G Kraus in Rubber Chemistry and Technology, 44, 1287 ( 1971), m 2/gm; N 2 SA is the surface area of the carbon black measured using nitrogen in accordance with the ASTM method D-3037-71 T, m 2 lgm; 15 DBP is the structure of the carbon black in cc/100 g and is measured in accordance with U S Patent 3,548,454 and, after crushing, by method B in accordance with ASTM D-241470, (This property is also referred to as 24 M 4 DBP): and T is the tint or tinting strength of the carbon black 20 measured by arbitrarily assigning the reference black IRB No 3 the value of 100; the tint is measured in accordance with ASTM 3265-75.
Among the carbon blacks defined by the formula given above, those that are further 25 characterized by having surface area and structure properties within the following ranges are particularly preferred:
CTAB 73 to 140 square meters/gram DBP 67 to 111 cc/100 g 30 (N 2 SA CTAB): 23 square meters/gram or less All these properties, namely CTAB, DBP and N 2 SA, are defined and measured as disclosed above.
For best overall performance in tubber compositions, a carbon black as defined above is 35 presently preferred that has a tint residual TR as defined of -6 to -20, and a tint, as above defined, of from 70 100.
In accordance with another embodiment of this invention, there is provided a rubber composition exhibiting both low heat buildup and satisfactory tread wear properties This rubber composition comprises 100 parts by weight of rubber and from 1 to 200, preferably 40 to 120 and more preferably 20 80, parts by weight of a carbon black having a tint residual of -6 or less The tint residual is defined as above The preferred rubber compositions are those incorporating the preferred carbon blacks as defined above.
The rubber in the rubber composition of this invention can be natural rubber or a synthetic rubber Among the synthetic rubbers the homo-polymers and copolymers of at 45 least one conjugated acryclic alkadiene having 4 to 8 carbon atoms, as well as the copolymers of at least one conjugated acyclic alkadiene having 4 to 8 carbon atoms and at least one monovinyl arene with the vinyl substituent attached to an arene ring carbon atom are presently preferred Particularly preferred are polymers and copolymers of butadiene, isoprene and piperylene with styrene or a methylstyrene so Yet more specifically, and in accordance with another embodiment of this invention, there is provided a rubber composition which is particularly useful for tire tread apaplications and which is essentially composed of ingredients and quantities as shown in the following tabulation, contaning in addition standard additives such as antioxidants, etc: 55 Tread Black Rubber Parts by weight Rubber 100 Carbon black 65-90 Extender oil 15-65 60 The carbon black in this composition is, again, defined by having a tint residual of -6 or less.
Similarly, and in accordance with still a further embodiment of this invention, a rubber composition is provided which is particularly applicable in the tire carcass applications This 65 3 1 565 144 3 rubber composition consists essentially of the ingredients listed in the following tabulation and, in addition, also contains standard additives such as antioxidants, etc:
Carcass Black Rubber Parts by Weight 5 Rubber 100 Carbon black 30-60 Extender oil 5-10 10 In this carcass rubber composition, too, the carbon black is defined by having a tint residual of -6 or less.
