CN102352203B - Preparation method of novel adhesive for energy-saving lamps - Google Patents
Preparation method of novel adhesive for energy-saving lamps Download PDFInfo
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- CN102352203B CN102352203B CN2011102692874A CN201110269287A CN102352203B CN 102352203 B CN102352203 B CN 102352203B CN 2011102692874 A CN2011102692874 A CN 2011102692874A CN 201110269287 A CN201110269287 A CN 201110269287A CN 102352203 B CN102352203 B CN 102352203B
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Abstract
The invention discloses a preparation method of an adhesive for energy-saving lamps. The adhesive prepared by the existing method has the defect of high price and can easily lose effect. The method disclosed by the invention comprises the following steps: respectively preparing an acrylate modified polyvinyl acetate emulsion and an organosilicon emulsion; evenly stirring the acrylate modified polyvinyl acetate emulsion, the organosilicon emulsion and polyethylene glycol propyltrimethoxy silane; adding a filler powder; and mechanically mixing to obtain a white viscous heat-resistant adhesive for energy-saving lamps. 10-50 parts of organosilicon emulsion, 0.5-1 part of polyethylene glycol propyltrimethoxy silicon and 200-300 parts of filler powder are added to every 100 parts of acrylate modified polyvinyl acetate emulsion. The method disclosed by the invention has simpler technique, and can implement industrial production. By compounding the acrylate modified polyvinyl acetate emulsion and the organosilicon emulsion, the prepared adhesive for energy-saving lamps has the advantages of high adhesive strength, high heat resistance, high aging resistance and the like.
Description
Technical field
The invention belongs to the chemical material technical field, be specifically related to a kind of preparation method of electricity-saving lamp caking agent.
Background technology
Electric consumption on lighting accounts for 12 ﹪ of whole society's electricity consumption total amount, and along with the raising of Economic development and living standards of the people, power consumption also can further increase.Electricity-saving lamp many 4～6 times of work-ing life is a kind of efficient energy-saving lighting product than ordinary incandescent lamp economize on electricity 60～80 ﹪, and China promotes electricity-saving lamp and uses as the energy-conserving product of state key development.According to the manufacture craft of electricity-saving lamp, in electricity-saving lamp production, must use caking agent to the electricity-saving lamp plastic component and the bonding between the tube glass is housed.At present the most of electricity-saving lamp of China manufacturer uses white glues, yellow glue to have high-temperature discoloration, phenomenon such as ftracture, come unstuck, though and the silicone sealant adhesive property is better, have price problem high, that lost efficacy easily.A kind of electricity-saving lamp of the medium invention of Xu Zhi is with caking agent and preparation method thereof (CN101481592A); Trevira, vinylon, tynex, polyacrylonitrile fibre, spun glass, wynene, lignin fibre etc. are added in proposition in benzene emulsion, acrylate and vinyl acetate emulsion, polyvinyl acetate emulsion or Vinyl Acetate Copolymer-vac emulsion, only the resistance to cleavage to tackiness agent has some improvement.
Summary of the invention
The object of the invention is exactly the deficiency to prior art, and the preparation method of a kind of electricity-saving lamp with caking agent is provided.
