GB1603160A – Process for removing layers of selenium
– Google Patents
GB1603160A – Process for removing layers of selenium
– Google Patents
Process for removing layers of selenium
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Publication number
GB1603160A
GB1603160A
GB23140/78A
GB2314078A
GB1603160A
GB 1603160 A
GB1603160 A
GB 1603160A
GB 23140/78 A
GB23140/78 A
GB 23140/78A
GB 2314078 A
GB2314078 A
GB 2314078A
GB 1603160 A
GB1603160 A
GB 1603160A
Authority
GB
United Kingdom
Prior art keywords
amine
mercaptan
base
selenium
layer
Prior art date
1977-05-26
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
GB23140/78A
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.)
Hoechst AG
Original Assignee
Hoechst AG
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.)
1977-05-26
Filing date
1978-05-26
Publication date
1981-11-18
1978-05-26
Application filed by Hoechst AG
filed
Critical
Hoechst AG
1981-11-18
Publication of GB1603160A
publication
Critical
patent/GB1603160A/en
Status
Expired
legal-status
Critical
Current
Links
Espacenet
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Classifications
G—PHYSICS
G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
G03G15/00—Apparatus for electrographic processes using a charge pattern
G03G15/75—Details relating to xerographic drum, band or plate, e.g. replacing, testing
G—PHYSICS
G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
G03G21/00—Arrangements not provided for by groups G03G13/00 – G03G19/00, e.g. cleaning, elimination of residual charge
G—PHYSICS
G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
G03G5/005—Materials for treating the recording members, e.g. for cleaning, reactivating, polishing
Description
PATENT SPECIFICATION ( 11) 1 603 160
O ( 21) Application No 23140/78 ( 22) Filed 26 May 1978 ( 19) 4 ( 31) Convention Application No 2723799 ( 32) Filed 26 May 1977 in z» ( 33) Fed Rep of Germany (DE) & o ( 44) Complete Specification Published 18 Nov 1981 ú ( 51) INT CL 3 C 23 G 5/02 ( 52) Index at Acceptance C 7 E 152 188 192 200 214 i o ( 54) PROCESS FOR REMOVING LAYERS OF SELENIUM ( 71) WE, HOECHST AKTIENGESELLSCHAFT, a body corporate organised according to the laws of the Federal Republic of Germany, of 6230 Frankfurt/Main 80, Postfach 80 03 20, Federal Republic of Germany, 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: 5
The invention relates to a process for removing a layer containing or consisting of amorphous selenium from a metal base.
In electrophotography, metal bases are used as supports for selenium layers, in the form of plates, cylindrical drums or flexible tapes The metals used are, for example, aluminum, brass, chromium and stainless steel The surfaces of the bases are in most cases pretreated 10 Thus, aluminum drums may be anodized at least in the edge zones Because of the necessary surface smoothness and the dimensional accuracy, the metal bases, in particular drums, are sufficiently valuable to be reclaimed when the photoconductor layer has worn out.
Methods of recovery of the carrier base, after an applied layer of selenium has worn out 15 or has been damaged, are therefore of great interest.
The applied photoconductor layer is used for the production of latent electrostatic charge images Amorphous selenium is frequently used Doped selenium or selenium alloys may also be used, extending the sensitivity of the selenium into the red region of the spectrum.
Usually, arsenic is present and halogens, phosphorus, antimony, tellurium and sulfur may 20 also be added The metal base may carry a single layer or a series of layers.
Various processes have been proposed for separating selenium-containing layers from metal bases For example, the photoconductor layer can be separated from the base using oxidising acids, concentrated solutions of alkali metal sulfides or fused alkali metal hydroxides (U S Patent Specification 2,816,008) Another process involves cooling the 25 drum to a low temperature in liquid nitrogen (U S Patent Specification 3, 837,815).
Subsequently, the drum is immersed in water and the ice layer formed is then thawed In this case, the selenium layer adheres not to the metal but to the ice layer It has also been proposed to heat the selenium layer together with the carrier base to a temperature just below the melting point of the selenium layer and subsequently to spray the coated surface 30 (DT-AS 2,549,947).
