CN105131176A - Glass fiber engineering plastic yarn film forming agent and preparation method thereof - Google Patents
Glass fiber engineering plastic yarn film forming agent and preparation method thereof Download PDFInfo
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- CN105131176A CN105131176A CN201510663346.4A CN201510663346A CN105131176A CN 105131176 A CN105131176 A CN 105131176A CN 201510663346 A CN201510663346 A CN 201510663346A CN 105131176 A CN105131176 A CN 105131176A
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Abstract
The invention discloses a glass fiber engineering plastic yarn film forming agent and a preparation method thereof. The film forming agent is a copolymer formed by polymerizing diacetone acrylamide, acrylic monomers, methacrylic acid monomers, methyl methacrylate and butyl acrylate monomers. The preparation method comprises the steps that 1, 7-9 parts of the diacetone acrylamide, 7-9 parts of the acrylic monomers, 7-9 parts of the methacrylic acid monomers, 120-140 parts of the methyl methacrylate, 220-240 parts of the butyl acrylate monomers and 14-25 parts of emulsifying agents are mixed evenly to obtain pre-emulsified liquid; 2, an emulsion polymerization reaction is performed on pre-emulsified liquid accounting for 3-10% of the mass of the pre-emulsified liquid obtained in the step 1 and initiating agents to obtain latex particle seeds; 3, the surplus pre-emulsified liquid is dropwise added in the latex particle seeds to enable the latex particle seeds to be largened, the initiating agents are added to remove the residual monomers, and the glass fiber engineering plastic yarn film forming agent is prepared. The film forming agent can be matched with other auxiliaries to prepare a glass fiber soakage agent which is good in glass fiber bundling property, capable of resisting high temperature and yellowing, good in heat stability and high in composite property.
Description
Technical field
The invention belongs to the technical field that glass fibre membrane-forming agent manufactures, be specifically related to a kind of glass fibre engineering plastics yarn membrane-forming agent and preparation method thereof.
Background technology
As everyone knows, the key of development of glass fibre new variety is treating compound technology, and in treating compound, important component is membrane-forming agent.Membrane-forming agent is except shielding to fiber, and it plays keying action to the stiffness, convergency, choppability, dispersiveness, impregnability etc. of glass fibre; Treating compound not only can make glass fibre better mate in chemical property with plastic basis material, greatly can also improve the value of the product of glass fibre simultaneously.
Polyacrylate Emulsion can give the good hardness of glass fibre, convergency, cutting, static resistance etc. as the membrane-forming agent of glass fiber infiltration agent, but the acrylic ester emulsion overwhelming majority domestic at present belongs to anionic, very bad with the cationic lubricant in glass fiber treating compound, static inhibitor matching, have a strong impact on the stability for the treatment of compound, directly affect the quality of glass fibre engineering plastics yarn thus.Further, engineering plastics yarn membrane-forming agent also will be considered and consistency between engineering plastic composite material and chemical bonding effect.Therefore, exploitation can give the fine good stiffness of engineering plastics, convergency, cutting, static resistance non-ionogenic polyacrylate copolymer emulsion economical and technically all very important.
Summary of the invention
For solving prior art Problems existing, the object of the present invention is to provide a kind of glass fibre engineering plastics yarn membrane-forming agent and preparation method thereof.
For achieving the above object, the invention provides a kind of glass fibre engineering plastics yarn membrane-forming agent, this membrane-forming agent is the multipolymer be polymerized by diacetone-acryloamide(DAA), Acrylic Acid Monomer, methacrylic acid monomer, methyl methacrylate, Butyl Acrylate Monomer.
Present invention also offers a kind of preparation method of glass fibre engineering plastics yarn membrane-forming agent, the method comprises the following steps:
(1) diacetone-acryloamide(DAA) 7-9 part, Acrylic Acid Monomer 7-9 part, methacrylic acid monomer 7-9 part, methyl methacrylate 120-140 part, Butyl Acrylate Monomer 220-240 part, emulsifying agent 14-25 part are mixed, obtain pre-emulsion, above number is mass parts;
(2) 3-10% of pre-emulsion quality and initiator are carried out emulsion polymerization, obtain latex particle seed;
(3) drip remaining pre-emulsion, make latex particle seed become large, add initiator and carry out residual monomer elimination, sieve after stirring, obtained glass fibre engineering plastics yarn membrane-forming agent.
