CN103073810A - Method for improving styryl carbon powder resin compatibility - Google Patents
Method for improving styryl carbon powder resin compatibility Download PDFInfo
- Publication number
- CN103073810A CN103073810A CN2012105795769A CN201210579576A CN103073810A CN 103073810 A CN103073810 A CN 103073810A CN 2012105795769 A CN2012105795769 A CN 2012105795769A CN 201210579576 A CN201210579576 A CN 201210579576A CN 103073810 A CN103073810 A CN 103073810A
- Authority
- CN
- China
- Prior art keywords
- copolymer
- acrylic ester
- cinnamic acrylic
- styryl
- flour
- Prior art date
- 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.)
- Granted
Links
- -1 styryl carbon powder Chemical compound 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 42
- 229920005989 resin Polymers 0.000 title claims abstract description 30
- 239000011347 resin Substances 0.000 title claims abstract description 30
- 229920001577 copolymer Polymers 0.000 claims abstract description 44
- 229920002521 macromolecule Polymers 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 36
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 22
- 125000005504 styryl group Chemical group 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 10
- 239000008096 xylene Substances 0.000 claims description 10
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 9
- 239000004593 Epoxy Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 19
- 239000000843 powder Substances 0.000 abstract description 4
- 239000000049 pigment Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000005007 epoxy-phenolic resin Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000002861 polymer material Substances 0.000 abstract 1
- 238000007790 scraping Methods 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 239000000428 dust Substances 0.000 description 17
- NJVOHKFLBKQLIZ-UHFFFAOYSA-N (2-ethenylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C=C NJVOHKFLBKQLIZ-UHFFFAOYSA-N 0.000 description 6
- 230000002194 synthesizing effect Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000012966 redox initiator Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Abstract
The invention discloses a method for improving styryl carbon powder resin compatibility, which belongs to the technical field of polymer material processing and application. The method for improving the styryl carbon powder resin compatibility uses a main body method to synthesize macromolecule phenethylene-acrylate copolymer, uses a solution method to synthesize micromolecule phenethylene-acrylate copolymer, and mingles the macromolecule and the micromolecule phenethylene-acrylate copolymer; and during the mixing process of the macromolecule and the micromolecule phenethylene-acrylate copolymer, modified epoxy-phenolic resin is added to improve the styryl carbon powder resin compatibility. The method has the characteristics that the styryl carbon powder resin treated by the method has good compatibility and good crushability; the pigment is dispersed uniformly; the waste powder rate is low; the carbon powder prepared has uniform particle size distribution, and does not stick to scraping plate; and the quality of carbon powder is high. The method can be widely used in the fields such as preparation of carbon powder of printers and copying machines.
Description
Technical field
The present invention relates to the processing of high molecular material method, particularly relate to a kind of method that improves styryl flour-carbon resin consistency.
Background technology
Carbon dust can be divided into two large classes according to the difference of the mode of production---polymerization carbon dust and pulverizing carbon dust.Pulverize carbon dust and be again the physics carbon dust, production process is first the auxiliary agents such as the resin of solid, magneticsubstance, pigment, charge control agent, wax to be mixed roughly, heat at mixing roll again, resin is melted, simultaneously being distributed in the resin with not melting homogeneous chemical composition, carrying out again coarse reduction, classification, surface modification after the cooled and solidified and get final product.
The more styryl flour-carbon resin of using of physics carbon dust, the preparation method of styryl flour-carbon resin is, substance law synthetic macromolecule copolymer in cinnamic acrylic ester, the synthetic low molecule copolymer in cinnamic acrylic ester of solution method mixes high low-molecular-weight copolymer in cinnamic acrylic ester.Because high low-molecular-weight copolymer in cinnamic acrylic ester mixture consistency is poor, the carbon dust of production in use low molecule melting clings scraper plate, affects printing effect, affects the carbon dust quality.Now production is generally adopted and add linking agent in mixture, makes incompatible resin crosslinked, improves the consistency of system.This method of improving consistency is produced in the carbon dust process, and comminuted bad, pigment is bad in resin dispersion, takes the powder rate high, prepares carbon dust pattern corner angle many, the carbon dust poor quality.The present invention is in the low-molecular-weight copolymer in cinnamic acrylic ester mixing process of height, adds epoxy modified phenolic resin, improves styryl flour-carbon resin consistency.It is comminuted good that modified resin is produced in the carbon dust process, and colo(u)rant dispersion is even, take the powder rate low, prepares the carbon dust size distribution even.
