A kind of preparation method of silica gel carrier

A technology of carrier and silica gel, which is applied in the direction of catalyst carrier, chemical instrument and method, catalyst activation/preparation, etc. It can solve the problems of cumbersome operation steps, large solvent consumption, and long time for distilling and removing water.

Active Publication Date: 2022-01-04
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The azeotropic distillation method has the problems of long time for distilling and removing water, expensive solvents, and high energy consumption; the organic solvent replacement method has the disadvantages of cumbersome operation steps, large solvent consumption, and difficult recovery.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Put 60ml of dilute sulfuric acid solution with a concentration of 1.1mol / L in a closed reactor, add 3.0ml of 5.0mol / L ammonia solution at 30°C and react for 20min; raise the temperature to 50°C under stirring conditions, and add the mass fraction at a flow rate of 8ml / min It is 16mL of 4% magnesium nitrate and aluminum nitrate aqueous solution (the molar ratio of the two nitrates is 1:1). Add a 1.2mol / L sodium silicate aqueous solution at a flow rate of 3ml / min, adjust the pH of the reaction solution to 7, add distilled water to disperse the sol thoroughly, and react at a constant temperature for 0.5h. Add 20ml of ethanol aqueous solution of sodium carbonate with a mass fraction of 6% at a flow rate of 4ml / min (the volume ratio of ethanol to water is 1:6), and react at a constant temperature for 0.5h. Add a 1.2 mol / L sodium silicate aqueous solution at a flow rate of 4 ml / min, adjust the pH of the reaction solution to 11, and react at a constant temperature for 1.0 h. ...

Embodiment 2

[0043] The preparation process was the same as in Example 1, except that 6.0ml of 5.0mol / L ammonia solution was added at 30°C to react for 20min; the temperature was raised to 50°C, and 16mL of 4% magnesium nitrate and aluminum nitrate aqueous solution ( The molar ratio of the two nitrates is 1:1). Add a potassium silicate aqueous solution with a concentration of 1.2 mol / L at a flow rate of 3 ml / min, adjust the pH value of the reaction solution to 6, add distilled water to completely disperse the sol, and react at a constant temperature for 0.5 h. Other conditions are identical with embodiment 1. The test results are shown in Table 1.

Embodiment 3

[0045] The preparation process was the same as in Example 1, except that 20 ml of potassium carbonate ethanol aqueous solution with a mass fraction of 8% was added at a flow rate of 4 ml / min (the volume ratio of ethanol to water was 1:9), and the reaction was performed at a constant temperature for 0.5 h. Add 1.2 mol / L sodium silicate water solution at a flow rate of 4 ml / min, adjust the pH value of the reaction solution to 12, and react at a constant temperature for 1.0 h. Other conditions are identical with embodiment 1. The test results are shown in Table 1.

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Abstract

The invention relates to a preparation method of a silica gel carrier. During the preparation of the silica gel carrier, two kinds of nitrate aqueous solution and carbonate ethanol aqueous solution are added; during the gel reaction, the reaction is regulated by adding an organic alcohol aqueous solution of an inorganic acid The pH value of the solution is adjusted, and the preparation of silica gel is completed through high-temperature hydrothermal reaction. This process greatly increases the specific surface area of ​​silica gel, improves the pore volume and distribution of silica gel, and improves the basic physical properties of silica gel carrier.

Description

technical field [0001] The invention relates to a preparation method of a silica gel carrier, in particular to a preparation method of a high specific surface area silica gel carrier. Background technique [0002] Silicone is extremely versatile. Among them, silica gel is particularly suitable as a catalyst carrier because of its high specific surface area. At present, carrier silica gel is mainly used in traditional Ziegler-Natta catalysts and metallocene olefin polymerization catalysts. There are also many reports at home and abroad on the preparation process of inorganic methods, such as using silicate as the mother liquor, and then adding silicate and inorganic acid to react; Or use silicate and inorganic acid as the mother liquor, add inorganic acid to adjust its pH value; or use parallel flow mode, add silicate and inorganic acid at the same time for reaction. As a catalyst carrier, silica gel has a suitable pore volume, pore size and distribution, and a high specifi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/08B01J21/14B01J23/04B01J35/10B01J37/00B01J37/10B01J32/00
Inventor 王海刘文霞王玲玲任峰徐人威董万卓张鹏陈雪蓉郝萍曹庚振李忠
Owner PETROCHINA CO LTD
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