Preferably, the emulsifying agent in step (1) is polyethenoxy ether class emulsifying agent.
Preferably, in step (2), at temperature 55-60 DEG C, emulsion polymerization is carried out.
Preferably, the initiator in step (2) and (3) is redox initiator, Potassium Persulphate or ammonium persulphate.
Preferably, in step (3), at temperature 60-65 DEG C, remaining pre-emulsion is dripped.
Preferably, in step (3), pre-emulsion drips off rear insulation 60-120min.
Preferably, in step (3), cross 200 mesh sieves, obtained glass fibre engineering plastics yarn membrane-forming agent.
Beneficial effect of the present invention is: membrane-forming agent of the present invention can coordinate with other auxiliary agents, prepares good, the high temperature resistant non yellowing of glass fiber bundling, Heat stability is good, glass fiber infiltration agent that composite property is high.The preparation method of membrane-forming agent of the present invention uses acrylic compounds and cross-linking monomer to carry out emulsion polymerization, prepares the membrane-forming agent with good, the high temperature resistant non yellowing of glass fiber bundling.
Embodiment
Below in conjunction with embodiment, in detail explanation is explained to the present invention.
Embodiment 1
Letex polymerization is carried out in four mouthfuls of reaction flasks that agitator, reflux exchanger, thermometer and dropping funnel are housed.189g (10.5mol) deionized water, 0.68g (0.005mol) sodium acetate trihydrate are dropped in reaction flask; 117g (6.5mol) deionized water, 6g (0.0135mol) alkyl polyoxyethylene ether, 8g (0.0176mol) Soxylat A 25-7 sorbitan monostearate, 7g (0.0414mol) diacetone-acryloamide(DAA), 7g (0.097mol) Acrylic Acid Monomer, 7g (0.0814mol) methacrylic acid monomer, 120g (1.198mol) methyl methacrylate, 220g (1.716mol) Butyl Acrylate Monomer are dropped into and drip in bottle, obtained pre-emulsion, stirs and mixes half an hour.
Reaction flask stirs and is warming up to 55 DEG C, drip the pre-emulsion of 3%, add 0.108g (0.0012mol) tertbutyl peroxide, 0.185g (0.0012mol) sodium hydrosulfite, 3% pre-emulsion 20min drips off simultaneously, then is incubated 30min and carries out initial stage polyreaction.
After temperature of reaction kettle is stable, start dropping residue 97% pre-emulsion, 0.54g (0.006mol) tertbutyl peroxide, 0.924g (0.006mol) sodium hydrosulfite simultaneously and carry out polyreaction, continuous dropping 4 hours, temperature controls at 60 DEG C.Dropwise insulation 1 hour, temperature controls at 60 DEG C.Then add 0.18g (0.002mol) tertbutyl peroxide and 0.308g (0.002mol) sodium hydrosulfite carries out residual monomer elimination, after stirring half an hour, be cooled to less than 40 DEG C 200 order net filtration dischargings.
This membrane-forming agent 1 rotor viscosity is 41 centipoises, pH value 4.91, effective size of grain 350nm.
Embodiment 2
Letex polymerization is carried out in four mouthfuls of reaction flasks that agitator, reflux exchanger, thermometer and dropping funnel are housed.195g (10.83mol) deionized water, 1.2g (0.0088mol) sodium acetate trihydrate are dropped in reaction flask; 120g (6.67mol) deionized water, 8g (0.018mol) alkyl polyoxyethylene ether, 10g (0.022mol) Soxylat A 25-7 sorbitan monostearate, 8g (0.047mol) diacetone-acryloamide(DAA), 8g (0.111mol) Acrylic Acid Monomer, 8g (0.093mol) methacrylic acid monomer, 120g (1.198mol) methyl methacrylate and 236g (1.841mol) Butyl Acrylate Monomer being dropped into drips in bottle, and obtained pre-emulsion stirs and mixes half an hour.
Reaction flask stirs and is warming up to 55 DEG C, drip the pre-emulsion of 3%, add 0.126g (0.0014mol) tertbutyl peroxide, 0.216g (0.0014mol) sodium hydrosulfite, 3% pre-emulsion 20min drips off simultaneously, then is incubated 30min and carries out initial stage polyreaction.After temperature of reaction kettle is stable, start dropping residue 97% pre-emulsion, 0.559g (0.0062mol) tertbutyl peroxide, 0.96g (0.0062mol) sodium hydrosulfite simultaneously and carry out polyreaction, continuous dropping 4 hours, temperature controls at 60 DEG C.Dropwise insulation 1 hour, temperature controls at 60 DEG C.Then add 0.198g (0.0022mol) tertbutyl peroxide and 0.34g (0.0022mol) sodium hydrosulfite carries out residual monomer elimination, after stirring half an hour, be cooled to less than 40 DEG C 200 order net filtration dischargings.
