CN105585648A - Polyvinyl chloride for battery separators, and production device and method thereof - Google Patents
Polyvinyl chloride for battery separators, and production device and method thereof Download PDFInfo
- Publication number
- CN105585648A CN105585648A CN201610077824.8A CN201610077824A CN105585648A CN 105585648 A CN105585648 A CN 105585648A CN 201610077824 A CN201610077824 A CN 201610077824A CN 105585648 A CN105585648 A CN 105585648A
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- CN
- China
- Prior art keywords
- polyvinyl chloride
- battery separator
- initator
- copper sulphate
- potassium peroxydisulfate
- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/02—Monomers containing chlorine
- C08F114/04—Monomers containing two carbon atoms
- C08F114/06—Vinyl chloride
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
Abstract
The invention relates to the field of vinyl chloride monomer emulsion polymerization methods, and particularly relates to a polyvinyl chloride for battery separators, and a production device and method thereof. The polyvinyl chloride is prepared from the following raw materials in parts by weight: a vinyl chloride monomer, an emulsifier, an initial initiator, an initiator, an after-treatment agent and soft water. The device for producing the polyvinyl chloride powder for battery separators is a polymerization kettle. The polymerization kettle comprises a motor, a transmission structure, a stirring system and a bracket, wherein the length-diameter ratio of the device is (4-6):1, stirring blades of the stirring system are spiral, the motor is provided with a frequency converter, and the capacity of the device is 13.5m<3>. By redesigning and testing the stirring blades, the length-diameter ratio of the reaction kettle is improved, so that the product with stable quality is generated.
Description
Technical field
The present invention relates to VCM emulsion polymerisation process field, be specifically related to a kind of battery separator polyvinyl chlorideAnd process units and method.
Background technology
The polyvinyl chloride powder of producing in the past battery separator is to adopt 14m3Polymeric kettle is produced, and this production technology is mainAdopt pyknic polymeric kettle to produce, draw ratio is 5:2. Because its production technology, equipment are optimized not, this production dressBe placed in and forever closed for 2012, at present the domestic polyvinyl chloride powder production line that there is no emulsion method battery separator.And quality is stable not, each index parameter fluctuates greatly up and down. User uses and should not operate, the product shelves of producingInferior low.
Summary of the invention
In view of the deficiencies in the prior art, the object of the invention is to provide a kind of battery separator polyvinyl chloride and production thereofApparatus and method.
The technical solution used in the present invention is:
A kind of battery separator polyvinyl chloride, described polyvinyl chloride is made up of following raw material by weight:
VCM 25-43 part;
Emulsifying agent: stearic acid 0.05-0.8 part, dodecyl acid 0.05-0.5 part, solid caustic soda 0.03-0.15 part;
Initial initator: potassium peroxydisulfate 0.01-0.05 part, sodium hydrogensulfite 0.03-0.15 part, copper sulphate 0.15-0.25Part;
Initator: potassium peroxydisulfate 0.1-0.25 part, copper sulphate 0.03-0.2 part;
Post-treatment agent: potassium hydroxide 0.05-0.15 part, dodecyl acid 0.1-0.25 part;
Soft water: 50-70 part.
Described polyvinyl chloride is made up of following raw material by weight:
VCM 30-35 part;
Emulsifying agent: stearic acid 0.1-0.2 part, dodecyl acid 0.1-0.2 part, solid caustic soda 0.05-0.08 part;
Initial initator: potassium peroxydisulfate 0.01-0.02 part, sodium hydrogensulfite 0.05-0.1 part, copper sulphate 0.15-0.2Part;
Initator: potassium peroxydisulfate 0.1-0.15 part, copper sulphate 0.05-0.1 part;
Post-treatment agent: potassium hydroxide 0.05-0.1 part, dodecyl acid 0.1-0.15 part;
Soft water: 55-60 part.
A device of producing battery separator polyvinyl chloride powder, described device is polymeric kettle, described polymeric kettle bagDraw together motor, drive mechanism, stirring system and support, described device draw ratio is 4～6:1.
The paddle of described stirring system is spirality.
Described motor is provided with frequency converter.
