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Method and system for producing 1, 3-propylene glycol by multi-step method

A technology of propylene glycol and multi-step method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve unsatisfactory problems and achieve low cost and mild reaction conditions

Active Publication Date: 2021-01-26
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, although China has made considerable progress in the production of 1,3-propanediol by biological methods, and some research results are being industrialized and demonstrated for production, it still cannot meet the demand for 1,3-propanediol in my country's high-end polyester industry.

Method used

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  • Method and system for producing 1, 3-propylene glycol by multi-step method
  • Method and system for producing 1, 3-propylene glycol by multi-step method
  • Method and system for producing 1, 3-propylene glycol by multi-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0102] (1) Dehydration reaction of 1,3-dichloropropanol

[0103] refer to figure 1 As shown, the raw material 1,3-dichloropropanol 2 is transported to the preheating furnace 4 by the transport pump 3, preheated and gasified, and then mixed with the protective gas nitrogen and transported to the dehydration catalyst (Beta Molecular sieve) in the dehydration reactor 5, and at 500 ° C, the liquid hourly space velocity is 3.0h -1 Pass through the dehydration catalyst bed in the dehydration reactor under the conditions and dehydration reaction occurs, and then transported to the dehydration product storage tank 7 after being cooled by the condenser 6 to obtain 1,3-dichloropropanol, 1,3-dichlorohydrin The dehydration product composed of chloropropene, water and other organic matter was analyzed by gas chromatography, and the conversion rate of 1,3-dichloropropanol was measured to be 75%, and the selectivity of 1,3-dichloropropene was 90%;

[0104] (2) Hydrolysis reaction of 1,3-di...

Embodiment 2

[0111] (1) Dehydration reaction of 1,3-dichloropropanol

[0112] refer to figure 1 As shown, the raw material 1,3-dichloropropanol 2 is transported to the preheating furnace 4 by the delivery pump 3, preheated and gasified, and then mixed with the protective gas nitrogen and transported to the dehydration catalyst (Al 2 o 3 Loaded phosphotungstic acid, 30%H 3 o 40 PW 12 / Al 2 o 3 ) in the dehydration reactor 5, and at 200°C, the liquid hourly space velocity is 0.1h -1 Pass through the catalyst bed of the dehydration reactor under certain conditions and dehydration reaction occurs, then after being cooled by the condenser 6, it is transported to the dehydration product storage 7 to obtain 1,3-dichloropropene, a small amount of 1,3-dichloropropanol The dehydration product composed of , water and other organic matter was analyzed by gas chromatography, and the conversion rate of 1,3-dichloropropanol was measured to be 83%, and the selectivity of 1,3-dichloropropene was 93%...

Embodiment 3

[0120] (1) Dehydration reaction of 1,3-dichloropropanol

[0121] refer to figure 1 As shown, the raw material 1,3-dichloropropanol 2 is transported to the preheating furnace 4 by the delivery pump 3, preheated and gasified, and then mixed with the protective gas nitrogen and transported to the dehydration catalyst (solid state) loaded with the pipeline through the pipeline. Phosphoric acid, 10% H 3 PO 4 / SiO 2 ) in the dehydration reactor 5, and at 300°C, the liquid hourly space velocity is 2.0h -1 Under the condition of passing through the dehydration reactor and the dehydration reaction takes place, then after being cooled by the condenser 6, it is transported to the dehydration product storage tank 7 to obtain 1,3-dichloropropene, water, a small amount of 1,3-dichloropropanol and other The dehydration product composed of organic matter was analyzed by gas chromatography, and the conversion rate of 1,3-dichloropropanol was measured to be 63%, and the selectivity of 1,3-d...

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Abstract

The invention discloses a method and a system for producing 1, 3-propylene glycol by a multi-step method. The method comprises the following steps: carrying out dehydration reaction on 1, 3-dichloropropanol and a dehydration catalyst to prepare 1, 3-dichloropropene; carrying out a first hydrolysis reaction on a first mixed reaction system containing the 1, 3-dichloropropene, a first hydrolysis agent and a first solvent to prepare 3-chloro-2-propene-1-alcohol; carrying out hydrogenation reaction on the 3-chloro-2-propene-1-alcohol and a hydrogenation catalyst to prepare 3-chloropropanol; and carrying out a second hydrolysis reaction on a second mixed reaction system containing the 3-chloropropanol, a second hydrolysis agent and a second solvent to prepare the 1, 3-propylene glycol. According to the method, 1, 3-dichloropropanol is used as a raw material, the important chemical raw material 1, 3-propylene glycol is prepared through a dehydration, hydrolysis, hydrogenation and hydrolysisfour-step method, and the method has the advantages of mild reaction conditions, low cost, environmental protection, economy and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method and system for producing 1,3-propanediol by a multi-step method. Background technique [0002] 1,3-propanediol (1,3-Propandiol, referred to as 1,3-PDO, chemical formula: CH 2 OHCH 2 CH 2 OH) is an important organic chemical raw material, mainly used in ink, paint, cosmetics, pharmaceuticals, antifreeze and other industries, and its most important use is to produce poly(trimethylene terephthalate) fiber (abbreviated as PTT) main raw material. The prepared PTT fiber not only has the properties of polyethylene terephthalate (PET), but also has good resilience and anti-pollution properties of nylon. It is widely used in carpets, engineering plastics, clothing fabrics and other fields, and has become the current international A hotspot in the development of synthetic fibers. However, the high price and insufficient production capacity of 1,3-propan...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/09
CPCC07C29/09C07C17/23C07C29/172C07C31/205C07C21/073C07C33/423C07C31/36Y02P20/52
Inventor 李通尹宏峰严波李梦珠张洁励斌
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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