Process for in-situ quiclely preparing crystalline polyester using nano silicon dioxide

A nano-silica, in-situ preparation technology, applied in the field of polyester preparation, can solve problems such as poor color, limited performance and range of composite materials, etc., to achieve increased crystallization speed, increased compatibility, and improved dispersibility Effect

Inactive Publication Date: 2005-05-18
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of dark brown silicate in this method, the color of the product is relatively poor, which limits the performance and scope of the composite material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 95% ethanol to a 2000mL beaker, add 10 grams of polyvinylpyrrolidone while stirring, and heat to 70°C. After stirring and reacting for 1 hour, filter, wash and activate in an oven at 100° C. for 1 hour, then dry and set aside.

[0019] Disperse the above-mentioned organically modified nano-silica in 500 grams of ethylene glycol to form a slurry with a concentration of 20%, first disperse it in a high-speed disperser, and then grind it in a circulating sand mill. Use a laser particle size analyzer to test the particle size of the slurry. When the average particle size of nano-silica in the slurry is less than 100 nanometers, stop grinding and discharge the slurry for later use.

[0020] 8,000 grams of terephthalic acid, 3,812 grams of ethylene glycol, and 235 grams of the above-mentioned nano-silica slurry were beaten together and then added to a 30-liter polyester polymerization kettle. Antimony ethylene glycol was used as a polycondensation catalyst, and trimethyl ...

Embodiment 2

[0022] The difference from the method described in Example 1 is that the surface modification of nano silicon dioxide uses silane coupling agent KH-560, and the amount of silane coupling agent is 15% of that of nano silicon dioxide.

[0023] Disperse the above-mentioned organically modified nano-silica powder in 1000 grams of ethylene glycol to form a slurry with a concentration of 20%, first disperse it in a high-speed disperser, and then grind it in a circulating sand mill, During the grinding process, use a laser particle size analyzer to test the particle size of the slurry. When the average particle size of nano-silica in the slurry is less than 100 nanometers, stop the grinding and discharge the slurry for later use. 8000 grams of terephthalic acid, 3616 grams of ethylene glycol and 480 grams of the above-mentioned nano-silica slurry are beaten together and added to a 30-liter polyester polymerization kettle, using ethylene glycol antimony as a polycondensation catalyst a...

Embodiment 3

[0025] The difference from the methods described in Examples 1 and 2 is that the surface of the nano-silica is not subjected to drying and activation after the organic modification, and the average particle size is always kept below 100 nanometers. First, dissolve the silane coupling agent KH-560 in water, stir well, then add it into 500 grams of 20% silicon dioxide aqueous solution, keep the solution temperature at 60°C, and fully stir for 0.5 hours to react. The dosage of the silane coupling agent is 10% of the mass of nano silicon dioxide. After fully reacting, the above-mentioned organically modified nano silicon dioxide is dispersed in 400 grams of ethylene glycol, and a large amount of water is removed to form a 20% nano silicon dioxide ethylene glycol solution.

[0026] 8000 grams of terephthalic acid, 3600 grams of ethylene glycol and 500 grams of the above-mentioned nano-silica slurry are beaten together and added to a 30-liter polyester polymerization kettle, using e...

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PUM

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Abstract

The present invention relates to composite material preparing technology. The production process of nano composite silica / polyester material includes the following steps: coating nano silica as crystallizing nucleartor with organic matter for surface modification to make it capable of distribute well in ethylene glycol as one monomer for polyester; high temperature pre-treating compounded nano silica / ethylene glycol slurry to make nano silica possess average size smaller than 100 nm; and polymerization or copolymerization between nano silica / ethylene glycol slurry and other monomer for polyester inside reactor to obtain in-situ nano composite silica / polyester material. The composite material with 1 wt% of nanometer silica contained has non-isothermal crystallization melting peak temperature raised to 213.4 deg.c and 4-8 times raised isothermal crystallization rate at 185-200 deg.c.

Description

technical field [0001] The invention relates to a method for preparing polyester, in particular to a method for preparing rapid crystallization polyester in situ by using nano silicon dioxide. Used in the field of composite materials. technical background [0002] As a thermoplastic engineering plastic, polyester has comprehensive properties such as high strength, high rigidity, good heat resistance, excellent dimensional stability, and chemical resistance. It is widely used in the fields of electronic and electrical components, machinery, and automotive components. . Especially in recent years, due to the excellent properties of polyester, lower production costs and higher performance-price ratio, the proportion of polyester used in car plastics has been increasing. However, as an engineering plastic application, polyester has disadvantages such as slow crystallization rate, large shrinkage rate of molded products, and brittle quality. For this reason, extensive research...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78C08K3/36C08K9/04C08L67/00
Inventor 杨永喆徐宏古宏晨
Owner SHANGHAI JIAO TONG UNIV
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