Described installed capacity is 13.5m3。
Adopt described device to produce the method for described battery separator polyvinyl chloride, it is characterized in that: described method bagDraw together following steps:
1) in described polymeric kettle, add the soft water of initial initator and 1/3 to add in still, start and stir;
2) emulsifying agent is added in still, stir;
3) add VCM, stir, add initator, remaining water, polymerization reaction take place, treats to fall in stillAfter pressure, add post-treatment agent to obtain latex;
4) the spray-dried polyvinyl chloride powder that obtains battery separator.
Described step 1) mixing speed is turn/min of 10-30, time 20-30 minute.
Described step 3) mixing speed is turn/min of 60-80,
Described step 3) polymeric reaction temperature is 50-65 DEG C, the reaction time is 400-500 minute.
A kind of battery separator polyvinyl chloride and process units and method provided by the invention, beneficial effect is as follows:
1, the present invention adopts the emulsion polymerisation process of 13.5m3 polymeric kettle to produce the polyvinyl chloride powder of battery separatorEnd, redesigns, tests stirring blade, explores the agitating auger paddle that is applicable to battery separator material property energy;
2, the motor attached with frequency converters of the present invention to stirring blade, adjusts the rotating speed stirring, and explores battery separatorThe mixing speed of material property energy;
3, the present invention is to changing in still type, and polymeric kettle is designed to asthenic, and its draw ratio is 4～6:1, of the present inventionStill attenuates than reactor still footpath in the past, and still attenuates and is elongatedly conducive to mass transfer (pass cold, conduct heat), because when still reactionThe extraneous still of constantly giving is interior to heat, to cold, ensures that reactor temperature is constant, and product quality is better like this, cold or heatAmount is accelerated to the speed of propagating in still, makes reaction better controlled, and the powder particle of generation is more even, qualityHigher;
4, stir and used frequency converter and stirring blade, can regulate the speed of stirring and the effect of mixing, furtherReach and control reaction, generate stay-in-grade product;
5, the stage of reaction of the present invention is more excellent, and the present invention divides initial initator and initator, adds at twice, allows anti-Should evenly carry out, avoid vigorous reaction wayward and produce low-grade product;
6, the present invention is optimized the auxiliary agent of formula, use, makes uniform in quality, and indices reaches useThe desired parameter in family.
Brief description of the drawings
Fig. 1: the present invention produces the device schematic diagram of battery separator polyvinyl chloride powder;
Fig. 2: the present invention produces the paddle schematic diagram of the device of battery separator polyvinyl chloride powder;
Wherein: motor 1, drive mechanism 2, paddle 3, support 4.
Detailed description of the invention
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to enforcementThe scope of example statement.
Embodiment 1
A kind of battery separator polyvinyl chloride, described polyvinyl chloride is made up of following raw material by weight:
25 parts of VCMs;
0.05 part of stearic acid, 0.05 part of dodecyl acid, 0.03 part of solid caustic soda;
0.01 part of potassium peroxydisulfate, 0.03 part of sodium hydrogensulfite, copper sulphate 0.15-part;
0.1 part of potassium peroxydisulfate, 0.03 part, copper sulphate;
0.05 part, potassium hydroxide, 0.1 part of dodecyl acid;
Soft water: 50 parts.
Embodiment 2
A kind of battery separator polyvinyl chloride, described polyvinyl chloride is made up of following raw material by weight:
30 parts of VCMs;
0.1 part of stearic acid, 0.1 part of dodecyl acid, 0.05 part of solid caustic soda;
0.01 part of potassium peroxydisulfate, 0.05 part of sodium hydrogensulfite, 0.15 part, copper sulphate;
0.1 part of potassium peroxydisulfate, 0.05 part, copper sulphate;
0.05 part, potassium hydroxide, 0.1 part of dodecyl acid;
Soft water: 55 parts.
Embodiment 3
A kind of battery separator polyvinyl chloride, described polyvinyl chloride is made up of following raw material by weight:
35 parts of VCMs;
0.2 part of stearic acid, 0.2 part of dodecyl acid, 0.08 part of solid caustic soda;
0.02 part of potassium peroxydisulfate, 0.1 part of sodium hydrogensulfite, 0.2 part, copper sulphate;
0.15 part of potassium peroxydisulfate, 0.1 part, copper sulphate;
0.1 part, potassium hydroxide, 0.15 part of dodecyl acid;
Soft water: 60 parts.
