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Process method for synthesizing polyoxymethylene dimethyl ether from methanol and paraformaldehyde

A technology of polyoxymethylene dimethyl ether and process method, which is applied in the field of synthesis of polyoxymethylene dimethyl ether, can solve problems such as low yield, and achieve the effects of low production cost, high yield and selectivity, and good technical effects

Active Publication Date: 2022-04-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by the present invention is to provide a new synthesis method of polyoxymethylene dimethyl ether based on the low yield of polyoxymethylene dimethyl ether synthesis process products using methanol and paraformaldehyde as raw materials in the prior art

Method used

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  • Process method for synthesizing polyoxymethylene dimethyl ether from methanol and paraformaldehyde
  • Process method for synthesizing polyoxymethylene dimethyl ether from methanol and paraformaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1. Preparation of catalyst

[0035] Wash the sodium sulfonate polystyrene cation exchange resin 7320 with deionized water until clear water flows out, then soak it with 4w% hydrochloric acid four times, each use is equivalent to 10 times the dry weight of sodium sulfonate polystyrene cation exchange resin 7320 4w% hydrochloric acid, soaked for 4 hours each time, and then washed with deionized water until there is no chloride ion in the eluate, and dried at 60°C to obtain a sulfonic acid polystyrene cation exchange resin with a total exchange capacity of 4.10 mmol / g. Get the sulfonic acid type polystyrene cation exchange resin that is equivalent to dry base resin 98 grams and 300ml contain Cu and be 2 grams of Cu(OH) 2 Mix the aqueous suspension, add 1 drop of glacial acetic acid, mix, let stand at room temperature for 24 hours, and dry to constant weight in a vacuum oven to obtain a catalyst with a Cu content of 2w%.

[0036] 2. Synthesis of polyoxymethylene dimethyl ...

Embodiment 2

[0041] 1. Preparation of catalyst

[0042] Wash the sodium sulfonate polystyrene cation exchange resin 7320 with deionized water until clear water flows out, then soak it with 4w% hydrochloric acid four times, each use is equivalent to 10 times the dry weight of sodium sulfonate polystyrene cation exchange resin 7320 4w% hydrochloric acid, soaked for 4 hours each time, and then washed with deionized water until there is no chloride ion in the eluate, and dried at 60°C to obtain a sulfonic acid polystyrene cation exchange resin with a total exchange capacity of 4.10 mmol / g. Get the sulfonic acid type polystyrene cation exchange resin that is equivalent to 98 grams of dry base resin, under nitrogen protection, be 2 grams of Mn(OH) containing Mn with 300ml 2 Mix the aqueous suspension, add 1 drop of glacial acetic acid, mix, let stand at room temperature for 24 hours, and dry to constant weight in a vacuum oven to prepare a catalyst with a Mn content of 2w%.

[0043] 2. Synthes...

Embodiment 3

[0046] 1. Preparation of catalyst

[0047] Sodium sulfonate polystyrene cation exchange resin 7320 was washed with deionized water until clear water flowed out, then soaked in 4w% hydrochloric acid four times, each use was equivalent to 10 times the dry weight of sodium sulfonate polystyrene cation exchange resin 7320 4w% hydrochloric acid, soaked for 4 hours each time, and then washed with deionized water until there is no chloride ion in the eluate, and dried at 60°C to obtain a sulfonic acid polystyrene cation exchange resin with a total exchange capacity of 4.10 mmol / g. Get the sulfonic acid type polystyrene cation exchange resin equivalent to 98 grams of dry base resin, under nitrogen protection, with 300ml of Cu(OH) containing 1 gram of Cu and 1 gram of Mn 2 and Mn(OH) 2 Mix the aqueous suspension, add 1 drop of glacial acetic acid, mix, let stand at room temperature for 24 hours, and dry to constant weight in a vacuum oven to prepare a catalyst with a Cu content of 1w...

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Abstract

The invention relates to a process method for synthesizing polyoxymethylene dimethyl ether, which solves the problem of low yield of polyoxymethylene dimethyl ether synthesis process products using methanol and paraformaldehyde as raw materials. The method includes a reaction zone and a separation zone. The reaction zone includes a nitrogen storage Tank, methanol storage tank, mixing tank with heater, drying pipe and bubbling reactor. The process step in the reaction zone is that paraformaldehyde is heated in the mixing tank to become formaldehyde gas, which is sent to the drying pipe to remove water after being purged with nitrogen. Enter the bubbling reactor, under the action of solid acid catalyst, react with methanol and recover the mixture passed into the reactor to generate polyoxymethylene dimethyl ether, the separation zone includes anion exchange resin bed, rectification module and product storage tank, separation The process steps in the zone are that the discharge from the reactor enters the rectification module after being deacidified by the anion exchange resin bed, and the trimer and tetramer of polyoxymethylene dimethyl ether enter the product storage tank, which better solves this technical problem .

Description

technical field [0001] The invention relates to a method for synthesizing polyoxymethylene dimethyl ether, in particular to a method for synthesizing polyoxymethylene dimethyl ether with paraformaldehyde as a raw material. Background technique [0002] my country's resource structure has the characteristics of "rich coal, less oil, and gas", and my country's vigorous industrial development has put forward increasing requirements for oil supply. However, in recent years, my country's oil resources have become increasingly tense, and the pressure on oil supply has increased unprecedentedly. According to statistics, in 2011 my country's dependence on foreign oil reached 56.5%, an increase of 1.7 percentage points compared with 2010. Since my country became a net oil importer for the first time in 1993, China's dependence on foreign oil has been rising from 6% in that year, and broke through the warning line of 50% in 2009. How to use our country's rich coal resources to solve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/56C07C41/58C07C43/30B01J31/10
CPCC07C41/56C07C41/58B01J31/10C07C43/30
Inventor 高晓晨柏诗哲高焕新
Owner CHINA PETROLEUM & CHEM CORP