In accordance with still a further embodiment of this invention, there is provided a carbon black reactor in which the low tint residual carbon black can be made This carbon black reactor is basically a tubular carbon black reactor with a wide precombustion section 15 followed by a narrow first reaction section which in turn is followed by a wider second reaction section The diameter of the precombustion section is from 9 to 12 inches whereas the axial length of this precombustion section is from 3 to 6 inches The first reaction section, which is a narrow section, has an upstream diameter of 2 to 4 inches and an axial length of 3 to 15 inches The second reaction section has an upstream diameter which is 2 to 20 times as wide as the downstream diameter of the first reaction section, so that the cross section of the reaction sections abruptly widens from said first section to said second section Means for generating a hot combustion gas vortex in the precomnbustion section, as well as means for introducing hydrocarbon feedstock are provided for The hydrocarbon feedstock can be introduced either at the upstream confining wall of the precombustion 25 section at the axis or can be introduced at a local at the tubular reactor wall within the downstream portion of the first reaction section or at the reactor wall immediately adjacent the abrupt diameter change from the first to the second reaction section.
The first reaction section, in accordance with a first embodiment of this reactor in accordance with his invention, is from 3 to 8 inches long and frustoconically shaped The 30 first reaction secton in this embodiment converges in downstream direction at an angle between the reactor axis and the frustoconical surface in the range of from 10 to 18 degrees, and the downstream diameter of this first reaction section is from 1 to 2 inches.
In another embodiment of the reactor of this invention, the first reaction section is essentially a cylindrical reaction section having a venturi-shaped choke therein The length 35 of the first reaction section in this embodiment is from 6 to 18 inches, and the venturi-shaped choke located at the upstream portion of the first reaction section is from 3 to 9 inches long in axial direction The throat diameter of the venturishaped choke is from 1 to 2 inches.
The invention will be still more fully understood from the following description made 40 with reference to the accompanying drawings in which Figures 1 and 3 are longitudinal sections through two reactors according to this invention, and Figure 2 is a transverse section taken on line 2-2 of either Figure 1 or Figure 2.
In the drawings, two specific reactors are shown in cross section Figures 1 and 2 show a 45 tubular carbon black reactor confined by a shell 1 or heat-resistant material such as ceramic.
The internal shape of the reactor is essentially rotationally symmetric around the reactor axis 2 The reactor is composed of a precombustion section 3, a first reaction section 4 and a second reaction section 5 All these sections are in open communication, axially aligned and operatively connected with each other The first reaction section 4 is essentially a 50 frustoconically shaped section converging in downstream direction The precombustion section 3 is a cylindrical section confined by an upstream wall 31, a cylindrical wall 32 and a downstream confining wall 33.
Normally liquid hydrocarbon feedstock can be introduced into the reactor along line 5 which is equipped with a discharge nozzle 7, which is arranged flush with the upstream wall 55 31 of the precombustion section 3 The hydrocarbon feed line 6, as well as the nozzle 7, are surrounded by a pipe 8 through which a relatively small quantity of air can be introduced into the reactor This so-called jacket air is introduced in oder to protect the nozzle and the hydrocarbon feed pipe 6.
A vortex of hot combustion gases can be generated within the precombustion section 3 60 Gas is introduced into the precombustion section 3 for this purpose from gas discharge nozzles 34 and 35 (see Figure 2) This gas, which usually is natural gas, is combusted with air which is introduced via channels 36 and 37, respectively, which surround the gas discharge nozzles 34 and 35.
