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Method of preparing polylactic acid/silicon dioxide nano composite material from acidic silicasol

A technology of nanocomposite material and acidic silica sol is applied in the field of preparing polylactic acid/silica nanocomposite material, which can solve the problems of high cost of silica nanoparticles, high cost of nanoparticles, long route and the like, and achieves low cost, Realize the effect of commercial production and simple process

Inactive Publication Date: 2007-08-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for the in-situ blending method, toxic organic solvents need to be used, and the cost of in-situ generation of nanoparticles by the sol-gel method is high; while for the in-situ ring-opening polymerization method, in order to incorporate hydrophilic The silica nanoparticles are dispersed into the hydrophobic lactide monomer, which must be hydrophobically modified in a volatile organic solvent. In addition to the inherent defects of the aforementioned ring-opening polymerization, the in-situ ring-opening polymerization method is not suitable. An ideal method for preparing polylactic acid / silica nanocomposites
Therefore, in view of the high cost of silica nanoparticles in the prior art for preparing polylactic acid / silica nanocomposites or the need to hydrophobically modify silica nanoparticles or the need to use organic solvents or long polymerization routes, etc., It is necessary to study and develop new methods for preparing polylactic acid / silica nanocomposites

Method used

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  • Method of preparing polylactic acid/silicon dioxide nano composite material from acidic silicasol
  • Method of preparing polylactic acid/silicon dioxide nano composite material from acidic silicasol
  • Method of preparing polylactic acid/silicon dioxide nano composite material from acidic silicasol

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Experimental program
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Effect test

Embodiment 1

[0046] Mix 10 grams of acidic silica sol (the amount of silica nanoparticles is 5wt%) and 55.6 grams of 90wt% L-lactic acid aqueous solution under magnetic stirring, and then ultrasonically disperse; , oil bath heating. Dehydrate at 110°C and normal pressure for 2 hours; then gradually reduce the pressure to 0.1atm, raise the temperature to 130°C, dehydrate for 2 hours, and then continue to dehydrate at 150°C and 400Pa for 4 hours to obtain silica containing The lactic acid prepolymer of nanoparticle; 0.23 gram (1mmol) stannous chloride dihydrate and 0.17 gram (1mmol) p-toluenesulfonic acid are joined in this prepolymer, mix well, be warming up to 180 ℃ gradually, gradually Reduce the pressure to 400 Pa, carry out melt polycondensation, and react for 10 hours to obtain a polylactic acid / silicon dioxide nanocomposite material. The yield of polylactic acid is 82.5%, the weight average molecular weight is 70300, and the content of silica nanoparticles is 5.8wt%.

Embodiment 2-7

[0048]0.2 gram, 3 gram, 6 gram, 20 gram, 40 gram, 60 gram of acidic silica sol (silicon dioxide nanoparticle consumption is respectively 0.1wt%, 1.5wt%, 3wt%, 10wt%, 20wt%, 30wt%) Mix with 55.6 grams of 90wt% L-lactic acid aqueous solution under magnetic stirring, and then ultrasonically disperse; then add to a 250mL three-neck round bottom flask, magnetically stir, heat in an oil bath, and dehydrate at 110°C for 2 hours under normal pressure. Then gradually reduce the pressure to 0.1atm, raise the temperature to 130°C, dehydrate for 2 hours, and then continue to dehydrate for 4 hours at 150°C and 400Pa to obtain a lactic acid prepolymer containing silica nanoparticles; (1mmol) tin protochloride dihydrate and 0.17 gram (1mmol) p-toluenesulfonic acid join in the lactic acid prepolymer, mix uniformly, be warming up to 180 ℃ gradually, step down to 400Pa gradually, carry out melting polycondensation, reaction 10 Hours, polylactic acid / silicon dioxide nanocomposites were obtained....

Embodiment 8-10

[0050] 2 grams of silica sol (containing 0.5 grams of silica nanoparticles, and the amount of silica nanoparticles is 1 wt%) was added to 55.6 grams of L-lactic acid aqueous solution, ultrasonically dispersed; transferred to a 250mL three-neck round bottom flask, and magnetically stirred Heated in an oil bath, dehydrated at 110°C and normal pressure for 2 hours, then gradually reduced the pressure to 0.1atm, raised the temperature to 130°C, dehydrated for 2 hours, and then continued to dehydrate at 150°C and 400Pa for 4 hours to obtain Lactic acid prepolymer containing silica nanoparticles. Add 0.23 grams (1 mmol) of stannous chloride dihydrate and 0.17 grams (1 mmol) of p-toluenesulfonic acid into the three-necked flask containing the oligomer, mix well, gradually raise the temperature to 180 ° C, and gradually reduce the pressure to 400Pa, carry out melt polycondensation, and react for 5 hours to obtain a polylactic acid / silicon dioxide nanocomposite material. The yield of ...

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Abstract

The invention discloses a preparing method of polylactic acid / silica dioxide nanometer composite material with acidic silicasol, which comprises the following steps: (1) mixing acidic silicasol lactic acid raw material under the condition of agitation and hypersonic or agitation and hypersonic; getting nanometer grade dispersing mixture; (2) dewatering and prepolying the mixture from step (1); getting lactic acid prepolymer with silica dioxide nanometer particle; (3) adding into activator; proceeding original position melting polycondensation or original position melting solid phase polycondensation; getting the product. The raw material of this invention is cheap and available, which can used to plastic, packing material, agricultural film, fiber and biological material domain.

Description

technical field [0001] The invention relates to the preparation of polymer nanocomposite materials, in particular to a method for preparing polylactic acid / silicon dioxide nanocomposite materials. Background technique [0002] Biodegradable polymer refers to that its chain structure breaks under the action of water, enzymes, microorganisms, etc., and becomes a small molecular monomer or oligomer, which is finally decomposed by microorganisms in the ecological environment and transformed into carbon dioxide and water or Biomass, or a class of polymer materials that eventually participate in the metabolic process of human and animal bodies and are converted into carbon dioxide and water and excreted from the body. Common biodegradable polymer materials include degradable natural polymers (such as cellulose, starch, chitin, chitosan, etc.), microbially synthesized polymers (such as PHBV) and chemically synthesized polymers (such as polylactic acid, polyhexene, etc.) lactones, ...

Claims

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Application Information

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IPC IPC(8): C08L67/04C08K3/36C08G63/06C08G63/80C08G63/85
Inventor 吴林波曹丹李伯耿黄源
Owner ZHEJIANG UNIV
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