For realizing goal of the invention, the present invention adopts following technical scheme:
Prepare acrylate modified aqueous polyvinyl acetate emulsion and organic silicon emulsion at first respectively; Then acrylate modified aqueous polyvinyl acetate emulsion, organic silicon emulsion and polyoxyethylene glycol propyl trimethoxy silicane are stirred; Carry out mechanically mixing after adding the filler powder, promptly get white thickness electricity-saving lamp and use tackiness agent.More than the parts by weight of each component be:
Acrylate modified aqueous polyvinyl acetate emulsion 100
Organic silicon emulsion 10～50
Polyoxyethylene glycol propyl trimethoxy silicane 0.5～1
Filler powder 200～300
The concrete grammar for preparing acrylate modified aqueous polyvinyl acetate emulsion is:
1. be that 10～30 parts Z 150PH and 150～200 parts deionized water add in the reaction kettle with parts by weight, reaction kettle is warming up to 70～90 ℃, is stirred to Z 150PH and all dissolves;
2. reaction kettle is cooled to 50～60 ℃, and adding parts by weight is 1～3 part tensio-active agent OP-1O, the X 2073 that parts by weight are 1～3 part, the Vinyl Acetate Monomer that parts by weight are 70～100 parts; Be warming up to 70～75 ℃ after stirring, the adding parts by weight are 2～5 parts initiator solution, stir; Continue to stir, in 3～4 hours, evenly splashing into parts by weight is 10～20 parts of acrylate monomers, and adding total amount for 3～4 times with the time-division is 5～10 parts initiator solution, forms intermediate liquid;
3. be warming up to 80～85 ℃, be incubated 0.5～1 hour, be cooled to then use NaHCO below 50 ℃
3It is 6～7 that the aqueous solution is regulated intermediate liquid pH value, and the adding parts by weight are 5～15 parts Witcizer 300, stir the postcooling discharging;
The concrete grammar of preparation organic silicon emulsion is:
1. be that 250～300 parts deionized water, 80～100 parts octamethylcyclotetrasiloxane, 30～60 parts emulsifier mix are even with parts by weight, homogeneous obtains pre-emulsion in high pressure homogenizer;
2. pre-emulsion is poured in the reactor drum, the adding parts by weight are 30～50 parts Witco 1298 Soft Acid, are 65～85 ℃ in temperature and react 2～4 hours down, form milk sap;
3. be cooled to use NaHCO below 50 ℃
3It is 6～7 that the aqueous solution is regulated milk sap pH value, stirs the postcooling discharging.
Described filler powder is one or more in light calcium carbonate, water-ground limestone, Natural manganese dioxide, aluminum oxide or the talcum powder;
Described initiator solution be weight percentage Potassium Persulphate or the ammonium persulfate aqueous solution of 10～20 ﹪.
Described acrylate monomer be ethyl propenoate, Bing Xisuandingzhi and 2-Hydroxy ethyl acrylate in one or more.
Described emulsifying agent is X 2073 or sodium lauryl sulphate.
The inventive method technology is simple relatively, can realize suitability for industrialized production.This method is compound through acrylate modified aqueous polyvinyl acetate emulsion and organic silicon emulsion are carried out, and not only cohesive strength is high with tackiness agent for the electricity-saving lamp of preparation, and over-all propertieies such as thermotolerance and stability to aging are also better simultaneously.
Embodiment
Below through embodiment the present invention is described further.
Embodiment 1.
Prepare acrylate modified aqueous polyvinyl acetate emulsion: at first the Z 150PH of 10kg and the deionized water of 200kg are added in the reaction kettle, reaction kettle is warming up to 70 ℃, is stirred to Z 150PH and all dissolves; Then reaction kettle is cooled to 50 ℃; Add the tensio-active agent OP-1O of 1kg, the X 2073 of 1kg, the Vinyl Acetate Monomer of 70kg, be warming up to 70 ℃ after stirring, the weight percent that adds 2kg is the persulfate aqueous solution of 20 ﹪; Stir; In 3 hours, evenly splash into Bing Xisuandingzhi and the 10kg ethyl propenoate mix monomer of 10kg then, the weight percent of adding 5kg with the time-division for 3 times is the persulfate aqueous solution of 20 ﹪, forms intermediate liquid; Be warming up to 80 ℃, be incubated 1 hour, be cooled to then use NaHCO below 50 ℃
3It is 6 that the aqueous solution is regulated intermediate liquid pH value, adds the Witcizer 300 of 5kg, stirs the postcooling discharging.
