Catalyst used in preparation of acrylic acid and/or acrylic acid ester from lactic acid or lactate through dehydration

An acrylate and lactate technology, applied in the field of catalysis, can solve the problems of low catalyst stability, inability to meet industrial requirements, and many by-products of lactic acid dehydration, and achieve good reproducibility, good industrial application prospects, and easy process control. Effect

Inactive Publication Date: 2014-12-03
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Catalysts with better results are generally supported phosphate catalysts or modified molecular sieve catalysts, but there is still no industrialized production example of lactic acid (ester) to prepare acrylic acid (ester). Very low, far from meeting the needs of industrialization, so it is urgent to design a new high-efficiency catalyst

Method used

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  • Catalyst used in preparation of acrylic acid and/or acrylic acid ester from lactic acid or lactate through dehydration

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Catalyst preparation

[0041] First weigh CuSO according to the loading amount of 10wt% 4 , add water to dissolve according to the excess impregnation method, and 5g of dried silica gel (specific surface area 320m 2 / g) was added to the solution; dried at 100°C for 4h, then transferred to a muffle furnace and roasted at 500°C for 3h to obtain CuSO loaded on silica gel 4 Material.

[0042] Then take Na by weighing 30wt% load 2 HPO 4 , add a certain amount of water to mix and dissolve according to the same amount of impregnation method, and the silica gel-loaded CuSO prepared in the above steps 4 The material was immersed; dried at 100°C for 4h, then transferred to a muffle furnace, and baked at 500°C for 3h to make a silica gel-loaded composite Na 2 HPO 4 / CuSO 4 catalyst.

[0043] Catalyst application

[0044] Weigh 2g of the catalyst prepared in the above preparation process, put it into a 8mm×400mm quartz glass tube fixed-bed microreactor, and carry out the r...

Embodiment 2

[0046] Catalyst preparation

[0047] In embodiment 2, this process is different from embodiment 1 in that, by weighing CuSO 4 , using a specific surface area of ​​200m 2 / g of silica gel; dry at 120°C for 3 hours, then bake.

[0048] Weigh K according to 10wt% load 3 PO 4 , and take the cocatalyst cobalt acetate by 0.5wt% load and weigh Pd(NO by 0.1wt% load 3 ) 2 , add a certain amount of water to mix and dissolve according to the same amount of impregnation method, and then add CuSO loaded on silica gel 4 The material was immersed; after drying, it was baked at 700°C for 2h, and the other reaction conditions were the same as in Example 1 to make a silica gel-loaded composite K 3 PO 4 / CuSO 4 / Co / Pd catalyst.

[0049] Catalyst application

[0050] Example 2 In the same reactor as in Example 1, the reaction of lactic acid dehydration to produce acrylic acid is carried out. The difference between this process and Example 1 is that during the reaction, the concentration...

Embodiment 3

[0052] Catalyst preparation

[0053] In embodiment 3, this process is different from embodiment 1 in that, by weighing FeSO 4 , using a specific surface area of ​​320m 2 / g of MCM-41 all-silicon molecular sieve; dry at 100°C for 6 hours, and bake at 350°C for 4 hours.

[0054] Then weigh KH by 50wt% load 2 PO 4 , and weigh the cocatalyst Ce(NO 3 ) 3 , weigh the cocatalyst Y (NO 3 ) 3 , add a certain amount of water to mix and dissolve according to the same amount of impregnation method, and then add FeSO loaded on silica gel 4 Material immersion; drying at 100°C for 6 hours, roasting at 600°C for 3 hours, and other reaction conditions are the same as in Example 1 to make a composite KH compound supported by MCM-41 all-silicon molecular sieve 2 PO 4 / FeSO 4 / Ce / Y catalyst.

[0055] Catalyst application

[0056] Embodiment 3 carries out the reaction that ethyl lactate is dehydrated to produce acrylic acid and ethyl acrylate in the reactor identical with embodiment 1,...

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Abstract

The invention discloses a catalyst used in preparation of acrylic acid and / or acrylic acid ester from lactic acid or lactate through dehydration. The catalyst comprises a composite phosphate / sulfate main catalyst, a rare earth metal cocatalyst and a silica gel, silica sol or total silicon molecular sieve carrier. The invention also discloses a preparation method for the catalyst, and the method comprises the steps of loading the phosphate / sulfate main catalyst and a metal salt of the cocatalyst on the carrier by using an impregnation method or a mixed precipitation method after dissolving the main catalyst and the metal salt and carrying out drying and roasting activation. The catalyst is used in preparation of acrylic acid and / or acrylic acid ester from lactic acid or lactate through dehydration, and through control of reaction conditions, the catalyst enables a conversion rate of raw materials to reach 100% and selectivity of products to reach 80.4% and to maintain at more than 70% for a long time. The catalyst has the advantages of a long service life, low cost, good reproducibility and wide industrial application prospects.

Description

technical field [0001] The invention belongs to the field of catalyst preparation and bio-based chemicals, and relates to a catalyst for preparing acrylic acid and / or acrylate by dehydration of lactic acid or lactic acid ester and its preparation and application, in particular, to a loaded compound Salt catalyst and its preparation method, and the application of the catalyst in preparing acrylic acid and / or acrylic acid ester through dehydration reaction of lactic acid or lactate. Background technique [0002] Acrylic acid and its esters are an important basic raw material and intermediate in modern organic chemical industry, and occupy an extremely important position in the fine chemical industry. Acrylic acid (ester) is the main structural unit of acrylic polymers, etc. Its polymers have excellent weather resistance, water resistance, heat resistance, etc., so that they can be obtained in coatings, plastics, papermaking, textiles, leather, super absorbent resins, etc. Wid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/182B01J27/185B01J29/03C07C57/065C07C51/377C07C69/54C07C67/327
CPCY02P20/584
Inventor 谭天伟莫志朋刘广黄辉韩超
Owner BEIJING UNIV OF CHEM TECH
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