The hydrocarbon feedstock axially introduced from nozzle 7 is contracted with the vortex 65 1 565 144 of hot combustion gases and the reaction mixture is passed through the first reaction section 4 and, after an abrupt expansion, through the second reaction section 5 At the end of the reaction section 5, the reaction mixture is contacted with a quenching fluid, e g, water or cold smoke injected in radial direction into the second reaction section 5 from lines 51 and 52, respectively Thus quenched carbon black-containing smoke can be withdrawn from the 5 reactor via a smoke withdrawal line 60.
A similar reactor as that shown in Figures 1 and 2 is shown in Figure 3 The cross section taken along line 2-2 of this reactor is the same as of the reactor in Figure 1, and reference is therefore also made for this reactor to Figure 2 The main difference between the reactors shown in Figures 1 and 3 is the shape of the first reaction section and the location for the 10 introduction of the hydrocarbon feed The first reaction section 4 is an essentially cylindrically-shaped section which is provided with a venturi-shaped choke 41 In addition, two different means for the introduction of hydrocarbon feedstock are provided for which can be used individually or in combination the first means for introducing hydrocarbon feedstock into this reactor consist of radial spray nozzles 71 surrounded by cooling pipes 81 15 through which cooling “jacket” air can be injected The second means for introduced hydrocarbon feedstock are located proximate to the abrupt expansion between the first reaction section 4 and the second reaction section 5 These hydrocarbon feedstock injection means also consist of spray nozzles 72 for radial injection of hydrocarbon feed surrounded by cooling jacket 32 for injection of a small quantity of cooling or “jacket” air Thus, as 20 shown by these two ebodiments of the reactors, the hydrocarbon feedstock can be injected into the reactors either upstream flush with the upstream wall or relatively far downstream in the first reaction section or even close to the abrupt diameter change into the second reaction section at the upstream end thereof In this sense the term “first reaction section” is not to be understood in a technically limiting sense With these exceptions, the second 25 reactor shown in Figure 3 is the same as that shown in Figure 1 and the same reference numerals have been used so that a details dexplanation of the other elements of this reactor can be avoided.
A typical reactor in accordance with this invention and in accordance with Figures 1 and 2 will have the following dimensions: 30 P (diameter of precombustion section 3): 10-1/4 inches D (diameter of upstream end of first reaction section 4) 3 inches d (diameter of downstream end of first reaction section 4) 1 6 inches S (diameter of second reaction section 5) 6 inches a (axial length of the precombustion section 3) 4 inches b (axial length of the first reaction section 4) 3-3/4 inches c (axial length of the second reaction section 4) 52 inches A typical reactor in accordance with Figures 2 and 3 will have the dimensions shown in the following tabulation:
P (diameter of precombustion section 3) 10-3/8 inches D (diameter of upstream end of first reaction section 4) 3 inches d (diameter of downstream end of first reaction section 4) 3 inches A 1 565 144 5 S (diameter of second reaction section 5) 6 inches a (axial length of the precombustion section 3) 4 inches 5 b (axial length of the first reaction section 4) 12 inches c (axial length of the second 10 reaction section 4) 42 inches i (diameter of the venturi throat) 1 6 inches 1 (angle between venturi and axis) 12 degrees 15 The invention will be yet more fully understood from the following examples.
Example I
Three runs to produce a low tint residual carbon black in accordance with this invention 20 were carried out in a reactor as described in connection with Figures 1 and 2 and as specified with respect to the dimensions thereof above The feed oil used in all the runs was Ponca #7 : BMCI = 120; mid-boiling point ( 50 %) = 7550 F, average boiling point = 804 ‘F The reactants introduced into the reactor, as well as the properties of the carbon black produced are shown in the following table: 25 TABLE I
