CN104193866A - Preparation method of polyvinyl acetate resin - Google Patents
Preparation method of polyvinyl acetate resin Download PDFInfo
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- CN104193866A CN104193866A CN201410414120.6A CN201410414120A CN104193866A CN 104193866 A CN104193866 A CN 104193866A CN 201410414120 A CN201410414120 A CN 201410414120A CN 104193866 A CN104193866 A CN 104193866A
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Abstract
The invention discloses a preparation method of a polyvinyl acetate resin. The preparation method comprises the following steps: sequentially adding vinyl acetate, butanone, acetic acid and a composite redox initiator into a kettle, heating to 50-70 DEG C, reacting for 4-6 hours, and continuing the reaction for 4-6 hours while controlling the temperature at 75-90 DEG C, wherein the mass ratio of the butanone to the vinyl acetate is (0.6-2):1, the mass ratio of the acetic acid to the vinyl acetate is (0.3-0.6):1, the composite redox initiator is a mixture of cyclohexanone peroxide, dibenzoyl peroxide and tert-butyl hydroperoxide, and the mass ratio of the composite redox initiator to the vinyl acetate is (0.01-0.05):1. The polyvinyl acetate resin has the advantages of favorable toughness, favorable plasticity, favorable stability, favorable aging resistance, high safety and no toxicity, is free of arsenic, lead or mercury, and is a preferable material for a chewing gum base.
Description
Technical field
The present invention relates to chemical industry resin deep process technology field, especially a kind of preparation method of polyvinyl acetate resin.
Background technology
Polyvinyl acetate resin is taking vinyl acetate between to for plastic as raw material, and the amorphous polymer generating through polyreaction, its appearance transparent, is soluble in benzene, acetone and trichloromethane equal solvent.Polyvinyl acetate resin itself is nontoxic, green safety, and water insoluble and oily polymer substance, cannot be absorbed by the body.Therefore, polyvinyl acetate resin Chang Zuowei chewing gum base is applied to food service industry.
The preparation method of traditional polyvinyl acetate resin is using benzoyl peroxide as initiator, and vinyl acetate between to for plastic obtains polyvinyl acetate resin by mass polymerization.This method adopts single initiator, and the toughness of products therefrom and plasticity are all poor, does not reach the requirement of edible rank polyvinyl acetate resin.
Summary of the invention
The object of this invention is to provide a kind of preparation method of polyvinyl acetate resin, this method is by adopting compound oxidizing reduction initiator, and the toughness of products and the plasticity that obtain are good.
In order to address the above problem, the technical solution used in the present invention is:
The preparation method of this polyvinyl acetate resin, comprise the following steps: successively by vinyl acetate between to for plastic, butanone, acetic acid and compound oxidizing reduction initiator add in still, be warming up to 50 ° of C～70 ° C, react 4 hours～6 hours, then controlling temperature is 75 ° of C～90 ° C, continues reaction 4 hours～6 hours; Wherein, the mass ratio of butanone and vinyl acetate between to for plastic is 0.6～2:1; The mass ratio of acetic acid and vinyl acetate between to for plastic is 0.3～0.6:1; Compound oxidizing reduction initiator is cyclohexanone peroxide, the mixture of dibenzoyl peroxide and three kinds of materials of tertbutyl peroxide; The mass ratio of compound oxidizing reduction initiator and vinyl acetate between to for plastic is 0.01～0.05:1.
In technique scheme, technical scheme can also be more specifically: the mass ratio of butanone and vinyl acetate between to for plastic is 0.8～1:1; The mass ratio of compound oxidizing reduction initiator and vinyl acetate between to for plastic is 0.03:1.
Further, the mass ratio of butanone and vinyl acetate between to for plastic is 1.2～1.5:1; The mass ratio of compound oxidizing reduction initiator and vinyl acetate between to for plastic is 0.01:1.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
1, in polyreaction of the present invention, adopt compound oxidizing reduction initiator, compared with the polymerization temperature of lower 80 DEG C～120 DEG C of traditional single initiator, the present invention is starting polymerization reaction at 50 DEG C, thereby reduces energy consumption of reaction, saves production cost; The present invention adopts the segmentation mode of temperature control step by step, and polyreaction is carried out more stably, thereby softening temperature and the molecular weight of regulation and control product that can be stable reach the effect that improves toughness of products and plasticity.
2, this polyvinyl acetate resin polymerization degree is higher, and molecular-weight average is higher than 40,000, and monomer residue is less, and toughness, plasticity, stability and ageing-resistant performance are good, and or not containing arsenic and heavy metal, safety non-toxic, does not reach food rank, is the preferred material of chewing gum base.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
Respectively by 0.5 ton of vinyl acetate between to for plastic, 0.3 ton of butanone, 0.25 ton of acetic acid and 5 kilograms of compound oxidizing reduction initiators add in still, heating, be warming up to 50 ° of C, react after 6 hours and be warming up to 75 ° of C, continue reaction 6 hours, stopped reaction, distillation, dry, granulation packaging, obtains polyvinyl acetate resin.
Compound oxidizing reduction initiator in the present embodiment is cyclohexanone peroxide, the mixture of dibenzoyl peroxide and three kinds of materials of tertbutyl peroxide.
