CN101781535B - Solvent based flame-retardant pressure-sensitive binding agent and preparation method thereof - Google Patents
Solvent based flame-retardant pressure-sensitive binding agent and preparation method thereof Download PDFInfo
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- CN101781535B CN101781535B CN2010101145387A CN201010114538A CN101781535B CN 101781535 B CN101781535 B CN 101781535B CN 2010101145387 A CN2010101145387 A CN 2010101145387A CN 201010114538 A CN201010114538 A CN 201010114538A CN 101781535 B CN101781535 B CN 101781535B
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Abstract
The invention discloses a solvent based flame-retardant pressure-sensitive binding agent and a preparation method thereof and belongs to the field of binding agents. The flame-retardant pressure-sensitive binding agent is prepared by blending the solvent based flame-retardant binding agent and an organic flame retardant in a weight ratio of 10:0.5-2.0, wherein the organic flame retardant is a phosphoric flame retardant; and the solvent based pressure-sensitive binding agent comprises the following components in percentage by weight: 20 to 35 percent of olefine acid soft monomer, 5 to 20 percent of olefine acid hard monomer, 0.5 to 5 percent olefine acid of functional monomer, 42 to 70 percent of organic solvent, 0.1 to 3 percent of oil soluble initiator and 0.05 to 0.5 percent of chain transfer agent. A solvent system is adopted in the flame-retardant pressure-sensitive binding agent. A flame-retardant coating in the flame-retardant pressure-sensitive binding agent adopts a solvent based coating. The solvent based coating is melted to form a film so that the fusing performance of an auxiliary agent and the solvent based flame-retardant pressure-sensitive binding agent in a film forming process is guaranteed to be more uniform, flame-retardant efficiency of the flame retardant with the same amount is higher, and the solvent based flame-retardant pressure-sensitive binding agent has high initial tack and high-efficiency retardant effectiveness.
Description
Technical field
The present invention relates to adhesive field, particularly relate to a kind of solvent based flame-retardant pressure-sensitive binding agent and preparation method thereof.
Background technology
At present, the vinylformic acid that adopt prepare flame-retardant pressure-sensitive binding agent more, but progress along with the Water-borne modification polymerization technique of acrylate monomer, prior art more is tending towards Water-borne modification more and more on the development technique of oleic series pressure sensitive adhesive, this must cause the initial bonding strength of pressure sensitive adhesive significantly to reduce.And cause dissociating mutually of fire retardant and latex particle because the particle packing film former of water-based emulsion is comprehended, make existing flame-retardant pressure-sensitive binding agent flame retardant effect also can't guarantee.
Summary of the invention
Based on the problem that above-mentioned prior art exists, the embodiment of the invention provides a kind of solvent based flame-retardant pressure-sensitive binding agent and preparation method thereof, makes pressure-sensitive fire retardant glue can guarantee to reach high just sticking and flame retardant effect efficiently in use.
The objective of the invention is to be achieved through the following technical solutions:
The embodiment of the invention provides a kind of solvent based flame-retardant pressure-sensitive binding agent, and this flame-retardant pressure-sensitive binding agent is made up of by 10: 0.5~2.0 part by weight blend solvent-borne type pressure sensitive adhesive and organic fire-retardant;
Wherein, described organic fire-retardant adopts phosphorus flame retardant;
Described solvent-borne type pressure sensitive adhesive is made up of following components in percentage by weight: alkene esters of gallic acid soft monomer 20~35%, alkene esters of gallic acid hard monomer 5~20%, alkene esters of gallic acid function monomer 0.5~5%, organic solvent 42~70%, oil-soluble initiator 0.1~3%, chain-transfer agent 0.05~0.5%.
Described phosphorus flame retardant comprises:
In triphenylphosphate, trimethyl phosphite 99, triethyl phosphate, trioctyl phosphate, phosphotriester, the di(2-ethylhexyl)phosphate phenyl 2-ethylhexyl any or several arbitrarily.
The used esters of acrylic acid soft monomer of described solvent-borne type pressure sensitive adhesive comprises:
In butyl acrylate, ethyl propenoate, ethyl acrylate, the Isooctyl acrylate monomer any or several arbitrarily.
