Catalyst for preparing unsaturated acid or unsaturated acid ester

A technology of catalysts and compounds, which is applied in the direction of molecular sieve catalysts, physical/chemical process catalysts, and carboxylate preparations, etc. It can solve the problems of unsatisfactory large-scale production, easy loss of active components, and complex influencing factors, and achieves good industrial application prospects. , low cost, simple effect of industrial preparation

Active Publication Date: 2018-06-01
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the catalysts used in the above studies are basic catalysts or acid-base bifunctional catalysts. The preparation process generally uses methods such as impregnation, ion exchange, and co-precipitation to load the active components on the carrier. There are cumbersome preparations, complex influencing factors and The shortcomings of low repeatability and easy loss of active ingredients cannot meet the needs of industrial mass production

Method used

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  • Catalyst for preparing unsaturated acid or unsaturated acid ester
  • Catalyst for preparing unsaturated acid or unsaturated acid ester
  • Catalyst for preparing unsaturated acid or unsaturated acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] The preparation of embodiment 1 catalyst

[0059] Na-Molecular sieves with FER configuration

[0060] Na-FER molecular sieves were purchased from Shanghai Zhuoyue Chemical Technology Co., Ltd.

[0061] Table 1 Na-FER molecular sieves with three different average particle sizes

[0062] Na-FER

Si / Al

Grain size (μm)

D. 50 (μm)

Sample A

2 / 6.5

0.1-0.5

1.6

Sample B

30 / 7

0.5-1.5

3.0

Sample C

50 / 6.5

1.5-3.5

4.8

[0063] Preparation of H-FER

[0064] Na-FER catalyst was purchased from Shanghai Zhuoyue Chemical Technology Co., Ltd. 10 grams of calcined Na-molecular sieves with FER configuration were exchanged three times with 0.5mol / L ammonium nitrate for 2 hours each time, washed with deionized water, dried, calcined at 550°C for 4 hours, and prepared by extrusion into 20 ~40 mesh H-FER catalyst, samples A, B, and C were prepared as catalyst samples 1#, 2#, and 3#, respectively.

[0065] Preparatio...

Embodiment 2

[0091] Embodiment 2 methylal DMM reacts with methyl acetate MAc

[0092]10g of the above-mentioned catalyst samples 1# to 10# and catalyst samples D0# to D10# were respectively loaded into a fixed-bed reactor with a tube inner diameter of 28mm, and the temperature was raised to 550°C at 5°C / min under a nitrogen atmosphere and kept for 4 hours. Then the nitrogen atmosphere was lowered to the reaction temperature of 350° C., and the pressure of the reaction system was raised to the reaction pressure of 3 MPa with nitrogen. The reaction raw materials (wherein the molar ratio of methylal and methyl acetate is 2:1) from top to bottom at a total feed space velocity of 0.3h -1 Through the catalyst bed, the catalyst evaluation results are shown in Table 3. After 30 hours of reaction time, samples were taken and analyzed, and the results are shown in Table 3.

[0093] Table 3 Catalyst evaluation results for the reaction between methylal DMM and methyl acetate MAc

[0094]

Embodiment 3

[0095] Embodiment 3 different reaction conditions

[0096] Put 10g of the above-mentioned 10# catalysts into the column tubes respectively, pass through a 28mm fixed bed reactor, raise the temperature to 550°C at 5°C / min under nitrogen atmosphere, and keep it for 4 hours. Then the nitrogen atmosphere is lowered to a reaction temperature of 200°C to 400°C, the DMM / MAc molar ratio is 2 / 1, and the pressure of the reaction system is raised to a reaction pressure of 0.2Mpa to 15.0Mpa with nitrogen. Feed the raw materials from top to bottom at a total feed space velocity of 0.05h -1 to 10.0h -1 through the catalyst bed. The specific reaction conditions are shown in Table 4. After 30 hours of reaction time, samples were taken for analysis, and the results are shown in Table 4.

[0097] Pretreatment and reaction conditions of the catalyst of table 4

[0098]

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Abstract

The invention relates to a catalyst for preparing unsaturated acid or unsaturated acid methyl ester, in particular to a molecular sieve with FER configuration and a method for preparing unsaturated acid or unsaturated acid methyl ester by using the molecular sieve. The catalyst contains the molecular sieve with FER configuration, and further, the median particle diameter D50 of the molecular sievewith FER configuration is smaller than or equal to 6 mu m; preferably, the molecular sieve with FER configuration has median particle diameter D50 of 0.15-3.5 mu m.

Description

technical field [0001] The invention relates to a catalyst for preparing unsaturated acid or unsaturated ester, in particular to a molecular sieve with FER configuration and a method for preparing unsaturated acid or unsaturated ester by using the catalyst. Background technique [0002] Acrylic acid and methyl acrylate are important chemical raw materials, which can be used as coatings, flocculants, dispersants and binders, and are widely used in construction, water treatment, daily chemical, soil treatment and leather industries. People's daily life is closely related. At present, the most commonly used method in the industry to prepare acrylic acid and methyl acrylate is the two-stage oxidation of propylene, that is, the first step of oxidizing propylene to acrolein, and further oxidation to obtain acrylic acid. However, the raw material propylene comes from petroleum, which is a non-renewable resource and does not conform to the concept of sustainable development. [00...

Claims

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Application Information

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IPC IPC(8): B01J29/68B01J29/67B01J29/65C07C27/00C07C51/09C07C57/04C07C67/343C07C69/54
CPCB01J29/65B01J29/67B01J29/68B01J2229/186C07C51/09C07C67/343C07C57/04C07C69/54
Inventor 马占玲朱文良马现刚刘红超刘勇倪友明刘世平陈其伟刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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