CN102850482B - Acrylic emulsion preparation method with improved monomer conversion rate, and prepared acrylic emulsion - Google Patents
Acrylic emulsion preparation method with improved monomer conversion rate, and prepared acrylic emulsion Download PDFInfo
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- CN102850482B CN102850482B CN201210218826.6A CN201210218826A CN102850482B CN 102850482 B CN102850482 B CN 102850482B CN 201210218826 A CN201210218826 A CN 201210218826A CN 102850482 B CN102850482 B CN 102850482B
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- 239000000839 emulsion Substances 0.000 title claims abstract description 40
- 239000000178 monomer Substances 0.000 title claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 39
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 230000003750 conditioning effect Effects 0.000 claims description 11
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 10
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 10
- 230000000977 initiatory effect Effects 0.000 claims description 9
- -1 acrylic ester Chemical class 0.000 claims description 7
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 6
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 6
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- OKIRBHVFJGXOIS-UHFFFAOYSA-N 1,2-di(propan-2-yl)benzene Chemical compound CC(C)C1=CC=CC=C1C(C)C OKIRBHVFJGXOIS-UHFFFAOYSA-N 0.000 claims description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004160 Ammonium persulphate Substances 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- 101000648997 Homo sapiens Tripartite motif-containing protein 44 Proteins 0.000 claims description 2
- 239000004159 Potassium persulphate Substances 0.000 claims description 2
- 102100028017 Tripartite motif-containing protein 44 Human genes 0.000 claims description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- 229940065472 octyl acrylate Drugs 0.000 claims description 2
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims 1
- 238000007720 emulsion polymerization reaction Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 3
- 230000001804 emulsifying effect Effects 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000004908 Emulsion polymer Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a preparation method of an acrylic emulsion. According to the invention, acrylic monomers are well mixed in a blending tank or kettle, such that a monomer mixture is obtained and is preserved for later use; deionized water with a specified amount and an emulsifying agent with a specified proportion are added into a reaction kettle, such that an emulsifying liquid is prepared, wherein the well mixed emulsifying liquid in the reaction kettle reaches a temperature and a pressure required by process requirements; the prepared monomer mixture is added to the reaction kettle, and a stirring rotation speed is regulated to a required rotation speed; when temperature and pressure in the kettle reach an initiator adding condition, an initiator is added, and a reaction is initiated, such that the acrylic emulsion is prepared. The method provided by the invention assists in improving acrylic emulsion polymerization monomer conversion rate, and in reducing residual monomer smell in the air.
Description
Technical field
The present invention relates to high molecular emulsion polymer technical field, be specifically related to
acrylic emulsion polymkeric substance and preparation method.
Background technology
High molecule emulsion polymerization is widely used in plastics at present, rubber, coating, many Industrialized processing technique fields such as synthon, is a kind of considerable chemical production processing technology.Specifically there is the letex polymerization of acrylate in additives for plastics, styrene-butadiene rubber(SBR) in rubber synthesis, textile auxiliary, the letex polymerization in coating for internal and external wall production for building.
Existing
acrylic emulsionproduction method, the polymerization under atmospheric pressure reaction of nitrogen is rushed outside most employing enamel reaction still or stainless steel cauldron, the subject matter that this reaction exists needs inflated with nitrogen to replace additional air in still to promote normally carrying out of reaction, but emulsion polymerization is a kind of slow initiation, the reaction mechanism of fast growth, the free reaction times can be very long, the mode of so rushing nitrogen by normal pressure controls reaction, inevitably produce waste, the still unreacted monomer of normal appearance is by the situation of taking out of outside still, so both waste raw material monomer, be difficult to improve yield, contaminate environment outside still can be discharged again because of monomer, be one not environmentally, there is the working method of unfavorable raising yield.
Summary of the invention
The technical problem that the present invention need solve is provide a kind of cost low and can improve letex polymerization transformation efficiency and product yield, can reach again the acrylic emulsion preparation method that better green technology requires.
The technical scheme that the present invention takes is:
A kind of acrylic emulsion preparation method improving monomer conversion
(1) acrylic ester monomer is mixed formation monomer mixture by formula rate in material-compound tank or still stand-by,
(2) emulsion made by the emulsifying agent of the deionized water and regulation ratio of squeezing into specified amount in reactor, and make the emulsion stirred in reactor reach the temperature and pressure of processing requirement, then the monomer mixture prepared is added in reactor, adjustment mixing speed is processing requirement rotating speed
(3) question response temperature in the kettle, pressure condition reach initiator when adding condition, add initiator and start initiation reaction and make
acrylic emulsion.
in technique scheme, the acrylic ester monomer described in step (1) istwo or more mix monomer in methyl methacrylate, butyl acrylate, ethyl propenoate, butyl methacrylate, β-dimethyl-aminoethylmethacrylate, Octyl acrylate, the temperature condition that emulsion in step (2) will reach technique is normal temperature, pressure condition is negative pressure, pressure range-0.08MPa--0 MPa.
