CN101077901A - High-strength polyvinyl acetate and preparing method thereof - Google Patents
High-strength polyvinyl acetate and preparing method thereof Download PDFInfo
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- CN101077901A CN101077901A CN 200710086659 CN200710086659A CN101077901A CN 101077901 A CN101077901 A CN 101077901A CN 200710086659 CN200710086659 CN 200710086659 CN 200710086659 A CN200710086659 A CN 200710086659A CN 101077901 A CN101077901 A CN 101077901A
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Abstract
The high strength white latex is the emulsion polymer of ethyl acetate prepared with PVA 4-6 weight portions, vinyl acetate 18-36 weight portions, OP-10 0.1-0.3 weight portions, 10 % concentrate ammonium persulfate solution 0.8-1.5 weight portions, sodium bicarbonate 0.1-0.2 weight portions, 2-ethoxyl ethyl acetate 0.6-1.2 weight portions, dibutyl phthalate 3-5 weight portions, glycol 0.08-0.15 weight portions, and water 50-75 weight portions. The present invention also discloses the preparation process of the white latex. The high strength white latex has homogeneous latex grain, high initial adhesion and high toughness, and may be used in adhering leather, timber, paper, etc.
Description
Technical field
The invention belongs to high molecular polymer technical field for building, relate in particular to the preparation method of a kind of high-strength polyvinyl acetate for building and this kind latex.
Background technology
The existing building white glue with vinyl is the emulsion polymer of vinyl acetate, is white in color or ivory-white stringy liquid, so claim white glue with vinyl.Its raw materials for production mainly contain vinyl acetate, water, initiator, emulsifying agent, protective colloid, pH value and molecular weight regulator, softening agent etc.But prepare in the process of white glue with vinyl at Vinyl Acetate Monomer and polyvinyl alcohol polymerization, during as initiator, polymerization time reaches 6-8 hour with hydrogen peroxide etc., and polymerization temperature need be strict controlled in 75-78 ℃.Polymerization time is longer, and the polymerization temperature narrow range of Yao Qiuing is difficult to control simultaneously.Because the temperature of reaction harshness is difficult to control, can have part unreacted monomer and other starting monomer in the final white glue with vinyl, influences the cohesive strength of white glue with vinyl, the existence of this organic monomer simultaneously also can cause white glue with vinyl can't reach environmental protection standard.
In addition because the raw material of existing white glue with vinyl mostly is the solvent borne product, in the production process " three wastes " discharging very big, have a strong impact on the healthy of staff, also can cause great pollution to environment; Existing white glue with vinyl product is because polymerization temperature requires harshness, and the requirement condition of tackling conversion unit mutually is higher, and the proportion of raw materials scope is also relatively harsher, and this can cause, and facility investment is big, quality product is not easy control, and the quality guaranteed period is shorter.Existing white glue with vinyl can only be used for bonding wood, and corresponding timber floor is bonding, the bonding of bonding, the leather of material jigsaw, cotton spinning cloth and leather all needs to produce the product that matches.
Goal of the invention
The purpose of this invention is to provide a kind of high-strength polyvinyl acetate and preparation method thereof, it has wide, the simple environment-friendly type high intensity power of the preparation technology white glue with vinyl and preparation method thereof simultaneously of cohesive strength height, raw material sources, its production cost is low, anti-freezing property is stronger, and range of application is comparatively extensive.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of high-strength polyvinyl acetate is the emulsion polymer of vinyl acetate, it is characterized in that it comprises that following materials of weight proportions is prepared from:
Polyvinyl alcohol 4～6
Vinyl acetate between to for plastic 18～36
OP-10 0.1～0.3
10% ammonium persulfate solution 0.8～1.5
Sodium bicarbonate 0.1～0.2
2-ethoxyethyl amyl acetate 0.6～1.2
Dibutyl phthalate (DBP) 3～5
Ethylene glycol 0.08～0.15
Water 50～75
Described polyvinyl alcohol comprises polyvinyl alcohol 17-88 type, polyvinyl alcohol 17-99 type or polyvinyl alcohol 20-99 type.
Described 10% ammonium persulfate solution can substitute with 10% Sodium Persulfate solution.
Described feed composition also comprises the card pine of 1.0～1.5 weight proportions.
