CN101660276A - Aqueous silicon-acrylate textile adhesive coating and preparation method thereof - Google Patents
Aqueous silicon-acrylate textile adhesive coating and preparation method thereof Download PDFInfo
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- CN101660276A CN101660276A CN200910186073A CN200910186073A CN101660276A CN 101660276 A CN101660276 A CN 101660276A CN 200910186073 A CN200910186073 A CN 200910186073A CN 200910186073 A CN200910186073 A CN 200910186073A CN 101660276 A CN101660276 A CN 101660276A
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Abstract
The invention relates to an aqueous silicon-acrylate textile adhesive coating and a preparation method thereof; the aqueous silicon-acrylate textile adhesive coating is polymer emulsion which is formed by the following raw materials through core-shell polymerization; the raw materials include: lauryl sodium sulfate, alkyl phenol polyoxyethylene ether, methacrylic acid, butyl acrylate, ethyl acrylate, N-methacrylamide, acrylic acid, vinyl acetate monomer, vinyltrimethoxysilane, ammoniumpersulfate and deionized water. High-low temperature rangeability of resonance frequency f0 of audio frequencyof the cloth-edge cone of a loudspeaker which is prepared by the aqueous silicon-acrylate textile adhesive coating can be greatly improved.
Description
Technical field
The present invention relates to a kind of coating adhesive and preparation method thereof, relate in particular to a kind of aqueous silicon-acrylate textile adhesive coating and preparation method thereof.
Background technology
Modern loudspeaker preparation industry is owing to be subjected to the dual-pressure of industry competition and environmental protection, and the user is more and more higher to the requirement of loudspeaker quality, so the used adhesive of loudspeaker is had higher requirement.The sound basin selvedge of loudspeaker adopts polyacrylate dispersion as coating glue, generally require prepared sound basin high and low temperature resistance good, the high low temperature amplitude of variation that shows as the loudspeaker audio resonant frequency is little, thereby guarantee higher tonequality output, this product quality, lifting product specification to improving sound basin selvedge, and satisfy the demand of special environment condition and part high-end user, have great importance.
The research work of emulsion polymerisation has obtained more rapidly development over nearly 20 years, from research contents, people have further investigated the one-tenth nuclear issue rather crucial in the emulsion polymerisation, and the whole process of polymerization has been had understanding more clearly; Semi-continuous emulsion polymerizing is a kind of New Emulsion polymerization technique that just obtains broad research and application in recent years.So-called semi-continuous emulsion polymerizing, the monomer (or monomer emulsions) that to participate in polymerization exactly splashes in the reactor with certain speed continuously, with the speed of control polymerization, the copolymerization composition of polymer, the structure of polyalcohol emulsion particle, and the molecular weight of polymer etc.Early stage semi-continuous emulsion polymerizing almost all selects monomer to splash into reactor with relative very slow speed, make reaction system not contain free monomer droplet in the most of the time of reaction, thereby nuclear is in " starvation " always.In this case, the reaction rate of whole system equates that with the feed rate of monomer this control for polymerization rate control and polymerization exotherm provides effective means, also makes the adjusting of emulsion particle size and form more convenient simultaneously.When this method is applied to the emulsion copolymerization system, be expected to obtain to form the copolymer of homogeneous.
In recent years, polarity is differed the seeded emulsion polymerization of bigger monomer to people and the structural form of emulsion particle has carried out deep research, find to be easy to form seed polymer at interior, other monomer-polymer nucleocapsid structure emulsion particle outside when seed polymer hydrophily during less than other polymer of monomers; Otherwise, with the hydrophilic monomer is nuclear layer monomer, and be the seeded emulsion polymerization of shell monomers with the hydrophobic monomer, in polymerization process, the shell hydrophobic polymer may be to seed latex particle internal migration, thereby might form (as: careless mould type, fabric of island-in-sea type, flip type etc.) latex particle of improper structural form.Because nucleocapsid latex particle particular structure form has two kinds of polymer properties concurrently, its particular structure form can be improved polymer properties, give micelle certain functional characteristic, as the high-low temperature resistant that can improve polymer significantly, wear-resisting, weather resistance and adhesive strength etc.
Adopt the polyacrylate dispersion of conventional method preparation, prepared loudspeaker cloth lateral basin, the high low temperature vary within wide limits of loudspeaker audio resonant frequency under the bigger environmental condition of variations in temperature, is difficult to obtain satisfied tonequality.The high low temperature amplitude of variation of the loudspeaker audio resonant frequency of external like product is minimum, and the disclosed technical data of its related coatings glue is actually rare.
Summary of the invention
The object of the present invention is to provide a kind of aqueous silicon-acrylate textile adhesive coating and preparation method thereof, this method has improved tensile strength and the high-low temperature resistant characteristic behind the polymer film forming.In complex, contain crosslinkable N-methylol and carboxylic group, can improve the adhesive force of polymer after crosslinked fabric.