Embodiment 4
A kind of battery separator polyvinyl chloride, described polyvinyl chloride is made up of following raw material by weight:
43 parts of VCMs;
0.8 part of stearic acid, 0.5 part of dodecyl acid, 0.15 part of solid caustic soda;
0.05 part of potassium peroxydisulfate, 0.15 part of sodium hydrogensulfite, 0.25 part, copper sulphate;
0.25 part of potassium peroxydisulfate, 0.2 part, copper sulphate;
0.15 part, potassium hydroxide, 0.25 part of dodecyl acid;
Soft water: 70 parts.
Embodiment 5
A kind of battery separator polyvinyl chloride, described polyvinyl chloride is made up of following raw material by weight:
28 parts of VCMs;
0.15 part of stearic acid, 0.18 part of dodecyl acid, 0.07 part of solid caustic soda;
0.015 part of potassium peroxydisulfate, 0.058 part of sodium hydrogensulfite, 0.18 part, copper sulphate;
0.13 part of potassium peroxydisulfate, 0.08 part, copper sulphate;
0.08 part, potassium hydroxide, 0.13 part of dodecyl acid;
Soft water: 58 parts.
Embodiment 6
A device of producing battery separator polyvinyl chloride powder, described device is polymeric kettle, described polymeric kettle bagDraw together motor 1, drive mechanism 2, stirring system and support 4, it is characterized in that: described device draw ratio is 5:1.
The paddle 3 of described stirring system is spirality.
Described motor 1 is provided with frequency converter.
Described installed capacity is 13.5m3。
Embodiment 7
The method of producing battery separator polyvinyl chloride, said method comprising the steps of:
1) add in still to the soft water that adds potassium peroxydisulfate, sodium hydrogensulfite, copper sulphate and 1/3 in described polymeric kettle,Starting stirring setting speed is turn/min of 10-30, time 20-30 minute;
2) stearic acid, dodecyl acid, solid caustic soda are added in still;
3) add VCM, adjusting rotating speed is turn/min of 60-80, adds potassium peroxydisulfate, copper sulphate, at 50-65 DEG CLower polymerization reaction take place 400-500 minute adds potassium hydroxide, the sour latex that obtains of dodecyl after step-down in still;
4) the spray-dried polyvinyl chloride powder that obtains battery separator.
Described step 1) mixing speed is turn/min of 10-30.
The battery separator that polyvinyl chloride of the present invention is made the results are shown in Table 1 with commercially available, Comparison of standards.
Several baffle material contrasts of table 1
As shown in Table 1, the battery separator intensity that polyvinyl chloride of the present invention is made is the highest, and heat endurance is best, porosityHeight, powder particle is more even, and quality is higher.
The above embodiments are only the preferred technical solution of the present invention, and should not be considered as for restriction of the present invention this ShenPlease in embodiment and feature in embodiment in the situation that not conflicting, can mutually be combined. Guarantor of the present inventionThe scope of protecting should with claim record technical scheme, comprise claim record technical scheme in technical characterictic etc.Be protection domain with alternative. Being equal within the scope of this, replaces and improves, also within protection scope of the present invention.
Claims (10)
1. a battery separator polyvinyl chloride, is characterized in that: described polyvinyl chloride is made up of following raw material by weight:
VCM 25-43 part;
Emulsifying agent: stearic acid 0.05-0.8 part, dodecyl acid 0.05-0.5 part, solid caustic soda 0.03-0.15 part;
Initial initator: potassium peroxydisulfate 0.01-0.05 part, sodium hydrogensulfite 0.03-0.15 part, copper sulphate 0.15-0.25 part;
Initator: potassium peroxydisulfate 0.1-0.25 part, copper sulphate 0.03-0.2 part;
Post-treatment agent: potassium hydroxide 0.05-0.15 part, dodecyl acid 0.1-0.25 part;
Soft water: 50-70 part.
2. battery separator polyvinyl chloride according to claim 1, is characterized in that: described polyvinyl chloride is made up of following raw material by weight:
VCM 30-35 part;
Emulsifying agent: stearic acid 0.1-0.2 part, dodecyl acid 0.1-0.2 part, solid caustic soda 0.05-0.08 part;
Initial initator: potassium peroxydisulfate 0.01-0.02 part, sodium hydrogensulfite 0.05-0.1 part, copper sulphate 0.15-0.2 part;
Initator: potassium peroxydisulfate 0.1-0.15 part, copper sulphate 0.05-0.1 part;
Post-treatment agent: potassium hydroxide 0.05-0.1 part, dodecyl acid 0.1-0.15 part;
Soft water: 55-60 part.
