Method for continuously preparing 1,3-propanediol by one-step glycerol conversion

A technology of propylene glycol and glycerin, which is applied in the fields of chemical instruments and methods, elimination of hydroxyl groups, organic chemistry, etc., can solve the problems of limiting the wider application of microbial fermentation methods, low initial concentration of glycerin, complicated separation and purification, etc., to achieve continuous process Low cost of production, separation and purification, simple and easy purification process

Active Publication Date: 2009-04-15
ZHANGJIAGANG GLORY CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the common problem of microbial fermentation is that during the fermentation process, higher concentrations of glycerol and fermentation products will inhibit the activity of enzymes or engineered bacteria. In order to maintain the activity of microorganisms in the fermentation broth, the initial concentration of glycerol generally Very low (maximum concentration cannot exceed 17%)
It can be seen that the separation and purification of the product 1,3-propanediol is complicated and costly, which limits the wider ap

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A tubular fixed-bed reactor with a length of 60 cm and an inner diameter of 12 mm was used. The catalyst is zirconia / tungsten oxide composite oxide with platinum attached, the particle size is 20-40 mesh, and the weight ratio of three metal elements is: platinum: tungsten: zirconium = 2: 10: 64.7.

[0023] The above-mentioned catalyst was first passed through hydrogen at 250° C., and then activated for 1 hour. Take 2 ml of the activated catalyst and put it into the reactor.

[0024] The reaction raw materials are glycerol aqueous solution with a weight concentration of 60% and hydrogen, and the hydrogen / glycerol volume ratio is 1200; the glycerin volume space velocity is 0.25h -1 , the reaction temperature is 130°C, and the reaction pressure is 4MPa.

[0025] The raw material glycerol and hydrogen are continuously input from the upper inlet of the reactor. After the reaction, the reaction product is continuously discharged from the lower outlet of the reactor. After ga...

Embodiment 2

[0028] The reaction temperature is 120° C., and other conditions are the same as in Example 1.

[0029] Reaction product obtains through chromatographic analysis, and glycerol transformation rate is 34.8%, contains 7.5% (weight) of 1,3-propanediol, 0.7% (weight) of 1,2-propanediol, 5.9% (weight) of n-propanediol in the reaction mixture alcohol and 1.2% by weight isopropanol. The yield of 1,3-propanediol was 15.3% relative to the charged amount of glycerin (excluding water).

[0030] Compared with Example 1, this example shows that reducing the reaction temperature reduces the conversion rate of glycerol, and the content of 1,3-propanediol and the yield of 1,3-propanediol in the mixture after the reaction are also slightly reduced.

Embodiment 3

[0032] Reaction temperature is 140 ℃, and other conditions are all identical with embodiment 1.

[0033]The reaction product obtains 60.5% of glycerol conversion ratio through chromatographic analysis, contains 10.7% (weight) of 1,3-propanediol, 0.9% (weight) of 1,2-propanediol, 12.4% (weight) of n-propanol and 2.1% by weight isopropanol. The yield of 1,3-propanediol was 21.6% relative to the charged glycerol (water not included).

[0034] Compared with Example 1, this example shows that the temperature of reaction is increased, and the conversion rate of glycerol increases, which improves the weight content of 1,3-propylene glycol and the productive rate of 1,3-propylene glycol in the reaction mixture, but the product 1,3-propylene glycol selectivity is reduced.

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Abstract

The invention relates to a method for continuously preparing 1, 3-propylene glycol by glycerin through one step of conversion. With the presence of metal/ solid acid bifunctional catalyst, glycerin water solution and hydrogen are simultaneously and continuously led into a fixed bed reactor and have a catalytic reaction at the temperature of 100-150 DEG C, and a pressure of 2-8MPa, wherein, the volume ratio of hydrogen and glycerin water solution is 600-1200; volume air speed of glycerin water solution is 0.15-1h<-1>; the reaction product is collected and has a gas liquid separation to remove gas hydrogen; the liquid phase is distilled and separated to remove the side product to obtain the 1, 3-propylene glycol product; the metal/ solid acid bifunctional catalyst is functioned by zirconia/ tungsten oxide complex oxide with attachment of platinum; and weight ratio of each metallic element in the catalyst is: Pt: W: Zr=1-5:5-20:69-55. The process of the reaction is simple; the production can be continuous; high concentration glycerin can be converted under a relatively moderate reaction condition; content of 1, 3-propylene glycol is high, while content of side product is low; and 1, 3-propylene glycol separation and purification cost is low.

Description

technical field [0001] The invention provides a method for continuously preparing 1,3-propanediol by one-step catalytic conversion of glycerin, a by-product of biodiesel, belonging to the field of biomass chemical industry. Background technique [0002] 1,3-propanediol (1,3-PDO), the molecular formula is HO-CH 2 -CH 2 -CH 2 -OH, it is an important raw material in the field of fine chemicals, it can be used in solvents, antifreeze agents, protective agents, lubricants, especially for the production of polyester materials, it and terephthalic acid produce polytrimethylene terephthalate (PTT ), compared to polyesters formed by other diols (such as ethylene glycol, 1,4-butanediol), such as polyethylene terephthalate (abbreviated as PET), polybutylene terephthalate (abbreviated PBT), PTT has more unique properties, such as excellent elasticity, dyeability, stain resistance, good anti-ultraviolet discoloration performance, antistatic, good biodegradability, etc., in carpets, en...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/60B01J23/652
Inventor 陈长林秦丽珍徐南平陈晓蓉宋敏洁
Owner ZHANGJIAGANG GLORY CHEM IND CO LTD
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