The present invention is achieved like this, and it is characterized in that, the material component mass percent is:
The material component mass percent of solution I is:
Monomer 20～50%
The material component mass percent of solution II is:
Lauryl sodium sulfate SDS 0.5～5.0%
Alkylphenol polyoxyethylene OP-10 1.0～6.0%
Deionized water 30～60%
The material component mass percent of solution III is:
Ammonium persulfate APS 0.2～2.0%
The deionized water surplus.
Monomer of the present invention, its weight percentages is:
Component weight nucleocapsid
Methacrylic acid MAA 0.5～5.0 0.5～5.0 0
Butyl acrylate BA 30～80 10～40 10～40
Ethyl acrylate EA 0.5～5.0 0 0.5～5.0
Vinylacetate VAc 1.0～10 1.0～10 0
N methacrylamide NMA 1.0～14.0 1.0～7.0 1.0～7.0
Acrylic acid AA 2.0～18 1.0～9.0 1.0～9.0
Vinyltrimethoxy silane A-171 0.5～5.0 0 0.5～5.0.
A kind of preparation method of aqueous silicon-acrylate textile adhesive coating is characterized in that, concrete steps are:
(1) preparation of pre-emulsion
Nuclear monomer I1 slowly is added dropwise among the aqueous solution II of 1/3 emulsifying agent while stirring successively, at room temperature stirs fully and mix, emulsification 0.5～2 hour obtains nuclear monomer pre-emulsion I1-1; In like manner, shell monomer I2 slowly is added dropwise among the aqueous solution II of other 1/3 emulsifying agent while stirring successively, stirs fully under the room temperature and mix, emulsification 0.5～2 hour obtains shell monomer pre-emulsion I2-1;
(2) preparation of seed emulsion
Agitator is being housed, thermometer, the aqueous solution II that adds residue 1/3 emulsifying agent in the 500ml four-hole boiling flask of condenser pipe, 1/2 nuclear monomer emulsion I1-1,1/3 initiator solution III, about 50～80 ℃ of temperature control, start stirring, in water bath with thermostatic control, be heated to 50～80 ℃ and make it polymerization, time 30～50min, after blue-fluorescence occurring, with two dropping funels respectively synchronously, splash into remaining nuclear monomer emulsion I1-1 and 1/3 initiator solution III lentamente, 60～90 ℃ of temperature controls, 1～2h dropwises, continue to be incubated about 30～90min in 60～95 ℃, promptly get seed emulsion;
(3) polymerization of shell
In above-mentioned seed emulsion, splash into shell monomer emulsion I2-1 and 1/3 remaining initiator solution III respectively synchronously, lentamente by two dropping funels, 60～95 ℃ of temperature controls, 0.5-2h dropwise, continue insulation 1～2h in 60～95 ℃, reaction finishes, and is cooled to 20～45 ℃ of polyacrylate dispersions that obtain core/shell structure.
Advantage of the present invention is: improved tensile strength and the high-low temperature resistant characteristic behind the polymer film forming.In complex, contain crosslinkable N-methylol and carboxylic group, can improve the adhesive force of polymer after crosslinked fabric.When providing carboxylic group with crosslinked ability by reasonable use acrylic acid addition, can make product pass through the thickening of alkali condition swelling, particularly use volatile alkali (as ammoniacal liquor) to make its thickening, and do not need to use again thickener, alkali volatilizees in drying course after the coating, and can not be retained on the fabric of coating.Add silane coupler, improve the weatherability of particle, anti-staining property and protect the light colour retention.By particle structure being carried out the orientation design, particularly design different monomer prescription of nucleocapsid and amount ratio, make it have certain flexibility at low temperatures, at high temperature has certain rigid again, like this, apparent is existing certain resistance to low temperature, and certain resistance to elevated temperatures is arranged again.Utilize the loudspeaker cloth lateral basin of this aqueous silicon-acrylate textile adhesive coating preparation, the high low temperature amplitude of variation of loudspeaker audio resonant frequency has greatly improved.
The specific embodiment
The specific embodiment of a kind of aqueous silicon-acrylate textile adhesive coating of the present invention and preparation method thereof below is provided.
