CN107226883A - A kind of core shell structure aqueous silicone acrylic emulsion and preparation method thereof - Google Patents
A kind of core shell structure aqueous silicone acrylic emulsion and preparation method thereof Download PDFInfo
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- CN107226883A CN107226883A CN201710532348.9A CN201710532348A CN107226883A CN 107226883 A CN107226883 A CN 107226883A CN 201710532348 A CN201710532348 A CN 201710532348A CN 107226883 A CN107226883 A CN 107226883A
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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Abstract
A kind of core shell structure aqueous silicone acrylic emulsion and preparation method thereof, acrylic acid ester emulsion includes following component methyl methacrylate, butyl acrylate, acrylic acid, emulsifying agent, initiator, organosilicon, ammoniacal liquor and deionized water.Using semi-continuous seed emulsion polymerization method, various monomers are added in polymerization system in the different phase of polymerisation with reference to trace inequality charging production technology, it is prepared for the organic silicon acrylic ester emulsion with core shell structure, nontoxic pollution-free of the present invention, have the advantage of both organosilicon and acrylate polymer concurrently, improve hardness, adhesive force, the heat endurance of latex film, the performance such as hydrophobicity and water resistance；Moulding property, water resistance, the pollution resistance of emulsion are improved, the performances such as the MFT of emulsion are reduced；The gel fraction of emulsion polymerization is effectively reduced, the conversion ratio and stability of emulsion polymerization is improved.
Description
Technical field
The invention belongs to chemical technology field, it is related to the preparation and application of water paint.
Background technology
As the appearance and people of a series of environmentally friendly laws and regulations are to environmental protection and healthy pay attention to day by day, pass
Solvent based coating unite because containing substantial amounts of organic volatile, having substantial amounts of VOC to volatilize during solidification, easily environment being polluted, because
This its application is gradually restricted, and environment-friendly aqueous coating replaces organic solvent as decentralized medium using water, and environment is dirty
Dye is small, receives significant attention in recent years, just gradually replaces traditional solvent based coating.
The species of in the market water paint is various, there is aqueous polyurethane, water-and acrylate, aqueous epoxy resins etc., and
Water-and acrylate because its there is excellent adhesiveness, weatherability and corrosion resistance the advantages of, while raw material sources are abundant, it is easy to
Production and construction, it has also become the important kind of paint field.Conventional acrylates emulsion poor heat resistance, " heat is glutinous cold short " and water resistance
Poor the shortcomings of, limits its further development and uses.
The content of the invention
It is poly- using semi-continuous seed emulsion the invention provides a kind of core shell structure aqueous silicone acrylic emulsion and preparation method thereof
It is legal, with reference to trace inequality feed production technology according to " particle design " concept by various acrylate monomers be added to stratum nucleare or
In shell, organosilicon A-174 is added in the outermost layer of core-shell latex particles, the organosilicon propylene with core shell structure is prepared for
Acid esters emulsion.Core shell structure organic silicon acrylic ester emulsion improves the defect of conventional emulsions " heat is glutinous cold short ", improves latex
The combination properties such as the heat endurance of film, hydrophobicity and mechanical property.
The present invention is to be achieved by the following technical programs.
A kind of core shell structure aqueous silicone acrylic emulsion of the present invention, it is characterised in that by the component of following mass fraction
Prepare：40-50 parts of methyl methacrylate, 50-60 parts of butyl acrylate, 1.5-3.6 parts of emulsifying agent, initiator 0.4-
0.8 part, 1-8 parts of acrylic acid, 1-8 parts of organosilicon, 0.4-0.6 parts of sodium acid carbonate, 140-160 parts of deionized water.
Described emulsifying agent is anionic emulsifier and nonionic emulsifier, and its mass ratio is 2 ﹕ 1.
Further, described anionic emulsifier is lauryl sodium sulfate, and nonionic emulsifier is OP-10.
Further, described initiator is ammonium persulfate or potassium peroxydisulfate.
Further, described organosilicon is γ-methacryloxypropyl trimethoxy silane.