Summary of the invention
The objective of the invention is to improve the consistency of styryl carbon dust with epoxy modified phenolic resin in order to overcome the deficiency of above-mentioned background technology, a kind of method that improves styryl flour-carbon resin consistency is provided.In order to achieve the above object, technical scheme of the present invention is achieved in that
The method of raising styryl flour-carbon resin consistency provided by the invention, described method comprises following approach: the preparation of (one) copolymer in cinnamic acrylic ester mixture: with substance law synthetic macromolecule copolymer in cinnamic acrylic ester 1000-1200kg, with the synthetic xylene solution 1600-2000kg that contains low molecule copolymer in cinnamic acrylic ester of solution method, wherein copolymer in cinnamic acrylic ester and dimethylbenzene are pressed the 1:1 preparation, contain in described macromolecule styrene-acrylate copolymer that low molecular xylene solution joins melting described, in the low-molecular-weight copolymer in cinnamic acrylic ester mixing process of height, the 3%-6% by high low-molecular-weight copolymer in cinnamic acrylic ester total amount adds epoxy modified phenolic resin again; (2) copolymer in cinnamic acrylic ester mixture devolatilization: with the copolymer in cinnamic acrylic ester of above-mentioned reaction, under 80-100 ℃ of temperature slaking 2-4 hour, be warming up to again under 140-160 ℃, distilled desolventizing dimethylbenzene and residual monomer 2-4 hour; With the described copolymer in cinnamic acrylic ester of distillation devolatilization, vacuum volatilization, temperature rises to 160-180 ℃, devolatilization 2-6 hour, obtains the mixed flour-carbon resin of epoxide modified phenolic aldehyde increase-volume copolymer in cinnamic acrylic ester.
In technique scheme, the synthetic low molecule copolymer in cinnamic acrylic ester number-average molecular weight of described solution method is 3 * 10
3-5 * 10
3
In technique scheme, substance law synthetic macromolecule copolymer in cinnamic acrylic ester number-average molecular weight is 2 * 10
5-4 * 10
5
In technique scheme, add epoxy modified phenolic resin by 4% of the low-molecular-weight copolymer in cinnamic acrylic ester total amount of described height.
In technique scheme, the described curing time is 3 hours, and temperature is 85 ℃; Described distillation time is 2.5 hours, and temperature is 155 ℃; The described vacuum volatilization time is 4 hours, and temperature is 170 ℃.
In technique scheme, described is 1100kg with substance law synthetic macromolecule copolymer in cinnamic acrylic ester; Described is 1800kg with the synthetic xylene solution that contains low molecule copolymer in cinnamic acrylic ester of solution method.
Described vacuum operating, can select reciprocating type, water circulation type, or water ring and all kinds of vacuum apparatuss of lobe pump built-up type, vacuum tightness is greater than-0.08Mpa, final vacuum reaches-0.099Mpa.
The method of raising styryl flour-carbon resin consistency of the present invention, have following beneficial effect: characteristics of the present invention are that the styryl flour-carbon resin consistency of processing through the method is good, in the carbon dust course of processing, sticking scraper plate takes that the powder rate is low, the carbon dust quality is high.The system that the present invention can be widely used in printer and duplicator carbon dust such as joins at the field.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but this embodiment should not be construed as limitation of the present invention.