Run 1 Run 2 Run 3 30 Tangential air, SCF/hr 11,000 7,500 6,000 Tangential natural gas, SCF/hr 732 500 400 Ratio A/G)volume ratio) 15/1 15/1 15/1 % Excess air 50 50 50 Axial air, SCF/hr 0 200 175 35 Oil, pounds/hr 101 69 6 47 3 Nozzle for oil 2 radial spray angle spray angle jets 900 900 40 Nozzle position flush flush flush Air/oil, SCF/pound 108 9 110 9 130 5 45 Carbon black product:
N 2 SA, m 2/gm 90 93 125 CTAB, m /gm 88 88 104 5 24 M 4 DBP, cc/100 gm 87 100 103 50 Tint 88 91 96 5 Tint residual, TR -12 8 -9 8 -9 1 “Flush” means oil nozzle was at upstream face of the precombustion chamber 55 Stoichiometric for air/natural gas is 10/1.
The above data show that in a carbon black reactor as shown in Figures 1 and 2, the low tint residual carbon black can be made Furthermore, the data shown above indicate that the tint residual is particularly low for low air-to-oil ratios 60 Example II
In a reactor as shown in Figures 2 and 3, the particular dimensions of which have been described in the above tabulation, low tint residual carbon black, as well as high tint residual carbon black were made The only difference between the reactor used for this 65 0 1 565 144 example and the reactor shown in Figures 2 and 3 is that the oil injection nozzle and the oil injection nozzle position were the same as that shown in connection with the reactor of Figures 1 and 2 for Runs 4 and 6 Thus, the hydrocarbon feedstock was injected into the reactor essentially in axial direction at a location where the spray nozzle was arranged flush 5 with the upstream confining wall of the precombustion section and the nozzle was arranged on the reactor axis In Run 5, made by way of comparison, the nozzle was inserted 2 inches into the precombustion zone The ingredients injected into the reactor, their quantities and ratios, as well as the properties of the carbon black made in accordance with this exaple, are shown in the following Table II 10 TABLE II
Run 4 Run 5 Run 6 Tangential air, SCF/hr 9,000 6,000 6,000 15 Tangential propane, SCF/hr 255 6 213 170 4 Ratio of air/fuel (volratio) 36 2/1 28 9/1 36 1/1 % Excess air 44 8 15 6 44 4 Axial air, SCF/hr 262 4 175 175 20 Oil pounds/hr 70 6 45 56 3 Nozzle for oil spray angle spray angle spray angle 900 900 900 25 Nozzle position flush 2 ” in pre flush combustion zone Air/oil, SCF/pound 131 2 137 2 109 7 30 Carbon black product:
N 2 SA, m 2/gm 130 119 99 CTAB, m 2/gm 117 116 97 24 M 4 DBP, cc/100 gm 98 5 97 96 Tint 107 1 128 99 7 Tint residual, TR -6 8 + 12 1 -7 7 40 “Flush” means the nozzle is at upstream end of precombustion chamber.
Stoichiometric for air/propane is 25/1.
The carbon black made in accordance with this example for Runs 4 and 6 showed a low 45 tint residual, whereas the carbon black made in accordance with Run 5 howed a very high tint residual.
Ir /1 1 565 144 / Example III
The three carbon blacks made in accordance with Example I were compared to three commercially available carbon blacks that were matchied to the carbon blacks prepared in accordance with Example I as far as the structure and surface area were concerned but that differed essentially from these blacks as far as the tint was concerned Therefore in 5 accordance with the formula of this invention, the tint residual of the carbon blacks to be compared was quite different The properties of the carbon blacks which were compared are listed in the following Table Ill.
TABLE III 10
N 330 N 347 N 220 Low Regular Low Regular Low Regular Hyst (IRB #3) Hyst (#1 Control)Hvst (#7 Control) 15 Run 1 Run 2 Run 3 CTAB m 2/g 83 83 88 01 105 11) 24 M 4 cc/100 lg 87 88 100 100 103 100 20 Tint 88 100))91 105 97 lt) Tint residual, -13 -2 -t) + 2 -9 O TR H.I (Ultra 3 50 2 35 18 2 17 3 10 2 20 filtration) 25 Heterogeneity index determined by ultrafiltration as described in Rubber Chemistry Technology Vol 48 No 4, September-October 1975 pages 542-545 30 3 The regular IRB #3 is an industry reference black coimmierciallh available in the industry.
