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PTMEG polymerization catalyst preparation method

A technology of catalyst and complexing agent, which is applied in the field of preparing 12-tungstophosphoric acid catalyst for PTMEG polymerization, which can solve the problems of polymerization catalytic activity, selective PTMEG product quality, yield less than 30%, and industrialization difficulties. , to achieve the effects of easy control, stable catalytic activity and good selectivity

Active Publication Date: 2004-11-10
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the heteropolyacid catalyst that this method produces usually contains the sodium ion of 200~500PPM and a small amount of iron, aluminium, chromium, lead etc. etc. have a great influence
[0006] Russian patent RU1559773 (1994) invented by КупиковаOM et al. The method of electrodialysis to synthesize 12-tungstophosphoric acid, the product produced has high purity, but industrialization is difficult, and the yield is less than 30%
Strengthen the acid (hydrochloric acid, sulfuric acid, nitric acid, etc.) to adjust the pH, extract with a large amount of ether to form an ether compound of heteropoly acid, add water to heat and decompose the ether compound to obtain an aqueous solution of heteropoly acid, concentrate and crystallize to obtain heteropoly acid crystals, the The method uses a large amount of solvent ether, the yield is not high, and the impurities harmful to the polymerization reaction of PTMEG in industrial sodium tungstate are brought into the 1 2-tungstophosphoric acid crystal, which affects the polymerization catalysis of PTMEG

Method used

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Examples

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Embodiment 1

[0027] Weigh 509 grams of sodium tungstate and add it to a container containing 5200 mL of water to dissolve, add 30% H 2 o 2 Solution 120ml, stirring ice bath to cool down to 10°C, slowly add 0.75L of 6N hydrochloric acid, keep the temperature in the range of 6-8°C during the whole process, slowly introduce SO2 through the gas sparger 2 , after the reaction reaches the end point, use a Buchner funnel to suction and filter, wash the filter cake continuously through 4L of 1N, 0.6N, 0.2N dilute hydrochloric acid and 6L of deionized water, and immediately add the washed and filtered filter cake to 0.13mol / In the L phosphoric acid aqueous solution, the concentration of active tungstic acid is controlled at 1.15mol / L, fully stirred for 2 hours, and then slowly heated up to 50°C according to the heating curve. Cool the crystallizer for crystallization, centrifuge the 12-tungstophosphoric acid crystals containing a small amount of mother liquor, prepare the obtained crystals into a...

Embodiment 2

[0029] Weigh 509 grams of sodium tungstate and add it to a container containing 3200 mL of water to dissolve, add 30% H 2 o 2 Solution 107ml, stirring ice bath to cool down to 5°C, slowly add 0.68L of 6N hydrochloric acid, keep the temperature in the range of 4-5°C during the whole process, slowly introduce SO2 through the gas sparger 2 , after the reaction reaches the end point, use a Buchner funnel to suction and filter, wash the filter cake continuously through 4 L of 1N, 0.5 N, 0.1 N dilute hydrochloric acid and 6.5 L of deionized water, and immediately add the washed and filtered filter cake to 0.12 mol / L phosphoric acid aqueous solution, the concentration of active tungstic acid is controlled at 1.15mol / L, fully stirred for 2 hours, and then slowly heated up to 50°C according to the heating curve. Cool the crystallizer for cooling crystallization, centrifuge the 12-tungstophosphoric acid crystals containing a small amount of mother liquor, prepare the obtained crystals...

Embodiment 3

[0031] Weigh 1,000 grams of sodium tungstate and add it to a container containing 7,200 mL of water to dissolve it, add 30% H 2 o 2 Solution 219ml, stirring ice bath to cool down to 10°C, slowly add 1.6L of 6N hydrochloric acid, keep the temperature in the range of 7-10°C during the whole process, slowly inject SO through the gas sparger 2, after the reaction reaches the end point, use a Buchner funnel to suction and filter, wash the filter cake continuously through 10 L of 1N, 0.5 N, 0.1 N dilute hydrochloric acid and 12 L of deionized water, and immediately add the washed and filtered filter cake to 0.12 mol / In the L phosphoric acid aqueous solution, the concentration of active tungstic acid is controlled at 1.14mol / L, fully stirred for 3 hours, and then slowly heated up to 50°C according to the heating curve. The crystallizer is cooled and crystallized, and the 12-tungstophosphoric acid crystals containing a small amount of mother liquor are centrifuged, and the obtained ...

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Abstract

The invention relates to a process for preparing 12-tungstophosphoric acid catalyst for PTMEG polymerization comprising the steps in sequence, (1) dissolving sodium tungstate crystal of industrial grade into water, and charging hydrogen dioxide complexing agent, cooling down, (2) heat preservation, filling definite quantity of dilute hydrochloric acid, (3) letting in SO2 slowly, washing with dilute hydrochloric acid and water after reaction, (4) charging the prepared active tungstic acid with rather high purity immediately into phosphoric water solution, agitating, elevating temperature, condensing, controlling process end spot according to weight, the invention is characterized in that the process also comprises, (5) subjecting the concentration liquid to cooling crystallization, separating mother liquid by centrifugal separation, (6) adding equal volumn of C3-C20 ether to the water solution of the dissolved crystal for extraction to obtain HPA ether addition product, rinsing the ether addition product by the diluted acid of the equal volume, the high purity 12-tungsten phosphoric catalyst is thus obtained through heating and concentrating the ether addition product.

Description

(1) Technical field [0001] The present invention relates to a method for preparing a catalyst for PTMEG polymerization. Specifically, it relates to a method for preparing a 12-tungstophosphoric acid catalyst for PTMEG polymerization. (2) Background technology [0002] 12-tungstophosphoric acid is a new type of catalyst that has attracted people's attention. It has both acidic and redox properties. It is superior to traditional catalysts in industrial applications. It can be used in hydration, ester (ester decomposition) and transesterification in the field of organic synthesis. , decomposition, alkylation-dealkylation, acetic acid acid hydrolysis, poly(condensation), epoxide etherification, acylation, isomerization, nitration, etc., 12-tungstophosphoric acid as a catalyst has high catalytic activity and selectivity It has the advantages of good performance, small pollution and easy control, especially the selection of 12-tungstophosphoric acid as the catalytic system in the...

Claims

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Application Information

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IPC IPC(8): B01J27/18B01J27/188C08F4/22C08G65/20
Inventor 张艺苏亚贵范天民周正波朱毓群吕涛贺天禄
Owner 中国中化股份有限公司
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