CN100560649C - The electrolytical method of in-situ polymerizing organic rectorite stone/polymethyl methacrylate gel polymer - Google Patents
The electrolytical method of in-situ polymerizing organic rectorite stone/polymethyl methacrylate gel polymer Download PDFInfo
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- CN100560649C CN100560649C CNB2006100431262A CN200610043126A CN100560649C CN 100560649 C CN100560649 C CN 100560649C CN B2006100431262 A CNB2006100431262 A CN B2006100431262A CN 200610043126 A CN200610043126 A CN 200610043126A CN 100560649 C CN100560649 C CN 100560649C
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- organic rectorite
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- polymethyl methacrylate
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Abstract
The present invention relates to the electrolytical method of a kind of in-situ polymerizing organic rectorite stone/polymethyl methacrylate gel polymer.Be to adopt high speed shear that the modification organic rectorite is dispersed among organic plasticizer P C, methyl methacrylate is as monomer, Diisopropyl azodicarboxylate is as initiator, lithium perchlorate is as lithium salts, plasticizer components propylene carbonate PC in the gel electrolyte directly as the solvent of polymerization system, the employing free radical causes, and the in-situ polymerization mode prepares stable gel type organic rectorite/poly methyl methacrylate polymer ionogen.Condition required for the present invention is simple, simple, the easy row of technology; Be a kind of directly, simple, pollution is little, suitability is wide, operating procedure simply prepares gel electrolyte method.The organic rectorite of preparing/polymethyl methacrylate gel polymer electrolyte system not only has gratifying ionic conductivity, and has good dimensional space stability and electrochemical stability.
Description
Technical field
The present invention relates to the electrolytical method of a kind of in-situ polymerizing organic rectorite stone/polymethyl methacrylate gel polymer, belong to the interdisciplinary field of electricity and materialogy.
Background technology
In gel polymer electrolyte, add nanoparticle, not only can improve its mechanical property, improve its gel stability, can also improve its chemical property, this preparation nano-composite gel polymer dielectric (NGPE) is the feasible and effective method of modifying of a kind of convenience.Nanoparticle commonly used has clay, SiO
2, zeolite, Al
2O
3Deng.
Rectorite leng is a kind of natural clay with layered silicate character.By suitable organically-modified, form the modified Nano particle that excellent compatibility is arranged with polymkeric substance, this nanoparticle is used for mechanics and the thermal characteristics that polymer modification can be improved polymkeric substance than the highland.
This laboratory once in the number of applying for a patent is 200510041814.0 patent, had applied for adopting the mode of organic rectorite and polymer blending to prepare the nano-composite gel method for preparing polymer electrolytes,
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes the electrolytical method of a kind of in-situ polymerizing organic rectorite stone/polymethyl methacrylate gel polymer, synthetic from polymeric matrix adopts the method for in-situ polymerization to prepare the OREC/PMMA gel polymer electrolyte with good ionic conductivity and dimensional stability.
Technical scheme
Organic rectorite provided by the invention/polymethyl methacrylate gel polymer ionogen, be to adopt high speed shear that the modification organic rectorite is dispersed among organic plasticizer P C, methyl methacrylate (MMA) is as monomer, Diisopropyl azodicarboxylate (AIBN) is as initiator, lithium perchlorate (LiClO
4) as lithium salts, plasticizer components propylene carbonate PC in the gel electrolyte directly as the solvent of polymerization system, the employing free radical causes, and the in-situ polymerization mode prepares stable gel type organic rectorite/polymethylmethacrylate (OREC/PMMA) polymer dielectric.
Technical characterictic of the present invention is:
A) lithium perchlorate salt is dissolved in is made into organic electrolyte among the propylene carbonate PC, become component one;
B) organic rectorite is dispersed in the part softening agent (PC) by high speed shear becomes component two
C) with the methyl methacrylate be monomer, Diisopropyl azodicarboxylate is as initiator, directly mix mutually with component one and component two or four, heating in water bath carries out in-situ polymerization to 65-85 ℃, react after 2.5 hours, reaction gel liquid is prolonged the stream film forming on sheet glass, can obtain the gel-type electrolytic thin-membrane at 60 ℃ of vacuum-drying 8h.
Above-mentioned each component is mixed by following proportioning:
Methyl methacrylate 20-30g
Organic rectorite clay 2～8g
Propylene carbonate 18-50g
Lithium perchlorate 1.8-7g
Diisopropyl azodicarboxylate 0.04-0.1g
Beneficial effect
The home polymerization mode that the present invention adopts, required condition is simple, simple, the easy row of technology; Be a kind of directly, simple, pollution is little, suitability is wide, operating procedure simply prepares gel electrolyte method.The organic rectorite of preparing/polymethyl methacrylate gel polymer electrolyte system not only has gratifying ionic conductivity, and has good dimensional space stability and electrochemical stability.
Description of drawings
Fig. 1: be the electrolytical process flow sheet of preparation organic rectorite/polymethyl methacrylate gel polymer
Embodiment
Now in conjunction with the accompanying drawings the present invention is further described:
The preparation of organic rectorite: sodium base rectorite leng 50g stirring pulping soluble in water, and with 30g organic surface active agent C
12Quaternary ammonium salt is soluble in water under 40～50 ℃, water phase surfactant mixture is slowly poured in the slurries again, and homogeneous changes in the there-necked flask after disperseing 10min, is incubated 12h down in 80～85 ℃.Change in the beaker, again with deionized water wash to using AgNO
3Solution procuratorial work is less than Cl
-Till, drying, grinding promptly obtain organic rectorite 12-OREC.
