CN105713149A - Vinyl acetate-acrylic emulsion and preparation method thereof - Google Patents
Vinyl acetate-acrylic emulsion and preparation method thereof Download PDFInfo
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- CN105713149A CN105713149A CN201410736935.6A CN201410736935A CN105713149A CN 105713149 A CN105713149 A CN 105713149A CN 201410736935 A CN201410736935 A CN 201410736935A CN 105713149 A CN105713149 A CN 105713149A
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Abstract
The invention provides vinyl acetate-acrylic emulsion and a preparation method thereof. The preparation method comprises the following steps: mixing (meth)acrylate, vinyl acetate, carboxylic acid monomers, and a chain transferring agent to prepare monomers; evenly mixing mixed monomers obtained in the previous step with a weight percentage of 80 to 100%, a reaction type emulsifier with a weight percentage of 40 to 90%, an initiator with a weight percentage of 40 to 90%, and functional monomers; reacting the mixed monomers obtained in the previous step with a weight percentage of 0 to 20% with an emulsifier with a weight percentage of 10 to 60% and an initiator with a weight percentage of 10 to 60% for 10 to 40 minutes at a temperature of 70 to 95 DEG C, dropwise adding a mixed solution within 1 to 5 hours; maintaining a temperature of 70 to 95 DEG C for 1 to 2 hours, then cooling to a temperature of 25 DEG C, and adjusting the pH to 5-8 to obtain the vinyl acetate-acrylic emulsion. The vinyl acetate-acrylic emulsion is used as a paint for coated paper, can obviously enhance the surface strength of coated paper, and improves the phenomenon of powder falling.
Description
Technical field
The present invention relates to a kind of coating being coated with paper, particularly relate to a kind of acetic acid acrylic emulsion and preparation method thereof.
Background technology
Emulsion is widely used in the bonding of coating for paper, in application process, the performance requirement of emulsion is more and more higher.Improvement and development along with emulsion applications Technology, it is desirable to emulsion has the good technique suitability, wherein, the most important or caking property of styrene-acrylic emulsion.Emulsion applications can significantly improve the surface strength of paper in coating for paper, reduces paper hair and powder dropping phenomenon.
The preparation method that Chinese patent CN101280035A discloses a kind of emulsion, with styrene, butyl acrylate, methyl methacrylate, acrylic acid, containing the functional monomer of urea groups, compound emulsifying agent, thermal decomposition initiating for raw material, adopt hud polymerization method polymerization obtain Wet-rub resistant styrene-acrylic emulsion.The emulsion applications prepared is in coating for paper, and coating mobility, resistance to water are better, but after coating, surface strength of paper is poor on paper.Therefore, it is badly in need of a kind of coating for paper and had both met good fluidity, water-tolerant, also want paper surface to have enough intensity.
Summary of the invention
It is an object of the invention to for above technical problem, it is provided that one had both met good fluidity, water-tolerant, the coating for paper of also enough surface strengths.
Technical scheme is specific as follows:
The preparation method of a kind of acrylate and vinyl acetate emulsion, specifically comprises the following steps that
1) (methyl) acrylate, vinylacetate, carboxylic acid monomer and chain-transferring agent are mixed and made into mix monomer;
2) by step 1) 80-100% and the 40-90% of reactive emulsifier gross weight of described mix monomer gross weight, the 40-90% of initiator gross weight, functional monomer, water gross weight 40-70% be uniformly mixed into mixed solution;
3) by step 1) in mix monomer and the reactive emulsifier of all the other weight of all the other weight, the initiator of all the other weight, all the other weight water mix, react 10-40 minute under 70 DEG C of-95 DEG C of conditions, then dropping step 2) in mixed solution, at least dropwised in 1 hour;
4), after being incubated 1-2 hour at 70-95 DEG C, it is cooled to room temperature, pH is adjusted to 5-8, obtain acrylate and vinyl acetate emulsion.
A kind of preparation method of acrylate and vinyl acetate emulsion, the weight proportion of each component is:
The preparation method of a kind of acrylate and vinyl acetate emulsion, described initiator is selected from any one or a few in peroxide, persulfide, persulfuric acid, persulfate.
The preparation method of a kind of acrylate and vinyl acetate emulsion, described persulfate is selected from any one or a few in potassium peroxydisulfate, sodium peroxydisulfate, Ammonium persulfate..
A kind of preparation method of acrylate and vinyl acetate emulsion, described (methyl) acrylate any acrylic or methacrylic acid alkyl ester in C1-C18 straight or branched.
