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Preparation method of dual-mode pore size distribution silica gel carrier

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 problems such as unfavorable, narrow difference in dual-mode pore size distribution, and poor fluidity of supported catalysts.

Active Publication Date: 2016-05-11
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 particle size. Large aperture peaks are generally smaller than It is not conducive to the support of the methylalumoxane / metallocene catalyst system with a relatively large molecular weight, and it is easy to cause poor fluidity of the supported catalyst

Method used

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  • Preparation method of dual-mode pore size distribution silica gel carrier
  • Preparation method of dual-mode pore size distribution silica gel carrier

Examples

Experimental program
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Embodiment 1

[0026]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 until the pH is 0.5-1, let stand for 3 hours, then add ethanol and F68PEO-PPO-PEO ternary block copolymer, stir to fully dissolve F68, The ratio of ethanol to water is 1:10, and the amount of F68 added is 10% of the total solution. At 30°C, add 20% silicon dioxide sodium silicate solution dropwise until the pH rises to 3, and the second stage gel is obtained. High temperature to 80°C, aging for 6 hours to obtain dual-mode silica gel slurry. After washing with deionized water for 3 times in a plate and frame filter press, dry it with a GLP-150 high-speed centrifugal spray dryer. The inlet and outlet temperatures ...

Embodiment 2

[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 stand for 1 hour, then add ethanol and F68PEO-PPO-PEO ternary block copolymer, stir to fully dissolve F68, The ratio of ethanol to water is 1:5, the amount of F68 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, and the second stage gel is obtained. The temperature was raised to 80° C. and aged 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 with a GLP-150 high-speed centrifuga...

Embodiment 3

[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 until the pH is 0.5-1, let it stand for 3 hours, then add 1-butanol and F68PEO-PPO-PEO ternary block copolymer, stir to make F68 fully Dissolve, the ratio of 1-butanol to water is 1:4, the amount of F68 added is 8% 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 90° 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 frame filter press, dry it with a GLP-150 high-speed centrifugal s...

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Abstract

The invention discloses a preparation method of a double-mould-pore-size-distribution silica-gel carrier through two stage gel reactions by using an inorganic silicate and an inorganic acid as raw materials. In the first stage, a sol-gel technology is adopted, and silica gel pore size distribution of which ranges from 50 angstroms and 500 angstroms is prepared by adjusting the pH value, the reaction temperature and the ageing time. In the second phase, the pore size of the silica gel is adjusted by adding a ternary block copolymer of polyethylene oxide-polypropylene oxide-polyethylene oxide (PEO-PPO-PEO) as a template reagent. The pore size distribution in the second phase ranges from 20 angstroms and 150 angstroms. The silica-gel carrier, the difference of the average pore sizes of which in the two stages is larger than 50 angstroms, is prepared. Olefin copolymer with wide molecular weight distribution can be obtained by polymerization by utilization of a catalyst prepared by the carrier.

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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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/02C08F4/02
Inventor 王雄姚培洪徐人威朱博超韩晓昱任峰郝萍葛汉青刘文霞吴江王丹丹王海巨娟侠高冬梅
Owner PETROCHINA CO LTD