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Preparation method of large-pore volume flatting agent

A matting agent and macroporous volume technology, applied in the chemical industry, can solve the problems of high porosity of silica, unsatisfactory silica, and easily damaged structure, and achieve the reduction of surface area, firm structure, transparency and transparency. high effect

Inactive Publication Date: 2012-01-25
嘉兴市博豪家纺有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the silica produced by the wet method, the product properties obtained by different process routes are different: the silica prepared by the gel method has a firm structure, narrow pore size distribution, good transparency, but low porosity; The silica prepared by the precipitation method has a high porosity, but the structure is loose, the structure is easily destroyed under high shear, and the transparency is also poor (for reference, see the invention patent application number 02156478.7 of the State Intellectual Property Office)
[0004] So far, the silica produced by the existing technology of the liquid phase method cannot meet the requirements of firm structure and high porosity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The raw material components are by mass: 15 g tetraethyl orthosilicate (TEOS purity 28%), 0.20 g 2nd generation HPAE (10 -4 mol, pentaerythritol as the core), water (deionized water) 100 g, concentrated hydrochloric acid 25 g.

[0021] Preparation of high-efficiency silica matting agent with large pore volume: Dissolve 2nd generation HPAE in the prepared hydrochloric acid solution, adjust pH=1, stir for 30 minutes to dissolve until a uniform solution is formed; then slowly add TEOS dropwise into the solution And then stirred for 30 minutes; put the above mixed solution into a sealed reaction vessel, raised the temperature to 60 °C, kept stirring for 24 hours, and obtained a light yellow gel. The obtained gel was aged for 4 h, then washed, dried, and placed in 400 o C was calcined in a muffle furnace for 3 h, and finally the finished product was obtained by crushing and grading.

Embodiment 2

[0023] The raw material components are by mass: 13 g of orthosilicate methyl ester (TMOS purity is 30%), 0.46 g of 3rd generation HPAE (10 -4 mol, pentaerythritol as the core), water (deionized water) 100 g, concentrated hydrochloric acid 25 g.

[0024] Preparation of high-efficiency silica matting agent with large pore volume: Dissolve the third-generation HPAE in the prepared hydrochloric acid solution, adjust the pH=2, stir for 30 minutes to dissolve until a uniform solution is formed; then slowly add TEOS dropwise into the solution Then stir for 45 min; put the above mixed solution into a sealed reaction vessel, raise the temperature to 70°C, keep stirring for 18 h, and obtain a light yellow gel. The obtained gel was aged for 3 h, then washed, dried, and placed in 450 o C was calcined in a muffle furnace for 4 h, and finally the finished product was crushed and classified.

Embodiment 3

[0026] The raw material components are by mass: 20 g of orthobutyl silicate (TBOS purity is 32%), 0.97 g of 4th generation HPAE (10 -4 mol, pentaerythritol as the nucleus), water (deionized water) 100g, concentrated hydrochloric acid 25g.

[0027] Preparation of high-efficiency silica matting agent with large pore volume: Dissolve the 4th generation HPAE in the prepared hydrochloric acid solution, adjust the pH=3, stir for 30 minutes to dissolve until a uniform solution is formed; then slowly add TEOS dropwise into the solution And then stirred for 45 minutes; put the above mixed solution into a sealed reaction vessel, raised the temperature to 50 °C, kept stirring for 36 hours, and obtained a yellow gel. The obtained gel was aged for 4 h, then washed, dried, and placed in 500 o C was calcined in a muffle furnace for 5 h, and finally the finished product was crushed and classified.

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Abstract

The invention relates to a preparation method of a large-pore volume flatting agent, belonging to the field of chemical industry. The preparation process thereof comprises the following steps: a. dissolving a template agent in an acid solution at room temperature, adjusting the pH value to 1-3, and stirring to form a homogeneous solution; b. slowly and dropwise adding a silicon source to the homogeneous solution while stirring, pouring into a sealed reaction vessel after uniformly stirring, heating up to 40-80 DEG C, and stirring to make the materials to react for 18-48 hours so as to obtain a gel; and aging the gel obtained in step b for 3-8 hours, washing, drying, calcining in a muffle furnace at 350-550 DEG C for 2-6 hours, and finally crushing and classifying to obtain the finished large-pore volume flatting agent. The invention has the advantage of simple and reasonable process design, and the product has the advantages of large pore volume, large specific area, high purity, moderate DBP absorption value, favorable dispersibility, high transparency and the like.

Description

technical field [0001] The invention relates to a preparation method of a large pore volume matting agent, which belongs to the field of chemical industry. Background technique [0002] In the coatings industry, silica is used due to its refractive index being similar to that of most resins used in this industry (DE-PS 24 14 478, DE-PS 17 67 332, DE-OS 16 69 123, DE-AS 15 92 865, DE-A 38 15 670), used in lacquer has good optical properties, so silica becomes the first choice for high-grade paint matting agent. The main characteristic parameters affecting the silica matting agent are pore volume (void ratio), average particle size and pore size distribution, surface treatment, etc. What was used as matting agent earlier was amorphous silica produced by gas phase method. For example, Chinese patent application CN2822370.5 discloses a silica matting agent of amorphous granular silica, wherein the silica is oxidized Polyolefin wax to be treated. [0003] The current methods o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12
Inventor 丁海燕陈枫帅宏喜
Owner 嘉兴市博豪家纺有限公司
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