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 compl

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0018] Example 1

[0019] (1) Preparation of seed emulsion: add 0.15g of emulsifier sodium dodecyl biphenyl sulfonate (DSB) and 260g of deionized water to 500ml four ports equipped with stirring, reflux condenser, thermometer and nitrogen inlet pipe 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; increase the temperature to 70℃, add 0.165g An aqueous solution of ammonium persulfate (APS) and 5g of water and an aqueous solution of 0.075g of sodium bisulfite (SBS) and 5g of water are incubated and matured for 2 hours to obtain seed latex particles, which are cooled for later use.

[0020] (2) Preparation of core layer latex particles: 25g seed latex particles and 185g deionized water are added to a 500ml four-necked flask equipped with a stirring, reflux condenser, thermometer and nitrogen inlet tube, and 40.5g methyl methacrylate (MMA) ), 22.5g butyl methacrylate (BA) and 27g meth

Example Embodiment

[0025] Example 2

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

[0027] (2) Preparation of core layer latex particles: 25g seed latex particles and 185g deionized water are added to a 500ml four-necked flask equipped with a stirring, reflux condenser, thermometer and nitrogen inlet tube, and 40.5g 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 Mix 20 g of deionized water, heat up to 70°C, and add the monomer mixture solution and the initiator mixture solution dropwise at the same time. After 2 hours of dripping, the core layer latex particles are obtained by heat preservation and curing for 2 hours, and the temperature is lowered for later use.

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

Example Embodiment

[0032] 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-shell latex particles and 140g of deionized water were added to a 500ml four-necked flask equipped with stirring, reflux condenser, thermometer and nitrogen inlet, 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) were mixed with 20g of deionized water, heated to 70°C, while dripping the monomer mixture solution and the initiator mixture solution, dripping 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 swelling gradually: same as example 1.

[0037] (5) Preparation of cross-linked shell

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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

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Claims

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Application Information

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Owner BEIJING UNIV OF CHEM TECH
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