A preparation method of modified polysiloxane microspheres with controllable particle size

A technology of polysiloxane and siloxane monomer, which is applied in the field of preparation of modified polysiloxane microspheres, which can solve the problems of limited application range and achieve the effect of narrow particle size distribution and uniform particle size

Active Publication Date: 2020-03-10
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Although polysiloxane microspheres have many excellent properties, the scope of application is still limited, such as difficult to apply in some high refractive index, oily medium and other fields

Method used

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  • A preparation method of modified polysiloxane microspheres with controllable particle size
  • A preparation method of modified polysiloxane microspheres with controllable particle size
  • A preparation method of modified polysiloxane microspheres with controllable particle size

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preparation example Construction

[0048] The invention provides a preparation method of modified polysiloxane microspheres, comprising the following steps:

[0049] A) mixing siloxane monomers, acid catalysts and water, and hydrolyzing to obtain a silanol solution;

[0050] The electrical conductivity of the water is 5-60 μs / cm;

[0051] B) Putting a basic catalyst into the silanol solution obtained in the above steps to carry out a condensation reaction, then raising the temperature and adding a modifying agent, and reacting again to obtain modified polysiloxane microspheres.

[0052]In the invention, the siloxane monomer, the acidic catalyst and water are firstly mixed, and after hydrolysis, a silanol solution is obtained.

[0053] The electrical conductivity of the water in the present invention is preferably 5-60 μs / cm, more preferably 15-50 μs / cm, more preferably 25-40 μs / cm, most preferably 30-35 μs / cm.

[0054] The present invention has no special restrictions on the siloxane monomers, and the siloxan...

Embodiment 1

[0075] 2μm microspheres

[0076]In a 2L four-neck flask equipped with a stirring, thermometer and reflux condenser, add 1404g of water with a conductivity of 5μs / cm, add 0.8g of hydrochloric acid, raise the temperature to 50°C, and add methyl trimethoxyl dropwise at a stirring speed of 200rpm Base silane 163g, equilibrate reaction for 0.5 hours, then add ammonia water 30g, 20rmp reaction 8h. The reaction solution was heated to 90°C, 15g of double-capped heads were added, reacted for 9h, centrifuged and washed with water until neutral, and dried in a drying oven at 150°C to obtain hydrophobically modified polysiloxane microspheres.

[0077] The hydrophobically modified polysiloxane microspheres prepared in Example 1 of the present invention were characterized and counted, and the yield was 92.8%.

[0078] see figure 1 , figure 1 Scanning electron micrograph of the hydrophobically modified polysiloxane microspheres prepared in Example 1 of the present invention. Depend on f...

Embodiment 2

[0086] 3μm microspheres

[0087] In a 2L four-neck flask equipped with a stirring, thermometer and reflux condenser, add 1404g of water with a conductivity of 7μs / cm, add 0.9g of acetic acid, raise the temperature to 30°C, and add methyl trimethoxyl at a stirring speed of 300rpm Silane 176.8g, equilibrated for 1 hour, then added KOH 20g and stirred evenly, 25rmp for 10 hours. Heat the reaction solution to 80°C, add 5g of KH570, react for 7h, centrifuge and wash with water until neutral, and dry in a drying oven at 150°C to obtain acrylic modified silicone resin microspheres.

[0088] The acrylic-modified silicone resin microspheres prepared in Example 2 of the present invention were characterized and counted, and the yield was 94.5%.

[0089] see image 3 , image 3 Scanning electron microscope image of the acrylic modified silicone resin microspheres prepared in Example 2 of the present invention. Depend on image 3 It can be seen that the particle size of the acrylic mo...

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Abstract

The invention provides a preparation method of modified polysiloxane microspheres. The preparation method comprises steps as follows: firstly, a silanol solution is obtained by mixing and hydrolyzing siloxane monomers, an acidic catalyst and water; the electrical conductivity of the water is 5-60 mu s / cm; an alkaline catalyst is added to the silanol solution obtained in the step, a condensation reaction is performed, the mixture is heated, a modifier is added for a reaction again, and the modified polysiloxane microspheres are obtained. The modified polysiloxane microspheres containing multiple active genes are prepared by adding the modifier; the particle sizes of the modified polysiloxane microspheres are controlled by adjusting the electrical conductivity of the raw material water, so that the prepared modified polysiloxane microspheres have narrower particle size distribution, are uniform in particle size and meet the demands of different products. Besides, the provided preparation method has higher product yield, adopts a simple process, is easy to operate, doesn't require organic solvents, is environment-friendly and facilitates large-scale production.

Description

technical field [0001] The invention belongs to the technical field of organosilicon materials, and relates to a preparation method of modified polysiloxane microspheres, in particular to a preparation method of modified polysiloxane microspheres with controllable particle size. Background technique [0002] Polysiloxane, the general formula is (R n SiO 4-n / 2 ) m , also known as silicone, is a type of polymer with repeated Si-O bonds as the main chain and organic groups directly connected to silicon atoms, where R represents organic groups, such as methyl, phenyl, etc.; n is The number of organic groups connected to the silicon atom (between 1 and 3), m is the degree of polymerization (m is not less than 2). The main chain structure of polysiloxane is Si-O-Si structure, which is the same as quartz in essence, the difference is that organic groups are connected to its side groups. Silane monomers and polysiloxanes are generally referred to as organosilicon compounds, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/08C08G77/06
CPCC08G77/06C08G77/08C08G77/38
Inventor 尤小姿张迪宋丹丹童锋白俊玲刘继
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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