CN104558367A - Method for synthesizing core-shell acrylate emulsion - Google Patents
Method for synthesizing core-shell acrylate emulsion Download PDFInfo
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- CN104558367A CN104558367A CN201410579621.XA CN201410579621A CN104558367A CN 104558367 A CN104558367 A CN 104558367A CN 201410579621 A CN201410579621 A CN 201410579621A CN 104558367 A CN104558367 A CN 104558367A
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Abstract
The invention relates to a method for synthesizing a core-shell acrylate emulsion. The method comprises the following steps: dividing an emulsifier water solution into three parts; dropwise adding a core monomer to one part of emulsifier water solution under high-speed stirring, and pre-emulsifying to prepare a core monomer pre-emulsified liquid I; dropwise adding the core monomer to another part of emulsifier water solution under high-speed stirring, and pre-emulsifying to prepare a core monomer pre-emulsified liquid II; adding the third part of emulsifier water solution to a buffer agent to obtain an emulsifier buffer agent water solution III; sequentially adding the emulsifier buffer agent III, the core monomer pre-emulsified liquid I, the core monomer pre-emulsified liquid II and a 1/3 initiator water solution to a four-opening flask, and reacting to obtain a core layer emulsion; dropwise adding a shell monomer pre-emulsified solution II and the rest of 1/3 initiator water solution to the core layer emulsion to react; ending reaction, adjusting the pH value with ammonium hydroxide, and filtering to obtain the core-shell acrylate emulsion. The method disclosed by the invention is simple and easy to control; the stain resistance of the synthesized core-shell acrylate emulsion is obviously improved.
Description
Technical field
The present invention relates to a kind of synthetic technology of organic coating, particularly relate to a kind of core-shell acrylic-resin emulsion synthetic method.
Background technology
Acrylic emulsion coating is the principal item of domestic and international building external paint, but its contamination resistance is poor, greatly constrains Acrylic emulsion coating applying at China's external wall.Affect the many factors of acrylate exterior wall latex coating contamination resistance, but the contamination resistance of acrylic ester emulsion base-material is the deciding factor in many factors.Based on " latex particle design " thought, carry out core-shell emulsion polymerization, soft in core-shell emulsion film has lower minimum film-forming temperature mutually, makes to have good film forming properties during coating normal temperature; Hard in core-shell emulsion film has higher hardness and lower surface energy mutually, thus improves the contamination resistance of acrylate exterior wall latex coating.
Summary of the invention
It is simple that technical problem to be solved by this invention is to provide a kind of method, easy to control, the synthetic method that the core-shell acrylic-resin emulsion contamination resistance of synthesis significantly improves.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of core-shell acrylic-resin emulsion synthetic method, comprises the steps:
Emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, pre-emulsification, obtained nuclear monomer pre-emulsion I;
Under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification, obtained shell monomer pre-emulsion II;
3rd part of emulsifier aqueous solution obtains emulsifying agent aqueous solution of buffer agent III after adding buffer reagent;
In four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, be obtained by reacting stratum nucleare emulsion;
In stratum nucleare emulsion, drip 1/3 initiator solution reaction of shell monomer pre-emulsion II and remainder;
Reaction terminates, and uses ammoniacal liquor adjust ph, filters and obtain core-shell acrylic-resin emulsion.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, pre-emulsification, being implemented as follows of obtained nuclear monomer pre-emulsion I step:
Emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, is at room temperature fully uniformly mixed, pre-emulsification 1 ~ 2h, obtained nuclear monomer pre-emulsion I.
Further, describedly under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification, being implemented as follows of obtained shell monomer pre-emulsion II step:
Under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification 1 ~ 2h, obtained shell monomer pre-emulsion II.
Further, being implemented as follows of emulsifying agent aqueous solution of buffer agent III step is obtained after described 3rd part of emulsifier aqueous solution adds buffer reagent:
Be 1:1 ~ 1:3 according to emulsifying agent and buffer reagent mass ratio, after the 3rd part of emulsifier aqueous solution adds buffer reagent emulsifying agent aqueous solution of buffer agent III.
Further, described in four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, be obtained by reacting being implemented as follows of stratum nucleare emulsion step:
In four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, react under 60 ~ 70 DEG C of conditions, after there is blue-fluorescence, instill remaining 1/2 nuclear monomer pre-emulsion I and 1/3 initiator solution with 2 dropping funnels are synchronous, slow respectively, dropwise in 1.5 ~ 2h, be warmed up to 70 ~ 80 DEG C, and continue insulation about 10 ~ 30min, obtain stratum nucleare emulsion.
Further, described in stratum nucleare emulsion, drip being implemented as follows of 1/3 initiator solution reactions steps of shell monomer pre-emulsion II and remainder:
Stratum nucleare emulsion in, by 2 dropping funnels synchronous, 1/3 initiator solutions of slowly dripping shell monomer pre-emulsions II and remainder respectively, temperature control is at 75 ~ 80 DEG C, and 2 ~ 2.5h dropwises, and is warming up to 80 ~ 85 DEG C of insulation 0.5 ~ 1h.
