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Method for preparing special silica gel carrier with large pore volume and large specific surface area

A technology with large specific surface area and large pore volume, applied in the field of preparation of special silica gel carrier for high-activity gas-phase ethylene polymerization catalyst, to prevent the shrinkage of pore size

Inactive Publication Date: 2011-04-06
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In CN02127599.8, a preparation method of macroporous granular silica gel is introduced. The method described is not suitable for ethylene polymerization catalyst carrier because the pore volume is only 0.8-1.1ml / g.

Method used

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  • Method for preparing special silica gel carrier with large pore volume and large specific surface area
  • Method for preparing special silica gel carrier with large pore volume and large specific surface area
  • Method for preparing special silica gel carrier with large pore volume and large specific surface area

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 1. Dilute industrial sodium silicate with a modulus of 3.1 to a concentration of 10% industrial sodium silicate solution with a mass content of silicon dioxide; add dropwise a sulfuric acid solution with a mass content of 25% at an initial temperature of 20°C to adjust System pH to 2-4, keep the final adjusted pH value at 3.5-4;

[0021] 2. Raise the temperature to the final temperature of 95-100°C, add the specific surface control agent glycerin, and the addition amount of the specific surface control agent is 1% of the mass content of sodium silicate;

[0022] 3. Insulate at the final temperature for 2 hours to carry out hydrothermal reaction; then age at room temperature for 2 hours; wash with water until the mass content of sodium ions is below 0.05%; dry by spray drying: keep the temperature at 400°C; Then carry out particle size classification, the average particle size is 75-150 microns, to obtain the final product of macroporous microsphere silica gel with water...

Embodiment 2

[0027] 1. Dilute industrial sodium silicate with a modulus of 3.2 to a concentration of 15% industrial sodium silicate solution with a mass content of silicon dioxide; add dropwise a sulfuric acid solution with a mass content of 20% at an initial temperature of 30°C to adjust System pH to 2-4, keep the final adjusted pH value at 3.5-4;

[0028] 2. Raise the temperature to the final temperature of 80-85°C, add the specific surface control agent ethyl acetate, and the addition amount of the specific surface control agent is 3% of the mass content of sodium silicate;

[0029] 3. Insulate at the final temperature for 3 hours to carry out hydrothermal reaction; then age at room temperature for 1 hour; wash with water until the mass content of sodium ions is below 0.05%; dry by spray drying: keep the temperature at 500°C; Then carry out particle size classification, the average particle size is 75-150 microns, to obtain the final product of macroporous microsphere silica gel with wa...

Embodiment 3

[0034] 1. Dilute the industrial sodium silicate with a modulus of 3.3 to a concentration of 20% industrial sodium silicate solution with a mass content of silicon dioxide; add dropwise a sulfuric acid solution with a mass content of 18% at an initial temperature of 40°C to adjust System pH to 2-4, keep the final adjusted pH value at 3.5-4;

[0035] 2. Raise the temperature to the final temperature of 90-95°C, add the specific surface control agent ethylene glycol, and the addition amount of the specific surface control agent is 3% of the mass content of sodium silicate;

[0036] 3. Insulate at the final temperature for 2 hours to perform hydrothermal reaction; then age at room temperature for 2 hours; wash with water until the mass content of sodium ions is below 0.05%; dry by spray drying: keep the temperature at 600°C; Then carry out particle size classification, the average particle size is 75-150 microns, to obtain the final product of macroporous microsphere silica gel wi...

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Abstract

The invention relates to a method for preparing a special silica gel carrier with a large pore volume and a large specific surface area. The method is characterized by comprising the following process steps of: diluting industrial sodium silicate; adding inorganic acid solution dropwise at the initial temperature of between 20 and 40 DEG C, adjusting the pH value of a system to be 2 to 4, heating to the final temperature of between 80 and 100 DEG C and adding a specific surface control agent which may be one or more of glycol, ethyl acetate, glycerol, acetone and trichloroethane; preserving the heat for 2 to 4 hours and performing a hydro-thermal reaction; ageing for 1 to 2 hours; washing; drying; and performing particle size classification to obtain the final product.

Description

technical field [0001] The invention relates to a preparation method of silica gel, more specifically, relates to a preparation method suitable for special silica gel carrier used as a highly active gas-phase method ethylene polymerization catalyst. Background technique [0002] At present, in the preparation process of gas-phase polymerization polyethylene catalyst, silica gel has been widely used as a carrier. The catalyst made of this carrier is mainly used in the production of LLDPE. The pore characteristics of the currently used silica gel carrier are: pore volume 1.6ml / g, specific surface area 300-350m2 / g, average particle size: 40-50 microns. The catalyst activity prepared by using this carrier can only reach 3000-4000gPE / gcat, which makes the production cost of polyethylene remain high. The latest foreign research shows that the catalyst activity prepared by using the special silica gel carrier with large pore volume and large specific surface area can reach It can...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F2/34C08F4/02
Inventor 胡毅刘红光于海斌郑书忠尹世容郑秋红
Owner CHINA NAT OFFSHORE OIL CORP
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