CN101735357A - Method for improving ageing whiteness of vinyl chloride resin - Google Patents
Method for improving ageing whiteness of vinyl chloride resin Download PDFInfo
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- CN101735357A CN101735357A CN200810202352A CN200810202352A CN101735357A CN 101735357 A CN101735357 A CN 101735357A CN 200810202352 A CN200810202352 A CN 200810202352A CN 200810202352 A CN200810202352 A CN 200810202352A CN 101735357 A CN101735357 A CN 101735357A
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Abstract
The invention provides a method for improving ageing whiteness of vinyl chloride resin. The method comprises the following steps: adding water, dispersing agent, vinyl chloride monomer, initiator, fisheye resisting agent and pH regulator in a reaction kettle for polymerization, and adding terminator and antioxidant in the reaction system simultaneously to obtain vinyl chloride resin, wherein the pH regulator is ammonium hydrogen carbonate, the antioxidant is imperfectly hindered phenol chain terminator antioxidant, the weight ratio of pH regulator to antioxidant is 1:1.76-2. In the inventive method, the resin particle size distribution width is lowered, resin particle shape is more regular, the heat resistance of the produced vinyl chloride resin is enhanced, the ageing whiteness index is obviously improved, and inherent quality of resin is enhanced. The polymerization in the production process is stable, quality repeatability of resin of each batch is good, and the new aid adopting composite preparation method can be applied in cauldron industrialized production.
Description
Technical field
The present invention relates to the preparation method of polyvinyl chloride (PVC) RESINS, particularly in the polyvinyl chloride resin production process, improve the method for aging of product whiteness.
Background technology
In the polyvinyl chloride resin production,, for example, require polyvinyl chloride (PVC) RESINS that higher ageing whiteness is arranged, and require resin that good plasticizing capacity is arranged, just need to improve production method, use New-type adjuvant for obtaining the polyvinyl chloride (PVC) RESINS product of better quality.Existing manufacturing technique only adopts reaction later stage adding sodium hydroxide solution to come stable polymerization system pH value mostly, and the back adds the mode of terminator termination reaction, and it is relatively poor that the product aging whiteness is improved effect.
Summary of the invention
The technical issues that need to address of the present invention provide a kind of method that improves ageing whiteness of vinyl chloride resin, improve difficult defective to overcome the ageing whiteness of vinyl chloride resin that exists in the prior art.
Method of the present invention, comprise the steps: water, dispersion agent, vinyl chloride monomer, initiator, anti-flake agent and pH regulator agent are added in the reactor, 50～65 ℃, reaction times is 4.5～5.5 hours, carry out polyreaction, then terminator and oxidation inhibitor are added in the reaction system simultaneously, obtain polyvinyl chloride (PVC) RESINS; The parts by weight of component are:
1000 parts of vinyl chloride monomers
1000～1500 parts in water
0.2～0.35 part of dispersion agent
0.15～0.25 part of initiator
0.4～0.7 part of anti-flake agent
0.005～0.015 part of pH regulator agent
0.2～0.3 part of terminator;
Described pH regulator agent is a bicarbonate of ammonia;
Described dispersion agent is selected from polyvinyl alcohol (KH20) that Japanese synthetic chemistry company produces or in the Vltra tears (being called for short HPMC) more than one;
Described initiator is selected from more than one among the own ester abbreviation EHP of peroxy dicarbonate two (2-ethyl) and TX-99 (peroxidation neodecanoic acid isopropyl benzene ester) or the TX-36 (bis oxide (3,5, the 5-trimethylammonium) hexanoyl);
Described anti-flake agent is a Tert. Butyl Hydroquinone;
Described terminator is the acetone amido thiocarbamide (be called for short ATSC) that contracts, and can adopt the product of Hua Lian, Beijing chemical industry company limited;
Described oxidation inhibitor is non-complete Hinered phenols chain terminator and oxidation inhibitor (being called for short EB44-34), and can adopt the Ciba company trade mark is the product of EB44-34, is the oxidation inhibitor of 40% water base corpuscle emulsion form for a kind of weight concentration;
What need specification sheets is that above-mentioned reaction conditions and dispersion agent, initiator and the anti-flake agent etc. adopted are technology well known in the art;
The weight ratio of pH regulator agent and oxidation inhibitor is:
PH regulator agent: oxidation inhibitor=1: 1.76～2;
According to the present invention, it is 5～10% solution that bicarbonate of ammonia is mixed with weight concentration earlier, adds reactor then;
The applicant finds that improving the rosin products whiteness generally has two methods, adds pH regulator agent, heat-resisting terminator.The height of the pH value of polymerization system is to influence one of the particle form of resin and key factor of resin ageing whiteness, and dispersion system is also had certain influence.