A kind of preparation method of core shell structure aqueous silicone acrylic emulsion of the present invention, it prepare in accordance with the following steps and
Into：
(1) preparation of pre-emulsion：42-48 mass parts deionized water, 0.5-1.2 mass parts breast are added in four-hole boiling flask
Agent, is stirred, and 12.5-15.6 mass parts MMA, 34.5-41.4 mass parts BA, high-speed stirred 30min are slowly added to successively,
Both core pre-emulsion is obtained；28-32 parts of deionized waters, 0.5-1.2 parts of emulsifying agents are added in another four-hole boiling flask, stirring is equal
It is even, 26.0-32.5 mass parts MMA, 11.7-14.0 mass parts BA, 1-8 mass parts AA high-speed stirred 30min are slowly added to successively,
Both shell pre-emulsion is obtained.
(2) preparation of core emulsion：In equipped with agitator, condenser pipe, the four-hole bottle of thermometer, nitrogen protection is lower to be added
26.3-30.0 mass parts deionized water, 0.5-1.2 mass parts emulsifying agents, 0.4-0.6 mass parts buffer sodium acid carbonates, stirring
1.5-1.8 mass parts MMA, 3.8-4.6 mass parts BA, initiator solution are added after uniform, 75 DEG C -85 DEG C are progressively warming up to,
After blue phase occurs in system, continue to be incubated 15min, both obtain seed emulsion.Then step is slowly added dropwise simultaneously in seed emulsion
(1) the core pre-emulsion and initiator solution prepared, about 2h is dripped off, and continues to be incubated 1h.
(3) preparation of shell emulsion：At 75 DEG C -85 DEG C, 30%-70% shell pre-emulsions are slowly added dropwise simultaneously in core emulsion
With 30%-70% initiator solutions, time for adding is 2h, and shell pre-emulsion and initiator solution are dripped off simultaneously.
(4) preparation of shell emulsion：By step (1) prepare shell pre-emulsion remainder mixed with organosilicon after and
Step (3) remaining initiator solution instills step (3) at 75 DEG C -85 DEG C, and time for adding 30min, completion of dropping is follow-up
Continue insurance temperature 1h, is then down to room temperature, adjusts pH value to 7-8 with ammoniacal liquor, is discharged with the strainer filtering of 300 mesh.
Initiator solution described in step (2), (3) by 0.13-0.27 mass parts initiator and 16.7 mass parts
Deionized water is constituted.It is preferred that the ratio of initiator and deionized water is 0.2：16.7 mass parts.
Contain the Si-O keys of higher bond energy in organic silicon monomer molecule, with many excellent performances, such as weatherability, resistance to height
Warm nature, stain resistant and organic solvent-resistant etc., therefore, using silicone modified polyacrylate, can have both concurrently
Advantage, improves moulding property, hydrophobicity, pollution resistance, weatherability, resistant of high or low temperature, water resistance and the mechanical strength of polymer etc. comprehensive
Close performance.
Core shell structure acrylic acid ester emulsion uses seed semi-continuous emulsion polymerization method, anti-in polymerization by substep emulsion polymerization
Various monomers are added in polymerization system by the different phase answered, and make the inner side and outer side of emulsion particle and have different compositions, from
And cause nuclear shell that there are different functions, moulding property, water resistance, the pollution resistance of emulsion are improved, the minimum of emulsion is reduced
The performances such as film-forming temperature.
The inventive principle of the present invention：The present invention uses semi-continuous seed emulsion polymerization method, with methyl methacrylate
(MMA), butyl acrylate (BA) and acrylic acid (AA) are principal monomer, are added to various monomers with reference to trace inequality feed way
In stratum nucleare or shell, organosilicon A-174 is added in the outermost layer of core-shell latex particles, is prepared for soft core monocoque
Organic silicon acrylic ester emulsion, TG shows that the heat endurance of the Acrylic emulsion film after organic-silicon-modified is greatly improved, DSC
Show it is organic-silicon-modified after the shell glass transition temperature of Acrylic emulsion film be improved, water contact angle test and SEM
Show that the addition of organosilicon reduces the surface energy of coating and adds the roughness of coating.
Compared with prior art, its advantage is the present invention：
(1) present invention utilizes organosilicon-modified acrylate emulsion, improve the moulding property of polymer, hydrophobicity, pollution resistance,
The combination properties such as weatherability, resistant of high or low temperature, water resistance and mechanical strength.
(2) present invention use seed semi-continuous emulsion polymerization method, by substep emulsion polymerization polymerisation not same order
Various monomers are added in polymerization system by section, and making the inner side and outer side of emulsion particle has different compositions, so that nucleocapsid
Layer has different functions, improves moulding property, water resistance, the pollution resistance of emulsion, reduces MFT of emulsion etc.