The regular #1 control carbon black is a carbon black commercially available from the Phillips Petroleum Company under the designation Philblack l N 347 Similarly the regular #7 control carbon black is a carbon black conmierciallv available from the Phillips Petroleum Company Bartlesville Oklahoma under the designation N 220 35 The three carbon blacks listed were incorporated into various rubber compositions of natural rubber and of synthetic rubber in accordance with the followving two recipes:
Recipe I Recipe 2 SBR/BR Tread NR Tread 40 SBR-1712 ) 96 25 Cis-4 1203 ()3 9 NR (SMR-5 LBD) ))100 Carbon black ( 4) 75 50 45 Philrich #5 () 13 75 7 Zinc oxide 3 3 Stearic acid 2 BLE-25 () I Santoflex AW 7) 1 5 1 5 50 Flexamine G s) 1 Sulfur 1 9 2 5 Santocure ( 9) 1 1 06 Cyuram MS (t) O 15 55 ( 1) A polybutadiene/stvrene ( 76 5/23 5 weight ratio) copolymer rubber, polvmerized at 41 F and commercially available under the tradeilark Philprene E 513 BR 1712 from Phillips Petroleum Company.
( 2) A high cis-polybutadiene rubber commerciallh available under the tradename Cis-4 60 polybutadiene 1203, Phillips I Petroleum Conipany.
( 3) Natural rubber, SMR-5 LBD is a natural rubber broken down to preselected Mooney value of 54 raw Mooney at 212 F.
( 4) The various carbon blacks listed above were incorporated into the rubber for comparative runs 65 7,, R 1 565 144 ( 5) A highly aromatic extender oil available from Phillips Petroleum Co, Bartlesville, Oklahoma.
( 6) A high temperature reaction product of diphenylamine and acetone, a commercially available antioxidant.
( 7) 6-ethoxy-1, 2-dihydro-2, 2, 4-trimethylquinoline, antioxidant and flex-cracking inhibi 5 tor ‘Santoflex’ is a Registered Trade Mark.
( 8) Complex diarylamine-ketone reaction product ( 65 %) and N, N’diphenyl-pphenylenediamine ( 35 %), an antioxidant ‘Flexamine’ is a Registered Trade Mark.
( 9) N-cyclohexyl-2-benzothiazole sulfenamide, an accelerator ‘Santocure’ is a Registered 10 Trade Mark.
( 10) Tetramethylthiuram monosulfide, an accelerator.
The twelve rubber compositions in accordance with Recipe 1 and Recipe 2 given above were then formed into test specimens and tested for various rubber properties The test results are shown in the following Table IV: 15 TABLE IV
Properties in NR Tread (Recipe 2) 20 N 330 N 347 N 220 Low Regular Low Regular Low Regular Hyst (IRB #3) Hyst (#1 Control)Hyst (#7 Control) 25 Run 1 Run 2 Run 3 AT F(Std test) 39 47 45 51 47 53 (Severe test) 53 83 90 104 112 121 Resilience, % 72 67 71 66 70 65 30 Modulus, psi 1600 1550 1900 1880 1850 1750 Tensile, psi 3950 3980 3650 3980 4030 4280 Elongation, % 580 590 510 550 560 610 212 F tear, lb/in 370 360 340 370 320 360 Hardness 58 58 60 63 61 61 Properties in SBR/BR Tread (Recipe 1) AT F(orig) 55 66 63 68 63 70 AT (aged) 53 66 61 68 61 68 40 Resilience, % (orig) 65 54 60 56 59 52 (aged) 67 57 64 59 64 59 Modulus, psi 1400 1300 1850 1800 1640 1440 Tensile, psi 2870 2940 3040 3030 3000 3130 Elongation, % 520 580 460 470 480 550 212 F tear, lb/in 230 260 190 210 220 250 Hardness 55 58 61 62 58 60 AT: This is the heat buildup in degrees F determined in accordance with the standard test 50 ASTM D-623-67 In the severe test, the operation as disclosed in ASTM D623-67 is followed.
Resilience: Determined in accordance with ASTM D-945-59.
Modulus: Determined in accordance with ASTM D-412-68 55 Tensile: Determined in accordance with ASTM D-412-68.
Elongation: Determined in accordance with ASTM D-412-68.
212 F tear: Determined in accordance with ASTM D-624, using Die A Hardness: Determined in accordance with ASTM D-676-59.
