Method for preparing 1,3 propanediol by 3-methyl lactate

A technology for the preparation of methyl hydroxypropionate and hydrogen, which is applied in the preparation of hydroxyl compounds, chemical instruments and methods, preparation of organic compounds, etc. Dehydration side reactions, uniform distribution of components, and good catalytic activity

Inactive Publication Date: 2011-03-30
GUANGDONG UNIV OF PETROCHEMICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, from the technical point of view, there are problems that the expensive high-boiling-point activation solvent must be recovered, and the alkali metal ions in the catalyst make the active components easy to sinter, thereby shortening the life and stability of the catalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Cu(NO 3 ) 2 , Mn(NO 3 ) 2 and Zr(NO 3 ) 2 Water is made into the solution of 15% of total mass concentration, then by the mass ratio of alkaline precipitant sodium carbonate and Cu, Mn and Zr salt three kinds of monomers total mass ratio is the ratio of 1: 1.2, at 42 ℃ and under stirring Add alkaline precipitant sodium carbonate to the solution for titration and co-precipitation to obtain a dark blue precipitate, stir and age at 67°C for 11 hours, filter, wash with water, dry at 120°C under normal pressure or vacuum for 10 hours, press the powder, and crush it 1. Screening and selecting particles smaller than 200 meshes and calcining at 450° C. for 4 hours to obtain the catalyst.

[0021] The catalyzer of above-mentioned 1g and the decahydronaphthalene of 50mL are packed in the reactor of 250mL, pass into volume ratio 5%H 2 / 95%N 2 The mixed gas was controlled at a flow rate of 75mL / min, and the temperature was slowly raised to 185°C for 11 hours of activation. ...

Embodiment 2

[0023] Adopt the catalyst that embodiment 1 makes.

[0024] The catalyzer of 1g and the pentadecane of 50mL are packed in the reactor of 250mL, pass into volume ratio 5%H 2 / 95%N 2 The mixed gas is controlled at a flow rate of 100mL / min, and the temperature is slowly raised to 180°C for activation for 20h. When the reaction temperature was adjusted to 140°C, the gas was switched to hydrogen, and at the same time, 41 mL of a mixture of methyl 3-hydroxypropionate: methanol at a volume ratio of 1:10 was pumped by HPLC, and the LHSV was 4.0 hr -1 , injected into the reactor simultaneously with hydrogen to react, the pressure in the kettle was maintained at 10MPa by hydrogen, and the reaction was carried out for 30 hours. The results of sampling analysis showed that the conversion rate of methyl 3-hydroxypropionate was 64.53%, the selectivity of 1,3-propanediol was 82.41%, and the selectivity of propanol was 3.17%.

Embodiment 3

[0026] Adopt the catalyst that embodiment 1 makes.

[0027] The catalyzer of 1g and the decahydronaphthalene of 40mL are packed in the reactor of 250mL, pass into volume ratio 5%H 2 / 95%N 2 The mixed gas is controlled at a flow rate of 50mL / min, and the temperature is slowly raised to 250°C for 2h activation. When the reaction temperature was adjusted to 160°C, the activated solvent was not removed, and the gas was switched to hydrogen. At the same time, 75 mL of a mixture of methyl 3-hydroxypropionate: methanol at a volume ratio of 1:4 was pumped by HPLC, and the LHSV was 4.0 hr. -1 , Inject the reactor simultaneously with hydrogen to react, maintain the pressure in the kettle by hydrogen at 5Mpa, and react for 3 hours. The results of sampling analysis showed that the conversion rate of methyl 3-hydroxypropionate was 60.22%, the selectivity of 1,3-propanediol was 78.07%, and the selectivity of propanol was 5.11%.

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PUM

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Abstract

The invention discloses a method for preparing 1,3 propanediol by 3-methyl lactate. Under the presence of a reaction solvent, an activated solvent and a catalyst, 3-methyl lactate and hydrogen carries out hydrogenation, and active components of the catalyst can be oxides of Cu, Mn and Zr. The 1,3 propanediol is prepared by using the following methods: mixing Cu, Mn and Zr salt with water to obtain a solution with the total mass concentration of 10-20 percent; titrating and coprecipiting the solution and the alkali precipitator at 25 DEG C-90 DEG C while stirring; aging the precipitate for 2-20 hours at 40 DEG C-95 DEG C; washing, drying and baking for 2-6h at 300-900 DEG C; and pulverizing for over 200 meshes to obtain the catalyst, wherein the molar rate of Cu to Mn to Zr in Cu, Mn and Zr salt is 1 to (0.0.25-1.2) to (0.8-2), and the mass ratio of the alkali precipitator to the total mass of three monomers of Cu, Mn and Zr salt is 1 to (1-1.5). The invention is simple for operation, can be realized under the milder condition and can better inhibit the dehydration side reaction of beta-bit with hydroxide radicals.

Description

technical field [0001] The invention relates to a method for preparing 1,3-propanediol through catalytic hydrogenation of methyl 3-hydroxypropionate. Background technique [0002] 1,3-Propanediol is an important organic chemical raw material, which has been widely used as intermediates in coatings and various organic synthesis, as well as raw materials for the production of polyester (such as polytrimethylene terephthalate PTT). The performance of PTT produced by using it instead of 1,4-butanediol and ethylene glycol is better than that of PBT (1,4-butylene terephthalate) and PET (polyethylene terephthalate). It can also be used as a solvent, antifreeze and protective agent. [0003] At present, the known chemical production methods of 1,3 propanediol: ethylene oxide formylation (see U.S. Patents US5,770,776, US5,723,389, US5,731,478, US5,777,182;) Patents US6,232,511, US6,140543). These two kinds of synthetic methods with 3-hydroxy propionaldehyde as intermediate have th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/149B01J23/889
Inventor 陈小平王世琴马玉刚周海军刘春杰
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH
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