These processes, however, have various disadvantages Thus, when the selenium layer is stripped with aggressive chemical agents, the selenium is converted to toxic selenium compounds, the disposal of which raises problems Furthermore, recovery of selenium, which may be carried out, requires additional chemical processes On the other hand, the 35 surfaces of the metal base are attacked.
On stripping by generating large temperature differences, selenium is admittedly recovered in the elemental form but strains which lead to troublesome deformations of the outer surfaces are produced in the metal bases.
It has also been proposed in U S Patent Specification 3,990,907 to remove spent 40 selenium layers from metal carriers by treating the photoconductor drums with hot water, steam, trichloroethylene or perchloroethylene, in which case the layer of selenium loses its adhesion, due to the different thermal expansions of selenium and of the base, and can be stripped from the carrier.
A process of this type also utilizes relatively large temperature differences which make it 45 1,603,160 possible for strains to arise in the material, so that this process is also not without its problems Moreover, hot water and steam slightly attack carriers consisting of aluminum, while chlorinated ethylenes are toxic During the stripping process itself, sensitive carrier surfaces, for example surfaces of aluminum, are easily damaged.
The present invention is concerned with a process for removing the layer from a metal 5 base, if possible without a chemical reaction, and in which no damage to the metal base occurs.
The present invention provides a process for removing a layer containing or consisting of amorphous selenium from a base by treating the layer at a temperature within the range of from 60 WC to 150 WC with a fluid containing an amine or a mercaptan, and subsequently 10 cleaning the base with a fluid at a temperature of at most 40 WC.
The fluid used for cleaning is advantageously inert Preferably, the base is a metal base.
The process presumably causes a transformation of the selenium from the amorphous into the hexagonal state, as a result of which the layer flakes off and is finally removed completely, or almost completely, from the base by a cleaning process, such as, for 15 example, spraying Because of the relatively small temperature changes during the removal of the layer of selenium, no strains are generated in the metal so that deformation does not occur.
The fluid which contains an amine or mercaptan, may be applied to the layer of selenium in any desired manner, for example by dipping, dip-coating, spraying-on, rubbing-in or 20 pouring-on.
The amine or mercaptan may be employed by itself or dissolved in or mixed with a polyhydric alcohol.
The amines employed are advantageously those which, taking the environmental conditions into account, are free from noxious odor, do not possess an excessive basicity 25 and have a high boiling point Amines of a relatively high basicity can also be employed if direct contact with the metal base is avoided.
Preferred amines are those from the series of diprimary amines of the general formula NH,-(CH,-CH 2-NH)f H with X equal to or greater than 2 Diethylenetriamine and triethylenetetramine are particularly suitable Alkyldiamines with at least 5 carbon atoms 30 may be employed, e g, trimethylhexamethylenediamine Heterocyclic bases, e g, pyridine quinoline, morpholine and their alkyl derivatives, in particular those having up to 4 carbon atoms, are also suitable.
Preferably, 2,2,4-trimethylhexamethylenediamine is employed.
-35 The mercaptans employed are advantageously those which, like the preferred amines, 35 have little odor nuisance and a high boiling point.
Examples of mercaptans which can be used are those which correspond to the formula R-S-H, wherein R represents a straight or branched-chain alkyl group having more than 7 carbon atoms.
Preferably, lauryl mercaptan is employed 40 As already stated, amines or mercaptans may be employed by themselves as the fluid acting on the layer It has been found, however, that it is advantageous to apply the amine or mercaptan in a solution or mixture For this purpose, polyhydric alcohols are employed which, with respect to their boiling point, meet the temperature conditions required These include, in particular, glycols, glycerol or glycol ethers 45 Solvents or diluents which can be used are hexylene glycol, diethylene glycol, polyethylene glycol, trimethylene glycol, ethylene glycol, propylene glycol, glycerol and also glycol ethers, such, for example, as diethylene glycol monoethyl ether.
According to the invention, polyethylene glycol having a molecular weight below about 1,000 is preferably employed Polyethylene glycol having a molecular weight of 300 400 is 50 particularly suitable.
If a solution or mixture is used, it may contain the amine or mercaptan in any concentration Preferably, however, a 5 to 50 percent by weight solution or mixture of the amine or the mercaptan with a polyhydric alcohol is used.