The used esters of acrylic acid hard monomer of described solvent-borne type pressure sensitive adhesive comprises:
In methyl acrylate, methyl methacrylate, the methyl methacrylate any or any two kinds.
The used esters of acrylic acid function monomer of described solvent-borne type pressure sensitive adhesive comprises:
In vinylformic acid, methacrylic acid, Hydroxyethyl acrylate, hydroxyethyl methylacrylate, the Propylene glycol monoacrylate any or several arbitrarily.
The used organic solvent of described solvent-borne type pressure sensitive adhesive comprises:
In ethyl acetate, toluene, dimethylbenzene, the butanone any or several arbitrarily.
The used oil-soluble initiator of described solvent-borne type pressure sensitive adhesive comprises:
In azo diethyl butyronitrile, benzoyl peroxide, the isopropyl benzene hydroperoxide any or any two kinds; Perhaps any in azo diethyl butyronitrile, benzoyl peroxide, the isopropyl benzene hydroperoxide and tertbutyl peroxide.
The used chain-transfer agent of described solvent-borne type pressure sensitive adhesive adopts lauryl mercaptan.
The embodiment of the invention also provides a kind of preparation method of solvent based flame-retardant pressure-sensitive binding agent, comprising:
Preparation solvent-borne type pressure sensitive adhesive:
Get each component of preparation solvent-borne type pressure sensitive adhesive by the proportioning of aforesaid right requirement 1;
With the esters of acrylic acid soft monomer in the prescription, the esters of acrylic acid hard monomer, the esters of acrylic acid function monomer, account for the oil-soluble initiator of oil-soluble initiator gross weight 65~70% and whole chain-transfer agent mixing and obtain monomer mixed solution, to account for the monomer mixed solution of described monomer mixed solution gross weight 20~30% and occupy the organic solvent adding reactor of machine solvent gross weight 60~70%, be warming up to 75~80 ℃ of reactions 0.5~2 hour, drip remaining described monomer mixed solution, dripped off in 2 hours, remaining organic solvent is mixed the mixed solution that forms in 0.5 hour, slowly splash into reactor with remaining oil-soluble initiator, be incubated 2~4 hours, be cooled to room temperature, the viscosity that records reaction product is 500~1500mpa.s, solid content is 35~60%, and discharging promptly makes the solvent-borne type pressure sensitive adhesive;
The preparation flame-retardant pressure-sensitive binding agent: the described solvent-borne type pressure sensitive adhesive that will make with as the phosphorus flame retardant of organic fire-retardant by 10: 0.5~2.0 part by weight blend, after stirring, promptly obtain solvent based flame-retardant pressure-sensitive binding agent.
Used phosphorus flame retardant comprises in the described preparation flame-retardant pressure-sensitive binding agent step:
In triphenylphosphate, trimethyl phosphite 99, triethyl phosphate, trioctyl phosphate, phosphotriester, the di(2-ethylhexyl)phosphate phenyl 2-ethylhexyl any or several combination arbitrarily.
From the technical scheme of the invention described above as can be seen, in flame-retardant pressure-sensitive binding agent, adopt solvent system in the embodiment of the invention, flame retardant resistance coating selective solvent type coating in this flame-retardant pressure-sensitive binding agent, the fusion film forming of solvent-based coating has guaranteed auxiliary agent and this flame-retardant pressure-sensitive binding agent, and originally the amalgamation in film process is more even, make the fire retardant efficient of same amount higher, make this solvent based flame-retardant pressure-sensitive binding agent have high tack and flame retardant effect efficiently.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
Present embodiment 1 provides a kind of solvent based flame-retardant pressure-sensitive binding agent, and this flame-retardant pressure-sensitive binding agent is made up of by 10: 0.5~2.0 part by weight blend solvent-borne type pressure sensitive adhesive and organic fire-retardant;
Wherein, described organic fire-retardant adopts organic phosphorus flame retardant; Can adopt in triphenylphosphate, trimethyl phosphite 99, triethyl phosphate, trioctyl phosphate, tricresyl phosphate (2-chloroethyl) ester, the di(2-ethylhexyl)phosphate phenyl 2-ethylhexyl any or several arbitrarily.