Embodiment 1:
Lithium perchlorate salt LiCiO
45g is dissolved among the 15g propylene carbonate PC and is made into organic electrolyte, is component one; 0.5g (1phr) 12-OREC and 15g propylene carbonate are stirred through high speed shear, be component two; Take by weighing methyl methacrylate (MMA) and 0.08g Diisopropyl azodicarboxylate (AIBN) initiator of 20g, and itself and component one, two mixed, place 80 ℃ of stirred in water bath, react and to obtain colloidal state electrolytic solution curtain coating after 2.5 hours and become film, drying is 8 hours under 60 ℃ of vacuum, promptly gets organic rectorite/polymethyl methacrylate gel polymer ionogen (1phr-12-OREC/PMMA).Under concurrent this proportioning now, organic rectorite/polymethylmethacrylate of making (OREC/PMMA) gel polymer electrolyte has good spatial stability and mechanical mechanics property, and has satisfied well as the requirement of lithium ion battery electrolyte to ionic conductivity.
Embodiment 2:
Lithium perchlorate salt LiCiO
45g is dissolved among the 15g propylene carbonate PC and is made into organic electrolyte, is component one; 0.5g (1phr) 12-OREC and 15g propylene carbonate are stirred through high speed shear, be component two; Take by weighing methyl methacrylate (MMA) and 0.08g Diisopropyl azodicarboxylate (AIBN) initiator of 20g, and itself and component one, two mixed, place 80 ℃ of stirred in water bath, react and to obtain colloidal state electrolytic solution curtain coating after 2.5 hours and become film, drying is 8 hours under 60 ℃ of vacuum, promptly gets organic rectorite/polymethyl methacrylate gel polymer ionogen (3phr-12-OREC/PMMA).Under concurrent this proportioning now, organic rectorite/polymethylmethacrylate of making (OREC/PMMA) gel polymer electrolyte has good spatial stability and mechanical mechanics property, and has satisfied well as the requirement of lithium ion battery electrolyte to ionic conductivity.
Embodiment 3:
Lithium perchlorate salt LiCiO
45g is dissolved among the 15g propylene carbonate PC and is made into organic electrolyte, is component one; 0.5g (1phr) 12-OREC and 15g propylene carbonate are stirred through high speed shear, be component two; Take by weighing methyl methacrylate (MMA) and 0.08g Diisopropyl azodicarboxylate (AIBN) initiator of 20g, and itself and component one, two mixed, place 80 ℃ of stirred in water bath, react and to obtain colloidal state electrolytic solution curtain coating after 2.5 hours and become film, drying is 8 hours under 60 ℃ of vacuum, promptly gets organic rectorite/polymethyl methacrylate gel polymer ionogen (5phr-12-OREC/PMMA).Under concurrent this proportioning now, organic rectorite/polymethylmethacrylate of making (OREC/PMMA) gel polymer electrolyte has good spatial stability and mechanical mechanics property, and has satisfied well as the requirement of lithium ion battery electrolyte to ionic conductivity.
The specific performance of the gel electrolyte that three kinds of embodiments obtain is as follows:
※ all records under 25 ℃
Claims (1)
1. electrolytical method of in-situ polymerizing organic rectorite stone/polymethyl methacrylate gel polymer is characterized in that:
A) lithium perchlorate salt is dissolved in is made into organic electrolyte among the propylene carbonate PC, become component one;
B) the organic rectorite clay is dispersed among the part softening agent propylene carbonate PC by high speed shear becomes component two;
C) with the methyl methacrylate be monomer, Diisopropyl azodicarboxylate is as initiator, directly mix with component one and component two, heating in water bath carries out in-situ polymerization to 65-85 ℃, react after 2.5 hours, reaction gel liquid is prolonged the stream film forming on sheet glass, can obtain the gel-type electrolytic thin-membrane at 60 ℃ of vacuum-drying 8h;
Above-mentioned each component is mixed by following proportioning:
Methyl methacrylate 20-30g
Organic rectorite clay 2～8g
Propylene carbonate 18-50g
Lithium perchlorate 1.8-7g
Diisopropyl azodicarboxylate 0.04-0.1g.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100431262A CN100560649C (en) | 2006-07-10 | 2006-07-10 | The electrolytical method of in-situ polymerizing organic rectorite stone/polymethyl methacrylate gel polymer |
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|---|---|---|---|
| CNB2006100431262A CN100560649C (en) | 2006-07-10 | 2006-07-10 | The electrolytical method of in-situ polymerizing organic rectorite stone/polymethyl methacrylate gel polymer |
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| CN101104723A CN101104723A (en) | 2008-01-16 |
| CN100560649C true CN100560649C (en) | 2009-11-18 |
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| CN115403885A (en) * | 2022-08-20 | 2022-11-29 | 太仓市华鼎塑料有限公司 | High-flow PMMA material for automobile tail lamp cover |
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Non-Patent Citations (2)
| Title |
|---|
| 改性累托石对凝胶电解质组分相互作用的影响. 黄，韵，马晓燕，梁国正，林海军.硅酸盐学报，第34卷第1期. 2006 |
| 改性累托石对凝胶电解质组分相互作用的影响. 黄，韵，马晓燕，梁国正，林海军.硅酸盐学报，第34卷第1期. 2006 * |
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Granted publication date: 20091118 Termination date: 20120710 |