After the fluid has been applied to the selenium layer the whole is heated to a 55 temperature in the range of 60 and 150 C, for example in an oven, preferably at a temperature in the range from 70 130 C This temperature is advantageously maintained until the selenium layer starts to flake off.
Heating may also be carried out in any other desired manner, for example with hot air or by passing hot steam through the interior of the drum or provided the hot fluid does not 60 attack the metal base by dipping in a heated fluid, and this is preferred.
As a result of the treatment, amorphous selenium is converted into a form of metallic selenium which has poor adhesion to the base, and the action of the fluid is apparently to accelerate the rate of the thermally induced change.
After the thermal treatment, the metal bases are treated for cleaning with a fluid at a 65 3 1,603,160 3 temperature of at most 40 ‘C, as a result of which the seleniumcontaining layer, which has not yet flaked off, is removed from the base.
Suitable, preferably inert, fluids include those which have hitherto been used for similar purposes e g, lower alcohols or ketones and liquid lower hydrocarbons Preferably, however, water is employed Water at 10 20 MC has proved advantageous for removing the 5 selenium layer.
Any residue of selenium which may remain after flaking-off and removal of the selenium-containing layer may afterwards be removed using a solvent for selenium.
Examples of suitable solvents are aqueous solutions of alkali metal sulfides and alkali metal sulfites or, especially, mixtures of 40 98 % by weight of amine and 6 p 2 % by weight, of 10 alkyl mercaptan.
The present invention is explained in more detail by reference to the Examples.
Example 1
A copying drum consisting of aluminum and a photoconductor layer of selenium was 15 rubbed with a 1: 1 mixture by weight of 2,2,4trimethylhexamethylenediamine and polyethylene glycol having a molecular weight of 300, with the aid of a cotton wool pad and was then stored for 45 minutes in a drying cabinet heated to 90 ‘C and finally dipped into a basin filled with water The layer of selenium dropped off the aluminum drum, in the form of flakes The flakes were washed clean with water and acetone 20 A correspondingly heated selenium drum which had not been pre-treated with the mixture of fluids merely showed cracks in the selenium layer, the adhesion was, however, still good.
Example 2 25
Example 1 was successfully repeated using a mixture consisting of 95 parts by weight of a polyethylene glycol having a molecular weight of about 400 and 5 parts by weight of trimethylhexamethylenediamine.
Example 3 30
A worn-out copying drum, having a photoconductive layer of selenium, was dipped into a mixture of 95 parts by volume of a polyethylene glycol having a molecular weight of about 400 and 5 parts by volume of trimethylhexamethylenediamine maintained at 1000 C After about 15 minutes, the layer of selenium began to flake off When the drum was cooled in water at 20 ‘C, the photoconductor layer dropped off almost completely Remaining 35 residues of selenium were removed using a mixture of 50 parts by volume of morpholine and 50 parts by volume of lauryl mercaptan, at 20 ‘C.
Example 4
Example 3 was repeated with the polyethylene glycol/trimethylhexamethylenediamine 40 mixture at 130 MC The layer of selenium dropped off the aluminum drum after about 5 minutes The surface of the drum proved to be completely suitable for new coatings.
Example 5
A worn-out copying drum, having a photoconductive layer of selenium on a metal base, 45 was rubbed with lauryl mercaptan and then kept for 45 minutes in an oven at 90 ‘C When the drum was dipped, while still hot, into cold water, the layer dropped off the metal base almost completely The remaining residues were removed as described in Example 3.
It will be understood that the base from which the selenium layer is removed will be an electrically conductive material when the article to be treated is an electrophotographic 50 material The base may accordingly be one of those mentioned specifically above, or may be a non-conductive material having a conductive surface to which the selenium layer is to be removed, for example, a polyester film coated with, for example, aluminium.
Claims (1)
WHAT WE CLAIM IS:
1 A process for removing a layer containing or consisting of amorphous selenium from 55 a base which comprises treating the layer with a fluid containing an amine or a mercaptan at a temperature within the range of from 60 C to 150 C and subsequently cleaning the base with a fluid at a temperature of at most 40 C.
