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Preparation method of microspherical silica used as alkene polymerization catalyst carrier

A spherical silica and silica technology, which is applied in the treatment of dyed low molecular organic compounds, fibrous fillers, etc., can solve the problems of high temperature operation and residual impurities, and achieve the effects of no three wastes, low cost and simple preparation method.

Active Publication Date: 2005-08-24
吉化集团吉林市星云化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0028] Molten salt hole reaming method, there are problems such as high temperature operation and residual impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] 500ml (SiO 2 Tetraethoxysilane with a content ≥ 28%) was dissolved in 200ml of 30% (v / v) ethanol-water solution, under stirring, an acidic catalyst was added dropwise, and the hydrolysis and polycondensation reaction was carried out at 65°C. After the reaction, pour out The upper liquid, the reaction product was soaked in deionized water for 10 hours, then washed with ethanol, and the resulting gel was aged overnight at room temperature.

[0070] The above-mentioned gel was put into a colloid mill for refinement for one hour. At the beginning, dilute nitric acid (1.46mol / L) was slowly added to adjust the pH value to 1-2. Then add 20ml, the content is 3.42×10 -3 The surfactant of mol / L, surfactant is made up of 1 part (wt) fatty alcohol polyoxyethylene ether and 2 parts (wt) sodium dodecylbenzene sulfonate. Then add 50ml (17mol / L) of urea solution. Finally, it is processed with a high-speed shearing machine for 30 minutes, and the number of revolutions is controlled a...

Embodiment 2

[0074] 500ml (SiO 2 Tetraethoxysilane with a content ≥ 28%) was dissolved in 250ml of 30% (v / v) ethanol-water solution, under stirring, an acidic catalyst (0.5mol acid / mol tetraethoxysilane) was added dropwise, at 70°C After reacting for one hour, the resulting product was soaked in deionized water for 8 hours, washed with ethanol, and aged overnight at 60°C to obtain a silica gel.

[0075] Put the above-mentioned silica gel into a colloid mill and carry out a refinement treatment for 1.5 hours. At the initial stage of treatment, slowly add acrylic acid solution, the concentration of which is 1.46mol / L, adjust the pH value to 0.5-1.0, then add 10ml (3.42×10 -3 mol / L) surfactant composition. The surfactant composition is composed of 1 part (wt) of Tween and 1.5 parts (wt) of sodium dodecylbenzenesulfonate. Finally, add 30ml, 17mol / L formamide solution. After the colloid mill is processed, it is processed with a high-speed shearing machine for 30 minutes, and its rotation sp...

Embodiment 3

[0079] 500ml of 40% (wt / wt) liquid silicon dioxide was heated to 60°C under constant stirring, and ammonium chloride solution was slowly added dropwise. The concentration is 10%. After adding 30ml of ammonium chloride solution, keep it at 60°C and age it overnight to form a silica gel.

[0080] After soaking and washing the above-mentioned silica gel with deionized water, put it into a colloid mill for refining treatment for one hour. After being treated by colloid mill for 10 minutes, start to add dilute hydrochloric acid (2%) to adjust the pH value to 1-2. Then add the surfactant combination and weigh 20ml, and the content is 3.42×10 -3 mol / L, the surfactant composition is composed of 1 part (wt) of Span and 0.5 part (wt) of sodium dodecylbenzenesulfonate. Finally, 60ml (17mol / L) of urea aqueous solution was added. After the thinning process is finished, it is processed with a high-speed shearing machine for 20 minutes, and its number of revolutions is 7000 rpm. Silica s...

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Abstract

A SiO2 microball as the carrier of catalyst for polymerizing ethylene or alpha-olefin is prepared through preparing silicon gel, adding modifiers A, B and C, mechanical homogenizing and fining to become sol, spray drying to become dried microspherical SiO2 gel, and calcining. It has high specific surface area and porosity.

Description

technical field [0001] The invention relates to a preparation method and application of catalyst carrier microspherical silica suitable for ethylene polymerization or copolymerization with alpha-olefin. Background technique [0002] Microspherical SiO 2 (10-70 μm) as a catalyst carrier has been widely used in olefin polymerization catalysts, especially in gas-phase fluidized bed olefin polymerization catalysts. Many patents (US.4293673, US.4303565, US.4303566, US.4303771) have disclosed microspherical SiO 2 As a carrier, it is used in the catalyst of fluidized bed ethylene polymerization process. [0003] In order to adapt to the requirements of gas-phase fluidized bed fluidization engineering, micro-spherical SiO 2 It must have suitable bulk density, average particle size and particle size distribution, good fluidity and mechanical strength, etc. At the same time, as an olefin polymerization catalyst carrier SiO 2 , but also to meet the requirements of polymerization r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/02C08F10/02C08K7/18C09C1/28C09C3/08
Inventor 李长海于广臣郝春林李殿起
Owner 吉化集团吉林市星云化工有限公司