Described high-strength polyvinyl acetate is to be prepared from by following materials of weight proportions:
Polyvinyl alcohol 17-88 type 4～6
Vinyl acetate between to for plastic 18～36
OP-10 0.2
10% ammonium persulfate solution 1.2
Sodium bicarbonate 0.15
2-ethoxyethyl amyl acetate 1.0
Dibutyl phthalate (DBP) 4.0
Ethylene glycol 0.1
Card pine 1.2
Water 50～75
The preparation method of above-mentioned high-strength polyvinyl acetate is characterized in that preparation process is as follows:
(1) at first part or all of water, ethylene glycol are added reactor, start and stir and the adding polyvinyl alcohol, be heated to 80-95 ℃, polyvinyl alcohol is dissolved fully;
(2) add OP-10 again, be cooled to 60-65 ℃, be added dropwise to vinyl acetate between to for plastic then, and adding part initiator ammonium persulfate solution, the controlled polymerization temperature is carried out polyreaction for 70-80 ℃, adds the rest parts ammonium persulfate solution therebetween in batches, after vinyl acetate between to for plastic dropwises, the remaining ammonium persulfate solution of disposable adding, last temperature control to 85 kept 0.5-1.0 hour by ℃-90 ℃;
(3) be cooled to 45-55 ℃, add sodium hydrogen carbonate solution, 2-ethoxyethyl amyl acetate, the dibutyl phthalate of sodium bicarbonate or surplus water preparation, stir, obtain this high-strength polyvinyl acetate.
After being added dropwise to vinyl acetate between to for plastic in the described step (2), the ammonium persulfate solution that adds total amount 30% earlier, and then in batches the ammonium persulfate solution of adding total amount 60% in the reaction process, treat that vinyl acetate between to for plastic dropwises after, add the ammonium persulfate solution of residue 10% again.
Polyvinyl alcohol described in the transformation of the way Preparation Method comprises polyvinyl alcohol 17-88 type, polyvinyl alcohol 17-99 type or polyvinyl alcohol 20-99 type; Described 10% ammonium persulfate solution can substitute with 10% Sodium Persulfate solution.
After being cooled to 45-55 ℃ in the described step (3), also can add the card pine of 1.0～1.5 weight proportions.
After being cooled to 45-55 ℃ in the described step (3), the addition sequence successively of each raw material is sodium bicarbonate, 2-ethoxyethyl amyl acetate and dibutyl phthalate (DBP).
This high-strength polyvinyl acetate with polyvinyl alcohol and vinyl acetate between to for plastic as the principal reaction monomer, adopt OP-10 (polyoxyethylene octylphenol ether) as dispersion agent, do at persulphates such as ammonium persulphate or Sodium Persulfates under the condition of initiator, carry out the polyreaction in the wide temperature range, polymerization process is more stable, behind the initiated polymerization, still can carry out polyreaction under 70 ℃ temperature, speed of response can obviously not reduce yet.Under 80 ℃ temperature, polyreaction is relatively gentleer, and sudden and violent gathering can not take place, and therefore monomer content is very low in the polymer emulsion that finally obtains, and cohesive force can not be subjected to monomeric rigid, can meet and surpass the environmental protection standard of national regulation simultaneously again.
The raw material that this high-strength polyvinyl acetate adopted is the huge conventional industrial chemicals of output, and wherein dibutyl phthalate (DBP) is the softening agent of using always, also can replace with o-phthalic acid dibutyl ester here again.Safe, efficient, broad spectrum daily use chemicals product that card pine system generally acknowledges in the world limit the use of sanitas, external trade name " KATHONCG " (Ka Song and Kai Song), its active part is the isothiazolinone compounds, structure is: 2-methyl-4-isothiazoline-3-ketone and 5-chloro-2-methyl-4-isothiazoline-3-ketone, do not contain any heavy metal, can effectively suppress and go out except that mushroom and various microorganism.
The polyreaction of this high-strength polyvinyl acetate is medium with water, does not contain formaldehyde and other objectionable impuritiess, does not fire, the nonirritant taste, and is nontoxic, safety and environmental protection; Various proportion of raw materials controlled range are bigger, and technology is grasped easily, and production process is operated under safe pressure, and quality product is controlled easily, and product cost can be controlled flexibly.After having added mould inhibitor and emulsifying agent, this white glue with vinyl can be miscible with arbitrary proportion and other water-base cement liquid phase, do not precipitate, not stratified, do not have bad phenomenon such as gel, and the quality guaranteed period can reach more than 12 months, was 2 times of traditional white glue with vinyl.Owing to added antifreezing agent ethylene glycol, obviously improved its resistance to low temperature, this white glue with vinyl is after drying in addition, and rete compact structure after the film forming can effectively stop the infiltration of moisture, and water resistance improves greatly.
