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Preparation method of mono-dispersion polysiloxane microspheres with controllable particle size

A polysiloxane and monodispersity technology is applied in the field of preparation of polysiloxane microspheres, which can solve the problems of increased preparation cost and difficulty in washing, siloxane is prone to explosion, and product quality is uneven, etc. Guarantee the effects of monodispersity, high product yield, and simple treatment process

Inactive Publication Date: 2015-07-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the polysiloxane microspheres in domestic circulation are imported from Japan, Germany, the United States, South Korea and other countries. There are relatively few domestic products, and the quality of the products is uneven, and the particle size is single.
[0003] The Japanese patent (JP2000186148) is prepared by a two-step hydrolysis-condensation method, but has specific requirements for the conductivity of the acidic aqueous solution during the hydrolysis process; the Chinese patent (201310691799.9) uses surfactants and polymers in the process of preparing microspheres Stabilizer, although microspheres with low surface polarity are obtained, it increases the preparation cost and the difficulty of washing. The Chinese patent (CN102604100) only uses alkaline catalysts to prepare siloxane microspheres, although the patent obtains better sphericity and dispersion microspheres, but a single basic catalyst makes siloxane prone to implosion during hydrolysis

Method used

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  • Preparation method of mono-dispersion polysiloxane microspheres with controllable particle size
  • Preparation method of mono-dispersion polysiloxane microspheres with controllable particle size
  • Preparation method of mono-dispersion polysiloxane microspheres with controllable particle size

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 3Kg of deionized water into the reaction kettle, add 70% concentration of acetic acid aqueous solution, adjust the pH value of the aqueous solution to 4, then add 0.6KG of methyltrimethoxysilane, and stir and react at a speed of 200r / min for 2 hours. Then add 70% concentration of sodium hydroxide aqueous solution, adjust the pH of the solution to 11, stir and react for 1 hour under the rotating speed of 20r / min, the solution after the reaction is centrifuged, and with 30% ethanol aqueous solution (the mixing of ethanol and deionized water , the same below) for washing, placed in a vacuum drying oven to dry for 6 hours, the particle size of the obtained microspheres is about 1.5 microns, such as figure 1 shown.

Embodiment 2

[0025] Add 7Kg of deionized water to the reaction kettle, add 85% phosphoric acid aqueous solution, adjust the pH of the aqueous solution to 3, then add 0.7KG of methyltrimethoxysilane, stir and react at 150r / min for 1.5 hours, then add ammonia aqueous solution, adjust the pH of the solution to 9, stir and react at a speed of 30r / min for 2 hours, centrifuge the reacted solution, wash it with 20% ethanol aqueous solution, put it into a vacuum drying oven and dry it for 5 hours, and the obtained microspheres The particle size is about 2 microns.

Embodiment 3

[0027] Add 7Kg of deionized water into the reaction kettle, add concentrated hydrochloric acid, adjust the pH of the aqueous solution to 2, then add 0.35KG of methyltrimethoxysilane, stir and react at a speed of 200r / min for 0.5 hours, then add triethylamine aqueous solution, adjust the pH of the solution to 8, stir and react at a speed of 40r / min for 3 hours, centrifuge the reacted solution, wash it with 15% ethanol aqueous solution, put it into a vacuum drying oven and dry it for 4 hours, and the obtained microspheres The particle size is about 2-3 microns, such as figure 2 shown.

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Abstract

The invention discloses a preparation method of mono-dispersion polysiloxane microspheres with controllable particle size. The preparation method comprises the following three specific steps: (1) hydrolytic process: adding a certain amount of acidic catalyst into de-ionized water, mechanically mixing uniformly to form an acidic aqueous solution with a certain pH (potential of hydrogen) value, adding siloxane monomers according to a ratio, reacting for a period of time while stirring with a certain rotation speed, to form silanol solution; (2) polycondensation process: adding alkaline solution into the reaction system obtained in the step (1) to adjust the pH value of the system, keeping a certain mechanical rotation speed under a normal temperature condition, stirring and reacting for a period of time; and (3) drying process: centrifugally separating the solution obtained in the step (2), washing by mixed solution of ethanol and de-ionized water, drying in a vacuum drying oven, so as to obtain the polysiloxane microspheres with certain particle size. The method disclosed by the invention is simple, heating and nitrogen protecting device are not required, a toxic solvent is not required, and the controllability of the particle size of the microspheres is realized.

Description

technical field [0001] The invention relates to the technical field of preparation of polysiloxane microspheres, in particular to a method for preparing monodisperse polysiloxane microspheres with controllable particle diameters. Background technique [0002] Polysiloxane microspheres are multifunctional microspheres integrating organic and inorganic properties. They have excellent wear resistance, temperature resistance, hydrophobicity and special optical properties. They are often used in inks, cosmetics, coatings, Plastic products and other industries. When the polysiloxane microspheres are applied to the light diffusion plate, the haze of the diffusion plate can be increased without ensuring the excellent transparency of the diffusion plate, so as to achieve the function of protecting eyesight. At present, most of the polysiloxane microspheres in domestic circulation are imported from Japan, Germany, the United States, South Korea and other countries. There are relative...

Claims

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Application Information

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IPC IPC(8): C08G77/06C08G77/20
Inventor 王洪于栋李静张景
Owner SOUTH CHINA UNIV OF TECH
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