CN103864974A - Preparation method for core-shell-structured styrene-acrylate microemulsion - Google Patents
Preparation method for core-shell-structured styrene-acrylate microemulsion Download PDFInfo
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- CN103864974A CN103864974A CN201210542484.3A CN201210542484A CN103864974A CN 103864974 A CN103864974 A CN 103864974A CN 201210542484 A CN201210542484 A CN 201210542484A CN 103864974 A CN103864974 A CN 103864974A
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Abstract
The invention relates to the field of preparation of microemulsions. The objective of the invention is to provide a preparation method for a core-shell-structured styrene-acrylate microemulsion which is prepared through semi-continuous pre-emulsification seed microemulsion polymerization. The method comprises the following three steps: 1) preparation of a seed microemulsion; 2) pre-emulsification of a shell monomer; and 3) core-shell polymerization. The invention has the following beneficial effect: with the method, the styrene-acrylate microemulsion with a core-shell structure can be prepared.
Description
Technical field
The present invention relates to a kind of preparation field of microemulsion.
Background technology
The research field of styrene-acrylic microemulsion, the research work of Chinese scholars is mainly concentrated in the following areas:
1. the improvement of emulsification system: in traditional Styrene-Acrylate Emulsion Polymerization, the conventional emulsifier using is attached to emulsion particle surface in the mode of physical adsorption, thus realize the stability of emulsion system.What this conventional emulsifier molecule was easily subject to external environment affects generation desorb, result causes emulsion particle collision cohesion, and after emulsion film forming, emulsifying agent molecule remains in polymer solids, can in polymkeric substance, there is migration and cause the water tolerance of polymeric film to decline.
The feature of reactive emulsifier is that emulsifying agent molecule can persistent key be incorporated in latex molecule with monomer copolymerization on the one hand, this bonding has the following advantages: 1. emulsifying agent molecule can not move and cause emulsion condensation, and emulsifying agent molecule is still attached to particle surface after emulsion film forming or pressed powder, particle can be scattered in water again; 2. when reactive emulsifier consumption is suitable, improved reactive behavior, in the water after polymerization, just do not had emulsifying agent molecule, thereby accelerated film forming speed; 3. can improve the water tolerance of glued membrane.
2. the improvement of polymerization process: along with the development of emulsion polymerization technique, emerge many advanced persons' such as monomer pre-emulsification technology, seeded emulsion polymerization technology, core/shell emulsion polymerization technology, Emulsifier-free Emulsion Polymerization Technology and emulsion Interpenetrating Polymer Network Technology (LINP) polymerization technique.
Nineteen ninety, Puig etc. by semicontinuous dripping method, have carried out the copolymerization of vinylbenzene and Acrylic Acid Monomer and have studied in O/W type microemulsion, obtained the spherical monodisperse nano-particle microemulsion micelle that diameter is about 21nm, but its final monomer conversion are only 60%.Xu Xiangling etc. adopt seed emulsion polymerization, cause styrene polymerization with gamma-rays, obtain particle diameter in 30 nm left and right, ultra micro latex that solid content is higher.Wang Changchun etc. adopt a kind of improved microemulsion polymerization method, synthesize the acrylate ultra micro latex of high solids content, wherein emulsifier is 4%～8% of monomer total amount, assistant for emulsifying agent consumption is 4%～8% of monomer total amount, initiator amount is 0.2%～0.3% of monomer total amount, the ultra micro latex solid content (massfraction) making can reach more than 40%, and latex particle size is 20～40nm.
Summary of the invention
The object of this invention is to provide a kind of core-shell structure styrene-acrylic microemulsion preparation method, adopt semicontinuous pre-emulsification seed microemulsion polymerization method preparation, gathered by following three steps:
1) preparation of seed microemulsion: warming-in-water to 60～70 ℃, take the emulsifying agent of specified amount, buffer reagent joins in four-hole bottle, in the deionized water of specified amount, fully disperses.Take quantitative nuclear monomer (soft, hard monomer) and mix, join in above-mentioned four-hole bottle 1/5 of its total amount, make it to form transparent microemulsion.Take a certain amount of initiator potassium persulfate, be mixed with solution with a small amount of deionized water.Warming-in-water to 75 ℃, to the initiator that adds 1/3 in reactor, after reaction 15min, microemulsion gradually becomes blue transparent liquid from water white transparency state, illustrate that micro-emulsion polymerization reacts to carry out.Continue to drip residual nucleus monomer and initiator in reactor.Control rate of addition, it is dropwised at the appointed time.Then at 75 ℃ of insulation 1h, obtain blue transparent seed microemulsion.
2) pre-emulsification shell monomer: take the emulsifying agent of specified amount, fully disperse at the deionized water of specified amount.Take shell monomer (soft, hard, functional monomer) and add in the aqueous solution of emulsifying agent, pre-emulsification 30min under certain stirring velocity, obtains pre-emulsion.