All the data shown above indicate that a very significant improvement in the heat buildup 60 AT is achieved by the carbon blacks of this invention as compared to carbon blacks having similar properties but higher tint residual TR An improvement in the heat buildup of 6 to 8 degrees is very important and the results of the severe test further show an even higher improvement in the heat buildup or temperature change in a rubber composition incorporating the carbon black of this invention as compared to a rubber composition 65 R N 1 565 144 incorporating a similar carbon black with a higher tint residual.
Example IV
The carbon blacks made in accordance with Example II, as well as another carbon black having properties closely similar to the carbon black Run 6, but differing in the tint residual, were evalulated in rubber tests These carbon blacks were incorporated into rubber compositions as shown above in connection with Recipe No 1 The properties of the carbon blacks, as well as the rubber test results are shown in the following TABLE V 10
Run 4 Run 5 Run 6 Run 7 CTAB, m 2/gm, 114 118 99 105 24 M 4, cc/100 g 100 97 97 93 Tint 106 124 99 117 Tint residual, TR -6 8 -7 5 H.I (Ultrafiltration) 2 65 1 96 2 87 1 75 Cut growth, in () 0 068 0 124 0 033 0 108 2 AT OF (STD) 64 74 62 66 Resilience, % 59 53 60 57 Treadwear ( 2) 111 110 99 103 { 1} Cut growth: Determined in standard tire tests 25 2 Treadwear: Determined in standard tire tests.
The above-reported data again show that the heat buildup or hysteresis of a rubber composition incorporating a low tint residual carbon black os considerably improved as compared to a high tint residual carbon black In addition howefer, the rubber tests show that the treadwear remains unchanged for the carbon blacks compared.
Example V
In the following three recipes, typical compositions for passenger car tire tread, 35 passenger car tire carcasses and truck tire carcasses are given:
Passenger Car Tire Tread Component Pounds 40 Philprene SBR 1712 ( 2) 96 25 Cis-4 Polybutadiene 1203 ( 3) 30 Carbon black 75 Philrich () 5 ( 6) 13 75 45 Zinc oxide 3 Stearic acid 2 BLE-25 ( 8) 1 Santoflex AW ( 9) 1 5 Santocure ( 10) 1 1 5 Cyuram MS ( 11) 0 15 Sulfur 1 9 Passanger Car Tire Carcasses Natural rubber 49 55 Philprene (g) SBR 1708 ( 1) 41 25 Cis-4 Polybutadiene 1203 ( 3) 30 Carbon black 50 Rosin oil 3 Zinc oxide 4 60 Stearic acid 2 Agerite Resin D#( 4) 1 5 Amax #1 ( 5) 0 8 Diphenylguanidine O 1 Sulfur 2 5 65 a 1 in IU 1 565 144 Truck Tire Carcasses Natural rubber 80 Cis-4 Polybutadiene 1203 ( 3) 20 Carbon black 50 5 Philrich 5 ( 6) 7 Zinc oxide 5 Stearic acid 3 Sulfur 1 9 NOBS Special ( 7) 0 9 10 ( 1) Cold, oil-extended non-staining SBR rubber: 100 parts by weight low ash, low water absorption light-colored butadiene-styree ( 75-25 weight ratio) copolymer, emulsionpolymerized at 41 F using fatty acid soap and 37-1/2 parts by weight naphthenic 15 processing oil Commercially available from Phillips Petroleum Company, Bartlesville, Oklahoma.
( 2) A butadiene/styrene copolymer rubber ( 76 5/23 5 butadiene/styrene weight ratio) commercially available from Phillips Petroleum Company.
( 3) A high cis-polybutadiene rubber commercially available from Phillips Petroleum 20 Company.
{ 4) An antioxidant, 1,2-dihydro-2, 2, 4-trimethylquinoline.
5) N-oxydiethylene benzothiazole-2-sulfenamide and benzothiazyldisulfide, a delayedaction primary accelerator Amax is a Registered Trade Mark.
( 6) A highly aromatic extender oil commercially available from Phillips Petroleum 25 Company.
( 7) N-oxydiethylene-2-benzothiazyl sulfenamide.
) High-temperature reaction product of diphenylamine and acetone, an antioxidant.
9) 6-Ethoxy-1, 2-dihydro-2, 2, 4-trimethylquinoline, an antioxidant and flex-cracking inhibitor 30 10) An accelerator, N-cyclohexyl-2-benzothiazole sulfenamide.
11) An accelerator, tetramethylthiuram monosulfide.
The tire rubber compositions shown above incorporating the carbon black of the present invention will show reduced hysteresis or heat buildup, as has been shown in the previous examples This feature advantageously will decrease the risk of tire blowouts and the tires 35 catching fire.

