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Method for refining and purifying polyformaldehyde dialkyl ether

A formaldehyde dialkyl ether and product technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of poor extraction rate of extraction unit, poor extraction product purity, poor extraction efficiency, etc., and meet the reaction conditions Gentle, high operational safety effect

Active Publication Date: 2013-09-25
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
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  • Method for refining and purifying polyformaldehyde dialkyl ether

Examples

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Embodiment 1

[0051] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, which specifically includes the following steps:

[0052] S1. Add sodium percarbonate to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium percarbonate is 1% of the mass of the equilibrium product, heat to 50°C for reaction, and treat for 1 hour;

[0053] S2, performing solid-liquid separation on the product obtained after the reaction in step S1, and collecting the liquid phase product;

[0054] 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...

Embodiment 2

[0056] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, which specifically includes the following steps:

[0057] S1. Add sodium percarbonate to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium percarbonate is 3% of the mass of the equilibrium product, heat to 50°C for reaction, and treat for 1 hour;

[0058] S2, performing solid-liquid separation on the product obtained after the reaction in step S1, and collecting the liquid phase product;

[0059] 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 prod...

Embodiment 3

[0061] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, which specifically includes the following steps:

[0062] S1. Add sodium percarbonate to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium percarbonate is 5% of the mass of the equilibrium product, heat to 50°C for reaction, and treat for 1 hour;

[0063] S2, performing solid-liquid separation on the product obtained after the reaction in step S1, and collecting the liquid phase product;

[0064] 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 fract...

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Abstract

The invention provides a refining extraction technology capable of remarkably improving the extraction rate and the product purity after discovering the reason leading to the low extraction rate of an extraction unit and low purity of the extraction product through intensive study on the polyformaldehyde dialkyl ether extraction unit technology in the prior art. An aim of removing formaldehyde in a polyformaldehyde dialkyl ether balance system is achieved by adding sodium percarbonate into a polyformaldehyde dialkyl ether balance product; the method for refining and purifying polyformaldehyde dialkyl ether belongs to a solid-phase reaction; the impurities after reaction are easy to separate, the technology is simple, the reaction is mild, and the operation is easy; the sodium percarbonate increases a small number of peroxide chains on polyformaldehyde dialkyl ether while removing formaldehyde, and the peroxide chains are favorable for increasing the cetane number of the polyformaldehyde dialkyl ether; since the sodium percarbonate is added as a solid phase, the problem that materials such as methanol and the like are dissolved in an aqueous solution is avoided, and the recovery rate of the product is high; and therefore, the production cost can be effectively reduced.

Description

technical field [0001] The invention belongs to the fields of coal-based energy chemical industry, clean energy and chemical process refining, and 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 洪正鹏商红岩郭振国刘晨光
Owner DONGFANG HONGSHENG NEW ENERGY APPL TECH RES INST
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