The present invention is in the Production of PVC process, use new pH regulator agent-bicarbonate of ammonia, replace present NaOH pH value conditioning agent, in the stable polymerization system pH, add novel oxidation inhibitor EB44-34, to reach the purpose that the stable polymerization system improves the resin resistance toheat.
Adopt the prepared polyvinyl chloride (PVC) RESINS of aforesaid method, the particle diameter distribution width of resin decreases, and the resin particle form is more regular, and the polyvinyl chloride (PVC) RESINS resistance toheat of producing improves, and the ageing whiteness index improves significantly, and has promoted the inner quality of resin.And polyreaction is stable in the production process, and each batch resin quality good reproducibility is so this employing New-type adjuvant composite preparation process can be applicable in the big still industrial production.
Embodiment
Embodiment 1
Water, dispersion agent, vinyl chloride monomer, anti-flake agent Tert. Butyl Hydroquinone and initiator are added in the polymerization reaction kettle, and its ratio of weight and number is:
Vinyl chloride monomer: water: dispersion agent: initiator: anti-flake agent: bicarbonate of ammonia: terminator=1000: 1280: 0.28: 0.19: 0.55: 0.01: 0.25;
The weight ratio of pH regulator agent and oxidation inhibitor is:
PH regulator agent: oxidation inhibitor=1: 2;
Bicarbonate of ammonia is that weight concentration is 6% solution adding;
Temperature of reaction is 56.8 ℃, after 5 hours polyreaction, adds oxidation inhibitor with terminator in polymeric kettle, obtains polyvinyl chloride (PVC) RESINS.
Dispersion agent is the polyvinyl alcohol (KH20) produced of Japanese synthetic chemistry company and the mixture of Vltra tears (abbreviation HPMC), and weight ratio is 1: 0.68;
Initiator is that the own ester of peroxy dicarbonate two (2-ethyl) is called for short EHP and TX-99 (peroxidation neodecanoic acid isopropyl benzene ester) or TX-36 (bis oxide (3,5, the 5-trimethylammonium) more than one hexanoyl), anti-flake agent is a Tert. Butyl Hydroquinone, oxidation inhibitor is EB44-34;
Employing detects by GB/T 15595 required standards, and it is average more than 80 that the whiteness of polyvinyl chloride (PVC) RESINS product can reach, and the particle diameter of resin particle is thicker, and size distribution is concentrated relatively.
Embodiment 2
Adopt the method identical with embodiment 1, wherein:
1000 parts of vinyl chloride monomers
1500 parts in water
0.35 part of dispersion agent
0.25 part of initiator
0.7 part of anti-flake agent
0.015 part of pH regulator agent
0.3 part of terminator;
The weight ratio of pH regulator agent and oxidation inhibitor is: the pH regulator agent: oxidation inhibitor=1: 1.76;
Bicarbonate of ammonia is that weight concentration is 10% solution adding;
Adopt GB/T 15595 required standards to detect, it is average more than 79 that the whiteness of polyvinyl chloride (PVC) RESINS product can reach, and the particle diameter of resin particle is thicker, and size distribution is concentrated relatively.
Claims (4)
1. method that improves ageing whiteness of vinyl chloride resin, it is characterized in that, comprise the steps: water, dispersion agent, vinyl chloride monomer, initiator, anti-flake agent and pH regulator agent are added in the reactor, carry out polyreaction, add terminator and oxidation inhibitor in the reaction system simultaneously then, obtain polyvinyl chloride (PVC) RESINS, described pH regulator agent is a bicarbonate of ammonia, described oxidation inhibitor is non-complete Hinered phenols chain terminator oxidation inhibitor, and the weight ratio of pH regulator agent and oxidation inhibitor is: the pH regulator agent: oxidation inhibitor=1: 1.76～2.
2. method according to claim 1 is characterized in that, the parts by weight of component are:
1000 parts of vinyl chloride monomers
1000～1500 parts in water
0.2～0.35 part of dispersion agent
0.15～0.25 part of initiator
0.4～0.7 part of anti-flake agent
0.005～0.015 part of pH regulator agent
0.2～0.3 part of terminator.
3. method according to claim 1 is characterized in that, temperature of reaction is 50～65 ℃, and the reaction times is 4.5～5.5 hours.
