Method for refining and purifying polyformaldehyde dialkyl ether

A formaldehyde dialkyl ether and product technology, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of poor extraction rate of extraction unit, poor purity of extracted products, poor extraction efficiency, etc., so as to reduce production The effect of high cost, high recovery rate and simple process

Inactive Publication Date: 2013-10-02
DONGFANG HONGSHENG NEW ENERGY APPL TECH RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] For this reason, the technical problem to be solved by the present invention is to find out the influence reasons of the extraction rate of the extraction unit and the poor purity of the extraction product through in-depth research on the extraction unit process of polyoxymethylene dialkyl ether in the prior art, and then provide A refined extraction process that can significantly improve the extraction rate and product purity to solve the problem of poor extraction efficiency

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  • Method for refining and purifying polyformaldehyde dialkyl ether
  • Method for refining and purifying polyformaldehyde dialkyl ether
  • Method for refining and purifying polyformaldehyde dialkyl ether

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Embodiment 1

[0053] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, specifically:

[0054] S1. Add sodium sulfite to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium sulfite is 10% of the mass of the equilibrium product, heat to 40°C for reaction, and treat for 1 hour;

[0055] S2, performing solid-liquid separation on the reaction liquid obtained in step S1, and collecting liquid phase products;

[0056] S3. Carry out fractional atmospheric pressure distillation on the liquid phase product, and distill out the fraction before 60°C. The initial boiling point ~60°C is the unreacted raw material (formaldehyde, methanol and methylal), and the fraction collected at ~110°C is divided into two poly product (PODE 2 ), the fraction collected at ~160°C was the trimerization product (PODE 3 ), collecting fractions at ~200°C as tetramerization products (PODE 4 ); the fraction at ~250°C was collected as pentameric pro...

Embodiment 2

[0058] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, specifically:

[0059] S1. Add sodium bisulfite to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium bisulfite is 10% of the mass of the equilibrium product, heat to 40°C for reaction, and treat for 1 hour;

[0060] S2, performing solid-liquid separation on the reaction liquid obtained in step S1, and collecting liquid phase products;

[0061] S3. The liquid phase product is rectified at atmospheric pressure, the temperature at the bottom of the tower is 100° C., and the reflux ratio is 1. The production liquid at the top of the tower consists of methanol, methylal and a small amount of dimerization products; Then carry out fractional atmospheric pressure distillation on the polymer products with a degree of polymerization of 2 to 8, and collect the fractions at ~110°C as dimerization products (PODE 2 ), the fraction collected at ~160°C was ...

Embodiment 3

[0063] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, specifically:

[0064] S1. Add sodium metabisulfite to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium metabisulfite is 10% of the mass of the equilibrium product, heat to 40°C for reaction, and treat for 1 hour;

[0065] S2, performing solid-liquid separation on the reaction liquid obtained in step S1, and collecting liquid phase products;

[0066] S3. Carry out fractional atmospheric pressure distillation on the liquid phase product, distill out the fraction before 60°C, the initial boiling point ~60°C is the unreacted raw material (formaldehyde, methanol and methylal), and the fraction collected at ~110°C is dimerization Product (PODE 2 ), the fraction collected at ~160°C was the trimerization product (PODE 3 ), collecting fractions at ~200°C as tetramerization products (PODE 4 ); the fraction at ~250°C was collected as pentameric prod...

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Abstract

The invention relates to a method for refining and purifying polyformaldehyde dialkyl ether. By deeply researching the extraction unit technique of the polyformaldehyde dialkyl ether in the prior art, the invention finds out the reasons for influencing the extraction yield of the extraction unit and the purity of the extraction product, thereby providing a refinement extraction technique capable of enhancing the extraction yield and product purity. A proper amount of sulfite is added into the polyformaldehyde dialkyl ether balance product to remove formaldehyde in the polyformaldehyde dialkyl ether balance system. The method for refining and purifying polyformaldehyde dialkyl ether belongs to solid-phase reaction, the generated alpha-hydroxysulfonate is insoluble in the product, the impurities after reaction are easy to separate, and thus, the technique is simple. The method of adding sulfite several times is beneficial to breaking the adsorption balance between the sulfite and formaldehyde, so that the reaction proceeds forwards, thereby sufficiently removing the methanol by the reaction. Since the sulfite is added in a solid phase, the problem of dissolution of methanol and other materials in the water solution does not exists, and thus, the recovery rate of the product is high, thereby effectively lowering the production cost.

Description

technical field [0001] The invention belongs to the fields of coal-based energy chemical industry, clean energy and chemical process refining. It specifically relates to a refining and extraction process of polyoxymethylene dialkyl ether, a diesel additive. Background technique [0002] Surveys in recent years have shown that the apparent consumption of diesel in my country has reached about 167 million tons, resulting in frequent shortages of diesel supply (the domestic demand ratio of diesel and gasoline is about 2.5:1, while the current output ratio is about 2.3:1) . In addition to institutional reasons such as unreasonable pricing of different types of oil products and slow linkage between domestic refined oil prices and international crude oil prices, the fundamental reason is the constraints of resource shortages. Traditionally, oil is used as raw material for diesel production. China's relatively "rich in coal, poor in oil, and low in gas" resource endowment has made...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/303C07C41/58
Inventor 洪正鹏红岩郭振国刘晨光
Owner DONGFANG HONGSHENG NEW ENERGY APPL TECH RES INST
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