This membrane-forming agent 2 rotor viscosity is 49 centipoises, pH value 4.89, effective size of grain 328nm.
Embodiment 3
Letex polymerization is carried out in four mouthfuls of reaction flasks that agitator, reflux exchanger, thermometer and dropping funnel are housed.198g (11.00mol) deionized water, 1.36g (0.010mol) sodium acetate trihydrate are dropped in reaction flask; 126g (7.00mol) deionized water, 10g (0.0225mol) alkyl polyoxyethylene ether, 15g (0.033mol) Soxylat A 25-7 sorbitan monostearate, 9g (0.053mol) diacetone-acryloamide(DAA), 9g (0.125mol) Acrylic Acid Monomer, 9g (0.105mol) methacrylic acid monomer, 140g (1.398mol) methyl methacrylate and 240g (1.873mol) Butyl Acrylate Monomer being dropped into drips in bottle, obtained pre-emulsion, stirs and mixes half an hour.
Reaction flask stirs and is warming up to 55 DEG C, drip the pre-emulsion of 3%, add 0.189g (0.0021mol) tertbutyl peroxide, 0.324g (0.0021mol) sodium hydrosulfite, 5% pre-emulsion 20min drips off simultaneously, then is incubated 30min and carries out initial stage polyreaction.After temperature of reaction kettle is stable, start dropping residue 97% pre-emulsion, 0.703g (0.0078mol) tertbutyl peroxide, 1.20g (0.0078mol) sodium hydrosulfite simultaneously and carry out polyreaction, continuous dropping 4 hours, temperature controls at 60 DEG C.Dropwise insulation 1 hour, temperature controls at 60 DEG C.Then add 0.27g (0.003mol) tertbutyl peroxide and 0.462g (0.003mol) sodium hydrosulfite carries out residual monomer elimination, after stirring half an hour, be cooled to less than 40 DEG C 200 order net filtration dischargings.
This membrane-forming agent 3 rotor viscosity is 270 centipoises, pH value 4.98, effective size of grain 349nm.
Embodiment 4
Letex polymerization is carried out in four mouthfuls of reaction flasks that agitator, reflux exchanger, thermometer and dropping funnel are housed.189g (10.5mol) deionized water, 0.68g (0.005mol) sodium acetate trihydrate are dropped in reaction flask; 117g (6.5mol) deionized water, 6g (0.0135mol) alkyl polyoxyethylene ether, 8g (0.0176mol) Soxylat A 25-7 sorbitan monostearate, 7g (0.0414mol) diacetone-acryloamide(DAA), 7g (0.097mol) Acrylic Acid Monomer, 7g (0.0814mol) methacrylic acid monomer, 120g (1.199mol) methyl methacrylate, 220g (1.716mol) Butyl Acrylate Monomer are dropped into and drip in bottle, obtained pre-emulsion, stirs and mixes half an hour.
Reaction flask stirs and is warming up to 58 DEG C, drip the pre-emulsion of 3%, add 0.108g (0.0012mol) tertbutyl peroxide, 0.185g (0.0012mol) sodium hydrosulfite, 5% pre-emulsion 30min drips off simultaneously, then is incubated 40min and carries out initial stage polyreaction.
After temperature of reaction kettle is stable, start dropping residue 95% pre-emulsion, 0.54g (0.006mol) tertbutyl peroxide, 0.924g (0.006mol) sodium hydrosulfite simultaneously and carry out polyreaction, continuous dropping 4.5 hours, temperature controls at 62 DEG C.Dropwise insulation 1.5 hours, temperature controls at 62 DEG C.Then add 0.18g (0.002mol) tertbutyl peroxide and 0.308g (0.002mol) sodium hydrosulfite carries out residual monomer elimination, after stirring half an hour, be cooled to less than 40 DEG C 200 order net filtration dischargings.
This membrane-forming agent 4 rotor viscosity is 20 centipoises, pH value 4.78, effective size of grain 323nm.