Claims (1)

WHAT WE CLAIM IS:-
1 A carbon black having a tint residual (TR), as hereinbefore defined, of -6 or less and a tint (as hereinbefore defined) in the range 70 to 100.
2 A carbon black according to claim 1 having a TR in the range -6 to -20 40 3 A carbon black according to claim 1 or 2, having a CTAB surface area, as hereinbefore defined, in the range 73-140 m 2/g, a 24 M 4 DBP structure, as hereinbefore defined, in the range 67 to 111 cc/100 g, and a porosity (N 2 SA, as hereinbefore defined, less CTAB) of 23 m 2/g or less.
4 A carbon black according to claim 1, substantially as described in Example I or II 45 A synthetic or natural rubber when compounded with from 1 to 200 parts by weight, per 100 parts of rubber, of a carbon black according to any one of claims 1-4 and 19.
6 Synthetic or natural rubber according to claim 5, contaning from 20 to 80 parts by weight of said carbon black.
7 A rubber composition according to claim 5 or 6, in which the rubber component is a 50 homo polymer of a conjugated acyclic alkadiene of from 4-8 carbon atoms or a copolymer of two or more such dienes or of one or more such dienes with one or more monvinyl arenes.
8 A rubber composition according to claim 7 in which the rubber is a polybutadiene, a polyisoprene or polypiperylene or a copolymer of butadiene, isoprene or piperylene with 55 styrene or methyl styrene.
9 A rubber composition according to claim 5, 7 or 8 containing from 30120 parts by weight of carbon black per 100 parts of rubber.
A rubber composition according to claim 9 comprising, per 100 parts by weight of rubber, from 65-90 parts of carbon black and from 15-65 parts of extender oil 60 11 A rubber composition according to claim 9 comprising, per 100 parts by weight of rubber, from 30-60 parts of carbon black and from 5-10 parts of extender oil.
12 A rubber composition according to claim 5, substantially as hereinbefore described in Example III, IV or V.
13 A tyre comprising a rubber composition as claimed in any one of claims 5-12 65 1 ^ 1 1 1 565 144 l 14 A process for the manufacture of a carbon black as claimed in claim 1, which comprises pyrolysing a hydrocarbon feedstock in a generally tubular reactor, said reactor comprising a generally tubular elongated reactor shell closed at one end thereof, the upstream end, and open at the other end, the downstrtam end, for the recovery of the carbon black product, said shell having defined therein immediately adjacent the upstream 5 end thereof, a cylindrical precombustion chamber 9 to 12 inches in diameter and 3-6 inches in axial length, immediately downstream from said precombustion chamber a first generally tubular reaction section axially aligned and in open communication with said precombustion chamber and having an upstream diameter of 2 to 4 inches and an axial length of 3 to 15 inches, and immediately downstream from said first reaction section so that 10 the first reaction section opens abruptly thereinto, a second generally cylindrical reaction section axially aligned and in open communication with said first reaction section, the ratio of the diameter of said second reaction section to the downstream end of the first reaction section being in the range 2:1 to 5:1, said reactor further comprising fuel and air inlets into the periphery of said precombustion chamber for creating a vortex of combustion gas 15 therein, quench inlets into the downstream end of the second reaction section for introducing therein a quench medium, and either a single hydrocarbon feedstock inlet located in the upstream end wall of the tubular reactor and located on the axis thereof, or hydrocarbon feedstock inlet(s) radially located in the downstream portion of the first reaction section and/or in the upstream portion of the second reaction section immediately 20 adjacent the junction of the said first and second reaction sections.
A process according to claim 14, wherein the hydrocarbon feedstock inlet is located in the upstream end wall of the reactor on the axis thereof, and wherein the first reaction section is frusto conical, having a downstream end diameter of from 1-2 inches, an axial length of from 3-8 inches, and walls which converge on the axis at an angle of from 10-18 25 degrees.
16 A process according to claim 14, wherein the hydrocarbon feedstock inlet(s) is or are located in the downstream portion of the first reaction section and/or immediately adjacent the upstream end of the second reaction section and said first reaction section has a venturi-shaped choke positioned in the upstream portion thereof, said choke having a 30 throat diameter of from 1 to 2 inches an overal length of from 3-9 inches the overall length of said first reaction section being from 6-18 inches.
17 A process according to claim 14 wherein the reactor used is substantially as hereinbefore described with reference to the accmpanying drawings.
18 A process according to claim 14 substantially as hereinbefore described in Example 35 I or II.
19 Carbon black according to claim 1 when made by a process claimed in any one of claims 15-18.
A tubular carbon black reactor, comprising a generally tubular elongated reactor shell closed at one end thereof the upstream end and open at the other end the 40 downstream end, for the recovery of the carbon black product said shell having defined therein, immediately adjacent the upstream end thereof a cylindrical precmbustion chamber 9 to 12 inches in diameter and 3-6 inches in axial length immediately downstream from said precombustion chamber, a first generally tubular reaction section axially aligned and in open communication with said precombustion chamber, and having an upstream 45 diameter of 2 to 4 inches and an axial length of 3 to 15 inches and immediately downstream from said first reaction section so that the first reaction section opens abruptly thereinto, a second generally cylindrical reaction section axially aligned and in open communication with said first reaction section the ratio of the diameter of said second reaction section to the downstream end of the first reaction section being in the range 2:1 to 5:1, said reactor 50 further comprising fuel and air inlets into the periphery of said precombustion chamber for creating a vortex of combustion gas therein quench inlets into the downstream end of the second reaction section for introducing therein a quench medium and either a single hydro-carbon feedstock inlet located in the upstream end wall of the tubular reactor and located on the axis thereof, or hydrocarbon feedstock inlet(s) radially located in the 55 downstream portion of the first reaction section and/or in the upstream portion of the second reaction section immediately adjacent the junction of the said first and second reaction sections.
21 A reactor according to claim 20 wherein the hydrocarbon feedstock inlet is located in the upstream end wall of the reactor on the axis thereof, and wherein the first reaction 60 section is frusto conical, having a downstream end diameter of from 1-2 inches an axial length of from 3-8 inches, and walls which con\ erge on the axis at an angle of from 10-18 degrees.
22 A reactor according to claim 20 wherein the hydrocarbon feedstock inlet(s) is or are located in the downstream portion of the first reaction section and/or immediately 65 t 1 12 1 565 144 12 adjacent the upstream end of the second reaction section and said first reaction section has a venturi-shaped choke positioned in the upstream portion thereof, said choke having a throat diameter of from 1 to 2 inches an overal length of from 3-9 inches, the overall length ofsaid first reaction section being from 6-18 inches.
23 A reactor according to claim 20 substantially as hereinbefore described with 5 reference to the accmpanying drawings.
For the Applicants, D YOUNG & CO, Chartered Patent Agents, 10 9 & 10 Staple Inn, London WC 1 V 7RD.
Printed for Her Majesty’s Stationery Office, by Croydon Printing Company Limited Croydon, Surrey 1980.
Published by The Patent Office, 25 Southampton Buildings London, WC 2 A IAY,from which copies may be obtained.

