Catalyst for hydrogenation preparation of 1,3-propanediol from methyl 3-hydroxypropionate and preparation method of catalyst

A technology of methyl hydroxypropionate and catalyst, which is applied in the direction of preparation of hydroxy compounds, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., and can solve the problems that do not involve the order of addition and the method of addition, and are not clearly stated Hydrogenation conditions, poor catalytic effect, etc., to achieve the effects of enhanced interaction, prevention of sintering, and stable active centers

Inactive Publication Date: 2016-11-16
山东玉皇盛世化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the three different catalysts, the nickel-based catalyst represented by Raney nickel has the characteristics of complicated preparation, complicated reaction process and low catalyst activity.
Samsung Electronics Co., Ltd. discloses a method for preparing 1,3-propanediol from epoxides in patent US6348632. Using a copper chromate catalyst and reacting for 15 hours at 180°C, the conversion rate of methyl 3-hydroxypropionate is only 5%, 1 , The selectivity of 3-propanediol is only 3%, not only the catalytic effect is not good, but also there is the problem of chromium pollution. Special attention must be paid to the catalyst preparation, reaction process and post-treatment process
Although the method for preparing 1,3-propanediol from methyl 3-hydroxypropionate has been reported above, it does not involve the order and method of feeding in the preparation process, nor does it clearly state the hydrogenation conditions.

Method used

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  • Catalyst for hydrogenation preparation of 1,3-propanediol from methyl 3-hydroxypropionate and preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Dissolve 39.48g of copper nitrate and 4.12g of manganese nitrate in 400mL of deionized water, and 465ml of 0.7mol / L sodium hydroxide solution at 45°C and 200rpm under stirring at 0.8ml / min, then add 20g of silica sol, wait After the pH of the precipitate is 12.0, it is aged at 66°C for 1 hour, washed three times, then vacuum-dried at 100°C for 24 hours, calcined at 500°C for 4 hours, sieved into 20-40 mesh and packed, at 450°C, 8.0MPa, with hydrogen Volume concentration 20vol.% Hydrogen-nitrogen mixed gas reduction for 1 hour, pass through a methanol solution of 3-hydroxypropionate with a mass concentration of 5%, react at 200°C, 6.0MPa, for 4 hours, take out the reacted liquid and use GC -7890A gas chromatograph analysis and determination, the evaluation results are shown in Table 1.

Embodiment 2

[0029] Dissolve 27.34g of copper nitrate, 3.72g of lanthanum nitrate, 2.34g of nickel nitrate in 400mL of deionized water, and 400ml of 0.3mol / L sodium hydroxide solution at 30°C and 600rpm with stirring at 6ml / min, and then add 30g Silica sol, after the pH of the precipitate is 7.0, age at 40°C for 6h, wash three times, vacuum dry at 60°C for 40 hours, bake at 850°C for 4 hours, sieve into 20~40 mesh and fill, at 200°C, 6.0MPa After reducing for 20 hours with a hydrogen-nitrogen mixed gas with a hydrogen volume concentration of 5vol.%, pass through a methanol solution of 3-hydroxypropionate with a mass concentration of 20%, react at 160°C and 8.0MPa for 20 hours, and take out the reaction The final liquid was analyzed and determined by GC-7890A gas chromatograph, and the evaluation results are shown in Table 1.

Embodiment 3

[0031] Dissolve 33.41g of copper nitrate, 2.19g of zinc nitrate, 1.47g of ammonium molybdate, and 0.60g of ammonium phosphate in 400mL of deionized water, and 480ml of 1.3mol / L sodium hydroxide solution at 60°C and 800rpm at 8ml / min Co-precipitate, then add 23.33g of silica sol, after the pH of the precipitate is 13.0, age at 100°C for 10h, wash twice, vacuum dry at 140°C for 4 hours, roast at 700°C for 18 hours, sieve into 20~40 mesh equipment, at 400°C, 0.01MPa, after 48h reduction with a hydrogen-nitrogen mixed gas with a hydrogen volume concentration of 10vol.%. MPa, react at lower temperature for 15 hours, take out the liquid after reaction and adopt GC-7890A gas chromatograph to analyze and measure, and the evaluation results are shown in Table 1.

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Abstract

The invention relates to the field of hydrogenation catalysts, in particular to a catalyst for hydrogenation preparation of 1,3-propanediol from methyl 3-hydroxypropionate and a preparation method of the catalyst. The catalyst for hydrogenation preparation of 1,3-propanediol from methyl 3-hydroxypropionate is characterized in that SiO2 serves as a carrier, a Cu-based catalyst is adopted, one or more of the elements of Zn, Zr, Mn, La, P, Mo and Ni are added to serve as auxiliaries, and the catalyst comprises, by mass, 45%-75% of CuO, 15%-45% of SiO2 and 0.1%-25% of auxiliaries. The obtained catalyst is small in particle size, high in dispersity of active components and large in specific surface area; when the catalyst is used for hydrogenation preparation of 1,3-propanediol from methyl 3-hydroxypropionate, the activity and selectivity are high, and the repeatability is good.

Description

technical field [0001] The invention relates to the field of hydrogenation catalysts, in particular to a catalyst for hydrogenating 3-hydroxypropionate methyl ester to prepare 1,3-propanediol and a preparation method thereof. Background technique [0002] 1,3-Propanediol (1,3-PDO) is an important chemical raw material. It can be used to produce antifreeze, detergent, preservative, etc. It is the basic raw material of many polymers. The most important application developed at present is the synthesis of polytrimethylene terephthalate (PTT). Compared with PET (polyethylene terephthalate) and PBT (polybutylene terephthalate), PTT not only has excellent properties such as light resistance, less water absorption, and good stability, but also has good resilience. Due to the advantages of easy biodegradation and little environmental pollution, it is widely used in the field of fibers and plastics, and is the focus of current research and development. [0003] At present, there ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/889B01J23/83B01J23/88B01J23/72B01J23/80C07C29/149C07C31/20
CPCB01J23/8892B01J23/002B01J23/72B01J23/80B01J23/83B01J23/8873B01J2523/00C07C29/149B01J2523/17B01J2523/41B01J2523/72B01J2523/3706B01J2523/847B01J2523/27B01J2523/68B01J2523/48C07C31/205
Inventor 冯靓婧刘长城张勇帅王玉强陈双喜王胜伟
Owner 山东玉皇盛世化工股份有限公司
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