The preparation organic silicon emulsion: at first the deionized water of 250kg, the octamethylcyclotetrasiloxane of 100kg, the X 2073 of 40kg are mixed, homogeneous obtains pre-emulsion in high pressure homogenizer; Then pre-emulsion is poured in the reactor drum, added the Witco 1298 Soft Acid of 30kg, be 65 ℃ in temperature and reacted 4 hours down, form milk sap; Be cooled to use NaHCO below 50 ℃
3It is 6 that the aqueous solution is regulated milk sap pH value, stirs the postcooling discharging.
After getting the acrylate modified aqueous polyvinyl acetate emulsion of 100kg, 30kg organic silicon emulsion and 0.5kg polyoxyethylene glycol propyl trimethoxy silicane and stirring, add 250kg light calcium carbonate mechanically mixing and promptly get white thickness electricity-saving lamp and use heat-resistant adhesive.
Embodiment 2.
Prepare acrylate modified aqueous polyvinyl acetate emulsion: at first the Z 150PH of 30kg and the deionized water of 150kg are added in the reaction kettle, reaction kettle is warming up to 90 ℃, is stirred to Z 150PH and all dissolves; Then reaction kettle is cooled to 60 ℃; Add the tensio-active agent OP-1O of 3kg, the X 2073 of 3kg, the Vinyl Acetate Monomer of 100kg, be warming up to 75 ℃ after stirring, the weight percent that adds 5kg is the ammonium persulfate aqueous solution of 10 ﹪; Stir; In 4 hours, evenly splash into the Butyl Acrylate Monomer of 10kg then, the weight percent of adding 10kg with the time-division for 4 times is the ammonium persulfate aqueous solution of 20 ﹪, forms intermediate liquid; Be warming up to 85 ℃, be incubated 0.5 hour, be cooled to then use NaHCO below 50 ℃
3It is 7 that the aqueous solution is regulated intermediate liquid pH value, adds the Witcizer 300 of 15kg, stirs the postcooling discharging.
The preparation organic silicon emulsion: at first the deionized water of 300kg, the octamethylcyclotetrasiloxane of 80kg, the sodium lauryl sulphate of 60kg are mixed, homogeneous obtains pre-emulsion in high pressure homogenizer; Then pre-emulsion is poured in the reactor drum, added the Witco 1298 Soft Acid of 50kg, be 85 ℃ in temperature and reacted 2 hours down, form milk sap; Be cooled to use NaHCO below 50 ℃
3It is 7 that the aqueous solution is regulated milk sap pH value, stirs the postcooling discharging.
After getting the acrylate modified aqueous polyvinyl acetate emulsion of 100kg, 50kg organic silicon emulsion and 1kg polyoxyethylene glycol propyl trimethoxy silicane and stirring, add 100kg light calcium carbonate, 150kg water-ground limestone and 50kg Natural manganese dioxide mechanically mixing and promptly get white thickness electricity-saving lamp and use heat-resistant adhesive.
Embodiment 3.
Prepare acrylate modified aqueous polyvinyl acetate emulsion: at first the Z 150PH of 20kg and the deionized water of 180kg are added in the reaction kettle, reaction kettle is warming up to 80 ℃, is stirred to Z 150PH and all dissolves; Then reaction kettle is cooled to 55 ℃; Add the tensio-active agent OP-1O of 2kg, the X 2073 of 2kg, the Vinyl Acetate Monomer of 80kg, be warming up to 72 ℃ after stirring, the weight percent that adds 3kg is the persulfate aqueous solution of 15 ﹪; Stir; In 3.5 hours, evenly splash into 2-Hydroxy ethyl acrylate and the 10kg ethyl propenoate mix monomer of 5kg then, the weight percent of adding 8kg with the time-division for 3 times is the persulfate aqueous solution of 15 ﹪, forms intermediate liquid; Be warming up to 82 ℃, be incubated 0.8 hour, be cooled to then use NaHCO below 50 ℃
3It is 6.5 that the aqueous solution is regulated intermediate liquid pH value, adds the Witcizer 300 of 10kg, stirs the postcooling discharging.