Further, described reaction terminates, and uses ammoniacal liquor adjust ph, filters and obtain being implemented as follows of core-shell acrylic-resin emulsion step:
Reaction terminates, and is cooled to less than 30 ~ 40 DEG C, with ammoniacal liquor adjust ph to 8 ~ 9, filters and obtain core-shell acrylic-resin emulsion.
The invention has the beneficial effects as follows: method is simple, and easy to control, the core-shell acrylic-resin emulsion contamination resistance of synthesis significantly improves.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A kind of core-shell acrylic-resin emulsion synthetic method, comprises the steps:
Emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, pre-emulsification, obtained nuclear monomer pre-emulsion I;
Under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification, obtained shell monomer pre-emulsion II;
3rd part of emulsifier aqueous solution obtains emulsifying agent aqueous solution of buffer agent III after adding buffer reagent;
In four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, be obtained by reacting stratum nucleare emulsion;
In stratum nucleare emulsion, drip 1/3 initiator solution reaction of shell monomer pre-emulsion II and remainder;
Reaction terminates, and uses ammoniacal liquor adjust ph, filters and obtain core-shell acrylic-resin emulsion.
Embodiment 1:
Emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, is at room temperature fully uniformly mixed, pre-emulsification 1h, obtained nuclear monomer pre-emulsion I; Under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification 1h, obtained shell monomer pre-emulsion II; Be 1:1 according to emulsifying agent and buffer reagent mass ratio, after the 3rd part of emulsifier aqueous solution adds buffer reagent emulsifying agent aqueous solution of buffer agent III; In four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, react under 60 DEG C of conditions, after there is blue-fluorescence, instill remaining 1/2 nuclear monomer pre-emulsion I and 1/3 initiator solution with 2 dropping funnels are synchronous, slow respectively, dropwise in 1.5h, be warmed up to 70 DEG C, and continue to be incubated about 10min, obtain stratum nucleare emulsion; Stratum nucleare emulsion in, by 2 dropping funnels synchronous, 1/3 initiator solutions of slowly dripping shell monomer pre-emulsions II and remainder respectively, temperature control is at 75 DEG C, and 2h dropwises, and is warming up to 80 DEG C of insulation 0.5h; Reaction terminates, and is cooled to less than 30 DEG C, by ammoniacal liquor adjust ph to 8, filters and obtain core-shell acrylic-resin emulsion.
Embodiment 2:
Emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, is at room temperature fully uniformly mixed, pre-emulsification 1.5h, obtained nuclear monomer pre-emulsion I; Under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification 1.5h, obtained shell monomer pre-emulsion II; Be 1:2 according to emulsifying agent and buffer reagent mass ratio, after the 3rd part of emulsifier aqueous solution adds buffer reagent emulsifying agent aqueous solution of buffer agent III; In four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, react under 65 DEG C of conditions, after there is blue-fluorescence, instill remaining 1/2 nuclear monomer pre-emulsion I and 1/3 initiator solution with 2 dropping funnels are synchronous, slow respectively, dropwise in 1.7h, be warmed up to 75 DEG C, and continue to be incubated about 20min, obtain stratum nucleare emulsion; Stratum nucleare emulsion in, by 2 dropping funnels synchronous, 1/3 initiator solutions of slowly dripping shell monomer pre-emulsions II and remainder respectively, temperature control is at 78 DEG C, and 2.2h dropwises, and is warming up to 82 DEG C of insulation 0.6h; Reaction terminates, and is cooled to less than 35 DEG C, by ammoniacal liquor adjust ph to 8.5, filters and obtain core-shell acrylic-resin emulsion.
Embodiment 3:
Emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, is at room temperature fully uniformly mixed, pre-emulsification 2h, obtained nuclear monomer pre-emulsion I; Under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification 2h, obtained shell monomer pre-emulsion II; Be 1:3 according to emulsifying agent and buffer reagent mass ratio, after the 3rd part of emulsifier aqueous solution adds buffer reagent emulsifying agent aqueous solution of buffer agent III; In four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, react under 70 DEG C of conditions, after there is blue-fluorescence, instill remaining 1/2 nuclear monomer pre-emulsion I and 1/3 initiator solution with 2 dropping funnels are synchronous, slow respectively, dropwise in 2h, be warmed up to 80 DEG C, and continue to be incubated about 30min, obtain stratum nucleare emulsion; Stratum nucleare emulsion in, by 2 dropping funnels synchronous, 1/3 initiator solutions of slowly dripping shell monomer pre-emulsions II and remainder respectively, temperature control is at 80 DEG C, and 2.5h dropwises, and is warming up to 85 DEG C of insulation 1h; Reaction terminates, and is cooled to less than 40 DEG C, by ammoniacal liquor adjust ph to 9, filters and obtain core-shell acrylic-resin emulsion.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a core-shell acrylic-resin emulsion synthetic method, is characterized in that, comprises the steps:
Emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, pre-emulsification, obtained nuclear monomer pre-emulsion I;
Under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification, obtained shell monomer pre-emulsion II;
3rd part of emulsifier aqueous solution obtains emulsifying agent aqueous solution of buffer agent III after adding buffer reagent;
In four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, be obtained by reacting stratum nucleare emulsion;
In stratum nucleare emulsion, drip 1/3 initiator solution reaction of shell monomer pre-emulsion II and remainder;
Reaction terminates, and uses ammoniacal liquor adjust ph, filters and obtain core-shell acrylic-resin emulsion.
