Modified preparation method of silica gel carrier

A carrier, silica gel technology, applied in catalyst carriers, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of expensive solvent, large solvent consumption, difficult recovery, etc.

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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  • Modified preparation method of silica gel carrier
  • Modified preparation method of silica gel carrier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]Add 20ml of sodium carbonate ethanol aqueous solution with a mass fraction of 6% into the reaction kettle (the volume ratio of ethanol to water is 1:6), turn on the stirring, raise the temperature to 50°C, and add the concentration of 1.2mol / L at a flow rate of 3ml / min Sodium silicate aqueous solution and 1.0mol / L sulfuric acid aqueous solution, when the pH value of the solution in the reactor reaches 11, stop adding the mixed aqueous solution, and react at constant temperature for 0.5h. Add 16mL of magnesium nitrate and aluminum nitrate aqueous solutions with a mass fraction of 4% at a flow rate of 8ml / min (the molar ratio of the two nitrates is 1:1), and react at a constant temperature for 1.0h after the addition is complete; add a concentration of 1.0mol at a flow rate of 6mL / min / L sulfuric acid n-butanol aqueous solution (the volume ratio of n-butanol to water is 1:15), stop adding n-butanol sulfuric acid solution when the pH value of the solution is 9, and react at ...

Embodiment 2

[0039] The preparation process is the same as in Example 1, except that 20ml of potassium carbonate ethanol aqueous solution with a mass fraction of 6% is added to the reaction kettle (the volume ratio of ethanol to water is 1:6), the stirring is turned on, and the temperature is raised to 50° C., at 3ml / min At the same time, add a potassium silicate aqueous solution with a concentration of 1.2mol / L and a sulfuric acid aqueous solution with a concentration of 1.0mol / L. When the pH value of the solution in the reactor reaches 11, stop adding the mixed aqueous solution and react at a constant temperature for 0.5h. Add 16mL of zinc nitrate and aluminum nitrate aqueous solutions with a mass fraction of 4% at a flow rate of 8ml / min (the molar ratio of the two nitrates is 1:1), and react at a constant temperature for 1.0h after the addition; Other conditions are the same as in Example 1. The test results are shown in Table 1.

Embodiment 3

[0041] The preparation process is the same as in Example 1, except that 1,3-butanediol sulfuric acid aqueous solution with a concentration of 1.0mol / L is added at a flow rate of 4mL / min, and the volume ratio of 1,3-butanediol to water is 1:10 Other conditions Same as Example 1. The test results are shown in Table 1.

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Abstract

The invention relates to a modified preparation method of a silica gel carrier. The ethanol aqueous solution of carbonate is used as the bottom liquid, and silica sol is generated by adding silicate and inorganic acid in parallel, and two aqueous solutions of nitrate are added during the generation of the sol. ; During the gel reaction, the pH value of the reaction solution is adjusted by adding an organic alcohol aqueous solution of an inorganic acid, and the preparation of silica gel is completed through a high-temperature hydrothermal reaction. Without affecting the pore volume of silica gel, this process can greatly increase the specific surface area of ​​silica gel, thereby improving the basic physical properties of carrier silica gel; the process is simple to operate, has good repeatability, and low energy consumption, providing technical support for industrial device production. support.

Description

technical field [0001] The invention relates to a modified preparation method of a silica gel carrier, in particular to a modified 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. [0003] As a catalyst carrier, silica gel has a suitable pore volume, pore size and distr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/08B01J21/14B01J23/04B01J23/06B01J32/00B01J35/10B01J37/00B01J37/10
Inventor 王海王玲玲刘文霞任峰张鹏徐人威董万卓曹庚振陈雪蓉郝萍李忠
Owner PETROCHINA CO LTD
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