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Method for preparing silica gel carrier with dual-mode pore size distribution

A technology of pore size distribution and silica gel, which is applied in the field of preparation of silica gel carriers with dual-mode pore size distribution, which can solve the problems of narrow difference in dual-mode pore size distribution, poor fluidity and disadvantages of supported catalysts, etc.

Active Publication Date: 2014-04-02
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent uses a sol-gel process to prepare a silica gel carrier with a dual-mode pore size distribution. The pore size of the silica gel carrier is easily affected by reaction conditions such as aging time and pH value, resulting in a narrow difference in the dual-mode pore size distribution and a small pore size. The large pore diameter peak is generally smaller than , which is not conducive to the loading of the methylalumoxane / metallocene catalyst system with a relatively large molecular weight, and is easy to Poor fluidity of the supported catalyst

Method used

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  • Method for preparing silica gel carrier with dual-mode pore size distribution
  • Method for preparing silica gel carrier with dual-mode pore size distribution

Examples

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Embodiment 1

[0028] At 50°C, add 5% sulfuric acid solution dropwise to the sodium silicate solution containing 20% ​​silicon dioxide until the pH is 9-9.5 to form a silicon dioxide sol, continue stirring for 1 hour, and the sol hardens into silicon dioxide Gel, then raise the temperature to 90°C and age for 5 hours. After aging, lower the temperature to room temperature, add 5% sulfuric acid solution dropwise until the pH is 0.5-1, let it stand for 1 hour, then add ethanol and polyethylene glycol (Aladdin's reagent) with a commercially available average molecular weight of 4000, and stir Fully dissolve PEG, the ratio of ethanol to water is 1:5, the amount of PEG added is 12% of the total solution, and 20% sodium silicate solution of silicon dioxide is added dropwise at 35°C until the pH rises to 3.5 to obtain the second stage Gel, raise the temperature to 80° C., and age for 6 hours to obtain a dual-mode silica gel slurry. After washing with deionized water for 3 times in a plate and fram...

Embodiment 2

[0030] At 40°C, add 8% sulfuric acid solution dropwise to the sodium silicate solution with 15% silicon dioxide until the pH is 8.5-9 to form a silicon dioxide sol, continue to stir for 0.5 hours, and the sol hardens into silicon dioxide Gel, then raise the temperature to 70°C and age for 7 hours. After aging, lower the temperature to room temperature, add 8% sulfuric acid solution dropwise to pH 0.5-1, let it stand for 3 hours, then add 1-butanol and polyethylene glycol (Aladdin reagent) with an average molecular weight of 8000 in the market , Stir to fully dissolve PEG, the ratio of 1-butanol to water is 1:4, the amount of PEG added is 8% of the total solution, add 20% silicon dioxide sodium silicate solution dropwise at 35°C until the pH rises to 3.5 , to obtain the second-stage gel, raise the temperature to 90° C., and age for 6 hours to obtain a dual-mode silica gel slurry. After washing with deionized water for 4 times in a plate and frame filter press, dry it with a GL...

Embodiment 3

[0032] At 40°C, add 5% sulfuric acid solution dropwise to the sodium silicate solution containing 20% ​​silica until the pH is 8.5-9 to form a silica sol, continue stirring for 0.5 hours, the sol hardens into silica Gel, then raise the temperature to 80°C and age for 7 hours. After aging, lower the temperature to room temperature, add 5% sulfuric acid solution dropwise to pH 0.5-1, let it stand for 3 hours, then add ethanol and commercially available polypropylene glycol (Aladdin reagent) with an average molecular weight of 3000, and stir to make PPG Fully dissolved, the ratio of ethanol to water is 1:10, the amount of PPG added is 10% of the total solution, and 20% sodium silicate solution of silicon dioxide is added dropwise at 50°C until the pH rises to 3, and the second stage condensation is obtained. gel, raise the temperature to 80° C., and age for 6 hours to obtain a dual-mode silica gel slurry. After washing with deionized water for 4 times in a plate and frame filter...

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Abstract

Disclosed is a method for preparing silica gel with dual-mode pore size distribution by taking an inorganic silicate and an inorganic acid as raw materials and through two stages of gel reaction. In the first stage, silica gel with the pore size distribution of between 50 angstroms and 500 angstroms is prepared by adopting a sol-gel process and adjusting the pH value, the reaction temperature and the aging time; and in the second stage, the second-stage silica gel pore size is adjusted and controlled by adding polyethylene oxide or polypropylene oxide as a template reagent, the second-stage pore size distribution is between 20 angstroms and 150 angstroms, and the silica gel carrier having a difference between the average pore sizes of the two stages being greater than 50 angstroms is prepared. A catalyst prepared from the obtained carrier is polymerized to obtain an olefin polymer with wide molecular weight distribution.

Description

technical field [0001] The invention relates to a preparation method of a polyolefin catalyst carrier, in particular to a preparation method of a silica gel carrier with dual-mode pore size distribution. technical background [0002] Silica gel has a wide range of industrial applications, such as desiccants and catalyst supports, including olefin polymerization catalyst supports. These olefin polymerization catalysts generally contain a catalytic transition metal component, such as chromium, which can be deposited on a silica aerosol support by high temperature oxidation. Through olefin polymerization, controlling reaction temperature, pressure, solvent, catalyst and other polymerization processes, polyolefin products with different molecular weight distribution and melt index can be prepared. Among the many uses of polyolefin resins, hardness, strength and environmental stress (ESCR) are important indicators. These attributes increase correspondingly when the molecular we...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F4/02
Inventor 王雄王海徐人威韩晓昱葛汉青任峰郝萍马维丽刘文霞吴江王丹丹张翠玲巨娟侠高冬梅
Owner PETROCHINA CO LTD
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