Embodiment 2
Respectively by 1 ton of vinyl acetate between to for plastic, 1.2 tons of butanone, 0.3 ton of acetic acid and 0.03 ton of compound oxidizing reduction initiator add in still, heating, be warming up to 60 ° of C and start timing, react after 5 hours and be warming up to 80 ° of C, continue reaction 5 hours, stopped reaction, distillation, dry, granulation packaging, obtains polyvinyl acetate resin.
Compound oxidizing reduction initiator in the present embodiment is cyclohexanone peroxide, the mixture of dibenzoyl peroxide and three kinds of materials of tertbutyl peroxide.
Embodiment 3
Respectively by 1.5 tons of vinyl acetate between to for plastics, 3 tons of butanone, 1.2 tons of acetic acid and 75 kilograms of compound oxidizing reduction initiators add in still, heating, be warming up to 70 ° of C and start timing, react after 4 hours and be warming up to 90 ° of C, continue reaction 4 hours, stopped reaction, distillation, dry, granulation packaging, obtains polyvinyl acetate resin.
Compound oxidizing reduction initiator in the present embodiment is cyclohexanone peroxide, the mixture of dibenzoyl peroxide and three kinds of materials of tertbutyl peroxide.
Heavy metal content to the polyvinyl acetate resin product in above-mentioned 3 embodiment respectively, monomer residue, the projects such as molecular-weight average and the polymerization degree are measured, and measurement result is in table 1:
The detection index of table 1 polyvinyl acetate resin
From data in table 1, this polyvinyl acetate resin monomer residue is less, and molecular-weight average is higher than 40,000, and mean polymerisation degree is 500～600, and or not containing heavy metals such as arsenic, lead, mercury, safety non-toxic, does not reach food rank, can be used as the preferred material of chewing gum base.
Claims (3)
1. the preparation method of a polyvinyl acetate resin, it is characterized in that: successively by vinyl acetate between to for plastic, butanone, acetic acid and compound oxidizing reduction initiator add in still, be warming up to 50 ° of C～70 ° C, react 4 hours～6 hours, then controlling temperature is 75 ° of C～90 ° C, continues reaction 4 hours～6 hours; Wherein, the mass ratio of described butanone and described vinyl acetate between to for plastic is 0.6～2:1; The mass ratio of described acetic acid and described vinyl acetate between to for plastic is 0.3～0.6:1; Described compound oxidizing reduction initiator is cyclohexanone peroxide, the mixture of dibenzoyl peroxide and three kinds of materials of tertbutyl peroxide; The mass ratio of described compound oxidizing reduction initiator and described vinyl acetate between to for plastic is 0.01～0.05:1.
2. the preparation method of polyvinyl acetate resin according to claim 1, is characterized in that: the mass ratio of described butanone solvent and described vinyl acetate between to for plastic is 0.8～1:1; The mass ratio of described compound oxidizing reduction initiator and described vinyl acetate between to for plastic is 0.03:1.
3. the preparation method of polyvinyl acetate resin according to claim 1, is characterized in that: the mass ratio of described butanone and described vinyl acetate between to for plastic is 1.2～1.5:1; The mass ratio of described compound oxidizing reduction initiator and described vinyl acetate between to for plastic is 0.01:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410414120.6A CN104193866B (en) | 2014-08-21 | 2014-08-21 | The preparation method of polyvinyl acetate resin |
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| CN201410414120.6A CN104193866B (en) | 2014-08-21 | 2014-08-21 | The preparation method of polyvinyl acetate resin |
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| CN104193866A true CN104193866A (en) | 2014-12-10 |
| CN104193866B CN104193866B (en) | 2016-08-24 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3109837A (en) * | 1959-06-05 | 1963-11-05 | Kurashiki Rayon Co | Homopolymerization of vinyl acetate |
| CN101331161A (en) * | 2005-12-16 | 2008-12-24 | 3M创新有限公司 | Method of free radically polymerizing vinyl monomers |
| CN101544714A (en) * | 2009-05-05 | 2009-09-30 | 安徽皖维高新材料股份有限公司 | Polyvinyl acetate with low polymerization degree and polymerization method thereof |
| CN102863571A (en) * | 2011-07-07 | 2013-01-09 | 中国石油化工集团公司 | Method for preparing PVAC (Polyvinyl Acetate) |
-
2014
- 2014-08-21 CN CN201410414120.6A patent/CN104193866B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3109837A (en) * | 1959-06-05 | 1963-11-05 | Kurashiki Rayon Co | Homopolymerization of vinyl acetate |
| CN101331161A (en) * | 2005-12-16 | 2008-12-24 | 3M创新有限公司 | Method of free radically polymerizing vinyl monomers |
| CN101544714A (en) * | 2009-05-05 | 2009-09-30 | 安徽皖维高新材料股份有限公司 | Polyvinyl acetate with low polymerization degree and polymerization method thereof |
| CN102863571A (en) * | 2011-07-07 | 2013-01-09 | 中国石油化工集团公司 | Method for preparing PVAC (Polyvinyl Acetate) |
Non-Patent Citations (1)
| Title |
|---|
| 徐玲主编: "《高分子化学（第二版）》", 31 January 2010, article ""二、醋酸乙烯酯溶液聚合"", pages: 131-132 * |
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| CN104193866B (en) | 2016-08-24 |
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