Performance.
(3) present invention uses seed semi-continuous emulsion polymerization method, with reference to trace inequality feed way, effectively reduces emulsion and gathers
The gel fraction of conjunction, improves the conversion ratio and stability of emulsion polymerization.
(4) present invention is used as decentralized medium, nontoxic pollution-free using water instead of organic solvent.
Brief description of the drawings
Fig. 1 be emulsion of the present invention by the unmodified core shell structure water-and acrylate film (a) of the preparation process of embodiment 1 with having
The TG figures of machine Si modification core shell structure water-and acrylate film (b).
Fig. 2 be emulsion of the present invention by the unmodified core shell structure water-and acrylate emulsion (a) of the preparation process of embodiment 1 with having
The particle size distribution figure of machine Si modification core shell structure water-and acrylate emulsion (b).
Fig. 3 be emulsion of the present invention by the unmodified core shell structure water-and acrylate film (a) of the preparation process of embodiment 1 with having
The Static water contact angles figure of machine Si modification core shell structure water-and acrylate film (b).
Fig. 4 is SEM of the emulsion of the present invention by the unmodified core shell structure water-and acrylate film of the preparation process of embodiment 1
Figure.
Fig. 5 is emulsion of the present invention by the organic-silicon-modified core shell structure water-and acrylate film of the preparation process of embodiment 1
SEM schemes.
Embodiment
Below by specific embodiment, the invention will be further elaborated.
It will be understood to those of skill in the art that methods described of the embodiment of the present invention is merely to illustrate the present invention, without that should regard
To limit the scope of the present invention.In the examples where no specific technique or condition is specified, according to related technology in the art or
Condition is carried out.Agents useful for same or the unreceipted production firm person of instrument, being can be by buying the conventional products obtained.
Embodiment 1.
(1) preparation of pre-emulsion：48 mass parts deionized waters, 1 mass parts emulsifying agent are added in four-hole boiling flask, is stirred
Uniformly, 12.5 mass parts MMA, 41.4 mass parts BA, high-speed stirred 30min are slowly added to successively, both obtain core pre-emulsion；Another
32 mass parts deionized waters, 1 mass parts emulsifying agent are added in one four-hole boiling flask, stirs, 26 mass is slowly added to successively
Part MMA, 14 mass parts BA, 2 mass parts AA, high-speed stirred 30min, both obtain shell pre-emulsion.
(2) preparation of core emulsion：In equipped with agitator, condenser pipe, the four-hole bottle of thermometer, nitrogen protection is lower to add 30
Mass parts deionized water, 1 mass parts emulsifying agent, 0.5 mass parts buffer sodium acid carbonate, are stirring evenly and then adding into 1.5 mass parts
MMA, 4.6 mass parts BA, initiator solution, are progressively warming up to 80 DEG C, after blue phase occurs in system, continue to be incubated 15min, both
Obtain seed emulsion.Then the core pre-emulsion and initiator solution of step (1) preparation is slowly added dropwise simultaneously in seed emulsion,
About 2h is dripped off, and continues to be incubated 1h.
(3) preparation of shell emulsion：At 80 DEG C, 70% shell pre-emulsion and 70% initiation is slowly added dropwise simultaneously in core emulsion
The agent aqueous solution, time for adding is 2h, and shell pre-emulsion and initiator solution are dripped off simultaneously.
(4) preparation of shell emulsion：The remainder and 4 mass parts organosilicons of shell pre-emulsion prepared by step (1)
Instilled after mixing with step (3) remaining initiator solution at 80 DEG C after step (3), time for adding 30min, completion of dropping
Continue to be incubated 1h, be then down to room temperature, adjust pH value to 7-8 with ammoniacal liquor, discharged with the strainer filtering of 300 mesh.
