CN106008763A - Production method of polyvinyl acetate - Google Patents
Production method of polyvinyl acetate Download PDFInfo
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- CN106008763A CN106008763A CN201610484173.4A CN201610484173A CN106008763A CN 106008763 A CN106008763 A CN 106008763A CN 201610484173 A CN201610484173 A CN 201610484173A CN 106008763 A CN106008763 A CN 106008763A
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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
- C08F18/00—Homopolymers and copolymers 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 an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F18/02—Esters of monocarboxylic acids
- C08F18/04—Vinyl esters
- C08F18/08—Vinyl acetate
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- Polymers & Plastics (AREA)
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- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract
The invention discloses a production method of polyvinyl acetate. Tert-butyl hydroperoxide serves as an initiating agent, part of a reaction raw material is added in the first place for a prepolymerization reaction, and then the remaining reaction raw material is added for a polymerization reaction. The initiating agent is good in activity and high in reaction speed, purity of polyvinyl acetate is remarkably improved, and less monomer residues exist.
Description
Technical field
The present invention relates to technical field of polymer materials, the production method of a kind of polyvinyl acetate.
Background technology
Polyvinyl acetate is commonly used for coating, adhesive, paper, chewing gum base and fabric finishing agent, it is possible to as the raw material of the materials such as polyvinyl alcohol, vinyl acetate-chloride copolymer, vinyl acetate-ethylene copolymer.Polyvinyl acetate resin itself is nontoxic, green safety, and water insoluble and oily polymer substance, it is impossible to be absorbed by the body.
At present, monomer, initiator, solution etc. are put into and carry out polyreaction by the preparation process of polyvinyl acetate in the lump, but its course of reaction is more violent, and reaction temperature is higher, and side reaction is more, products obtained therefrom impure more, and monomer residue is more.
Summary of the invention
It is an object of the invention to provide the production method of a kind of polyvinyl acetate, this method can solve the problem that polyvinyl acetate product purity is low and monomer residue is many.
In order to solve the problems referred to above, the technical solution used in the present invention is:
The production method of this polyvinyl acetate comprises the following steps:
A, prepolymerization stage: 50 weight portions～100 weight portion VAMs, 5 weight portions～12 weight portion initiators, 70 weight portions～120 parts by weight acetic acid solution are added in reactor, regulation pH value is to 3～5, it is warming up to 75 DEG C～90 DEG C, arranging mixing speed is 150 revs/min～170 revs/min, enter the prepolymerization stage, react 1 hour～1.1 hours；
B, polymerization stage: in step A gained solution with 1 weight portion/point～2 weight portions/point speed add VAM, with 0.5 weight portion/point～1 weight portion/point speed add initiator, with 3 weight portions/point～5 weight portions/point speed add acetum, during adding VAM, initiator and acetum, arranging mixing speed is 220 revs/min～300 revs/min, keeping reaction temperature is 75 DEG C～90 DEG C, when the degree of polymerization of reaction extremely poly-ethyl acetate is 300～400, stopped reaction；The addition of polymerization stage VAM, initiator and acetum is respectively 100 weight portions～150 weight portions, 8 weight portions～15 weight portions, 200 weight portions～220 weight portions；
Wherein, described initiator is tert-butyl hydroperoxide.
In technique scheme, more specifically technical scheme is it may also is that the reaction temperature in prepolymerization stage is 85 DEG C～88 DEG C, and the reaction temperature of polymerization stage is 79 DEG C～83 DEG C.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
1, the present invention is firstly added partial monosomy, initiator and solvent and carries out prepolymerization, then adds residual monomer, initiator and solvent and carries out polyreaction, reacting balance, and in course of reaction, side reaction is less, and product purity significantly improves, and level of residual monomers is few.
, polymerization stage: in step A gained solution with 1 weight portion/point～2 weight portions/point speed add VAM, with 0.5 weight portion/point～1 weight portion/point speed add initiator, with 3 weight portions/point～5 weight portions/point speed add acetum, during adding VAM, initiator and acetum, arranging mixing speed is 220 revs/min～300 revs/min, keeping reaction temperature is 75 DEG C～90 DEG C, when the degree of polymerization of reaction extremely poly-ethyl acetate is 300～400, stopped reaction；The addition of polymerization stage VAM, initiator and acetum is respectively 100 weight portions～150 weight portions, 8 weight portions～15 weight portions, 200 weight portions～220 weight portions；
Wherein, described initiator is tert-butyl hydroperoxide.
In technique scheme, more specifically technical scheme is it may also is that the reaction temperature in prepolymerization stage is 85 DEG C～88 DEG C, and the reaction temperature of polymerization stage is 79 DEG C～83 DEG C.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
1, the present invention is firstly added partial monosomy, initiator and solvent and carries out prepolymerization, then adds residual monomer, initiator and solvent and carries out polyreaction, reacting balance, and in course of reaction, side reaction is less, and product purity significantly improves, and level of residual monomers is few.
/ kilogram, product purity is 92.5%.