4. method according to claim 1 is characterized in that described dispersion agent is selected from more than one in polyvinyl alcohol or the Vltra tears; Described initiator is selected from more than one among the own ester abbreviation EHP of peroxy dicarbonate two (2-ethyl) and TX-99 (peroxidation neodecanoic acid isopropyl benzene ester) or the TX-36 (bis oxide (3,5, the 5-trimethylammonium) hexanoyl); Described anti-flake agent is a Tert. Butyl Hydroquinone; Described terminator is the acetone amido thiocarbamide that contracts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810202352A CN101735357A (en) | 2008-11-06 | 2008-11-06 | Method for improving ageing whiteness of vinyl chloride resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810202352A CN101735357A (en) | 2008-11-06 | 2008-11-06 | Method for improving ageing whiteness of vinyl chloride resin |
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| CN101735357A true CN101735357A (en) | 2010-06-16 |
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| CN200810202352A Pending CN101735357A (en) | 2008-11-06 | 2008-11-06 | Method for improving ageing whiteness of vinyl chloride resin |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952219A (en) * | 2011-08-30 | 2013-03-06 | 中国石油化工股份有限公司 | Vinyl chloride monomer polymerization reaction system reaction termination method |
| CN102952225A (en) * | 2011-08-30 | 2013-03-06 | 中国石油化工股份有限公司 | Suspension polymerization method for reducing polyvinyl chloride resin fisheyes |
| CN105199026A (en) * | 2014-06-17 | 2015-12-30 | 上海氯碱化工股份有限公司 | Preparation method of special PVC resin for CPVC |
| CN106893011A (en) * | 2017-03-20 | 2017-06-27 | 青海盐湖工业股份有限公司 | A kind of whiteness Corvic high and preparation method thereof |
| CN107011589A (en) * | 2016-07-21 | 2017-08-04 | 佛山瑞箭体育器材有限公司 | A kind of method for improving polyvinyl chloride resin ageing whiteness |
| CN107011588A (en) * | 2016-07-20 | 2017-08-04 | 佛山瑞箭体育器材有限公司 | A kind of method for improving polyvinyl chloride resin ageing whiteness |
| CN108034015A (en) * | 2017-12-27 | 2018-05-15 | 山西阿科达化工科技有限公司 | A kind of preparation method of polyvinyl chloride |
| CN113651910A (en) * | 2021-09-15 | 2021-11-16 | 金川集团股份有限公司 | Preparation method of large-particle-size narrow-distribution polyvinyl chloride resin |
| CN115707719A (en) * | 2021-08-18 | 2023-02-21 | 中国石油化工股份有限公司 | PVC resin polymerization dispersing auxiliary agent, preparation method and resin preparation method |
-
2008
- 2008-11-06 CN CN200810202352A patent/CN101735357A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952219A (en) * | 2011-08-30 | 2013-03-06 | 中国石油化工股份有限公司 | Vinyl chloride monomer polymerization reaction system reaction termination method |
| CN102952225A (en) * | 2011-08-30 | 2013-03-06 | 中国石油化工股份有限公司 | Suspension polymerization method for reducing polyvinyl chloride resin fisheyes |
| CN102952225B (en) * | 2011-08-30 | 2014-12-10 | 中国石油化工股份有限公司 | Suspension polymerization method for reducing polyvinyl chloride resin fisheyes |
| CN105199026A (en) * | 2014-06-17 | 2015-12-30 | 上海氯碱化工股份有限公司 | Preparation method of special PVC resin for CPVC |
| CN107011588A (en) * | 2016-07-20 | 2017-08-04 | 佛山瑞箭体育器材有限公司 | A kind of method for improving polyvinyl chloride resin ageing whiteness |
| CN107011589A (en) * | 2016-07-21 | 2017-08-04 | 佛山瑞箭体育器材有限公司 | A kind of method for improving polyvinyl chloride resin ageing whiteness |
| CN106893011A (en) * | 2017-03-20 | 2017-06-27 | 青海盐湖工业股份有限公司 | A kind of whiteness Corvic high and preparation method thereof |
| CN108034015A (en) * | 2017-12-27 | 2018-05-15 | 山西阿科达化工科技有限公司 | A kind of preparation method of polyvinyl chloride |
| CN108034015B (en) * | 2017-12-27 | 2020-08-04 | 山西阿科达化工科技有限公司 | Preparation method of polyvinyl chloride |
| CN115707719A (en) * | 2021-08-18 | 2023-02-21 | 中国石油化工股份有限公司 | PVC resin polymerization dispersing auxiliary agent, preparation method and resin preparation method |
| CN115707719B (en) * | 2021-08-18 | 2023-10-20 | 中国石油化工股份有限公司 | PVC resin polymerization dispersion auxiliary agent, preparation method and resin preparation method |
| CN113651910A (en) * | 2021-09-15 | 2021-11-16 | 金川集团股份有限公司 | Preparation method of large-particle-size narrow-distribution polyvinyl chloride resin |
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Open date: 20100616 |