The water-and acrylate emulsion basic recipe of table 1
Fig. 1 is Unmodified propylene's acid esters (curve a), 4 parts of organosilicon-modified acrylates (TG songs of curve b) latex films
Line.As seen from the figure, the initial decomposition temperature of the acrylic acid ester emulsion film after organic-silicon-modified is from pure acrylate emulsion film
368.2 DEG C bring up to 374.8 DEG C；The decomposition mechanism temperature of pure acrylate film is 409.6 DEG C, and residual mass fraction is
15.01%, the decomposition mechanism temperature of organosilicon-modified acrylate emulsion film is 412.5 DEG C, and residual mass fraction is
17.67%；Under identical below-G conditions, the decomposition temperature of organic-silicon-modified acrylic acid ester emulsion film is more newborn than pure acrylate
The decomposition temperature of liquid film is high.The heat endurance of Acrylic emulsion film after this explanation is organic-silicon-modified is greatly improved, this be because
There is very high bond energy for the Si-O keys in organosilicon, the heat endurance of latex film can be improved, simultaneously because the addition of organosilicon,
The larger inorganic Si-O-Si networks of bond energy are formd in polymeric matrix, the effect of crosslinking is served.When polymer is thermally decomposed
When, these cross-linked networks can suppress the motion of polymer molecular chain, so as to effectively increase the heat decomposition temperature of polymer.
Curve a, b are respectively the grain of unmodified acrylic acid ester emulsion and organic-silicon-modified acrylic acid ester emulsion in Fig. 2
Footpath distribution map, as seen from the figure, the particle diameter distribution of pure-acrylic emulsion and silicone acrylic emulsion is Unimodal Distribution, is illustrated in emulsion polymerization process
New emulsion particle is not produced, understands that latex particle with core shell structure particle diameter is in 98nm or so, and particle diameter distribution index is all with reference to table 1
Smaller, distribution is narrower, illustrates that distribution emulsion polymerization can obtain the narrower emulsion particle of particle diameter distribution, while also demonstrating that various
Monomer all polymerize according to designed requirement in corresponding layer.
Fig. 3 is the organic silicon modified aqueous acrylate film and unmodified acrylate film that the present embodiment is obtained
(1) Static water contact angles.From figure, organosilicon can reduce the surface of water-based acrylic resin film to a certain extent certainly
By energy, water contact angle increases to 72.6 ° from 44.3 °.
Fig. 4, Fig. 5 are respectively the SEM of unmodified acrylic acid ester emulsion film and organic-silicon-modified acrylic acid ester emulsion film
Figure, as seen from the figure, unmodified acrylic acid ester emulsion film surface is more smooth, and through organic-silicon-modified acrylic acid ester emulsion film
Surface distributed some micron-sized particles, and surface is more coarse, because siliceous segment is moved in film forming procedure to surface
Move what is formed.
Embodiment 2.
(1) preparation of pre-emulsion；42 mass parts deionized waters, 0.5 mass parts emulsifying agent are added in four-hole boiling flask, is stirred
Mix uniform, 12.5 mass parts MMA, 41.4 mass parts BA, high-speed stirred 30min are slowly added to successively, both obtain core pre-emulsion；
28 mass parts deionized waters, 0.5 mass parts emulsifying agent are added in another four-hole boiling flask, stirs, 26 is slowly added to successively
Mass parts MMA, 14 mass parts BA, 3 mass parts AA, high-speed stirred 30min, both obtain shell pre-emulsion.
(2) preparation of core emulsion：In equipped with agitator, condenser pipe, the four-hole bottle of thermometer, nitrogen protection is lower to be added
26.25 mass parts deionized waters, 0.5 mass parts emulsifying agent, 0.4 mass parts buffer sodium acid carbonate, are stirring evenly and then adding into 1.5
Mass parts MMA, 4.6 mass parts BA, initiator solution, are progressively warming up to 75 DEG C, after blue phase occurs in system, continue to be incubated
15min, both obtains seed emulsion.Then core pre-emulsion and the initiation of step (1) preparation is slowly added dropwise simultaneously in seed emulsion
The agent aqueous solution, about 2h are dripped off, and continue to be incubated 1h.
(3) preparation of shell emulsion：At 75 DEG C, 50% shell pre-emulsion and 50% initiation is slowly added dropwise simultaneously in core emulsion
The agent aqueous solution, time for adding is 2h, and shell pre-emulsion and initiator solution are dripped off simultaneously.
(4) preparation of shell emulsion：The remainder of shell pre-emulsion prepared by step (1) is mixed with 2 parts of organosilicons
Instill after step (3), time for adding 30min, completion of dropping and continue at 75 DEG C with step (3) remaining initiator solution afterwards
1h is incubated, room temperature is then down to, pH value is adjusted to 7-8 with ammoniacal liquor, is discharged with the strainer filtering of 300 mesh.
Embodiment 3.
