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Method for preparing spherical catalyst for propylene polymerization

A propylene polymerization and catalyst technology, which is applied in the field of preparation of spherical catalysts, can solve the problems of increasing the rotation time of mechanical equipment, the large amount of titanium tetrachloride used, and the long production process route, so as to save raw materials, save energy, and improve fluidity. Good results

Inactive Publication Date: 2010-05-26
LIAONING DINGJIDE PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the conventional method: 1) when alcohol and magnesium chloride synthesize the magnesium chloride alcoholate carrier, magnesium chloride and alcohol will be divided into two steps and dispersed in white oil and silicone oil, and the white oil and silicone oil amount of use are large, and white oil and silicone oil are finally has to be washed away, thus wasting resources
2) In the catalyst synthesis step, the volume-to-mass ratio of titanium tetrachloride and magnesium chloride alkoxide carrier for titanium loading reaches 15-20L / kg, and the usage amount of titanium tetrachloride is large, and the subsequent recovery of excessive titanium tetrachloride , which increases the workload, not only wastes resources and energy, but also causes harm to the environment by using a large amount of titanium tetrachloride
3) The production process route is relatively long, which increases the rotation time of mechanical equipment
4) The product particles are uneven

Method used

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  • Method for preparing spherical catalyst for propylene polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 Spherical catalyst for propylene polymerization

[0025] The preparation method is as follows:

[0026] 1) Carrier preparation:

[0027] In a 500L white steel reaction kettle equipped with a mechanical stirrer and a thermometer fully replaced by nitrogen, add 300L of white oil and 60L of silicone oil, then put in 30kg of anhydrous magnesium chloride, and add 51L of absolute ethanol (the mixture of anhydrous magnesium chloride and absolute ethanol) The molar ratio is 1:2.8), heat up, melt at 100-130°C, and fully dissolve; then quickly emulsify the above-prepared mixture through an emulsifier and transfer it to the second reaction kettle that has previously added 1500L hexane and cooled to -30°C until the transfer of the material is completed, the final temperature does not exceed 0 °C and suction filtration; washing with hexane to remove silicone oil and white oil, and drying in a vacuum to obtain 60 kg of spherical particles, after screening by a vibrating si...

Embodiment 2

[0031] Example 2 Spherical catalyst for propylene polymerization

[0032] The preparation method is as follows:

[0033] 1) Vector preparation

[0034] The difference from Example 1 is that the addition of absolute ethanol is 55L (the molar ratio of anhydrous magnesium chloride to absolute ethanol is 1: 3.0); the carrier between 30 and 100 microns is taken after vibrating sieve screening, and the Analysis of its composition as MgCl 2 2.50C 2 h 5 Oh.

[0035] 2) Catalyst synthesis

[0036] Take the MgCl prepared in the above steps 2 2.50C 2 h 5 Add 50kg of OH spherical carrier into a stirred tank filled with 150L hexane after being fully replaced by nitrogen, cool down to -10°C, then slowly drop into a tank filled with 350L titanium tetrachloride for titanium and cool to - In the reactor at 10°C, control the pressure inside the kettle to 0.1Mpa, slowly raise the temperature to 40°C, then add 10L of diisobutyl phthalate (DIBP), continue to raise the temperature to 100°C...

Embodiment 3

[0037] Example 3 Spherical catalyst for propylene polymerization

[0038] The preparation method is as follows:

[0039] 1) Vector preparation

[0040] With embodiment 1.

[0041] 2) Catalyst synthesis

[0042] Take 50kg of spherical carrier, add it to a stirred tank filled with 150L hexane after being fully replaced by nitrogen, cool down to -20°C, and slowly drop it into a tank containing 400L titanium tetrachloride for titanium support and pre-cooled to -15°C In the reaction kettle, control the pressure inside the kettle to 0.25Mpa, slowly raise the temperature to 40°C, add 10L of diisobutyl phthalate, continue to heat up to 105°C, control the pressure inside the kettle to 0.3Mpa, keep the temperature constant for 1.5 hours, filter with suction, and then add 400L of titanium tetrachloride for washing was heated to 120°C, the pressure was controlled to 0.25Mpa, and the temperature was kept constant for 1.5 hours, and washed with hexane until the filtrate contained no chlo...

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Abstract

The invention relates to a method for preparing a spherical catalyst for propylene polymerization. The adopted technical scheme comprises the following steps of: adding white oil and silicone oil to a reaction kettle, throwing magnesium chloride and alcohol, the mole ratio of which is 1:2.8-3.0, into the reaction kettle and melting; transferring to a reaction kettle cooled to -30 DEG C after melting, to which hexane is added in advance, wherein the final temperature does not exceed 0 DEG C; performing pumping filtration and washing to obtain a spherical carrier; adding the spherical carrier to a stirred kettle holding the hexane, cooling to -10--20 DEG C, and then slowly dropping to a reaction kettle cooled to -10- -15 DEG C wherein the reaction kettle holds titanium tetrachloride for loading titanium; controlling the kettle pressure and heating to 40 DEG C; adding diisobutyl phthalate and heating to 100-105 DEG C; and controlling the kettle pressure, keeping the constant temperature for 1.5 hours, suction filtering, then adding titanium tetrachloride for washing; heating to 120 DEG C, keeping the constant temperature for 1.5 hours, and then washing until the filtrate does not contain chloride ions. The method is simple, saves raw materials, reduces production cost and is friendly to environment; and the prepared catalyst has even particles.

Description

technical field [0001] The invention belongs to the field of catalyst preparation methods, and in particular relates to a preparation method of a spherical catalyst for propylene polymerization. Background technique [0002] At present, the ZIELER-NATLA catalyst system is used to prepare the catalyst for propylene polymerization, which is composed of magnesium chloride as the carrier, titanium tetrachloride as the active material, and internal and external electron donors. In the conventional method: 1) when alcohol and magnesium chloride synthesize the magnesium chloride alcoholate carrier, magnesium chloride and alcohol will be divided into two steps and dispersed in white oil and silicone oil, and the amount of white oil and silicone oil used is large, and white oil and silicone oil are finally It also has to be washed away, thus wasting resources. 2) In the catalyst synthesis step, the volume-to-mass ratio of titanium tetrachloride and magnesium chloride alkoxide carrie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/06C08F4/654C08F4/16C08F4/02C08F10/02C08F10/08
Inventor 张再明
Owner LIAONING DINGJIDE PETROCHEM
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