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Polyester/mesoporous molecular sieve composite material and its preparing material

A technology of mesoporous molecular sieves and composite materials, which is applied in the field of polyester modified composite materials and its preparation, can solve problems such as the difficulty of combining inorganic particles, and achieve the effect of improving physical and mechanical properties and enhancing interface bonding

Inactive Publication Date: 2006-03-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention overcomes the disadvantage that inorganic particles are not easily combined with polymer matrix, solves the problem of interfacial combination between polymer matrix and inorganic particles, and proposes an in-situ polymerized polyester / mesoporous molecular sieve composite material and its preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Self-preparation of silicon-based mesoporous molecular sieves: react with ethyl orthosilicate and hexadecyltrimethylammonium bromide in a strong acidic aqueous solution at a temperature of 30°C, and use electric stirring and ultrasonic radiation. 40KHz, the pre-product is washed with deionized water, filtered, roasted at 600°C for 6 hours, and ground by a ball mill after cooling to obtain a silicon-based mesoporous molecular sieve powder with an average particle size of less than 1 micron and a pore size of about 3 nm;

[0026] Preparation of polyester / silicon-based mesoporous molecular sieve composites by direct esterification and polycondensation:

[0027] Add 100g of ethylene glycol, 200g of terephthalic acid, and 6g of fully dried silicon-based mesoporous molecular sieve particles into the reaction kettle, and perform electric stirring and ultrasonic dispersion. Kettle, ultrasonic frequency 100KHz, after ultrasonic dispersion for 20min, start heating to 2...

Embodiment 2

[0028] Example 2: Preparation of polyester / aluminum-based mesoporous molecular sieve composite material by direct esterification and polycondensation method:

[0029] Add 95g of ethylene glycol, 205g of terephthalic acid, and 12g of fully dried aluminum-based mesoporous molecular sieve particles into the reaction kettle. After electric stirring and ultrasonic dispersion, the ultrasonic frequency is 100KHz. After dispersing for 30 minutes, start heating to 260°C. After complete melting, add the stabilizer triphenyl phosphite and stir thoroughly to carry out the esterification reaction until the reaction no longer distills water, and the esterification reaction ends. Add 0.1g of Sb to the mixture 2 o 3 , the temperature is controlled at 260°C, the vacuum degree is 0.1Mpa, and stirred for 40min; when the vacuum degree is higher than 0.03Mpa, the temperature is raised to 285°C until the viscosity of the polymer reaches a certain level, the polycondensation reaction is over, and t...

Embodiment 3

[0030] Example 3: Preparation of polyester / silicon-based mesoporous molecular sieve composite material by transesterification polycondensation method:

[0031] Add 230g of refined dimethyl terephthalate, 170g of ethylene glycol, and 0.115g of zinc acetate into the reaction kettle, control the temperature at 190°C and stir it electrically. When the distilled amount of methanol reaches the theoretical amount, the transesterification reaction is considered to be over. Then add dry mesoporous molecular sieve 18g, catalyst antimony trioxide and heat stabilizer triphenyl phosphite, carry out thorough stirring and ultrasonic dispersion, radiation frequency 200KHz, dispersion time 40min. Then carry out pre-condensation, the temperature is 260°C, and the vacuum degree is 0.1MPa; when the vacuum degree rises to higher than 0.03MPa, the temperature is increased to 280°C. When the viscosity of the polymer reaches a certain value, it can be taken out of the kettle, cooled, and pelletized t...

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Abstract

This invention relates to polyester / mesoporous molecular sieve composite material and its preparing method. Using mesoporous molecular sieve fine particles with definite grain size, aperture and acid-base value, after drying, mixing with liquid polyesters, esterifying to obtain esterified mixed product, during reaction combining with ultrasonic dispersion technology to make monomer and molecular sieve fine partticles mix uniformly, by precondensation and endcondensation under constant temperature and pressure esterified product to obtain a product, by granulating and drying to be agglomerates. During prparation, under vacuum and ultrasonic action, monomer can enter to particle aperture, by in-situ polymerization, particles inside and outside is coated with polymer, bonding polyester and molecular sieve interface well to form polyester / mesoporous molecular sieve composite material with inorganic-organic interpenetrating network structure. The material properties, such as melt crystallization temperature, crystallinity, glass-transition temperature and bending strength, storage modulus elasticity modulus are obviously improved.

Description

technical field [0001] The invention relates to a polyester modified composite material and a preparation method thereof, in particular to a polyester / mesoporous molecular sieve composite material and an in-situ polymerization preparation method. Background technique [0002] Polyethylene terephthalate (PET) is widely used in fiber, packaging container, film, engineering plastics and other fields, but its application is affected to a certain extent due to its relatively low crystallization rate, deformation temperature and modulus. There are many reports on the modification of polyester with inorganic substances. At present, most of them are composite materials modified by blending and extruding polyester with inorganic particles. Due to the high energy consumption and easy degradation of PET blended melt, PET composite materials The crystallization rate is still unsatisfactory. In addition, because ordinary inorganic particles have no pores inside, their combination with po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/02C08G63/183C08G63/78C08K5/54
Inventor 吴刚闰明涛张大余
Owner CHINA PETROLEUM & CHEM CORP
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