3. a device of producing battery separator polyvinyl chloride powder, described device is polymeric kettle, described polymeric kettle comprises motor (1), drive mechanism (2), stirring system and support (4), it is characterized in that: described device draw ratio is 4 ~ 6:1.
4. device according to claim 3, is characterized in that: the paddle (3) of described stirring system is spirality.
5. device according to claim 3, is characterized in that: described motor (1) is provided with frequency converter.
6. device according to claim 3, is characterized in that: described installed capacity is 13.5m3。
7. adopt the method for installing battery separator polyvinyl chloride described in production claim 1 or 2 described in claim 3-6 any one, it is characterized in that: said method comprising the steps of:
1) in described polymeric kettle, add the soft water of initial initator and 1/3 to add in still, start and stir;
2) emulsifying agent is added in still, stir;
3) add VCM, stir, add initator, remaining water, polymerization reaction take place adds post-treatment agent to obtain latex after step-down in still;
4) the spray-dried polyvinyl chloride powder that obtains battery separator.
8. according to the method for claim 7, it is characterized in that: described step 1) mixing speed is turn/min of 10-30, time 20-30 minute.
9. according to the method for claim 7, it is characterized in that: described step 3) mixing speed is turn/min of 60-80.
10. according to the method for claim 7, it is characterized in that: described step 3) polymeric reaction temperature is 50-65 DEG C, the reaction time is 400-500 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610077824.8A CN105585648B (en) | 2016-02-03 | 2016-02-03 | A kind of battery separator polyvinyl chloride and its process units and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610077824.8A CN105585648B (en) | 2016-02-03 | 2016-02-03 | A kind of battery separator polyvinyl chloride and its process units and method |
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| Publication Number | Publication Date |
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| CN105585648A true CN105585648A (en) | 2016-05-18 |
| CN105585648B CN105585648B (en) | 2018-06-22 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2839284Y (en) * | 2005-09-08 | 2006-11-22 | 锦西化工机械(集团)有限责任公司 | Large polyfurnace for producing polyvinyl-chloride paste resin by emulsion polymerization |
| CN1978469A (en) * | 2006-11-23 | 2007-06-13 | 锦西化工机械(集团)有限责任公司 | Agitator of polymerizer for producing PVC resin paste by emulsion polymerization |
| CN101812148A (en) * | 2009-11-22 | 2010-08-25 | 天津渤天化工有限责任公司 | Method for producing polyvinyl chloride resin special for battery separator with moderate polymerization degree |
| CN101851309A (en) * | 2010-05-18 | 2010-10-06 | 武汉祥龙电业股份有限公司 | Production method for polyvinyl chloride powder for preparing baffle plate of lead acid storage battery |
-
2016
- 2016-02-03 CN CN201610077824.8A patent/CN105585648B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2839284Y (en) * | 2005-09-08 | 2006-11-22 | 锦西化工机械(集团)有限责任公司 | Large polyfurnace for producing polyvinyl-chloride paste resin by emulsion polymerization |
| CN1978469A (en) * | 2006-11-23 | 2007-06-13 | 锦西化工机械(集团)有限责任公司 | Agitator of polymerizer for producing PVC resin paste by emulsion polymerization |
| CN101812148A (en) * | 2009-11-22 | 2010-08-25 | 天津渤天化工有限责任公司 | Method for producing polyvinyl chloride resin special for battery separator with moderate polymerization degree |
| CN101851309A (en) * | 2010-05-18 | 2010-10-06 | 武汉祥龙电业股份有限公司 | Production method for polyvinyl chloride powder for preparing baffle plate of lead acid storage battery |
Non-Patent Citations (1)
| Title |
|---|
| 潘祖仁: "氯乙烯聚合釜的技术开发、引进技术消化和技术改造", 《聚氯乙烯》 * |
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Effective date of registration: 20180529 Address after: 443001 Dongshan Avenue 435-1-104, Wu Jia Gang District, Yichang, Hubei Applicant after: Yichang Bai Sichuan Environmental Testing Co., Ltd. Address before: No. 443003, Yichang, Hubei Province, victory No. three, 33-33-302 Applicant before: Xu Guangbin |
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