Described solvent-borne type pressure sensitive adhesive is made up of esters of acrylic acid soft monomer, esters of acrylic acid hard monomer, esters of acrylic acid function monomer, organic solvent, oil-soluble initiator and chain-transfer agent, the consumption of each component is by weight percentage: alkene esters of gallic acid soft monomer 20~35%, alkene esters of gallic acid hard monomer 5~20%, alkene esters of gallic acid function monomer 0.5~5%, organic solvent 42~70%, oil-soluble initiator 0.1~3%, chain-transfer agent 0.05~0.5%.
In the above-mentioned solvent based flame-retardant pressure-sensitive binding agent, each used in solvent-borne type pressure sensitive adhesive component is specially:
Used esters of acrylic acid soft monomer comprises: any in butyl acrylate, ethyl propenoate, ethyl acrylate, the Isooctyl acrylate monomer or several arbitrarily (using any several mixture arbitrarily that can be meant when several).
Used esters of acrylic acid hard monomer comprises: any in methyl acrylate, methyl methacrylate, the methyl methacrylate or any two kinds;
Used esters of acrylic acid function monomer comprises: any in vinylformic acid, methacrylic acid, Hydroxyethyl acrylate, hydroxyethyl methylacrylate, the Propylene glycol monoacrylate or several arbitrarily (using any several mixture arbitrarily that can be meant when several).
Used organic solvent comprises: any in ethyl acetate, toluene, dimethylbenzene, the butanone or several arbitrarily (using any several mixture arbitrarily that can be meant when several).
Used oil-soluble initiator comprises: any in azo diethyl butyronitrile, benzoyl peroxide, the isopropyl benzene hydroperoxide or any two kinds; Perhaps any in azo diethyl butyronitrile, benzoyl peroxide, the isopropyl benzene hydroperoxide and tertbutyl peroxide are used in combination.
Used chain-transfer agent mainly refers to lauryl mercaptan.
The concrete preparation process of above-mentioned solvent based flame-retardant pressure-sensitive binding agent is as follows:
Preparation solvent-borne type pressure sensitive adhesive: get each raw material by the proportioning of above-mentioned solvent-borne type pressure sensitive adhesive, with the esters of acrylic acid soft monomer, the esters of acrylic acid hard monomer, the esters of acrylic acid function monomer, the oil-soluble initiator and the whole chain-transfer agents that account for oil-soluble initiator gross weight 65~70% mix the formation monomer mixture, the monomer mixture that accounts for described monomer mixture gross weight 20~30% is added reactor with the organic solvent that occupies machine solvent gross weight 60~70%, be warming up to 75~80 ℃ of reactions 0.5~2 hour, drip the residual monomers mixture then, dripped off in 2 hours, after remaining organic solvent mixed the mixed solution that forms in 0.5 hour, slowly splash into reactor with remaining oil-soluble initiator, be incubated 2~4 hours, be cooled to room temperature, the viscosity that records reaction product is 500~1500mpa.s, solid content is 35~60%, and discharging promptly obtains the solvent-borne type pressure sensitive adhesive;
The preparation solvent based flame-retardant pressure-sensitive binding agent: will the above-mentioned solvent-borne type pressure sensitive adhesive that makes and as the phosphorus flame retardant of organic fire-retardant by 10: 0.5~2.0 part by weight blend, promptly obtain solvent based flame-retardant pressure-sensitive binding agent after stirring.
In the flame-retardant pressure-sensitive binding agent of the embodiment of the invention, adopt solvent system, flame retardant resistance coating selective solvent type coating in this flame-retardant pressure-sensitive binding agent, the fusion film forming of solvent-based coating has guaranteed auxiliary agent and this solvent based flame-retardant pressure-sensitive binding agent, and originally the amalgamation in film process is more even, make the fire retardant efficient of same amount higher, make this solvent based flame-retardant pressure-sensitive binding agent have high tack and flame retardant effect efficiently.