Embodiment 1
In the 4000L reactor, synthesize 1200kg cinnamic acrylic ester high-molecular copolymer with substance law, in the 4000L reactor, hang down molecule copolymer 1 600kg in total monomer and solvent xylene 1:1 ratio synthesizing styrene-acrylate, the xylene solution of the low molecule multipolymer of synthesizing styrene-acrylate is pumped in the reactor of synthesizing styrene-acrylate polymeric multipolymer with industry, adds 100kg epoxy modified phenolic resin system and be made into the copolymer in cinnamic acrylic ester mixture.Add redox initiation system, with the reaction the copolymer in cinnamic acrylic ester mixture after 85 ℃ of lower slakings 3 hours, be warming up to again 155 ℃, distilled desolventizing dimethylbenzene and remaining total monomer 2.5 hours, copolymer in cinnamic acrylic ester mixture with the distillation devolatilization, vacuum volatilization, vacuum tightness-0.097Mpa, temperature rises to 170 ℃, devolatilization 4 hours, discharging are pulverized and are obtained polystyrene-based flour-carbon resin.Described total monomer is copolymer in cinnamic acrylic ester.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, difference is: synthetic 1000kg cinnamic acrylic ester high-molecular copolymer, synthesizing styrene-acrylate hangs down molecule multipolymer 2000kg, the xylene solution of the low molecule multipolymer of synthesizing styrene-acrylate is pumped into the reactor of synthetic macromolecule multipolymer with industry, adds the 120kg epoxy modified phenolic resin.Add redox initiation system, 90 ℃ of lower slakings 2.5 hours, with the copolymer in cinnamic acrylic ester of reaction, under 160 ℃, distilled 2 hours, desolventizing dimethylbenzene and remaining total monomer are with the copolymer in cinnamic acrylic ester of distillation devolatilization, vacuum volatilization, vacuum tightness-0.097Mpa, temperature rises to 175 ℃, and devolatilization 5 hours, discharging are pulverized and obtained polystyrene-based flour-carbon resin.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, and difference is: synthetic 1100kg cinnamic acrylic ester high-molecular copolymer; The xylene solution 1800kg of the low molecule multipolymer of synthesizing styrene-acrylate; Add the 110kg epoxy modified phenolic resin; Curing temperature is 95 ℃, lasts 3 hours; Distillation temperature is 150 ℃, lasts 3 hours; The vacuum volatilization temperature is 165 ℃, lasts 5.5 hours.
Obviously, those skilled in the art can carry out various changes and modification to the present invention and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
The content that is not described in detail in this specification sheets belongs to the known prior art of this area professional and technical personnel.
Claims (6)
1. method that improves styryl flour-carbon resin consistency, it is characterized in that: described method comprises following approach: the preparation of (one) copolymer in cinnamic acrylic ester mixture: with substance law synthetic macromolecule copolymer in cinnamic acrylic ester 1000-1200kg, with the synthetic xylene solution 1600-2000kg that contains low molecule copolymer in cinnamic acrylic ester of solution method, wherein copolymer in cinnamic acrylic ester and dimethylbenzene are pressed the 1:1 preparation, contain in described macromolecule styrene-acrylate copolymer that low molecular xylene solution joins melting described, in the low-molecular-weight copolymer in cinnamic acrylic ester mixing process of height, the 3%-6% by high low-molecular-weight copolymer in cinnamic acrylic ester total amount adds epoxy modified phenolic resin again; (2) copolymer in cinnamic acrylic ester mixture devolatilization: with the copolymer in cinnamic acrylic ester of above-mentioned reaction, under 80-100 ℃ of temperature slaking 2-4 hour, be warming up to again under 140-160 ℃, distilled desolventizing dimethylbenzene and residual monomer 2-4 hour; With the described copolymer in cinnamic acrylic ester of distillation devolatilization, vacuum volatilization, temperature rises to 160-180 ℃, devolatilization 2-6 hour, obtains the mixed flour-carbon resin of epoxide modified phenolic aldehyde increase-volume copolymer in cinnamic acrylic ester.
2. the method for raising styryl flour-carbon resin consistency according to claim 1 is characterized in that: the synthetic low molecule copolymer in cinnamic acrylic ester number-average molecular weight of described solution method is 3 * 10
3-5 * 10
3
3. the method for raising styryl flour-carbon resin consistency according to claim 1, it is characterized in that: substance law synthetic macromolecule copolymer in cinnamic acrylic ester number-average molecular weight is 2 * 10
5-4 * 10
5
4. the method for raising styryl flour-carbon resin consistency according to claim 1 is characterized in that: add epoxy modified phenolic resin by 4% of the low-molecular-weight copolymer in cinnamic acrylic ester total amount of described height.