3) hud polymerization: slowly drip pre-emulsification shell monomer and initiator solution in seed microemulsion system, control rate of addition, 2h dropwises, insulation 1～1.5h, ammoniacal liquor adjust pH to 6～7, cooling discharge.
The invention has the beneficial effects as follows: adopt present method can make the styrene-acrylic microemulsion with nucleocapsid structure.
Embodiment
The preparation method of core-shell structure styrene-acrylic microemulsion, is characterised in that: adopt semicontinuous pre-emulsification seed microemulsion polymerization method preparation, be divided into three steps:
1) preparation of seed microemulsion: warming-in-water to 60～70 ℃, take the emulsifying agent of specified amount, buffer reagent joins in four-hole bottle, in the deionized water of specified amount, fully disperses.Take quantitative nuclear monomer (soft, hard monomer) and mix, join in above-mentioned four-hole bottle 1/5 of its total amount, make it to form transparent microemulsion.Take a certain amount of initiator potassium persulfate, be mixed with solution with a small amount of deionized water.Warming-in-water to 75 ℃, to the initiator that adds 1/3 in reactor, after reaction 15min, microemulsion gradually becomes blue transparent liquid from water white transparency state, illustrate that micro-emulsion polymerization reacts to carry out.Continue to drip residual nucleus monomer and initiator in reactor.Control rate of addition, it is dropwised at the appointed time.Then at 75 ℃ of insulation 1h, obtain blue transparent seed microemulsion.
2) pre-emulsification shell monomer: take the emulsifying agent of specified amount, fully disperse at the deionized water of specified amount.Take shell monomer (soft, hard, functional monomer) and add in the aqueous solution of emulsifying agent, pre-emulsification 30min under certain stirring velocity, obtains pre-emulsion.
3) hud polymerization: slowly drip pre-emulsification shell monomer and initiator solution in seed microemulsion system, control rate of addition, 2h dropwises, insulation 1～1.5h, ammoniacal liquor adjust pH to 6～7, cooling discharge.
Claims (1)
1. the preparation method of core-shell structure styrene-acrylic microemulsion, is characterized in that: adopt semicontinuous pre-emulsification seed microemulsion polymerization method preparation, be divided into three steps:
(1) the preparation of seed microemulsion: warming-in-water to 60～70 ℃, take the emulsifying agent of specified amount, buffer reagent joins in four-hole bottle, in the deionized water of specified amount, fully disperses; Take quantitative nuclear monomer (soft, hard monomer) and mix, join in above-mentioned four-hole bottle 1/5 of its total amount, make it to form transparent microemulsion; Take a certain amount of initiator potassium persulfate, be mixed with solution with a small amount of deionized water, warming-in-water to 75 ℃ adds 1/3 initiator in reactor, and after reaction 15min, microemulsion gradually becomes blue transparent liquid from water white transparency state; Continue to drip residual nucleus monomer and initiator in reactor, control rate of addition, it is dropwised at the appointed time; Then at 75 ℃ of insulation 1h, obtain blue transparent seed microemulsion;
(2) pre-emulsification shell monomer: take the emulsifying agent of specified amount, fully disperse at the deionized water of specified amount; Take shell monomer (soft, hard, functional monomer) and add in the aqueous solution of emulsifying agent, pre-emulsification 30min under certain stirring velocity, obtains pre-emulsion;
(3) hud polymerization: slowly drip pre-emulsification shell monomer and initiator solution in seed microemulsion system, control rate of addition, 2h dropwises, insulation 1～1.5h, ammoniacal liquor adjust pH to 6～7, cooling discharge.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210542484.3A CN103864974A (en) | 2012-12-14 | 2012-12-14 | Preparation method for core-shell-structured styrene-acrylate microemulsion |
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| CN201210542484.3A CN103864974A (en) | 2012-12-14 | 2012-12-14 | Preparation method for core-shell-structured styrene-acrylate microemulsion |
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| CN103864974A true CN103864974A (en) | 2014-06-18 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108822241A (en) * | 2018-06-07 | 2018-11-16 | 华东理工大学 | A kind of preparation method of environment-friendly type wet strength agent |
| CN113930123A (en) * | 2021-12-04 | 2022-01-14 | 恩平市捷威创新材料有限公司 | Water-based mirror back paint and processing technology thereof |
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2012
- 2012-12-14 CN CN201210542484.3A patent/CN103864974A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108822241A (en) * | 2018-06-07 | 2018-11-16 | 华东理工大学 | A kind of preparation method of environment-friendly type wet strength agent |
| CN113930123A (en) * | 2021-12-04 | 2022-01-14 | 恩平市捷威创新材料有限公司 | Water-based mirror back paint and processing technology thereof |
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Application publication date: 20140618 |