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Phillips Petroleum Company
Rubber compositions and method therefor

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1979-06-11
1980-12-18
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1983-07-22
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1976-04-30
US
US05/681,977
patent/US4071496A/en
not_active
Expired – Lifetime

1976-12-16
CA
CA268,033A
patent/CA1103897A/en
not_active
Expired

1977

1977-04-05
ZA
ZA00772091A
patent/ZA772091B/en
unknown

1977-04-05
IN
IN504/CAL/77A
patent/IN145988B/en
unknown

1977-04-22
BR
BR7702528A
patent/BR7702528A/en
unknown

1977-04-25
JP
JP4776977A
patent/JPS52133099A/en
active
Pending

1977-04-28
DE
DE19772718986
patent/DE2718986A1/en
not_active
Withdrawn

1977-04-29
IT
IT23024/77A
patent/IT1075098B/en
active

1977-04-29
FR
FR7713077A
patent/FR2349628A1/en
active
Granted

1977-04-29
TR
TR19691A
patent/TR19691A/en
unknown

1977-04-29
GB
GB18061/77A
patent/GB1565144A/en
not_active
Expired

1977-04-29
SE
SE7704989A
patent/SE7704989L/en
not_active
Application Discontinuation

Also Published As

Publication number
Publication date

BR7702528A
(en)

1977-11-29

TR19691A
(en)

1979-10-11

SE7704989L
(en)

1977-10-31

CA1103897A
(en)

1981-06-30

FR2349628A1
(en)

1977-11-25

IN145988B
(en)

1979-02-03

DE2718986A1
(en)

1977-11-03

JPS52133099A
(en)

1977-11-08

ZA772091B
(en)

1978-03-29

US4071496A
(en)

1978-01-31

FR2349628B1
(en)

1980-04-04

AU2410977A
(en)

1978-03-23

IT1075098B
(en)

1985-04-22

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