Embodiment 1
The design of monomer prescription is as following table 1 and 2
The total prescription design of table 1
The design of table 2 monomer prescription
| Monomer | Weight | Nuclear | Shell |
| ??MMA | ??3.9 | ??3.9 | ??0 |
| ??BA | ??51.8 | ??23.8 | ??28.0 |
| ??EA | ??3.7 | ??0 | ??3.7 |
| ??VAc | ??5.5 | ??5.5 | ??0 |
| ??NMA | ??2.2 | ??0.9 | ??1.3 |
| ??AA | ??2.2 | ??0.9 | ??1.3 |
| ??A-171 | ??0.7 | ??0 | ??0.7 |
| Total amount | ??70.0 | ??35.0 | ??35.0 |
The technical process of preparation is:
(1), the preparation of pre-emulsion:
Press table 1 and table 2 prescription, with nuclear monomer I
1Slowly be added dropwise to successively among the aqueous solution II of 1/3 emulsifying agent while stirring, at room temperature stir fully and mix, emulsification 0.5 hour obtains nuclear monomer pre-emulsion I
1-1; In like manner, with shell monomer I
2Slowly be added dropwise to successively while stirring among the aqueous solution II of other 1/3 emulsifying agent, stir fully under the room temperature and mix, emulsification 0.5 hour obtains shell monomer pre-emulsion I
2-1;
(2), the preparation of seed emulsion:
The aqueous solution II that in the 500ml four-hole boiling flask of agitator, thermometer, condenser pipe is housed, adds residue 1/3 emulsifying agent, 1/2 nuclear monomer emulsion I
1-1,1/3 initiator solution III, about about 60 ℃ of temperature control, start stirring, in water bath with thermostatic control, be heated to about 65 ℃ and make it polymerization, about 20min of time after blue-fluorescence (meaning the generation of " seed ") occurring, splashes into remaining nuclear monomer emulsion I respectively synchronously, lentamente with two dropping funels
1-1 and 1/3 initiator solution III, about 90 ℃ of temperature controls, 1h dropwises, and continues to be incubated about 30min in 98 ℃, promptly gets seed emulsion;
(3), the polymerization of shell:
In above-mentioned seed emulsion, splash into shell monomer emulsion I respectively synchronously, lentamente by two dropping funels
2-1 and 1/3 remaining initiator solution III, about 90 ℃ of temperature controls, 1h dropwises, and continues insulation 1h in 98 ℃, and reaction finishes, and is cooled to 40～45 ℃ of polyacrylate dispersions that obtain core/shell structure.
Embodiment 2
The design of monomer prescription is as following table 3 and 4
The total prescription design of table 3
The design of table 4 monomer prescription
| Monomer | Weight | Nuclear | Shell |
| ??MMA | ??10.5 | ??9.0 | ??1.5 |
| ??BA | ??57.8 | ??36.8 | ??21.0 |
| ??EA | ??8.0 | ??2.0 | ??6.0 |
| ??NMA | ??3.0 | ??1.0 | ??2.0 |
| ??AA | ??3.0 | ??1.0 | ??2.0 |
| ??KH-570 | ??4.3 | ??0 | ??4.3 |
| Total amount | ??86.6 | ??49.8 | ??36.8 |
The preparation method is with embodiment 1.
Embodiment 3
The design of monomer prescription is as following table 5 and 6.
The total prescription design of table 5
The design of table 6 monomer prescription
| Monomer | Weight | Nuclear | Shell |
| ??MMA | ??5.0 | ??4.0 | ??1.0 |
| ??BA | ??51.0 | ??29.5 | ??21.5 |
| ??EA | ??7.0 | ??2.0 | ??5.0 |
| ??VAc | ??8.0 | ??5.5 | ??2.5 |
| ??NMA | ??2.5 | ??1.0 | ??1.5 |
| ??AA | ??2.5 | ??1.0 | ??1.5 |
| Total amount | ??76.0 | ??43.0 | ??33.0 |
The preparation method is with embodiment 1.
Performance test:
The aqueous silicon-acrylate textile adhesive coating of preparation, the ammoniacal liquor with 25% are regulated viscosity to 25000mPaS, directly are coated with the scraper type coating machine on base cloth, are coated with 6 layers by actual needs, and the frictioning amount is 60～75g/m
2, dry naturally.Select the cloth of same material for use, and adopt identical impregnation prescription,, prepare sound basin selvedge raw material, dry naturally, the frictioning cloth is prepared the sound basin under condition of the same race by same frictioning amount and frictioning mode.The resonant frequency of sound basin adopts the test of DF5996 resonant frequency tester, utilizes WGD4-0.2 high-low temperature test chamber simulated environment variations in temperature, and simulated determination is from-20 ℃ to 60 ℃ audio frequency resonant frequency f
0Variation.
Table 7 product audio frequency resonant frequency f
0With variation of temperature
As can be seen from the above results, in each temperature range, compare f of the present invention with domestic widely used like product
0Rate of change all improves to some extent, in temperature range-5～40 ℃, and f
0Rate of change reduce to 0.95 from 1.19 of like product, its rate of change is 80% of a like product.In temperature range-10～40 ℃, f
0Rate of change reduce to 1.22 from 1.62 of like product, its rate of change is 75% of a like product, referring to table 7.