The preparation method of a kind of acrylate and vinyl acetate emulsion, described (methyl) acrylate is selected from propylene, acrylic acid methyl ester., ethyl acrylate, n-butyl acrylate, Isobutyl 2-propenoate, acrylic acid-2-ethyl caproite, methyl methacrylate, ethyl methacrylate, n-BMA, methacrylic acid-2-Octyl Nitrite.
The preparation method of a kind of acrylate and vinyl acetate emulsion, described carboxylic acid monomer is selected from any one or a few in acrylic acid, methacrylic acid, itaconic acid, fumaric acid;Described functional monomer be selected from 2-methyl-2 acrylic acid-2 hydroxyethyl ester phosphate ester, in N-acryl thiourea, N hydroxymethyl acrylamide any one or multiple;Described reactive emulsifier in allyl polyethenoxy ether ammonium sulfate, allyl polyethenoxy ether, the vinyl polyoxyethylene ether any one or multiple;Described chain-transferring agent in n-dodecyl mereaptan, tert-dodecyl mercaptan, the n-butyl mercaptan any one or multiple.
A kind of acrylate and vinyl acetate emulsion produced according to said method.
A kind of acrylate and vinyl acetate emulsion as mentioned above, is applied to the coating of coating paper.
The present invention adopts technique scheme, compared with prior art, and beneficial effects of the present invention:
It is known that medium-sized emulsifying agent is after emulsion film forming, compatible with polymer body because being difficult to, it is easy to the adhesion on the surface and paper-making fibre that move to film is deteriorated.And the present invention adopts reactive surfactant as emulsifying agent, this emulsifying agent can with the formal bond of chemical bond with on polymer chain, active group on emulsifier molecules can be combined by the group such as hydroxyl on fiber, increase macromolecular chain and fiber bonds, it is possible to strengthen the surface tension of paper.Add some functional monomers in the present invention, unexpected, it is possible to significantly improve the adhesion of emulsion and paper fibre.This is likely to be due to the hydroxyl on functional monomer, amino isoreactivity the group easily ester bond on vinylacetate, some groups on fiber surface and is combined, and the surface strength showing as paper is improved.
The acrylate and vinyl acetate emulsion of the present invention is a kind of product that can meet papermaking paint high-performance, environmental protection.This product is application in the coating of coating paper, can be remarkably reinforced the surface strength of coating paper, improve hair and powder dropping phenomenon.
Detailed description of the invention
The invention provides a kind of acetic acid acrylic emulsion and preparation method thereof.
Below by specific embodiment, the present invention being carried out detailed and concrete introduction, so that being better understood from the present invention, but following embodiment is not limiting as the scope of the invention.
Embodiment 1
The synthesis of acrylate and vinyl acetate emulsion:
A) 25g n-butyl acrylate, 70g vinylacetate, 2g acrylic acid and 0.1g n-dodecyl mereaptan are mixed and made into mix monomer, standby.
B) by 97.1ga) mix monomer in step adds 0.63g allyl polyethenoxy ether ammonium sulfate, 0.2g potassium peroxydisulfate, 3g2-methyl-2 acrylic acid-2 hydroxyethyl ester phosphate ester become aqueous solution with 35.7g deionized water dissolving, high-speed stirred 30 minutes, standby.
E) in the aqueous solution of 0.07g allyl polyethenoxy ether ammonium sulfate, 0.3g potassium peroxydisulfate and 15.3g deionized water, will react 40 minutes under 70 DEG C of conditions, then drip mixed liquor in b) step 5 hours.
F) 70 DEG C are incubated 2 hours.It is cooled to 25 DEG C, is that 10% ammonium hydroxide aqueous solution neutralizes with 4g weight solid content, continues stirring 10 minutes.Filtering through 100 eye mesh screens, obtain styrene-acrylic emulsion, solid content: 64.8wt%, mean diameter 290nm (uses Malven particle instrument to record), and pH=5.14 (uses PHS-3C Accurate pH to measure).
Embodiment 2
The synthesis of acrylate and vinyl acetate emulsion:
A) 68g ethyl acrylate, 30g vinylacetate, 1g methacrylic acid and 0.5g tert-dodecyl mercaptan are mixed and made into mix monomer.Standby.
B) by 79.6ga) mix monomer in step adds 1.8g allyl polyethenoxy ether, 4.05g sodium peroxydisulfate, 1gN-acryl thiourea and becomes aqueous solution, high-speed stirred 30 minutes with 65.7g deionized water dissolving.Standby.
C) by 19.9ga) mix monomer in step adds in the aqueous solution of 2.7g allyl polyethenoxy ether, 0.45g sodium peroxydisulfate and 98.55g deionized water, reacts 10 minutes under 95 DEG C of conditions, then drips mixed liquor in b) step 1 hour.