Beneficial effect of the present invention is that this high-strength polyvinyl acetate is a protective colloid with poly-ethanol, is polymerization single polymerization monomer with the vinyl acetate between to for plastic, and persulphate is an initiator, forms by letex polymerization, and polymeric micelle size is even, and initial bonding strength is good; Can prevent its fragility and increase toughness after increasing north agent having added; This white glue with vinyl can bonding preferably leather; Can be widely used in the timber jigsaw, bonding wood, wood-based plate processing, carton is bonding, and the fiber leather is bonding, paper product, the production of weaving and various coating.
Embodiment
The invention will be further elaborated below in conjunction with embodiment.
Embodiment 1 gets each raw material by following weight:
Polyvinyl alcohol 17-88 type 5kg vinyl acetate between to for plastic 24kg OP-10 0.2kg
10% ammonium persulfate solution 1.2kg sodium bicarbonate 0.15kg 2-ethoxyethyl amyl acetate 1.0kg
Dibutyl phthalate (DBP) 4.0kg ethylene glycol 0.1kg card pine 1.2kg
Water 60kg
Adopt above-mentioned raw materials to carry out the preparation of white glue with vinyl, the preparation method is as follows:
At first water and the 0.1kg ethylene glycol with 50kg adds in the reactor, starts whipping appts and adds 5kg17-88 type polyvinyl alcohol, is heated to 90 ℃, makes polyvinyl alcohol dissolve the formation clear solution fully;
Add 0.2kg nonionogenic tenside OP-10 again, stir and be cooled to 60-65 ℃; In reactor, drip vinyl acetate between to for plastic then, and the initiator ammonium persulfate solution of adding 0.36kg, the controlled polymerization temperature is between 70-80 ℃ simultaneously, polymerization time 6 hours, the ammonium persulfate solution that adds total amount 5% therebetween every half an hour, after treating that vinyl acetate between to for plastic dropwises, the remaining ammonium persulfate solution of disposable adding, and temperature control to 85 kept 30 minutes by ℃-90 ℃;
Reactant is cooled to 50 ℃, add solution, 1.0kg 2-ethoxyethyl amyl acetate, 4.0kg dibutyl phthalate and the 1.2kg card pine of the preparation of 10kg water and 0.15kg sodium bicarbonate successively, stir, be cooled to below 40 ℃, produce and pack, can obtain this high-strength polyvinyl acetate.
This high-strength polyvinyl acetate finished product is white milk, can't smell irritating smell, and micelle is more even, can be miscible with arbitrary proportion and other water-base cement liquid phase.Preserve do not precipitate after 12 months, not stratified, do not have bad phenomenon such as gel, can be used for the timber jigsaw, bonding wood, wood-based plate processing, carton is bonding, the fiber leather is bonding, paper product bonding, initial bonding force all is higher than the common white latex.Subzero 5 ℃ of low temperature can not solidify.
Embodiment 2 gets each raw material by following weight:
Polyvinyl alcohol 17-88 type 6kg vinyl acetate between to for plastic 18kg OP-10 0.1kg
10% ammonium persulfate solution 1.5kg sodium bicarbonate 0.20kg 2-ethoxyethyl amyl acetate 1.2kg
Dibutyl phthalate (DBP) 3.0kg ethylene glycol 0.08kg card pine 1.5kg
Water 75kg
Adopt above-mentioned raw materials to carry out the preparation of white glue with vinyl, the preparation method is as follows:
At first water and the 0.08kg ethylene glycol with 75kg adds in the reactor, and the startup whipping appts stirs with 60 rev/mins speed, and adds 6kg17-88 type polyvinyl alcohol, is heated to 80 ℃, makes polyvinyl alcohol dissolve the formation clear solution fully;
Add 0.1kg nonionogenic tenside OP-10 again, stir and be cooled to 60-65 ℃; In reactor, drip vinyl acetate between to for plastic then, the dropping time is about 6 hours, and the initiator ammonium persulfate solution of adding 0.40kg, the controlled polymerization temperature is between 70-80 ℃ simultaneously, polymerization time 6 hours added the ammonium persulfate solution of total amount 0.1kg therebetween every 1 hour, treat that vinyl acetate between to for plastic dropwises after, the remaining 0.5kg ammonium persulfate solution of disposable adding, and temperature control to 85 kept 1 hour by ℃-90 ℃;
Reactant is cooled to 55 ℃, adds 0.20kg sodium bicarbonate, 1.2kg 2-ethoxyethyl amyl acetate, 3.0kg dibutyl phthalate and 1.5kg card pine successively, stir, be cooled to below 40 ℃, the packing of producing can obtain this high-strength polyvinyl acetate.