Embodiment 5
Letex polymerization is carried out in four mouthfuls of reaction flasks that agitator, reflux exchanger, thermometer and dropping funnel are housed.195g (10.83mol) deionized water, 1.2g (0.0088mol) sodium acetate trihydrate are dropped in reaction flask; 120g (6.67mol) deionized water, 8g (0.018mol) alkyl polyoxyethylene ether, 10g (0.022mol) Soxylat A 25-7 sorbitan monostearate, 8g (0.047mol) diacetone-acryloamide(DAA), 8g (0.111mol) Acrylic Acid Monomer, 8g (0.093mol) methacrylic acid monomer, 120g (1.198mol) methyl methacrylate and 236g (1.841mol) Butyl Acrylate Monomer being dropped into drips in bottle, and obtained pre-emulsion stirs and mixes half an hour.
Reaction flask stirs and is warming up to 58 DEG C, and drip the pre-emulsion of 5%, add 0.378g (0.0014mol) Potassium Persulphate, 3% pre-emulsion 20min drips off simultaneously, then is incubated 30min and carries out initial stage polyreaction.After temperature of reaction kettle is stable, start dropping residue 95% pre-emulsion, 1.08g (0.004mol) Potassium Persulphate simultaneously and carry out polyreaction, drip 4 hours continuously, temperature controls at 60 DEG C.Dropwise insulation 1 hour, temperature controls at 60 DEG C.Then add 0.54g (0.002mol) Potassium Persulphate and carry out residual monomer elimination, after stirring half an hour, be cooled to less than 40 DEG C 200 order net filtration dischargings.
This membrane-forming agent 5 rotor viscosity is 40 centipoises, pH value 4.91, effective size of grain 400nm.
Embodiment 6
Letex polymerization is carried out in four mouthfuls of reaction flasks that agitator, reflux exchanger, thermometer and dropping funnel are housed.198g (11.00mol) deionized water, 1.36g (0.010mol) sodium acetate trihydrate are dropped in reaction flask; 126g (7.00mol) deionized water, 10g (0.0225mol) alkyl polyoxyethylene ether, 15g (0.033mol) Soxylat A 25-7 sorbitan monostearate, 9g (0.053mol) diacetone-acryloamide(DAA), 9g (0.125mol) Acrylic Acid Monomer, 9g (0.105mol) methacrylic acid monomer, 140g (1.398mol) methyl methacrylate and 240g (1.873mol) Butyl Acrylate Monomer being dropped into drips in bottle, obtained pre-emulsion, stirs and mixes half an hour.
Reaction flask stirs and is warming up to 60 DEG C, and drip the pre-emulsion of 10%, add 0.479g (0.0021mol) ammonium persulphate, 5% pre-emulsion 30min drips off simultaneously, then is incubated 60min and carries out initial stage polyreaction.After temperature of reaction kettle is stable, start dropping residue 90% pre-emulsion, 1.566g (0.0058mol) ammonium persulphate simultaneously and carry out polyreaction, drip 5 hours continuously, temperature controls at 65 DEG C.Dropwise insulation 2 hours, temperature controls at 65 DEG C.Then add 0.684g (0.003mol) ammonium persulphate and carry out residual monomer elimination, after stirring half an hour, be cooled to less than 40 DEG C 200 order net filtration dischargings.
This membrane-forming agent 6 rotor viscosity is 100 centipoises, pH value 4.92, effective size of grain 451nm.
Comparative example uses the polyacrylate dispersion bought as membrane-forming agent.
The membrane-forming agent respectively prepared by 3wt% embodiment of the present invention 1-6 or the membrane-forming agent of comparative example, 0.05% acetic acid, the white oil of 0.5%, the KH-550 silane coupling agent of 0.8% and 95.65wt% water mixing, obtain treating compound.The treating compound of above-mentioned preparation is coated on engineering plastics fiberglass surfacing, obtains the glass fibre after treating compound process.Detect the glass fibre performance of membrane-forming agent prepared by embodiment of the present invention 1-6 and comparative example, result is as shown in table 1.