Embodiment 2
Present embodiment 2 provides a kind of solvent based flame-retardant pressure-sensitive binding agent, and this flame-retardant pressure-sensitive binding agent is made up of by 10: 1 part by weight blend solvent-borne type pressure sensitive adhesive and organic fire-retardant; Wherein, organic fire-retardant adopts trioctyl phosphate;
Wherein, the solvent-borne type pressure sensitive adhesive is made up of each raw material in the following table:
Raw material (solvent-borne type pressure sensitive adhesive) | Weight percent (%) |
Ethyl acrylate | 20 |
Ethyl propenoate | 10 |
Methyl acrylate | 14 |
Vinylformic acid | 1.5 |
Hydroxyethyl acrylate | 2.0 |
Ethyl acetate | 40 |
Toluene | 10 |
Benzoyl peroxide | 2.3 |
Dodecyl Mercaptan | 0.2 |
The preparation method of above-mentioned solvent based flame-retardant pressure-sensitive binding agent, undertaken by following step:
Preparation solvent-borne type pressure sensitive adhesive: with ethyl acrylate, ethyl propenoate, methyl acrylate, vinylformic acid, Hydroxyethyl acrylate and the benzoyl peroxide and the whole Dodecyl Mercaptans that account for benzoyl peroxide gross weight 65% mix the formation monomer mixture, the monomer mixture of described monomer mixture gross weight 20% will be accounted for, mixed solvent with the mixed solvent gross weight 60% that accounts for toluene and ethyl acetate mixing formation adds reactor, be warming up to 75~80 ℃ of reactions 0.5~2 hour, drip the residual monomers mixed solution then, dripped off in 2 hours, after remaining mixed solvent mixed the mixed solution that forms in half an hour, slowly splash into reactor with remaining benzoyl peroxide, be incubated 2~4 hours, be cooled to room temperature, the viscosity that records reaction product is 500~2000mpa.s, solid content is 45~50%, and discharging promptly gets the solvent-borne type pressure sensitive adhesive;
The preparation flame-retardant pressure-sensitive binding agent: with the above-mentioned solvent-borne type pressure sensitive adhesive that makes with mix with 10: 1 part by weight as the trioctyl phosphate of organic fire-retardant after stir, promptly obtain solvent based flame-retardant pressure-sensitive binding agent.
Embodiment 3
Present embodiment 3 provides a kind of solvent based flame-retardant pressure-sensitive binding agent, and this flame-retardant pressure-sensitive binding agent is made up of by 10: 0.6 part by weight blend solvent-borne type pressure sensitive adhesive and organic fire-retardant; Wherein, organic fire-retardant adopts trimethyl phosphite 99;
Wherein, the solvent-borne type pressure sensitive adhesive is made up of each raw material in the following table:
Raw material (solvent-borne type pressure sensitive adhesive) | Weight percent (%) |
Butyl acrylate | 35 |
Methyl methacrylate | 9 |
Methacrylic acid | 1.5 |
Hydroxyethyl acrylate | 2.0 |
Ethyl acetate | 45 |
Dimethylbenzene | 5 |
Azo diethyl butyronitrile | 2.2 |
Dodecyl Mercaptan | 0.3 |
The preparation method of above-mentioned solvent based flame-retardant pressure-sensitive binding agent, undertaken by following step:
Preparation solvent-borne type pressure sensitive adhesive: with butyl acrylate, methyl acrylate, methacrylic acid, Hydroxyethyl acrylate and account for the azo diethyl butyronitrile of azo diethyl butyronitrile gross weight 68% and whole Dodecyl Mercaptans mixes and obtains monomer mixture, the monomer mixture of described monomer mixture gross weight 25% will be accounted for, mixed solvent with the mixed solvent gross weight 65% that accounts for dimethylbenzene and ethyl acetate mixing formation adds reactor, be warming up to 75~80 ℃ of reactions 0.5~2 hour, drip the residual monomers mixed solution then, dripped off in 2 hours, remaining mixed solvent is mixed the mixed solution that forms in half an hour, slowly splash into reactor with remaining benzoyl peroxide, be incubated 2~4 hours, be cooled to room temperature, the viscosity that records reaction product is 500~2000mpa.s, solid content is 45~50%, and discharging promptly makes the solvent-borne type pressure sensitive adhesive;
Preparation flame-retardant pressure-sensitive binding agent: press 10: 0.6 part by weight uniform mixing with the solvent-borne type pressure sensitive adhesive of above-mentioned preparation and as the triphenylphosphate of organic fire-retardant, promptly obtain solvent based flame-retardant pressure-sensitive binding agent.
