Silica gel supported polyolefin catalyst, and preparation method and application thereof

A polyolefin catalyst and silica gel technology, applied in the field of polymers, can solve the problems of increasing the type of active sites and reducing the activity of the catalyst, and achieve the effects of uniform pore size and particle size distribution, improved production efficiency, and large specific surface area

Inactive Publication Date: 2021-08-13
SHANGHAI HONGAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the metal catalyst will reduce the activity of the catalyst after loading, and it will also increase the types of active sites

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation steps of the silica gel carrier are as follows: add 10 g of carbon microspheres (particle size range 10-40 μm) into 400 ml of hydrochloric acid solution with a molar concentration of 1 mol / L and stir evenly to obtain a hydrochloric acid solution containing carbon microspheres; Slowly add methyl orthosilicate to the hydrochloric acid solution of carbon-containing microspheres prepared in the preceding steps and continue to stir, then add 50 g of sodium silicate aqueous solution with a mass concentration of 40% to obtain a silicon source solution; add 10g of template agent PVP (polyvinylpyrrolidone, K12) was stirred evenly to obtain a hydrated silicone gel, and then the resulting gel was transferred to a microwave reaction tank for thermal aging. The microwave power was 300W and the temperature was 90°C. Microwave reaction for 5h The gained product is filtered after cooling, and the gained solid is washed with ethanol / water (the volume ratio of ethanol and ...

Embodiment 2

[0025] The preparation steps for olefin polymerization catalyst are as follows (all operations are carried out under nitrogen protection):

[0026] (1) Put 4 g of the silica gel prepared in Example 1 into an oven at 110° C. to dry for 5 hours, and then add it to the drying reaction flask;

[0027] (2) Add 0.230g of chromium acetate and 0.568g of basic aluminum acetate (stabilized by 1% boric acid) into 25ml of methanol, and stir to obtain a Cr / Al-B composite solution;

[0028] (3) Add the Cr / Al-B composite solution prepared in step (2) to the silica gel obtained in step (1), move the resulting mixture into an ultrasonic reactor and vibrate ultrasonically at 30°C for 30min, filter and The obtained solid was dried in a vacuum oven at 110°C for 12 hours to obtain the catalyst for olefin polymerization, and the obtained catalyst was designated as Cr / Al-B / SG-1. The prepared catalyst was tested by ICP-OES to investigate the active metal components loaded on the catalyst. The test r...

Embodiment 3

[0030] Catalyzed ethylene polymerization steps are as follows (all operations are carried out under nitrogen protection):

[0031] In a fluidized bed reactor, using dry air as the fluidizing gas, activate 20 g of the catalyst Cr / Al-B / SG-1 prepared in Example 2 at 600°C for 8 hours, and cool to room temperature in a nitrogen atmosphere . 1.05g of the activated catalyst was transferred to a 30L isobutane slurry polymerization reactor, and the polymerization test was carried out with ethylene as a monomer: the total pressure of the reactor was 4MPa, the partial pressure of ethylene was 1.6MPa, and the reactor was maintained at 100 ℃, the slurry flow velocity is 2.5m / s, cooling down after maintaining the polymerization reaction for 1 hour, then pouring the reaction solution into 150ml mass concentration is 10% acidified ethanol solution (hydrochloric acid / ethanol=1 / 10) to terminate the reaction, after filtering, The resulting polymer was washed with 30ml of deionized water and 30...

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Abstract

The invention discloses a silica gel supported polyolefin catalyst. The catalyst takes silica gel as a carrier, transition metal salt as active metal and aluminum salt and boron compound as cocatalysts, the silica gel carrier is prepared by combining a sol-gel method with a soft and hard template method, the transition metal salt is selected from one of chromium acetate, chromium nitrate, chromium chloride, manganese acetate, manganese nitrate, manganese chloride, nickel acetate, nickel nitrate or nickel chloride, and the aluminum salt is one of basic aluminum acetate, basic magnesium aluminum carbonate or basic ammonium aluminum carbonate. The invention also discloses a preparation method of the silica gel loaded polyolefin catalyst. The preparation method comprises the following steps: dipping the silica gel carrier into a solution composed of transition metal salt, aluminum salt and a boron compound, carrying out ultrasonic oscillation, filtering, and drying to obtain a solid. The catalyst provided by the invention can be used for olefin polymerization reaction, and not only can improve the production efficiency of the polymerization reaction, but also can improve the melting point of the obtained polymer.

Description

technical field [0001] The invention belongs to the technical field of macromolecules, and in particular relates to a polyolefin catalyst supported by silica gel and a preparation method and application thereof. Background technique [0002] Since the discovery and industrialization of Ziegler-Natta catalysts and silica gel-supported chromium catalysts in the 1950s, catalyst technology has become one of the key core technologies in the polyolefin industry (Wang Wei. Single-site catalyst polyolefin materials Research progress [J]. Petrochemical Industry, 2013, 42(1): 95-103.). Catalysts for olefin polymerization can be divided into two categories: homogeneous catalysts and homogeneous catalysts; among them, although homogeneous catalysts have the advantages of mild reaction conditions, high catalytic activity and good selectivity, there are still difficulties in the separation of catalysts during polymerization reactions , The polymer and the catalyst stick to the kettle, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F110/02C08F4/02C08F4/22C08F4/26C08F4/12
CPCC08F10/00C08F110/02C08F4/025C08F4/22C08F4/26C08F4/12
Inventor 彭晓琪杜刚丁炎金建耀
Owner SHANGHAI HONGAN CHEM
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