2. a kind of core-shell acrylic-resin emulsion synthetic method according to claim 1, it is characterized in that, described emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, pre-emulsification, being implemented as follows of obtained nuclear monomer pre-emulsion I step:
Emulsifier aqueous solution is divided into 3 parts, under high velocity agitation nuclear monomer is added drop-wise in a copy of it emulsifier aqueous solution, is at room temperature fully uniformly mixed, pre-emulsification 1 ~ 2h, obtained nuclear monomer pre-emulsion I.
3. a kind of core-shell acrylic-resin emulsion synthetic method according to claim 1, it is characterized in that, describedly under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification, being implemented as follows of obtained shell monomer pre-emulsion II step:
Under high velocity agitation shell monomer is added drop-wise to wherein in another part of emulsifier aqueous solution, pre-emulsification 1 ~ 2h, obtained shell monomer pre-emulsion II.
4. a kind of core-shell acrylic-resin emulsion synthetic method according to claim 1, is characterized in that, after described 3rd part of emulsifier aqueous solution adds buffer reagent being implemented as follows of emulsifying agent aqueous solution of buffer agent III step:
Be 1:1 ~ 1:3 according to emulsifying agent and buffer reagent mass ratio, after the 3rd part of emulsifier aqueous solution adds buffer reagent emulsifying agent aqueous solution of buffer agent III.
5. a kind of core-shell acrylic-resin emulsion synthetic method according to claim 1, it is characterized in that, described in four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, be obtained by reacting being implemented as follows of stratum nucleare emulsion step:
In four-hole boiling flask, add emulsifying agent buffer reagent III, l successively, 2 nuclear monomer pre-emulsion I, 1/3 initiator solution, react under 60 ~ 70 DEG C of conditions, after there is blue-fluorescence, instill remaining 1/2 nuclear monomer pre-emulsion I and 1/3 initiator solution with 2 dropping funnels are synchronous, slow respectively, dropwise in 1.5 ~ 2 h, be warmed up to 70 ~ 80 DEG C, and continue insulation about 10 ~ 30 min, obtain stratum nucleare emulsion.
6. a kind of core-shell acrylic-resin emulsion synthetic method according to claim 1, is characterized in that, described in stratum nucleare emulsion, drips being implemented as follows of 1/3 initiator solution reactions steps of shell monomer pre-emulsion II and remainder:
Stratum nucleare emulsion in, by 2 dropping funnels synchronous, 1/3 initiator solutions of slowly dripping shell monomer pre-emulsions II and remainder respectively, temperature control is at 75 ~ 80 DEG C, and 2 ~ 2.5h dropwises, and is warming up to 80 ~ 85 DEG C of insulation 0.5 ~ 1h.
7. a kind of core-shell acrylic-resin emulsion synthetic method according to claim 1, is characterized in that, described reaction terminates, and uses ammoniacal liquor adjust ph, filters and obtain being implemented as follows of core-shell acrylic-resin emulsion step:
Reaction terminates, and is cooled to less than 30 ~ 40 DEG C, with ammoniacal liquor adjust ph to 8 ~ 9, filters and obtain core-shell acrylic-resin emulsion.
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| CN201410579621.XA CN104558367A (en) | 2014-10-25 | 2014-10-25 | Method for synthesizing core-shell acrylate emulsion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107400436A (en) * | 2017-08-01 | 2017-11-28 | 武汉工程大学 | A kind of water-based double microcapsules suppression weather-proof expansion steel-structure fireproofing coatings of cigarette and preparation method thereof |
| CN113698540A (en) * | 2021-08-27 | 2021-11-26 | 安徽聚合辐化化工有限公司 | Synthesis method of high-performance adhesive with core-shell structure |
-
2014
- 2014-10-25 CN CN201410579621.XA patent/CN104558367A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107400436A (en) * | 2017-08-01 | 2017-11-28 | 武汉工程大学 | A kind of water-based double microcapsules suppression weather-proof expansion steel-structure fireproofing coatings of cigarette and preparation method thereof |
| CN113698540A (en) * | 2021-08-27 | 2021-11-26 | 安徽聚合辐化化工有限公司 | Synthesis method of high-performance adhesive with core-shell structure |
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