5. the method for raising styryl flour-carbon resin consistency according to claim 1, it is characterized in that: the described curing time is 3 hours, temperature is 85 ℃; Described distillation time is 2.5 hours, and temperature is 155 ℃; The described vacuum volatilization time is 4 hours, and temperature is 170 ℃.
6. the method for raising styryl flour-carbon resin consistency according to claim 1, it is characterized in that: described is 1100kg with substance law synthetic macromolecule copolymer in cinnamic acrylic ester; Described is 1800kg with the synthetic xylene solution that contains low molecule copolymer in cinnamic acrylic ester of solution method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210579576.9A CN103073810B (en) | 2012-12-27 | 2012-12-27 | Method for improving styryl carbon powder resin compatibility |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210579576.9A CN103073810B (en) | 2012-12-27 | 2012-12-27 | Method for improving styryl carbon powder resin compatibility |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103073810A true CN103073810A (en) | 2013-05-01 |
| CN103073810B CN103073810B (en) | 2015-07-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210579576.9A Active CN103073810B (en) | 2012-12-27 | 2012-12-27 | Method for improving styryl carbon powder resin compatibility |
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| Country | Link |
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| CN (1) | CN103073810B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348426A (en) * | 2015-11-26 | 2016-02-24 | 宁波佛来斯通新材料有限公司 | Preparation method for low-temperature fixing chemical ink powder resin and method for preparing ink powders |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3065657B2 (en) * | 1990-06-08 | 2000-07-17 | 株式会社リコー | Dry type electrophotographic toner |
| CN1944485A (en) * | 2006-09-19 | 2007-04-11 | 张家港市威迪森油墨有限公司 | Blend polymerizing preparing method for copolymer resin |
-
2012
- 2012-12-27 CN CN201210579576.9A patent/CN103073810B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3065657B2 (en) * | 1990-06-08 | 2000-07-17 | 株式会社リコー | Dry type electrophotographic toner |
| CN1944485A (en) * | 2006-09-19 | 2007-04-11 | 张家港市威迪森油墨有限公司 | Blend polymerizing preparing method for copolymer resin |
Non-Patent Citations (3)
| Title |
|---|
| 姜真，等: "墨粉低温定影性能的影响因素分析", 《热固性树脂》, vol. 26, no. 5, 30 September 2011 (2011-09-30) * |
| 李求进，等: "苯乙烯-甲基丙烯酸甲酯共聚物与酚醛树脂共混体系相性态控制研究", 《功能材料》, vol. 38, 15 November 2007 (2007-11-15), pages 2864 - 2866 * |
| 范保荃: "试述墨粉及其共聚树脂", 《复印》, no. 4, 31 December 1997 (1997-12-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348426A (en) * | 2015-11-26 | 2016-02-24 | 宁波佛来斯通新材料有限公司 | Preparation method for low-temperature fixing chemical ink powder resin and method for preparing ink powders |
| CN105348426B (en) * | 2015-11-26 | 2018-04-27 | 宁波佛来斯通新材料有限公司 | The preparation method of low-temperature fixing chemistry ink powder resin and the method for preparing ink powder |
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| Publication number | Publication date |
|---|---|
| CN103073810B (en) | 2015-07-22 |
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Effective date of registration: 20231102 Address after: 438000 Building 5, No. 1 Xingang 1st Road, Huangzhou District, Huanggang City, Hubei Province (self declared) Patentee after: Zhongke Intelligent Technology (Huanggang) Co.,Ltd. Address before: 438000 Far East Industrial Park, No.1 Xingang 1st Road, Huanggang Economic Development Zone, Huanggang City, Hubei Province Patentee before: HUBEI FAREAST ZHUOYUE TECHNOLOGY Co.,Ltd. |