The glass fibre performance test results of membrane-forming agent prepared by table 1 the present invention and comparative example
| Stiffness | Convergency | Cutting property | Thermostability | Tension intensity | |
| Embodiment 1 | 155 | Good | 10 | Good | 0.42MPa |
| Embodiment 2 | 157 | Good | 9 | Good | 0.39MPa |
| Embodiment 3 | 158 | Good | 8 | Good | 0.40MPa |
| Embodiment 4 | 156 | Good | 9 | Good | 0.41MPa |
| Embodiment 5 | 153 | Good | 10 | Good | 0.45MPa |
| Embodiment 6 | 154 | Good | 7 | Good | 0.40MPa |
| Comparative example | 132 | Generally | 7 | Generally | 0.32MPa |
In table 1, the numerical value of stiffness is larger, represents that stiffness is better; Cutting property numerical value is larger, represents that cutting is better; Tension intensity is larger, represents that pulling force characteristic is better.Can be obtained by table 1, the performance of the membrane-forming agent that preparation method of the present invention obtains is better than the Polyacrylate Emulsion in comparative example.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.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 (8)
1. a glass fibre engineering plastics yarn membrane-forming agent, is characterized in that, the multipolymer that this membrane-forming agent is formed through polymerization by diacetone-acryloamide(DAA), Acrylic Acid Monomer, methacrylic acid monomer, methyl methacrylate and Butyl Acrylate Monomer.
2. a preparation method for glass fibre engineering plastics yarn membrane-forming agent, it is characterized in that, the method comprises the following steps:
(1) diacetone-acryloamide(DAA) 7-9 part, Acrylic Acid Monomer 7-9 part, methacrylic acid monomer 7-9 part, methyl methacrylate 120-140 part, Butyl Acrylate Monomer 220-240 part are mixed with emulsifying agent 14-25 part, obtain pre-emulsion, above number is mass parts;
(2) 3-10% and the initiator of getting step pre-emulsion quality carry out emulsion polymerization, obtain latex particle seed;
(3) remaining pre-emulsion being added dropwise to latex particle seed makes it become large, then adds initiator and carry out residual monomer elimination, sieves after stirring, obtained glass fibre engineering plastics yarn membrane-forming agent.
3. the preparation method of glass fibre engineering plastics yarn membrane-forming agent according to claim 2, it is characterized in that, the emulsifying agent in step (1) is polyethenoxy ether class emulsifying agent.
4. the preparation method of glass fibre engineering plastics yarn membrane-forming agent according to claim 2, is characterized in that, in step (2), at temperature 55-60 DEG C, carry out emulsion polymerization.
5. the preparation method of glass fibre engineering plastics yarn membrane-forming agent according to claim 2, is characterized in that, the initiator in step (2) and (3) is redox initiator, Potassium Persulphate or ammonium persulphate.
6. the preparation method of glass fibre engineering plastics yarn membrane-forming agent according to claim 2, is characterized in that, in step (3), at temperature 60-65 DEG C, drip remaining pre-emulsion.
7. the preparation method of glass fibre engineering plastics yarn membrane-forming agent according to claim 2, is characterized in that, in step (3), pre-emulsion drips off rear insulation 60-120min.
8. the preparation method of glass fibre engineering plastics yarn membrane-forming agent according to claim 2, is characterized in that, in step (3), crosses 200 mesh sieves, obtained glass fibre engineering plastics yarn membrane-forming agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116375361A (en) * | 2023-03-15 | 2023-07-04 | 重庆国际复合材料股份有限公司 | Active group-rich water-soluble resin film forming agent for glass fibers and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH06279707A (en) * | 1993-03-25 | 1994-10-04 | Mitsubishi Yuka Badische Co Ltd | Water-base undercoating agent for inorganic porous base material |
| CN103524669A (en) * | 2013-11-04 | 2014-01-22 | 常州天马集团有限公司（原建材二五三厂） | Acrylate emulsion and preparing method thereof |
| US20140323608A1 (en) * | 2011-12-15 | 2014-10-30 | Celanese Emulsions Gmbh | Polymer dispersions |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06279707A (en) * | 1993-03-25 | 1994-10-04 | Mitsubishi Yuka Badische Co Ltd | Water-base undercoating agent for inorganic porous base material |
| US20140323608A1 (en) * | 2011-12-15 | 2014-10-30 | Celanese Emulsions Gmbh | Polymer dispersions |
| CN103524669A (en) * | 2013-11-04 | 2014-01-22 | 常州天马集团有限公司（原建材二五三厂） | Acrylate emulsion and preparing method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116375361A (en) * | 2023-03-15 | 2023-07-04 | 重庆国际复合材料股份有限公司 | Active group-rich water-soluble resin film forming agent for glass fibers and preparation method thereof |
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