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3-methyl lactate hydrogenation catalyst and preparation method thereof

A technology of methyl hydroxypropionate and hydrogenation catalyst, which is applied in the preparation of hydroxyl compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of low concentration of methyl 3-hydroxypropionate, cumbersome catalyst washing, separation and Purification is difficult and other problems, to achieve the effect of less solvent content, simple preparation process, and less waste water treatment

Active Publication Date: 2014-09-10
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in hydrogenation, in order to improve the performance of the catalyst, a large amount of methanol and high-boiling organic matter are added to the hydrogenation raw material, resulting in a low concentration of methyl 3-hydroxypropionate in the raw material, which has a great impact on the subsequent separation and purification. Difficulties
At the same time, in the catalyst preparation process, sodium hydroxide is used as a precipitant, and the washing of the catalyst is cumbersome and consumes a large amount of deionized water.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Preparation of Cu:Mo:C weight ratio of 3-hydroxypropionate methyl ester hydrogenation catalyst of 45:18:7:

[0034] (1) Dissolve copper acetate and ammonium molybdate in deionized water according to the ratio, and stir and mix at room temperature;

[0035] (2) Weigh the starch by 3 times of the measured amount, then soak it with 2wt% acetic acid aqueous solution, the quality of the acetic acid aqueous solution is 5 times of the starch quality, then wash and filter three times with deionized water of the same quality;

[0036] (3) Quickly add the mixture obtained in step (1) to the starch obtained in step (2) and mix, then dry at 110°C for 10 hours, and then press into tablets;

[0037] (4) Then bake in the air at 130°C for 5 hours, and then bake in a nitrogen atmosphere at 700°C for 7 hours; then after cooling down to room temperature, air is introduced into the aforementioned nitrogen to make the volume of oxygen account for 1% of the total, and passivation After 8 ho...

Embodiment 2

[0040] Preparation of Cu:Mo:C weight ratio of 3-hydroxypropionate methyl ester hydrogenation catalyst of 3:1:1:

[0041] (1) Dissolve copper acetate and ammonium molybdate in deionized water according to the ratio, and stir and mix at room temperature;

[0042] (2) Weigh the starch according to 1.8 times of the measured amount, then soak it with 6wt% citric acid aqueous solution which is 4 times the mass of the starch, then wash and filter twice with deionized water of equal mass;

[0043] (3) Quickly add the mixture obtained in step (1) to the starch obtained in step (2) and mix, then dry at 120°C for 6 hours, and then press into tablets;

[0044] (4) Then roast in the air at 300°C for 4 hours, then roast at 800°C for 5 hours in a nitrogen atmosphere, then drop to room temperature, and feed oxygen into the aforementioned nitrogen so that the volume content of oxygen accounts for 2% of the total volume, Passivation for 4 hours; take out the catalyst, break it into 40-60 meshe...

Embodiment 3

[0047] Preparation of Cu:Mo:C weight ratio of 3-hydroxypropionate methyl ester hydrogenation catalyst of 49:14:27:

[0048] (1) Dissolve copper acetate and ammonium molybdate in deionized water according to the ratio, and stir and mix at room temperature;

[0049] (2) Weigh the starch according to 2.5 times of the measured amount, then soak it with 1wt% acetic acid aqueous solution which is 6 times the mass of the starch, then wash and filter twice with deionized water of equal mass;

[0050] (3) Quickly add the mixture obtained in step (1) to the starch obtained in step (2) and mix, then dry at 120°C for 6 hours, and then press into tablets;

[0051] (4) Then bake in the air at 250°C for 5 hours, then bake at 900°C for 4 hours in a nitrogen atmosphere; then lower it to room temperature, and let air flow into the aforementioned nitrogen so that the volume content of oxygen accounts for 1% of the total volume of the gas , passivated for 8 hours, took out the catalyst, crushed ...

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Abstract

The invention relates to a 3-methyl lactate hydrogenation catalyst which is composed of, by weight, 30-90% of Cu, 9-30% of Mo and 1-60% of C. The preparation steps include: (1) dissolving precursors of Cu and Mo elements in deionized water according to proportion, and mixing evenly; (2) weighing the precursors of a C element according to 1.8-3-times of stoichiometric ratio, then soaking in an organic acid solution, washing and filtering; (3) mixing substances in the step (1) and the step (2), then drying, tabletting and molding; and (4) roasting and passivating to obtain the catalyst. The catalyst is applied to hydrogenation preparing of 1,3-propylene glycol through 3- methyl lactate, conversion rate of the 3-methyl lactate is approximately 100%, and selectivity of 1,3-propylene glycol is more than 80%.

Description

technical field [0001] The invention relates to a hydrogenation catalyst for methyl 3-hydroxypropionate, a preparation method and application thereof, and belongs to the field of hydrogenation catalysts. technical background [0002] 1,3-propanediol is an important organic chemical raw material, and its biggest application is to polymerize with terephthalic acid to obtain PTT polyester. PTT polyester has excellent performance, good resilience, easy processing, easy dyeing and bulkiness, etc., and has a broad market prospect. [0003] At this stage, the synthesis routes of 1,3-propanediol mainly include: (1) The ethylene oxide method of Shell Company of the United States, using ethylene oxide hydroformylation to synthesize 3-hydroxypropionaldehyde, and then hydrogenating to synthesize 1,3- Propylene glycol, see patents US 5723389, US 6180838, US 8013192; (2) Degussa’s acrolein method, using acrolein hydration to generate 3-hydroxypropanal, and then hydrogenation to synthesiz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/22C07C31/20C07C29/149
Inventor 孙卫中张旭红焦国柱赵正康王志光梁铁
Owner SHANGHAI HUAYI ENERGY CHEM