The preparation organic silicon emulsion: at first the deionized water of 280kg, the octamethylcyclotetrasiloxane of 90kg, the X 2073 of 30kg are mixed, homogeneous obtains pre-emulsion in high pressure homogenizer; Then pre-emulsion is poured in the reactor drum, added the Witco 1298 Soft Acid of 40kg, be 75 ℃ in temperature and reacted 3 hours down, form milk sap; Be cooled to use NaHCO below 50 ℃
3It is 6.5 that the aqueous solution is regulated milk sap pH value, stirs the postcooling discharging.
After getting the acrylate modified aqueous polyvinyl acetate emulsion of 100kg, 10kg organic silicon emulsion and 0.8kg polyoxyethylene glycol propyl trimethoxy silicane and stirring, add 100kg water-ground limestone, 50kg aluminum oxide and 50kg talcum powder mechanically mixing and promptly get white thickness electricity-saving lamp and use heat-resistant adhesive.
Embodiment 4.
Prepare acrylate modified aqueous polyvinyl acetate emulsion: at first the Z 150PH of 15kg and the deionized water of 160kg are added in the reaction kettle, reaction kettle is warming up to 85 ℃, is stirred to Z 150PH and all dissolves; Then reaction kettle is cooled to 58 ℃; Add the tensio-active agent OP-1O of 1.5kg, the X 2073 of 2.5kg, the Vinyl Acetate Monomer of 90kg, be warming up to 75 ℃ after stirring, the weight percent that adds 4kg is the ammonium persulfate aqueous solution of 15 ﹪; Stir; In 4 hours, evenly splash into the vinylformic acid of 5kg and the Bing Xisuandingzhi mix monomer of 5kg then, the weight percent of adding 6kg with the time-division for 3 times is the ammonium persulfate aqueous solution of 15 ﹪, forms intermediate liquid; Be warming up to 83 ℃, be incubated 1 hour, be cooled to then use NaHCO below 50 ℃
3It is 7 that the aqueous solution is regulated intermediate liquid pH value, adds the Witcizer 300 of 7kg, stirs the postcooling discharging.
The preparation organic silicon emulsion: at first the deionized water of 260kg, the octamethylcyclotetrasiloxane of 95kg, the X 2073 of 35kg are mixed, homogeneous obtains pre-emulsion in high pressure homogenizer; Then pre-emulsion is poured in the reactor drum, added the Witco 1298 Soft Acid of 45kg, be 70 ℃ in temperature and reacted 3 hours down, form milk sap; Be cooled to use NaHCO below 50 ℃
3It is 7 that the aqueous solution is regulated milk sap pH value, stirs the postcooling discharging.
After getting the acrylate modified aqueous polyvinyl acetate emulsion of 100kg, 40kg organic silicon emulsion and 0.6kg polyoxyethylene glycol propyl trimethoxy silicane and stirring, add 150kg water-ground limestone, 50kg aluminum oxide and 80kg talcum powder mechanically mixing and promptly get white thickness electricity-saving lamp and use heat-resistant adhesive.