Embodiment 4
Present embodiment 4 provides a kind of solvent based flame-retardant pressure-sensitive binding agent, and this flame-retardant pressure-sensitive binding agent is made up of by 10: 2 part by weight blend solvent-borne type pressure sensitive adhesion profit and organic fire-retardant; Wherein, organic fire-retardant adopts di(2-ethylhexyl)phosphate phenyl 2-ethylhexyl;
Wherein, the solvent-borne type pressure sensitive adhesive is made up of each raw material in the following table:
Raw material (solvent-borne type pressure sensitive adhesive) | Weight percent (%) |
Ethyl acrylate | 25 |
Methyl acrylate | 19 |
Methacrylic acid | 1.5 |
Hydroxyethyl acrylate | 2.0 |
Ethyl acetate | 45 |
Butanone | 5 |
Azo diethyl butyronitrile and tertbutyl peroxide | 2.2 |
Dodecyl Mercaptan | 0.3 |
The preparation method of above-mentioned solvent based flame-retardant pressure-sensitive binding agent, undertaken by following step:
Preparation solvent-borne type pressure sensitive adhesive: with butyl acrylate, methyl acrylate, methacrylic acid, Hydroxyethyl acrylate and the tertbutyl peroxide and the whole Dodecyl Mercaptans that account for tertbutyl peroxide gross weight 70% mix the formation monomer mixture, the monomer mixture of described monomer mixture gross weight 30% will be accounted for, join in the reactor with accounting for butanone mixes the mixed solvent gross weight 70% that forms with ethyl acetate mixed solvent, be warming up to 75~80 ℃ of reactions 0.5~2 hour, drip the residual monomers mixed solution, dripped off in 2 hours, remaining mixed solvent is mixed the mixed solution that forms in half an hour, slowly splash into reactor with remaining benzoyl peroxide, be incubated 2~4 hours, be cooled to room temperature, recording the reaction product viscosity is 500~2000mpa.s, solid content is 45~50%, and discharging promptly makes the solvent-borne type pressure sensitive adhesive;
The preparation flame-retardant pressure-sensitive binding agent: will the above-mentioned solvent-borne type pressure sensitive adhesive that makes and as the di(2-ethylhexyl)phosphate phenyl 2-ethylhexyl of organic fire-retardant part by weight uniform mixing with 10: 2, promptly make solvent based flame-retardant pressure-sensitive binding agent.
Can know that the organic fire-retardant in the various embodiments described above also can adopt any in trimethyl phosphite 99, triethyl phosphate, tricresyl phosphate (2-chloroethyl) ester.
In sum, in flame-retardant pressure-sensitive binding agent, adopt solvent system in the embodiment of the invention, flame retardant resistance coating selective solvent type coating in this flame-retardant pressure-sensitive binding agent, the fusion film forming of solvent-based coating has guaranteed auxiliary agent and this flame-retardant pressure-sensitive binding agent, and originally the amalgamation in film process is more even, make the fire retardant efficient of same amount higher, make this solvent based flame-retardant pressure-sensitive binding agent have high tack and flame retardant effect efficiently.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (5)
1. a solvent based flame-retardant pressure-sensitive binding agent is characterized in that, this flame-retardant pressure-sensitive binding agent is made up of by 10: 0.5~2.0 part by weight blend solvent-borne type pressure sensitive adhesive and organic fire-retardant;
Wherein, described organic fire-retardant adopts phosphorus flame retardant;
Described solvent-borne type pressure sensitive adhesive is made up of following components in percentage by weight: esters of acrylic acid soft monomer 20~35%, esters of acrylic acid hard monomer 5~20%, esters of acrylic acid function monomer 0.5~5%, organic solvent 42~70%, oil-soluble initiator 0.1~3%, chain-transfer agent 0.05~0.5%;
Described phosphorus flame retardant is: any in triphenylphosphate, trimethyl phosphite 99, triethyl phosphate, trioctyl phosphate, the di(2-ethylhexyl)phosphate phenyl-2-ethylhexyl or several arbitrarily;
Described esters of acrylic acid soft monomer is: any in butyl acrylate, ethyl propenoate, ethyl acrylate, the Isooctyl acrylate monomer or several arbitrarily;
Described esters of acrylic acid hard monomer is: any in methyl acrylate, the methyl methacrylate or any two kinds;
Described esters of acrylic acid function monomer is: any in Hydroxyethyl acrylate, hydroxyethyl methylacrylate, the Propylene glycol monoacrylate or several arbitrarily.