D) 70 DEG C are incubated 1 hour.It is cooled to 25 DEG C, is that 40% sodium hydrate aqueous solution neutralizes with 20g weight solid content, continues stirring 10 minutes.Filtering through 100 eye mesh screens, obtain styrene-acrylic emulsion, solid content: 40.1wt%, mean diameter 104nm (uses Malven particle instrument to record), and pH=7.90 (uses PHS-3C Accurate pH to measure).
Embodiment 3
The synthesis of acrylate and vinyl acetate emulsion:
A) 20g methyl methacrylate, 27g acrylic acid-2-ethyl caproite, 50g vinylacetate, 1.5g itaconic acid and 0.3g n-butyl mercaptan are mixed and made into mix monomer.Standby.
B) by 88.92ga) mix monomer in step adds 1.5g vinyl polyoxyethylene ether, 1.5g Ammonium persulfate., 1.5gN-n-methylolacrylamide and becomes aqueous solution, high-speed stirred 30 minutes with 50.15g deionized water dissolving.Standby.
E) by 9.88ga) mix monomer in step adds in the aqueous solution of 1.5g vinyl polyoxyethylene ether, 1.5g Ammonium persulfate. and 50.15g deionized water, reacts 20 minutes under 80 DEG C of conditions, then drips mixed liquor in b) step 3 hours.
F) 70 DEG C are incubated 2 hours.It is cooled to 25 DEG C, is that 20% potassium hydroxide aqueous solution neutralizes with 10g weight solid content, continues stirring 10 minutes.Filtering through 100 eye mesh screens, obtain styrene-acrylic emulsion, solid content: 49.6wt%, mean diameter 201nm (uses Malven particle instrument to record), and pH=7.10 (uses PHS-3C Accurate pH to measure).
Embodiment 4
The synthesis of acrylate and vinyl acetate emulsion:
A) just 58g n-BMA, 20g styrene, 17.3g vinylacetate, 1.8g fumaric acid and 0.1g n-butyl mercaptan, 0.1g tert-dodecyl mercaptan are mixed and made into mix monomer.Standby.
B) by 82.8ga) mix monomer in step adds 1.0g vinyl polyoxyethylene ether, 0.4g allyl polyethenoxy ether ammonium sulfate, 1.4g Ammonium persulfate., 1.0gN-n-methylolacrylamide, 1.5g2-methyl-2 acrylic acid-2 hydroxyethyl ester phosphate ester become aqueous solution, high-speed stirred 30 minutes with 45.7g deionized water dissolving.Standby.
E) by 14.7ga) mix monomer in step adds in the aqueous solution of 0.6g vinyl polyoxyethylene ether, 0.6g Ammonium persulfate. and 30.5g deionized water, reacts 30 minutes under 85 DEG C of conditions, then drips mixed liquor in b) step 3 hours.
F) 70 DEG C are incubated 2 hours.It is cooled to 25 DEG C, be 15% potassium hydroxide aqueous solution, 10g weight solid content with 5g weight solid content is that 25% ammonium hydroxide aqueous solution neutralizes, continue stirring 10 minutes.Filtering through 100 eye mesh screens, obtain styrene-acrylic emulsion, solid content: 55.12wt%, mean diameter 148nm (uses Malven particle instrument to record), and pH=7.18 (uses PHS-3C Accurate pH to measure).
Embodiment 5
Comparative example: the emulsion prepared by the method for CN101280035A
By embodiment 1~4 and comparative example, prepare coating by following formula
95 grades of ground calcium carbonate 400g
Brazil china clay 100g
Emulsion (dry weight) 50g
Deionized water is appropriate, and adjusting coating weight solid content is 65%.
Experimentation: 1) 95 grades of ground calcium carbonate, Brazil's china clay and appropriate amount of deionized water are added high speed dispersor, high speed dispersion 20~30min after stirring, qualified to fineness, emulsion is added under low speed, after stirring, discharging, 100 eye mesh screens filter 2) by adopt embodiment 1~5 and comparative example emulsion preparation coating with 10# spreading rod at 75g/m2Art base paper is coated, coating weight 20g/m2, standby 3) and coating rolling condition: take the above-mentioned coating pattern hard press polish of small-sized calender twice (0.3Mpa, 85 DEG C) respectively.Standby.
A) above-mentioned coating paper adopt IGT printability instrument (Japan KRK) detect:
Criterion: surface strength shows that more greatly emulsion effect is more good
Surface strength m/s | |
Comparative example | 0.65 |
Embodiment 1 | 1.11 |
Embodiment 2 | 1.20 |
Embodiment 3 | 1.31 |
Embodiment 4 | 1.10 |
B) by OPP adhesive tape (OPPT04, Dongguan City Zong Wei Industrial Co., Ltd.) viscous 5cm strip on above-mentioned coating paper surface, moment pulls off OPP adhesive tape, checks whether have calcium carbonate powder or fiber on OPP adhesive tape.