This high-strength polyvinyl acetate finished product is white milk, can't smell any irritating smell, and micelle is more even, can be miscible with arbitrary proportion and other water-base cement liquid phase.Preserve do not precipitate after 12 months, not stratified, do not have bad phenomenon such as gel, can be used for the timber jigsaw, bonding wood, wood-based plate processing, carton is bonding, the fiber leather is bonding, paper product bonding, initial bonding force all is higher than the common white latex.Subzero 5 ℃ of low temperature can not solidify.
Embodiment 3 gets each raw material by following weight:
Polyvinyl alcohol 17-99 type 4kg vinyl acetate between to for plastic 36kg OP-10 0.3kg
10% Sodium Persulfate solution 0.8kg sodium bicarbonate 0.10kg 2-ethoxyethyl amyl acetate 0.6kg
O-phthalic acid dibutyl ester 5.0kg ethylene glycol 0.15kg water 50kg
Adopt above-mentioned raw materials to carry out the preparation of white glue with vinyl, the preparation method obtains the oyster white high-strength polyvinyl acetate at last with embodiment 1.
Claims (10)
1. a high-strength polyvinyl acetate is the emulsion polymer of vinyl acetate, it is characterized in that it comprises that following materials of weight proportions is prepared from:
Polyvinyl alcohol 4～6
Vinyl acetate between to for plastic 18～36
OP-10 0.1～0.3
10% ammonium persulfate solution 0.8～1.5
Sodium bicarbonate 0.1～0.2
2-ethoxyethyl amyl acetate 0.6～1.2
Dibutyl phthalate (DBP) 3～5
Ethylene glycol 0.08～0.15
Water 50～75
2. high-strength polyvinyl acetate according to claim 1 is characterized in that, described polyvinyl alcohol comprises polyvinyl alcohol 17-88 type, polyvinyl alcohol 17-99 type or polyvinyl alcohol 20-99 type.
3. high-strength polyvinyl acetate according to claim 1 is characterized in that, described 10% ammonium persulfate solution can substitute with 10% Sodium Persulfate solution.
4. high-strength polyvinyl acetate according to claim 1 is characterized in that, described feed composition also comprises the card pine of 1.0～1.5 weight proportions.
5. high-strength polyvinyl acetate according to claim 1 is characterized in that, described high-strength polyvinyl acetate is to be prepared from by following materials of weight proportions:
Polyvinyl alcohol 17-88 type 4～6
Vinyl acetate between to for plastic 18～36
OP-10 0.2
10% ammonium persulfate solution 1.2
Sodium bicarbonate 0.15
2-ethoxyethyl amyl acetate 1.0
Dibutyl phthalate (DBP) 4.0
Ethylene glycol 0.1
Card pine 1.2
Water 50～75
6. the preparation method of the described high-strength polyvinyl acetate of claim 1 is characterized in that preparation process is as follows:
(1) at first part or all of water, ethylene glycol are added reactor, start and stir and the adding polyvinyl alcohol, be heated to 80-95 ℃, polyvinyl alcohol is dissolved fully;
(2) add OP-10 again, be cooled to 60-65 ℃, be added dropwise to vinyl acetate between to for plastic then, and adding part initiator ammonium persulfate solution, the controlled polymerization temperature is carried out polyreaction for 70-80 ℃, adds the rest parts ammonium persulfate solution therebetween in batches, after vinyl acetate between to for plastic dropwises, the remaining ammonium persulfate solution of disposable adding, last temperature control to 85 kept 0.5-1.0 hour by ℃-90 ℃;
(3) be cooled to 45-55 ℃, add sodium hydrogen carbonate solution, 2-ethoxyethyl amyl acetate, the dibutyl phthalate of sodium bicarbonate or surplus water preparation, stir, obtain this high-strength polyvinyl acetate.
7. the preparation method of high-strength polyvinyl acetate according to claim 6, after it is characterized in that being added dropwise to vinyl acetate between to for plastic in the described step (2), the ammonium persulfate solution that adds total amount 30% earlier, and then in batches the ammonium persulfate solution of adding total amount 60% in the reaction process, after treating that vinyl acetate between to for plastic dropwises, add the ammonium persulfate solution of residue 10% again.
8. the preparation method of high-strength polyvinyl acetate according to claim 6 is characterized in that described polyvinyl alcohol comprises polyvinyl alcohol 17-88 type, polyvinyl alcohol 17-99 type or polyvinyl alcohol 20-99 type; Described 10% ammonium persulfate solution can substitute with 10% Sodium Persulfate solution.
9. the preparation method of high-strength polyvinyl acetate according to claim 6 after it is characterized in that being cooled to 45-55 ℃ in the described step (3), also can add the card pine of 1.0～1.5 weight proportions.
