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Method for preparing 1,3-methyl glycol

A technology for propylene glycol and dialkyl malonate, applied in 1 field, can solve the problems of low production efficiency, high concentration cost, low concentration of fermentation reactor products and the like

Active Publication Date: 2008-03-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common problems of the fermentation method are: the product concentration in the fermentation reactor is low, and the concentration is expensive. For example, many large reactors are required for commercial production, the equipment investment is large, and the production efficiency is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 52.2g Cu(NO 3 ) 2 .3H 2 O, 12.9g Zn(NO 3 ) 2 .6H 2 O, 56.9gAl(NO 3 ) 3 .9H 2 O was dissolved in 1000ml of deionized water as solution A, and 23wt% sodium carbonate solution was used as solution B. Under stirring at 60°C, drop A into B until the pH of the solution was 7±0.5 and titrated for aging 1 hour, then filter, wash with water, collect the precipitate, dry at 120°C for 3 hours, and roast at 350±10°C for 2 hours to obtain catalyst A: CuZn 0.2 Al 0.7 o 2.3 .

Embodiment 2

[0025] 52.2g Cu(NO 3 ) 2 .3H 2 O, 74.9gZn(NO 3 ) 2 .3H 2 O, 122gAl(NO 3 ) 3 .9H 2 O, dissolved in 500ml deionized water to make solution A. 20wt%Na 2 CO 3 as solution B. Put 200ml of deionized water into a 2000ml beaker, stir at room temperature, add the two solutions of A and B into the beaker at the same time, control the drop rate of A and B, keep the pH at 5.5±1, age for 1 hour after titration, then filter, wash with water, Collect the precipitate, dry at 120°C for 3 hours, and roast at 550±20°C for 2 hours to obtain catalyst B: CuZn 0.9 Al 1.5 o 4.2 .

Embodiment 3

[0027] 52.2g Cu(NO 3 ) 2 .3H 2 O, 146.7g Zn(NO 3 ) 2 .6H 2 O, 12.2gAl(NO 3 ) 3 .9H 2 O, dissolve in 400ml deionized water, stir at room temperature, add 20wt% ammonia water dropwise until the pH of the solution is 6±0.5, age for 1 hour, then filter, wash with water, collect the precipitate, dry at 120°C for 2hr, 350±10°C Calcined for 4 hours to obtain catalyst C: CuZn 1.9 Al 0.15 o 3.1 .

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PUM

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Abstract

The present invention provides 1, 3-propylene glycol preparing process, which includes the contact of dialkyl malonate with hydrogenating catalyst CuZnaAlbOc, where, a is 0.04-3, b is 0.04-3, and c is the atom number for reaching the electric neutrality of the compound; and reaction at temperature of 100-220 deg.c and pressure of 0.1-10.0 MPa, and in the space velocity of ester of 0.1-1 / hr and hydrogen / ester molar ratio of 100-700 to 1. The process has high 1, 3-propylene glycol selectivity, high reactor utilizing efficiency, and low cost.

Description

technical field [0001] The present invention relates to the preparation method of 1,3-propanediol. Background technique [0002] 1,3-Propanediol is an important organic chemical raw material, mainly used in the production of polymers such as thermoplastic polyurethane, polytrimethylene terephthalate (PTT), and can also be used as a solvent, antifreeze and protective agent. PTT prepared with 1,3 propylene glycol can be made into various elastic knitted fabrics with high elasticity and soft touch. It has been listed as one of the new fibers in the 21st century abroad. [0003] At present, the method for preparing 1,3-propanediol in the prior art mainly contains the following three kinds: [0004] (1) Use acrolein as raw material to prepare 1,3-propanediol through hydration and hydrogenation. EP544120 uses TiO 2 Using a phosphoric acid catalyst as a carrier, acrolein is hydrated to 3-hydroxyacrolein at 50°C-70°C, and then 3-hydroxyacrolein is used as a Raney Ni catalyst to p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/149B01J23/835B01J23/80
Inventor 王海京高国强刘易
Owner CHINA PETROLEUM & CHEM CORP
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