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Method and system for high-selectivity preparation of dipropylene glycol

A technology for reducing dipropylene glycol and propylene glycol, which is applied in the field of 1,2-propanediol synthesis, which can solve the problems of unsuitable automatic control, low price of crude products, and inability to achieve high selectivity, etc., and achieve easy control, mild conditions, and improved selectivity Effect

Inactive Publication Date: 2020-01-07
DONGYING HI TECH SPRING CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the selectivity of DPG and TPG reaches more than 80%, it is impossible to achieve high-selectivity DPG production
Patent CN 203382693 uses a high-pressure reactor to synthesize crude dipropylene glycol with propylene oxide and 1.2-propylene glycol as raw materials, and then obtains high-quality dipropylene glycol through refining and separation. However, the reaction is intermittent and the utilization rate of the equipment is not high. Not suitable for automatic control
Patents CN203393068 and CN201981142 also use propylene oxide and 1.2-propylene glycol as raw materials, and use continuous reaction technology to solve the defects of cumbersome synthesis process and high energy consumption. However, the series reaction is serious and produces a large number of by-products. Refined recycling
Another example is that patent CN101665414A synthesizes dipropylene glycol with propylene oxide and 1.2-propylene glycol under the condition of no catalyst, but there are long reaction times and defects such as high energy consumption
Therefore, most of the existing production enterprises can only sell crude products with a content of 50% to 80%, and the price of crude products is low, which also reduces the economic benefits of the whole set of devices

Method used

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  • Method and system for high-selectivity preparation of dipropylene glycol
  • Method and system for high-selectivity preparation of dipropylene glycol
  • Method and system for high-selectivity preparation of dipropylene glycol

Examples

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Effect test

preparation example Construction

[0060] The invention provides a kind of preparation method of dipropylene glycol, comprises the following steps:

[0061] 1) After mixing propylene oxide and propylene glycol, a mixed raw material is obtained;

[0062] 2) After carrying out the condensation reaction in the microchannel reactor with the mixed raw material that above-mentioned steps obtains, obtain dipropylene glycol.

[0063] The present invention firstly mixes propylene oxide and propylene glycol to obtain mixed raw materials.

[0064] The present invention has no special limitation on the addition ratio of the propylene oxide and propylene glycol, and the conventional addition ratio well known to those skilled in the art can be used, and those skilled in the art can select and adjust according to actual production conditions, raw material conditions and product requirements, The molar ratio of propylene glycol to propylene oxide in the present invention is preferably (1-10):1, more preferably (3-9):1, more p...

Embodiment 1

[0104] First, inject propylene oxide, 1.2-propanediol and benzenesulfonic acid catalysts into the microchannel mixer through the metering pump respectively, and the multi-strand raw materials are mixed by the microchannel mixer and then enter the raw material buffer tank, and the materials in the raw material buffer tank pass through the preheater After preheating to 80°C, enter the microchannel reactor for full reaction. Control the temperature in the microchannel reactor to 110°C, the pressure to 0.3MPa, and the residence time of the material to be 10 minutes. / h, 1.2-propanediol feed rate 152Kg / h, benzenesulfonic acid 0.5Kg / h.

[0105] The crude product after the reaction of Example 1 of the present invention was detected and analyzed.

[0106] see figure 2 , figure 2 It is the gas chromatogram of the crude product after the reaction of Example 1 of the present invention.

[0107] Referring to Table 1, Table 1 shows the specific composition of the crude product after t...

Embodiment 2

[0116] Firstly, propylene oxide, 1.2-propylene glycol and sodium bicarbonate catalyst are respectively injected into the microchannel mixer through the metering pump, and the multi-strand raw materials are mixed by the microchannel mixer and then enter the raw material buffer tank, and the materials in the raw material buffer tank pass through the preheater After preheating to 50°C, enter the microchannel reactor for full reaction. Control the temperature in the microchannel reactor to 120°C, the pressure to 0.2MPa, and the residence time of the material to be 2 minutes. / h, 1.2-propanediol feed rate 304Kg / h, sodium methoxide 0.5Kg / h.

[0117] The crude product after the reaction in Example 2 of the present invention was detected and analyzed, the content of dipropylene glycol in the crude product was 37%, and the selectivity of dipropylene glycol in the product was 98%.

[0118] Then the crude product is separated by rectification. Firstly, it is delightened by the first rect...

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Abstract

The invention provides a dipropylene glycol preparation method, which comprises: mixing propylene oxide and propylene glycol to obtain a mixed raw material; and carrying out a condensation reaction onthe mixed raw material obtained in the previous step in a micro-channel reactor to obtain dipropylene glycol. According to the invention, based on the fluid mechanics of the reaction process, particularly the micro-channel reactor is used as the reaction place, and has the characteristic of low channel diameter, so that the raw material is in a laminar flow state in the channel so as to reduce the back-mixing phenomenon, avoid the chance of the contact of the dipropylene glycol and the raw materials 1,2-propylene glycol and propylene oxide, and reduce the occurrence of the cascade reaction, such that the selectivity of the dipropylene glycol in the product is effectively improved; and the preparation method can further effectively reduce the reaction time and improve the yield of the dipropylene glycol product, and is simple in process, mild in condition, easy to control and suitable for industrial mass production.

Description

technical field [0001] The invention relates to the technical field of 1,2-propanediol synthesis, relates to a method and system for preparing dipropylene glycol, and in particular to a method and system for preparing dipropylene glycol with high selectivity. Background technique [0002] Dipropylene glycol, also known as dipropylene glycol, Dipropylene glycol, referred to as DPG), is a colorless, odorless liquid at room temperature, non-corrosive, very small irritation to the skin, low toxicity, and widely used. Dipropylene glycol can be divided into LO+ grade and industrial grade. The former is relatively expensive, and is mainly used in fields requiring high-quality raw materials such as spices, cosmetics, detergents, and food additives; the latter is relatively low in price, and is widely used in the production of industrial solvents and unsaturated resins that do not require high DPG quality. , Raw materials for the production of nitrocellulose varnish, etc. [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C41/34C07C43/11
CPCC07C41/03C07C41/34C07C43/11
Inventor 滕文彬王春梅杜桂强张风收
Owner DONGYING HI TECH SPRING CHEM IND
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