Described emulsifying agent is sodium lauryl sulphate, sodium laurylsulfonate, a kind of and several liquid and the mixture of solid; Described initiator is Potassium Persulphate, ammonium persulphate, Sodium Persulfate, oxidation diisopropylbenzene(DIPB) DCP and benzoyl peroxide in one or both.
The present invention has following unusual effect compared to existing technology:
Compared with prior art; the polymer emulsion transformation efficiency produced reaches 99-100%; and substantially without protection gas such as nitrogen in polymerization process; both reduce production cost and protect environment; reach the requirement of cleaner production, meet and belong to country and encourage Chemical Manufacture to be conducive to improving enterprise competitiveness and improving its economic benefit.
The present invention
acrylic emulsion preparation method'sunusual effect is: (1) described working method does not change existing manufacturing condition and equipment, other are not needed to invest, (2) raw materials is identical with existing technical recipe and easy and simple to handle, is beneficial to worker healthy, can avoid because the personnel that cause such as smooth base injure in production.(2) improve monomer conversion, reduce production cost.Operate easier.Decrease atmospheric pollution, realize resource circulation utilization simultaneously, be beneficial to environment protection.
Preparation method disclosed by the invention is
a kind of method that can improve acrylic emulsion polymerization single polymerization monomer transformation efficiency and reduce residual monomer smell in airconcise in technology, easy to operate, produce finished-product material excellent combination property, this method can be used for plastics, rubber, coating, the production operation field of the letex polymerizations such as textile printing and dyeing.
Embodiment
The ratio cubage by mass percentage of the raw material that acrylic emulsion preparation method of the present invention adopts includes: acrylic ester monomer mixture 40-50%, emulsifying agent 0.8-2.0%, initiator 0.1-0.2%, surplus is water.
Wherein, emulsifying agent is as tensio-active agent, have good coordinative role can improve emulsion polymerization systems surface tension well, conditioning agent with as tensio-active agent with deionized water oil-soluble monomer, the auxiliary agent such as initiator, oxidation inhibitor can be selected to add according to demand.
embodiment 1
Proportioning is carried out: methyl methacrylate 78% by following mass percent composition, butyl acrylate 22%, sodium lauryl sulphate 1.1%, conditioning agent 0.1%, time prepared by initiator 0.1%, first join in respective batching kettle and reactor by above-mentioned material, wherein initiator needs to add before starting the reaction, by methyl methacrylate after dilution, butyl acrylate, ethyl propenoate, conditioning agent etc. by processing requirement and formula rate before entering reactor with mix in material-compound tank or still stand-by
(2) by the emulsifying agent of the deionized water and specified requirement of squeezing into specified amount in reactor, and the temperature and pressure (negative pressure) making the emulsion stirred in reactor reach specified requirement is then by with the starting monomer compound prepared, add in this reactor successively, adjustment mixing speed is processing requirement rotating speed.Treat temperature of charge in still, when vacuum tightness reaches initiation conditions, add regulation initiator by technique, initiation reaction.Temperature of reaction controls, for 40-85 degree, to control well and remove the gentle reaction times, the technic indexs such as the limiting viscosity of product in reaction process.
The performance index of above-mentioned obtained acrylic emulsion polymkeric substance are as shown in the table:
Table 1 technical requirement
As can be seen from above table data, the acrylic polymer utilizing method described in patent of the present invention and formula rate to obtain all has good performance.
embodiment 2
Proportioning methyl methacrylate 83% is carried out, butyl acrylate 17%, sodium lauryl sulphate 1 by following mass percent composition, 1%, conditioning agent 0,0%, time prepared by initiator 0.1%, first join in respective batching kettle and reactor by above-mentioned material, wherein initiator needs to add before starting the reaction, by methyl methacrylate after dilution, butyl acrylate, ethyl propenoate, conditioning agent etc. by processing requirement and formula rate before entering reactor with mix in material-compound tank or still stand-by
(2) by the emulsifying agent of the deionized water and specified requirement of squeezing into specified amount in reactor, and the temperature and pressure (negative pressure) making the emulsion stirred in reactor reach specified requirement is then by with the starting monomer compound prepared, add in this reactor successively, adjustment mixing speed is processing requirement rotating speed.Treat temperature of charge in still, when vacuum tightness reaches initiation conditions, add regulation initiator by technique, initiation reaction.Temperature of reaction is 40-85 degree, controls well and removes the gentle reaction times, the technic indexs such as the limiting viscosity of product in reaction process.
Above-mentioned obtained
acrylic emulsion polymkeric substanceperformance is as shown in the table:
Table 2 technical requirement
embodiment 3
Proportioning methyl methacrylate 88% is carried out by following mass percent composition, butyl acrylate 12%, sodium lauryl sulphate 1,1%, conditioning agent 0,0%, time prepared by initiator 0.01-0.05%, first join in respective batching kettle and reactor by above-mentioned material, wherein initiator needs to add before starting the reaction, by methyl methacrylate after dilution, butyl acrylate, ethyl propenoate, conditioning agent etc. by processing requirement and formula rate before entering reactor with mix in material-compound tank or still stand-by
(2) by the emulsifying agent of the deionized water and specified requirement of squeezing into specified amount in reactor, and the temperature and pressure (negative pressure) making the emulsion stirred in reactor reach specified requirement is then by with the starting monomer compound prepared, add in this reactor successively, adjustment mixing speed is processing requirement rotating speed.(3) treat temperature of charge in still, when vacuum tightness reaches initiation conditions, add regulation initiator by technique, initiation reaction.Temperature of reaction is 40-85 degree, controls well and removes the gentle reaction times, the technic indexs such as the limiting viscosity of product in reaction process.