(1) preparation of pre-emulsion；45 mass parts deionized waters, 0.8 mass parts emulsifying agent are added in four-hole boiling flask, is stirred
Mix uniform, 15.63 mass parts MMA, 34.5 mass parts BA, high-speed stirred 30min are slowly added to successively, both obtain core pre-emulsion；
30 mass parts deionized waters, 0.8 mass parts emulsifying agent are added in another four-hole boiling flask, stirs, is slowly added to successively
32.5 mass parts MMA, 11.67 mass parts BA, 4 parts of AA, high-speed stirred 30min, both obtain shell pre-emulsion.
(2) preparation of core emulsion：In equipped with agitator, condenser pipe, the four-hole bottle of thermometer, nitrogen protection is lower to be added
28.13 mass parts deionized waters, 0.8 mass parts emulsifying agent, 0.4 mass parts buffer sodium acid carbonate, are stirring evenly and then adding into
1.75 mass parts MMA, 3.83 mass parts BA, initiator solution, are progressively warming up to 85 DEG C, after blue phase occurs in system, continue
15min is incubated, seed emulsion is both obtained.Then in seed emulsion simultaneously be slowly added dropwise step (1) preparation core pre-emulsion and
Initiator solution, about 2h are dripped off, and continue to be incubated 1h.
(3) preparation of shell emulsion：At 85 DEG C, 30% shell pre-emulsion and 30% initiation is slowly added dropwise simultaneously in core emulsion
The agent aqueous solution, time for adding is 2h, and shell pre-emulsion and initiator solution are dripped off simultaneously.
(4) preparation of shell emulsion：The remainder of shell pre-emulsion prepared by step (1) is mixed with 5 parts of organosilicons
Instill after step (3), time for adding 30min, completion of dropping and continue at 85 DEG C with step (3) remaining initiator solution afterwards
1h is incubated, room temperature is then down to, pH value is adjusted to 7-8 with ammoniacal liquor, is discharged with the strainer filtering of 300 mesh.
Embodiment 4.
(1) preparation of pre-emulsion；48 mass parts deionized waters, 1.2 mass parts emulsifying agents are added in four-hole boiling flask, are stirred
Mix uniform, 13.39 mass parts MMA, 35.84 mass parts BA, high-speed stirred 30min are slowly added to successively, both obtain core pre-emulsion；
32 mass parts deionized waters, 1.2 mass parts emulsifying agents are added in another four-hole boiling flask, stirs, is slowly added to successively
29.25 mass parts MMA, 12.83 mass parts BA, 8 mass parts AA, high-speed stirred 30min, both obtain shell pre-emulsion.
(2) preparation of core emulsion：In equipped with agitator, condenser pipe, the four-hole bottle of thermometer, nitrogen protection is lower to add 30
Mass parts deionized water, 1.2 mass parts emulsifying agents, 0.6 mass parts buffer sodium acid carbonate, are stirring evenly and then adding into 2.37 mass
Part MMA, 6.33 mass parts BA, initiator solution, are progressively warming up to 85 DEG C, after blue phase occurs in system, continue to be incubated
15min, both obtains seed emulsion.Then core pre-emulsion and the initiation of step (1) preparation is slowly added dropwise simultaneously in seed emulsion
The agent aqueous solution, about 2h are dripped off, and continue to be incubated 1h.
(3) preparation of shell emulsion：At 85 DEG C, 30% shell pre-emulsion and 30% initiation is slowly added dropwise simultaneously in core emulsion
The agent aqueous solution, time for adding is 2h, and shell pre-emulsion and initiator solution are dripped off simultaneously.
(4) preparation of shell emulsion：The remainder and 8 mass parts organosilicons of shell pre-emulsion prepared by step (1)
Instilled after mixing with step (3) remaining initiator solution at 85 DEG C after step (3), time for adding 30min, completion of dropping
Continue to be incubated 1h, be then down to room temperature, adjust pH value to 7-8 with ammoniacal liquor, discharged with the strainer filtering of 300 mesh.
Each embodiment test result of the core shell structure aqueous silicone acrylic emulsion of table 2
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Water absorption rate/% | 13.6 | 18.7 | 12.4 | 8.8 |
| Hardness | 2H | H | 3H | 4H |
| Adhesive force | 0 | 1 | 0 | 0 |
| Water resistance | Pass through | Pass through | Pass through | Pass through |
| Contact angle/。 | 72.6 | 62.1 | 73.9 | 75 |
| Calcium ion stability | Pass through | Pass through | Pass through | Pass through |
| Dewatering ability | Pass through | Pass through | Pass through | Pass through |
| Heat endurance | Pass through | Pass through | Pass through | Pass through |
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claim and its waits
Effect thing is defined.