2 A process as claimed in claim 1, wherein the base is a metal base.
3 A process as claimed in claim 1 or claim 2, wherein the treatment is carried out at a 60 temperature within the range of from 70 C to 130 C.
4 A process as claimed in any one of claims 1 to 3, wherein an amine is used, and wherein the amine is of the general formula NH 2-(CH 2-CH 2-NH)x H wherein X is at least 2.
A process as claimed in any one of claims 1 to 3, wherein an amine is used, and wherein the amine is an alkylenediamine having at least 5 carbon atoms 65 4 1,603,160 4 6 A process as claimed in any one of claims 1 to 3, wherein an amine is used, and wherein the amine is a heterocyclic base.
7 A process as claimed in any one of claims 1 to 3, wherein 2,2,4trimethylhexamethylenediamine is used.
8 A process as claimed in any one of claims 1 to 3, wherein diethylenetriamine, 5 triethylenetetraamine, trimethylhexamethylenediamine, pyridine, quinoline or morpholine is used.
9 A process as claimed in any one of claims 1 to 3, wherein a mercaptan is used, and wherein the mercaptan is of the formula R-S-H wherein R represents a straight or branched-chain alkyl group having at least 7 carbon atoms 10 A process as claimed in any one of claims 1 to 3, wherein lauryl mercaptan is used.
11 A process as claimed in any one of claims to 10, wherein the amine or mercaptan is used in the form of a solution or mixture with another fluid.
12 A process as claimed in claim 11, wherein the concentration of the amine or mercaptan is from 5 % to 50 % 15 13 A process as claimed in claim 11 or claim 12, wherein the solvent or other component of the mixture is a polyhydric alcohol.
14 A process as claimed in claim 13, wherein the alcohol is glycol, glycerol, a glycol ether, or a mixture containing any one or more of these compounds.
15 A process as claimed in claim 13, wherein the polyhydric alcohol is a polyethylene 20 glycol with a molecular weight within the range of from 300 to 400.
16 A process as claimed in any one of claims 1 to 15, wherein the cleaning fluid is inert to the layer.
17 A process as claimed in any one of claims 1 to 15, wherein water is used as the cleaning fluid 25 18 A process as claimed in claim 17, wherein the cleaning fluid is used at a temperature within the range of from 10 C to 20 C.
19 A process as claimed in any one of claims 1 to 18, which also comprises a treatment, subsequent to the cleaning, with a mixture of from 40 % to 98 % of an amine and 60 to 2 % of an alkyl mercaptan 30 A process as claimed in claim 1, substantially as described in any one of the Examples herein.
21 A base, whenever prepared by a process as claimed in any one of claims 1 to 20.
ABEL & IMRAY Chartered Patent Agents, 35 Northumberland House, 303-306 High Holborn, London WC 1 V 7 LH.
Printed for Her Majesty’s Stationery Office by Croydon Printing Company Limited, Croydon, Surrey 1981.
Published by The Patent Office, 25 Southampton Buildings London WC 2 A l AY, from which copies may be obtained.