10. the preparation method of high-strength polyvinyl acetate according to claim 6, after it is characterized in that being cooled to 45-55 ℃ in the described step (3), the addition sequence successively of each raw material is sodium bicarbonate, 2-ethoxyethyl amyl acetate and dibutyl phthalate (DBP).
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| CN 200710086659 CN101077901A (en) | 2007-03-29 | 2007-03-29 | High-strength polyvinyl acetate and preparing method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101265398B (en) * | 2008-04-28 | 2010-06-02 | 江苏德华兔宝宝装饰新材有限公司 | Environment-friendly type white emulsion glue |
| CN101838491A (en) * | 2010-05-21 | 2010-09-22 | 吴承斌 | Preparation method of water-soluble polishing varnish liquid |
| CN101314699B (en) * | 2008-07-16 | 2011-08-24 | 江苏黑松林粘合剂厂有限公司 | Water-based adhesion agent and preparation thereof |
| CN102250564A (en) * | 2010-12-21 | 2011-11-23 | 刘青 | Manufacture method of white latex |
| CN102295903A (en) * | 2011-06-24 | 2011-12-28 | 浙江农林大学 | Production method for rapidly-precured white latex |
| CN102372885A (en) * | 2010-08-24 | 2012-03-14 | 中国石油化工集团公司 | High viscosity polyvinyl acetate emulsion and preparation method thereof |
| CN103205222A (en) * | 2013-04-09 | 2013-07-17 | 桐乡市灵芝化工有限公司 | Paper tube adhesive and preparation method thereof |
| CN104231977A (en) * | 2013-06-24 | 2014-12-24 | 鲍震 | Method for producing white latex |
| CN105175638A (en) * | 2015-11-05 | 2015-12-23 | 贵州遵义铭东商贸有限公司 | Building adhesive and preparation method thereof |
| CN106047237A (en) * | 2016-07-01 | 2016-10-26 | 王锶源 | Latex adhesive |
| CN108219597A (en) * | 2018-01-03 | 2018-06-29 | 北京盛邦化工有限公司 | A kind of metope curing agent and preparation method thereof |
| CN110358479A (en) * | 2019-07-10 | 2019-10-22 | 东莞市冠力胶业有限公司 | A kind of antifreeze glue and its preparation process |
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2007
- 2007-03-29 CN CN 200710086659 patent/CN101077901A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101265398B (en) * | 2008-04-28 | 2010-06-02 | 江苏德华兔宝宝装饰新材有限公司 | Environment-friendly type white emulsion glue |
| CN101314699B (en) * | 2008-07-16 | 2011-08-24 | 江苏黑松林粘合剂厂有限公司 | Water-based adhesion agent and preparation thereof |
| CN101838491A (en) * | 2010-05-21 | 2010-09-22 | 吴承斌 | Preparation method of water-soluble polishing varnish liquid |
| CN102372885B (en) * | 2010-08-24 | 2015-08-05 | 中国石油化工集团公司 | A kind of high viscosity polyvinyl acetate emulsion and preparation method thereof |
| CN102372885A (en) * | 2010-08-24 | 2012-03-14 | 中国石油化工集团公司 | High viscosity polyvinyl acetate emulsion and preparation method thereof |
| CN102250564B (en) * | 2010-12-21 | 2012-10-10 | 刘青 | Manufacture method of white latex |
| CN102250564A (en) * | 2010-12-21 | 2011-11-23 | 刘青 | Manufacture method of white latex |
| CN102295903B (en) * | 2011-06-24 | 2012-09-05 | 浙江农林大学 | Production method for rapidly-precured white latex |
| CN102295903A (en) * | 2011-06-24 | 2011-12-28 | 浙江农林大学 | Production method for rapidly-precured white latex |
| CN103205222A (en) * | 2013-04-09 | 2013-07-17 | 桐乡市灵芝化工有限公司 | Paper tube adhesive and preparation method thereof |
| CN104231977A (en) * | 2013-06-24 | 2014-12-24 | 鲍震 | Method for producing white latex |
| CN105175638A (en) * | 2015-11-05 | 2015-12-23 | 贵州遵义铭东商贸有限公司 | Building adhesive and preparation method thereof |
| CN106047237A (en) * | 2016-07-01 | 2016-10-26 | 王锶源 | Latex adhesive |
| CN108219597A (en) * | 2018-01-03 | 2018-06-29 | 北京盛邦化工有限公司 | A kind of metope curing agent and preparation method thereof |
| CN110358479A (en) * | 2019-07-10 | 2019-10-22 | 东莞市冠力胶业有限公司 | A kind of antifreeze glue and its preparation process |
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