Claims (5)
1. the preparation method of an electricity-saving lamp caking agent; It is characterized in that this method prepares acrylate modified aqueous polyvinyl acetate emulsion and organic silicon emulsion at first respectively; Then acrylate modified aqueous polyvinyl acetate emulsion, organic silicon emulsion and polyoxyethylene glycol propyl trimethoxy silicane are stirred in proportion; Carry out mechanically mixing after adding the filler powder, promptly get white thickness electricity-saving lamp and use tackiness agent; More than the parts by weight of each component be:
Acrylate modified aqueous polyvinyl acetate emulsion 100
Organic silicon emulsion 10～50
Polyoxyethylene glycol propyl trimethoxy silicane 0.5～1
Filler powder 200～300
The concrete grammar for preparing acrylate modified aqueous polyvinyl acetate emulsion thing is:
1. be that 10～30 parts Z 150PH and 150～200 parts deionized water add in the reaction kettle with parts by weight, reaction kettle is warming up to 70～90 ℃, is stirred to Z 150PH and all dissolves;
2. reaction kettle is cooled to 50～60 ℃, and adding parts by weight is 1～3 part tensio-active agent OP-10, the X 2073 that parts by weight are 1～3 part, the Vinyl Acetate Monomer that parts by weight are 70～100 parts; Be warming up to 70～75 ℃ after stirring, the adding parts by weight are 2～5 parts initiator solution, stir; Continue to stir, evenly splashing into parts by weight in 3～4 hours is 10～20 parts of acrylate monomers, and adding total amount for 3～4 times with the time-division is 5～10 parts initiator solution, forms intermediate liquid;
3. be warming up to 80～85 ℃, be incubated 0.5～1 hour, be cooled to then use NaHCO below 50 ℃
3It is 6～7 that the aqueous solution is regulated intermediate liquid pH value, and the adding parts by weight are 5～15 parts Witcizer 300, stir the postcooling discharging;
The concrete grammar of preparation organic silicon emulsion is:
1. be that 250～300 parts deionized water, 80～100 parts octamethylcyclotetrasiloxane, 30～60 parts emulsifier mix are even with parts by weight, homogeneous obtains pre-emulsion in high pressure homogenizer;
2. pre-emulsion is poured in the reactor drum, the adding parts by weight are 30～50 parts Witco 1298 Soft Acid, are 65～85 ℃ in temperature and react 2～4 hours down, form milk sap;
3. be cooled to use NaHCO below 50 ℃
3It is 6～7 that the aqueous solution is regulated milk sap pH value, stirs the postcooling discharging.
2. the preparation method of a kind of electricity-saving lamp caking agent as claimed in claim 1 is characterized in that: described filler powder is one or more in light calcium carbonate, water-ground limestone, Natural manganese dioxide, aluminum oxide or the talcum powder.
3. the preparation method of a kind of electricity-saving lamp caking agent as claimed in claim 1 is characterized in that: described initiator solution be weight percentage Potassium Persulphate or the ammonium persulfate aqueous solution of 10～20 ﹪.
4. the preparation method of a kind of electricity-saving lamp caking agent as claimed in claim 1 is characterized in that: described acrylate monomer be ethyl propenoate, Bing Xisuandingzhi and 2-Hydroxy ethyl acrylate in one or more.
5. the preparation method of a kind of electricity-saving lamp caking agent as claimed in claim 1 is characterized in that: described emulsifying agent is X 2073 or sodium lauryl sulphate.
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| CN2011102692874A CN102352203B (en) | 2011-09-13 | 2011-09-13 | Preparation method of novel adhesive for energy-saving lamps |
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| CN108178993A (en) * | 2018-01-29 | 2018-06-19 | 佛山市三水永发洁具有限公司 | A kind of mirror sealed binder |
| CN108148531A (en) * | 2018-01-29 | 2018-06-12 | 佛山市三水永发洁具有限公司 | A kind of preparation method of mirror sealed binder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100575439C (en) * | 2006-04-17 | 2009-12-30 | 张恩天 | Environment friendly heat resistant adhesive for energy saving lamp holder |
| DE102008008421B4 (en) * | 2008-02-09 | 2014-06-26 | Celanese Emulsions Gmbh | Process for the preparation of polymer dispersions, the dispersions containing them and their use |
| CN101481592A (en) * | 2009-01-16 | 2009-07-15 | 上海漠王复合材料科技有限公司 | Anti-cracking adhesive for energy-saving lamp and preparation thereof |
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Effective date of registration: 20131018 Address after: 226600 No. 188, chemical Avenue, chemical industry zone, Haian hi tech Zone, Jiangsu Patentee after: Nantong Guangtai Biochemical Product Co., Ltd. Address before: Hangzhou City, Zhejiang province 310018 Xiasha Higher Education Park No. 2 street Patentee before: Hangzhou Electronic Science and Technology Univ |