GB23140/78A
1977-05-26
1978-05-26
Process for removing layers of selenium
Expired
GB1603160A
(en)
Applications Claiming Priority (1)
Application Number
Priority Date
Filing Date
Title
DE19772723799
DE2723799A1
(en)
1977-05-26
1977-05-26
METHOD OF REMOVING SELENIUM LAYERS
Publications (1)
Publication Number
Publication Date
GB1603160A
true
GB1603160A
(en)
1981-11-18
Family
ID=6009944
Family Applications (1)
Application Number
Title
Priority Date
Filing Date
GB23140/78A
Expired
GB1603160A
(en)
1977-05-26
1978-05-26
Process for removing layers of selenium
Country Status (7)
Country
Link
US
(1)
US4192692A
(en)
JP
(1)
JPS53147703A
(en)
AU
(1)
AU514959B2
(en)
DE
(1)
DE2723799A1
(en)
FR
(1)
FR2392138B1
(en)
GB
(1)
GB1603160A
(en)
NL
(1)
NL7805660A
(en)
Cited By (1)
* Cited by examiner, † Cited by third party
Publication number
Priority date
Publication date
Assignee
Title
GB2224750A
(en)
*
1988-09-26
1990-05-16
Fuji Xerox Co Ltd
Method for removing a selenium-containing layer from an electrophotographic photoreceptor
Families Citing this family (5)
* Cited by examiner, † Cited by third party
Publication number
Priority date
Publication date
Assignee
Title
US4556509A
(en)
*
1984-10-09
1985-12-03
Colgate-Palmolive Company
Light duty detergents containing an organic diamine diacid salt
DE3444293A1
(en)
*
1984-12-05
1986-06-05
Metallgesellschaft Ag, 6000 Frankfurt
AGENT FOR CLEANING PROCESSING PLANTS FOR HIGHLY VISCOSE REACTIVE MULTI-COMPONENT MIXTURES
DE102012011041A1
(en)
*
2012-06-05
2013-12-05
Leybold Optics Gmbh
Method for removing selenium precipitates on cold traps of solar cell production
EP3613835A1
(en)
2018-08-24
2020-02-26
The Procter & Gamble Company
Treatment compositions comprising a surfactant system and an oligoamine
EP3613834A1
(en)
2018-08-24
2020-02-26
The Procter & Gamble Company
Treatment compositions comprising low levels of an oligoamine
Family Cites Families (8)
* Cited by examiner, † Cited by third party
Publication number
Priority date
Publication date
Assignee
Title
DD92134A
(en)
*
1900-01-01
US2889206A
(en)
*
1953-09-30
1959-06-02
Kawecki Chemical Company
Recovery of selenium
US2816008A
(en)
*
1955-12-06
1957-12-10
American Smelting Refining
Recovery of selenium from scrap selenium rectifiers
FR1355159A
(en)
*
1962-04-10
1964-03-13
Du Pont
Method and composition for cleaning metals
US3992511A
(en)
*
1969-08-27
1976-11-16
Xerox Corporation
Recovery of selenium
GB1275355A
(en)
*
1969-08-27
1972-05-24
Xerox Corp
Recovery of selenium
US3837815A
(en)
*
1973-03-29
1974-09-24
Dick Co Ab
Method of reclaiming selenium and metal base from electrophotographic plates
JPS5087651A
(en)
*
1973-12-06
1975-07-14
1977
1977-05-26
DE
DE19772723799
patent/DE2723799A1/en
not_active
Withdrawn
1978
1978-05-23
JP
JP6159078A
patent/JPS53147703A/en
active
Pending
1978-05-23
FR
FR7815216A
patent/FR2392138B1/fr
not_active
Expired
1978-05-24
NL
NL7805660A
patent/NL7805660A/en
not_active
Application Discontinuation
1978-05-25
US
US05/909,561
patent/US4192692A/en
not_active
Expired – Lifetime
1978-05-25
AU
AU36462/78A
patent/AU514959B2/en
not_active
Expired
1978-05-26
GB
GB23140/78A
patent/GB1603160A/en
not_active
Expired
Cited By (3)
* Cited by examiner, † Cited by third party
Publication number
Priority date
Publication date
Assignee
Title
GB2224750A
(en)
*
1988-09-26
1990-05-16
Fuji Xerox Co Ltd
Method for removing a selenium-containing layer from an electrophotographic photoreceptor
US5085732A
(en)
*
1988-09-26
1992-02-04
Fuji Xerox Co., Ltd.
Method for removing a selenium-containing layer from a electrophotographic photoreceptor
GB2224750B
(en)
*
1988-09-26
1992-12-02
Fuji Xerox Co Ltd
Method for removing a selenium-containing layer from an electrophotographic photoreceptor
Also Published As
Publication number
Publication date
FR2392138B1
(en)
1981-01-23
DE2723799A1
(en)
1978-12-07
US4192692A
(en)
1980-03-11
AU3646278A
(en)
1979-11-29
AU514959B2
(en)
1981-03-05
FR2392138A1
(en)
1978-12-22
NL7805660A
(en)
1978-11-28
JPS53147703A
(en)
1978-12-22
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Legal Events
Date
Code
Title
Description
1982-02-10
PS
Patent sealed [section 19, patents act 1949]
1985-01-23
PCNP
Patent ceased through non-payment of renewal fee