Above result shows, utilizes the loudspeaker cloth lateral basin of aqueous silicon-acrylate textile adhesive coating preparation of the present invention, loudspeaker audio resonant frequency f
0High low temperature amplitude of variation have greatly improved.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention
Claims (3)
1, a kind of aqueous silicon-acrylate textile adhesive coating is characterized in that, the material component mass percent is:
The material component mass percent of solution I is:
Monomer 20～50%
The material component mass percent of solution II is:
Lauryl sodium sulfate SDS 0.5～5.0%
Alkylphenol polyoxyethylene OP-10 1.0～6.0%
Deionized water 30～60%
The material component mass percent of solution III is:
Ammonium persulfate APS 0.2～2.0%
The deionized water surplus.
2. a kind of aqueous silicon-acrylate textile adhesive coating according to claim 1 is characterized in that, in the described monomer, its weight percentages is:
Component weight nucleocapsid
Methacrylic acid MAA 0.5～5.0 0.5～5.0 0
Butyl acrylate BA 30～80 10～40 10～40
Ethyl acrylate EA 0.5～5.0 0 0.5～5.0
Vinylacetate VAc 1.0～10 1.0～10 0
N methacrylamide NMA 1.0～14.0 1.0～7.0 1.0～7.0
Acrylic acid AA 2.0～18 1.0～9.0 1.0～9.0
Vinyltrimethoxy silane A-171 0.5～5.0 0 0.5～5.0.
3. the preparation method of the described a kind of aqueous silicon-acrylate textile adhesive coating of claim 1 is characterized in that, concrete steps are:
(1), the preparation of pre-emulsion
Nuclear monomer I1 slowly is added dropwise among the aqueous solution II of 1/3 emulsifying agent while stirring successively, at room temperature stirs fully and mix, emulsification 0.5～2 hour obtains nuclear monomer pre-emulsion I1-1; In like manner, shell monomer I2 slowly is added dropwise among the aqueous solution II of other 1/3 emulsifying agent while stirring successively, stirs fully under the room temperature and mix, emulsification 0.5～2 hour obtains shell monomer pre-emulsion I2-1;
(2), the preparation of seed emulsion
Agitator is being housed, thermometer, the aqueous solution II that adds residue 1/3 emulsifying agent in the 500ml four-hole boiling flask of condenser pipe, 1/2 nuclear monomer emulsion I1-1,1/3 initiator solution III, about about 50～80 ℃ of temperature control, start stirring, in water bath with thermostatic control, be heated to 50～80 ℃ and make it polymerization, time 30～50min, after blue-fluorescence occurring, with two dropping funels respectively synchronously, splash into remaining nuclear monomer emulsion I1-1 and 1/3 initiator solution III lentamente, 60～90 ℃ of temperature controls, 1～2h dropwises, continue to be incubated about 30～90min in 60～95 ℃, promptly get seed emulsion;
(3), the polymerization of shell
In above-mentioned seed emulsion, splash into shell monomer emulsion I2-1 and 1/3 remaining initiator solution III respectively synchronously, lentamente by two dropping funels, 60～95 ℃ of temperature controls, 0.5-2h dropwise, continue insulation 1～2h in 60～95 ℃, reaction finishes, and is cooled to 20～45 ℃ of polyacrylate dispersions that obtain core/shell structure.
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| CN200910186073A CN101660276A (en) | 2009-09-21 | 2009-09-21 | Aqueous silicon-acrylate textile adhesive coating and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200801A (en) * | 2015-10-21 | 2015-12-30 | 江苏箭鹿毛纺股份有限公司 | Preparation method of skin care fabric capable of caring whole body skin |
| CN109180869A (en) * | 2018-09-26 | 2019-01-11 | 江门市金桥新材料有限公司 | A kind of silicone acrylic emulsion and its preparation process of ultra-fine grain diameter |
| CN117567912A (en) * | 2023-11-22 | 2024-02-20 | 江西科技师范大学 | Recyclable polyacrylate emulsion coating and preparation method and application thereof |
-
2009
- 2009-09-21 CN CN200910186073A patent/CN101660276A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200801A (en) * | 2015-10-21 | 2015-12-30 | 江苏箭鹿毛纺股份有限公司 | Preparation method of skin care fabric capable of caring whole body skin |
| CN109180869A (en) * | 2018-09-26 | 2019-01-11 | 江门市金桥新材料有限公司 | A kind of silicone acrylic emulsion and its preparation process of ultra-fine grain diameter |
| CN117567912A (en) * | 2023-11-22 | 2024-02-20 | 江西科技师范大学 | Recyclable polyacrylate emulsion coating and preparation method and application thereof |
| CN117567912B (en) * | 2023-11-22 | 2024-05-28 | 江西科技师范大学 | Recyclable polyacrylate emulsion coating and preparation method and application thereof |
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Open date: 20100303 |