Claims (7)
1. a kind of core shell structure aqueous silicone acrylic emulsion, it is characterised in that be made up of the component of following mass fraction：Methacrylic acid
40-50 parts of methyl esters, 50-60 parts of butyl acrylate, 1.5-3.6 parts of emulsifying agent, 0.4-0.8 parts of initiator, 1-8 parts of acrylic acid have
1-8 parts of machine silicon, 0.4-0.6 parts of sodium acid carbonate, 140-160 parts of deionized water.
2. a kind of core shell structure aqueous silicone acrylic emulsion according to claim 1, it is characterised in that described emulsifying agent is the moon
Ionic emulsifying agent and nonionic emulsifier, its mass ratio are 2 ﹕ 1.
3. a kind of core shell structure aqueous silicone acrylic emulsion according to claim 1 or 2, it is characterised in that described anion
Type emulsifying agent is lauryl sodium sulfate, and nonionic emulsifier is OP-10.
4. a kind of core shell structure aqueous silicone acrylic emulsion according to claim 1, it is characterised in that described initiator was
Ammonium sulfate or potassium peroxydisulfate.
5. a kind of core shell structure aqueous silicone acrylic emulsion according to claim 1, it is characterised in that described organosilicon is
γ-methacryloxypropyl trimethoxy silane.
6. the preparation method of a kind of core shell structure aqueous silicone acrylic emulsion described in claim 1, it is characterised in that by following step
Suddenly：
(1) 42-48 mass parts deionized water, 0.5-1.2 mass parts emulsifying agents are added in four-hole boiling flask, is stirred, successively
12.5-15.6 mass parts MMA, 34.5-41.4 mass parts BA, high-speed stirred 30min are slowly added to, core pre-emulsion is both obtained；
28-32 parts of deionized waters, 0.5-1.2 parts of emulsifying agents are added in another four-hole boiling flask, stirs, is slowly added to successively
26.0-32.5 mass parts MMA, 11.7-14.0 mass parts BA, 1-8 mass parts AA high-speed stirred 30min, both obtain shell pre-emulsion；
(2) in equipped with agitator, condenser pipe, the four-hole bottle of thermometer, nitrogen protection is lower add 26.3-30.0 mass parts go from
Sub- water, 0.5-1.2 mass parts emulsifying agents, 0.4-0.6 mass parts buffer sodium acid carbonates, are stirring evenly and then adding into 1.5-1.8 matter
Part MMA, 3.8-4.6 mass parts BA, initiator solution are measured, 75 DEG C -85 DEG C are progressively warming up to, after there is blue phase in system, after
Continue insurance temperature 15min, both obtains seed emulsion；Then the core pre-emulsion of step (1) preparation is slowly added dropwise simultaneously in seed emulsion
And initiator solution, about 2h drips off, and continues to be incubated 1h；
At (3) 75 DEG C -85 DEG C, 30%-70% shells pre-emulsion and 30%-70% initiators is slowly added dropwise simultaneously in core emulsion
The aqueous solution, time for adding is 2h, and shell pre-emulsion and initiator solution are dripped off simultaneously；
(4) with step (3) remaining initiator after the remainder for the shell pre-emulsion for preparing step (1) is mixed with organosilicon
The aqueous solution instills step (3) at 75 DEG C -85 DEG C, and then time for adding 30min, the follow-up continuation of insurance temperature 1h of completion of dropping are down to room
Temperature, adjusts pH value to 7-8 with ammoniacal liquor, is discharged with the strainer filtering of 300 mesh；
Initiator solution described in step (2), (3) by 0.13-0.27 mass parts initiator and 16.7 mass parts go from
Sub- water composition.
7. a kind of preparation method of core shell structure aqueous silicone acrylic emulsion according to claim 6, it is characterised in that initiator
Ratio with deionized water is 0.2：16.7 mass parts.
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| CN109627400A (en) * | 2018-12-07 | 2019-04-16 | 东联北方科技(北京)有限公司 | Acrylic acid series multi-layer core-shell polymer emulsion and its preparation method and application |
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| CN110551246A (en) * | 2018-06-04 | 2019-12-10 | 阜阳师范学院 | Acrylate emulsion and preparation method thereof |
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