Above-mentioned obtained
acrylic emulsion polymkeric substanceperformance is as shown in the table:
Table 3 technical requirement
embodiment 4
Proportioning methyl methacrylate 88% is carried out by following mass percent composition, butyl acrylate 12%, sodium lauryl sulphate 1,1%, conditioning agent 0,0%, time prepared by initiator 0.01-0.05%, first join in respective batching kettle and reactor by above-mentioned material, wherein initiator needs to add before starting the reaction, by methyl methacrylate after dilution, butyl acrylate, ethyl propenoate, conditioning agent etc. by processing requirement and formula rate before entering reactor with mix in material-compound tank or still stand-by
(2) by the emulsifying agent of the deionized water and specified requirement of squeezing into specified amount in reactor, and the temperature and pressure (negative pressure) making the emulsion stirred in reactor reach specified requirement is then by with the starting monomer compound prepared, add in this reactor successively, adjustment mixing speed is processing requirement rotating speed.Temperature of reaction is 40-85 degree, controls well and removes the gentle reaction times, the technic indexs such as the limiting viscosity of product in reaction process.Above-mentioned obtained
acrylic emulsion polymkeric substanceperformance is as shown in the table:
Table 4 technical requirement
Above are only the preferred embodiment of the present invention; these embodiments only can not be interpreted as limitation of the present invention for explaining the present invention; when not deviating from scope claimed in the claims in the present invention, various modifications and variations can be carried out to above-mentioned embodiment.
Claims (7)
1. improve an acrylic emulsion preparation method for monomer conversion, it is characterized in that:
(1) acrylic ester monomer is mixed formation monomer mixture by formula rate in material-compound tank or still stand-by,
(2) emulsion made by the emulsifying agent of the deionized water and regulation ratio of squeezing into specified amount in reactor, and make the emulsion stirred in reactor reach the temperature and pressure of processing requirement, then the monomer mixture prepared is added in reactor, adjustment mixing speed is processing requirement rotating speed
(3) question response temperature in the kettle, pressure condition reach initiator when adding condition, add initiator and start initiation reaction and make acrylic emulsion,
described acrylic ester monomer is two or more the mix monomer in methyl methacrylate, butyl acrylate, ethyl propenoate, butyl methacrylate, β-dimethyl-aminoethylmethacrylate, Octyl acrylate,
The temperature condition that emulsion in step (2) will reach technique is normal temperature, and pressure condition is negative pressure, pressure range-0.08MPa--0 MPa.
2. the acrylic emulsion preparation method of raising monomer conversion according to claim 1, is characterized in that, also added conditioning agent when acrylic ester monomer is mixed into monomer mixture, described conditioning agent comprise in mercaptan and CMC one or both.
3. the acrylic emulsion preparation method of raising monomer conversion according to claim 1, is characterized in that, is added with oxidation inhibitor in made acrylic emulsion, described oxidation inhibitor comprise in antioxidant 1010 or irgasfos 168 one or both.
4. the acrylic emulsion preparation method of raising monomer conversion according to claim 1, its characteristic is: described emulsifying agent is sodium lauryl sulphate.
5. the acrylic emulsion preparation method of raising monomer conversion according to claim 1, its characteristic is: described initiator is Potassium Persulphate, ammonium persulphate, Sodium Persulfate, oxidation diisopropylbenzene(DIPB) DCP and benzoyl peroxide in one or both.
6. improve the acrylic emulsion prepared by acrylic emulsion preparation method of monomer conversion according to claim 1, the ratio cubage by mass percentage of its raw material includes: acrylic ester monomer mixture 40-50%, emulsifying agent 0.8-2.0%, initiator 0.1-0.2%, surplus is water.
7. improve the acrylic emulsion prepared by acrylic emulsion preparation method of monomer conversion according to claim 6, it is characterized in that, acrylic emulsion solid content is 40-45%.
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| CN201210218826.6A CN102850482B (en) | 2012-06-29 | 2012-06-29 | Acrylic emulsion preparation method with improved monomer conversion rate, and prepared acrylic emulsion |
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Effective date of registration: 20160711 Address after: 512000, Ruyuan province Shaoguan Yao Autonomous County, Guangdong Province Feng Feng Road East Fuyuan Industrial Park Patentee after: Shaoguan Rui Environmental Protection Technology Co., Ltd. Address before: 516211, No. 27 West Wei Road, Huizhou Town, Huiyang District, Guangdong, China Patentee before: Ren Huiping |