2. solvent based flame-retardant pressure-sensitive binding agent as claimed in claim 1 is characterized in that, the used organic solvent of described solvent-borne type pressure sensitive adhesive comprises:
In ethyl acetate, toluene, dimethylbenzene, the butanone any or several arbitrarily.
3. solvent based flame-retardant pressure-sensitive binding agent as claimed in claim 1 is characterized in that, the used oil-soluble initiator of described solvent-borne type pressure sensitive adhesive comprises:
In benzoyl peroxide, the isopropyl benzene hydroperoxide any or any two kinds; Perhaps any in benzoyl peroxide, the isopropyl benzene hydroperoxide and tertbutyl peroxide.
4. solvent based flame-retardant pressure-sensitive binding agent as claimed in claim 1 is characterized in that, the used chain-transfer agent of described solvent-borne type pressure sensitive adhesive adopts lauryl mercaptan.
5. the preparation method of a solvent based flame-retardant pressure-sensitive binding agent is characterized in that, comprising:
Preparation solvent-borne type pressure sensitive adhesive:
Get each component of preparation solvent-borne type pressure sensitive adhesive by the proportioning of aforesaid right requirement 1;
With the esters of acrylic acid soft monomer in the prescription, the esters of acrylic acid hard monomer, the esters of acrylic acid function monomer, account for the oil-soluble initiator of oil-soluble initiator gross weight 65~70% and whole chain-transfer agent mixing and obtain monomer mixed solution, to account for the monomer mixed solution of described monomer mixed solution gross weight 20~30% and occupy the organic solvent adding reactor of machine solvent gross weight 60~70%, be warming up to 75~80 ℃ of reactions 0.5~2 hour, drip remaining described monomer mixed solution, dripped off in 2 hours, remaining organic solvent is mixed the mixed solution that forms in 0.5 hour, slowly splash into reactor with remaining oil-soluble initiator, be incubated 2~4 hours, be cooled to room temperature, the viscosity that records reaction product is 500~1500mPa.s, solid content is 35~60%, and discharging promptly makes the solvent-borne type pressure sensitive adhesive;
The preparation flame-retardant pressure-sensitive binding agent: the described solvent-borne type pressure sensitive adhesive that will make with as the phosphorus flame retardant of organic fire-retardant by 10: 0.5~2.0 part by weight blend, after stirring, promptly obtain solvent based flame-retardant pressure-sensitive binding agent.
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CN103013400B (en) * | 2012-12-26 | 2015-12-02 | 天津市新森焊材有限公司 | Welding wire tackiness agent |
Citations (3)
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CN1215409A (en) * | 1996-04-04 | 1999-04-28 | 日东电工株式会社 | Photopolymerizable composition, pressure-sensitive flame-retardant adhesive, and adhesive sheets |
WO2007058277A1 (en) * | 2005-11-21 | 2007-05-24 | Soken Chemical & Engineering Co., Ltd. | Adhesive composition for optical film, adhesive sheet, and optical member using such adhesive composition |
CN101591514A (en) * | 2008-05-28 | 2009-12-02 | 北京高盟燕山科技有限公司 | Emulsion for seal adhesive at normal temperature and preparation method thereof |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1215409A (en) * | 1996-04-04 | 1999-04-28 | 日东电工株式会社 | Photopolymerizable composition, pressure-sensitive flame-retardant adhesive, and adhesive sheets |
WO2007058277A1 (en) * | 2005-11-21 | 2007-05-24 | Soken Chemical & Engineering Co., Ltd. | Adhesive composition for optical film, adhesive sheet, and optical member using such adhesive composition |
CN101591514A (en) * | 2008-05-28 | 2009-12-02 | 北京高盟燕山科技有限公司 | Emulsion for seal adhesive at normal temperature and preparation method thereof |
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