Embodiment 2
The production method of the present embodiment polyvinyl acetate comprises the following steps:
A, prepolymerization stage: 70 parts of VAMs, 12 parts of tert-butyl hydroperoxide, 100 parts of acetums are added in reactor, regulation pH value, to 4～5, is warming up to 85 DEG C～88 DEG C, and arranging mixing speed is 160 revs/min, enter the prepolymerization stage, react 1.1 hours；
B, polymerization stage: in step A gained solution with 1.5 weight portions/point speed add VAM, with 1 weight portion/point speed add tert-butyl hydroperoxide, with 4 weight portions/point speed add acetum, during adding VAM, initiator and acetum, arranging mixing speed is 260 revs/min, keeping reaction temperature is 83 DEG C～88 DEG C, when the degree of polymerization of reaction to poly-ethyl acetate is 350～365, and stopped reaction；The addition of polymerization stage VAM, tert-butyl hydroperoxide and acetum is respectively 120 weight portions, 15 weight portions, 220 weight portions.
The present embodiment polyvinyl acetate monomer residual quantity is 1.7 mg/kg, and product purity is 93.2%.
Embodiment 3
The production method of the present embodiment polyvinyl acetate comprises the following steps:
A, prepolymerization stage: 100 parts of VAMs, 5 parts of tert-butyl hydroperoxide, 70 parts of acetums are added in reactor, regulation pH value, to 3～5, is warming up to 75 DEG C～80 DEG C, and arranging mixing speed is 170 revs/min, enter the prepolymerization stage, react 1 hour；
B, polymerization stage: in step A gained solution with 2 weight portions/point speed add VAM, with 0.5 weight portion/point speed add tert-butyl hydroperoxide, with 5 weight portions/point speed add acetum, during adding VAM, initiator and acetum, arranging mixing speed is 220 revs/min, keeping reaction temperature is 86 DEG C～90 DEG C, when the degree of polymerization of reaction to poly-ethyl acetate is 388～400, and stopped reaction；The addition of polymerization stage VAM, tert-butyl hydroperoxide and acetum is respectively 100 weight portions, 10 weight portions, 210 weight portions.
The present embodiment polyvinyl acetate monomer residual quantity is 1.8 mg/kg, and product purity is 92.7%.
Claims (2)
1. the production method of a polyvinyl acetate, it is characterised in that comprise the following steps:
A, 50 weight portions～100 weight portion VAMs, 5 weight portions～12 weight portion initiators, 70 weight portions～120 parts by weight acetic acid solution are added in reactor, regulation pH value is to 3～5, it is warming up to 75 DEG C～90 DEG C, arranging mixing speed is 150 revs/min～170 revs/min, reacts 1 hour～1.1 hours；
B, in step A gained solution with 1 weight portion/point～2 weight portions/point speed add VAM, with 0.5 weight portion/point～1 weight portion/point speed add initiator, with 3 weight portions/point～5 weight portions/point speed add acetum, during adding VAM, initiator and acetum, arranging mixing speed is 220 revs/min～300 revs/min, keeping reaction temperature is 75 DEG C～90 DEG C, when the degree of polymerization of reaction to poly-ethyl acetate is 300～400, and stopped reaction；The addition of VAM, initiator and acetum is respectively 100 weight portions～150 weight portions, 8 weight portions～15 weight portions, 200 weight portions～220 weight portions；
Wherein, described initiator is tert-butyl hydroperoxide.
The production method of polyvinyl acetate the most according to claim 1, it is characterised in that the reaction temperature in described prepolymerization stage is 85 DEG C～88 DEG C, the reaction temperature of polymerization stage is 79 DEG C～83 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610484173.4A CN106008763A (en) | 2016-06-28 | 2016-06-28 | Production method of polyvinyl acetate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610484173.4A CN106008763A (en) | 2016-06-28 | 2016-06-28 | Production method of polyvinyl acetate |
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| CN106008763A true CN106008763A (en) | 2016-10-12 |
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| CN201610484173.4A Pending CN106008763A (en) | 2016-06-28 | 2016-06-28 | Production method of polyvinyl acetate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350008A (en) * | 2000-10-20 | 2002-05-22 | 孙益成 | Modified polyvinyl acetate emulsion |
| CN1807471A (en) * | 2005-01-20 | 2006-07-26 | 常德市金芙蓉精细化工有限责任公司 | Vinyl acetate based high viscosity latex preparation method |
| CN102827316A (en) * | 2012-09-05 | 2012-12-19 | 安徽皖维集团有限责任公司 | Preparation method for polyvinyl alcohol with low crystallinity |
| CN104628960A (en) * | 2015-01-28 | 2015-05-20 | 海安县中丽化工材料有限公司 | Preparation method of white latex |
-
2016
- 2016-06-28 CN CN201610484173.4A patent/CN106008763A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350008A (en) * | 2000-10-20 | 2002-05-22 | 孙益成 | Modified polyvinyl acetate emulsion |
| CN1807471A (en) * | 2005-01-20 | 2006-07-26 | 常德市金芙蓉精细化工有限责任公司 | Vinyl acetate based high viscosity latex preparation method |
| CN102827316A (en) * | 2012-09-05 | 2012-12-19 | 安徽皖维集团有限责任公司 | Preparation method for polyvinyl alcohol with low crystallinity |
| CN104628960A (en) * | 2015-01-28 | 2015-05-20 | 海安县中丽化工材料有限公司 | Preparation method of white latex |
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Application publication date: 20161012 |