Sample | Result |
Comparative example | A small amount of white powder, a small amount of fiber |
Embodiment 1 | Nothing |
Embodiment 2 | Nothing |
Embodiment 3 | Nothing |
Embodiment 4 | Nothing |
From above-mentioned application result it can be seen that use the styrene-acrylic emulsion of the embodiment of the present invention 1~4 preparation, compared with comparative example, it is applied to the bottom-coating of coating paper, the surface strength of coating paper can be significantly improved and reduce coating paper hair and powder dropping phenomenon.
Above specific embodiments of the invention being described in detail, but it is intended only as example, the present invention is not restricted to particular embodiments described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and replacement are also all among scope of the invention.Therefore, the equalization made without departing from the spirit and scope of the invention converts and amendment, all should contain within the scope of the invention.
Claims (9)
1. the preparation method of an acrylate and vinyl acetate emulsion, it is characterised in that specifically comprise the following steps that
1) (methyl) acrylate, vinylacetate, carboxylic acid monomer and chain-transferring agent are mixed and made into mix monomer;
2) by step 1) 80-100% and the 40-90% of reactive emulsifier gross weight of described mix monomer gross weight, the 40-90% of initiator gross weight, functional monomer, water gross weight 40-70% be uniformly mixed into mixed solution;
3) by step 1) in mix monomer and the reactive emulsifier of all the other weight of all the other weight, the initiator of all the other weight, all the other weight water mix, react 10-40 minute under 70 DEG C of-95 DEG C of conditions, then dropping step 2) in mixed solution, at least dropwised in 1 hour;
4), after being incubated 1-2 hour at 70-95 DEG C, it is cooled to room temperature, pH is adjusted to 5-8, obtain acrylate and vinyl acetate emulsion.
2. method according to claim 1, it is characterised in that the weight proportion of each component is:
3. method according to claim 1 and 2, it is characterised in that described initiator is selected from any one or a few in peroxide, persulfide, persulfuric acid, persulfate.
4. method according to claim 3, it is characterised in that described persulfate is selected from any one or a few in potassium peroxydisulfate, sodium peroxydisulfate, Ammonium persulfate..
5. method according to claim 1 and 2, it is characterised in that described (methyl) acrylate any acrylic or methacrylic acid alkyl ester in C1-C18 straight or branched.
6. method according to claim 5, it is characterized in that, described (methyl) acrylate is selected from propylene, acrylic acid methyl ester., ethyl acrylate, n-butyl acrylate, Isobutyl 2-propenoate, acrylic acid-2-ethyl caproite, methyl methacrylate, ethyl methacrylate, n-BMA, methacrylic acid-2-Octyl Nitrite.
7. method according to claim 1 and 2, it is characterised in that described carboxylic acid monomer is selected from any one or a few in acrylic acid, methacrylic acid, itaconic acid, fumaric acid;Described functional monomer be selected from 2-methyl-2 acrylic acid-2 hydroxyethyl ester phosphate ester, in N-acryl thiourea, N hydroxymethyl acrylamide any one or multiple;Described reactive emulsifier in allyl polyethenoxy ether ammonium sulfate, allyl polyethenoxy ether, the vinyl polyoxyethylene ether any one or multiple;Described chain-transferring agent in n-dodecyl mereaptan, tert-dodecyl mercaptan, the n-butyl mercaptan any one or multiple.
8. the acrylate and vinyl acetate emulsion that a method according to claim 1 produces.
9. acrylate and vinyl acetate emulsion according to claim 8, it is characterised in that be applied to the coating of coating paper.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105985497A (en) * | 2015-02-28 | 2016-10-05 | 上海东升新材料有限公司 | Acetic acrylic emulsion and preparing method thereof |
CN107337758A (en) * | 2016-11-23 | 2017-11-10 | 佛山市传化富联精细化工有限公司 | A kind of water-fastness environmental-friendly stiffening agent and preparation method thereof |
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2014
- 2014-12-04 CN CN201410736935.6A patent/CN105713149A/en active Pending
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喻迪等: "交联型醋丙乳液用于汽车滤纸的增强", 《纸和造纸》 * |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105985497A (en) * | 2015-02-28 | 2016-10-05 | 上海东升新材料有限公司 | Acetic acrylic emulsion and preparing method thereof |
CN107337758A (en) * | 2016-11-23 | 2017-11-10 | 佛山市传化富联精细化工有限公司 | A kind of water-fastness environmental-friendly stiffening agent and preparation method thereof |
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Application publication date: 20160629 |