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Preparation method of large-size polymer hollow microspheres with high crosslinking degrees

A technology of hollow microspheres and high cross-linking degree, which is applied in the field of preparation of high-cross-linking degree hollow polymer microspheres and high-cross-linking degree polymer hollow microspheres, can solve problems such as unclean cavities, and avoid unnecessary problems. Stable, diameter-enhancing effect

Active Publication Date: 2012-09-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alkali-neutralized polymer chains are in a rigid stretching state due to the action of charges, and cannot completely shrink to the inner wall after being cooled and fixed, dried and dehydrated, resulting in an unclean cavity

Method used

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  • Preparation method of large-size polymer hollow microspheres with high crosslinking degrees
  • Preparation method of large-size polymer hollow microspheres with high crosslinking degrees
  • Preparation method of large-size polymer hollow microspheres with high crosslinking degrees

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0019] (1) Preparation of seed emulsion: Add 0.15g of emulsifier sodium dodecyl biphenyl sulfonate (DSB) and 260g of deionized water to a 500ml four-port tube equipped with stirring, reflux condenser, thermometer and nitrogen inlet tube In the bottle, after stirring for 10 minutes, add 21g methyl methacrylate (MMA), 7.5g butyl methacrylate (BA), 1.5g methacrylic acid (MAA) mixed monomer; heat up to 70°C, add 0.165g An aqueous solution of ammonium persulfate (APS) and 5 g of water and an aqueous solution of 0.075 g of sodium bisulfite (SBS) and 5 g of water were incubated for 2 hours to obtain seed latex particles, which were cooled for later use.

[0020] (2) Preparation of core latex particles: Add 25g of seed latex particles and 185g of deionized water into a 500ml four-necked bottle equipped with stirring, reflux condenser, thermometer and nitrogen inlet tube, and 40.5g of methyl methacrylate (MMA ), 22.5g butyl methacrylate (BA) and 27g methacrylic acid (MAA) were mixed, 0...

example 2

[0026] (1) Preparation of seed latex particles: same as Example 1.

[0027](2) Preparation of core latex particles: Add 25g of seed latex particles and 185g of deionized water into a 500ml four-necked bottle equipped with stirring, reflux condenser, thermometer and nitrogen inlet tube, and 40.5g of methyl methacrylate (MMA ), 22.5g butyl methacrylate (BA), 27g methacrylic acid (MAA) and 0.09g tripropylene glycol diacrylate (TPGDA) mixed, 0.6188g ammonium persulfate (APS), 0.2813g sodium sulfite (SBS) and 20g of deionized water was mixed, and the temperature was raised to 70°C. At the same time, the monomer mixed solution and the initiator mixed solution were added dropwise, and the drop was completed in 2 hours, and then incubated for 2 hours to obtain the core layer latex particles, and the temperature was lowered for later use.

[0028] (3) Preparation of core-shell latex particles: 75g of core layer latex particles and 128.75g of deionized water were added to a 500ml four-n...

example 3

[0033] (1) Preparation of seed latex particles: same as Example 1.

[0034] (2) Preparation of core layer latex particles: same as example 2

[0035] (3) Preparation of core-shell latex particles: 60g of core layer latex particles and 140g of deionized water were added to a 500ml four-necked bottle equipped with stirring, reflux condenser, thermometer and nitrogen inlet tube, and 54g of styrene (St) , 6g butyl methacrylate (BA) and 0.6g tripropylene glycol diacrylate (TPGDA) mixed, 0.4125g ammonium persulfate (APS), 0.1875g sodium sulfite (SBS) + 0.06g sodium dodecyl biphenyl sulfonate (DSB) was mixed with 20g of deionized water respectively, and the temperature was raised to 70°C. At the same time, the monomer mixed solution and the initiator mixed solution were added dropwise, and the drop was completed in 2 hours, and then continued to heat and mature for 2 hours to obtain core-shell latex particles, which were cooled for later use.

[0036] (4) Alkali / acid gradual expansi...

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Abstract

The invention provides a preparation method of large-size polymer hollow microspheres with high crosslinking degrees and belongs to the field of polymer materials. The large-size polymer hollow microspheres with high crosslinking degrees are prepared by adopting a multistep seeded emulsion polymerization method. The method is characterized by comprising the following steps: firstly preparing seeded emulsion particles with good compatibility with high acid polymers, secondly preparing high acid nuclear layer polymers, thirdly coating micro-crosslinked transitional crust layers on the surfaces of the high acid nuclear layer polymers, fourthly using volatile alkali / acid to carry out stepwise treatment to ensure the particles to have cavity structures and finally coating crosslinked crust layers on the surfaces of the particles with cavity structures and drying the particles, thus preparing emulsion particles with hollow structures. The method has the following advantages: the hollow microspheres prepared by the method have larger sizes; and with high crosslinking degrees of the crust layers, the polymer hollow microspheres not only have light weight and strong light-shielding performances, but also have good heat and solvent resistance, simultenously avoid high temperature and pressure and use of organic solvents and meet the requirements of low carbon, energy conservation and environmental friendliness.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a method for preparing hollow polymer microspheres with a high degree of crosslinking. More specifically, the method involves multi-step seed emulsion polymerization to prepare large particle size core-shell latex particles, wherein the core is a high-acid content hydrophilic polymer, the shell is a lightly cross-linked hydrophobic polymer, and then The latex particles with hollow structure are obtained by gradually expanding with alkali / acid, and finally the highly cross-linked shell layer is prepared on the surface by seed emulsion polymerization, that is, hollow polymer microspheres with high cross-linking degree are obtained. Background technique [0002] In recent years, the preparation methods and applications of hollow polymers have mostly appeared in the form of patents. Such as U.S. patent US6235810B1 (disclosure date: on May 22nd, 2001) discloses a kind of ...

Claims

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Application Information

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IPC IPC(8): C08F285/00C08F2/26C08J7/02C08J3/24
Inventor 李效玉汪琴宋春风何立凡邱藤
Owner BEIJING UNIV OF CHEM TECH
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