Catalyst for producing methyl-acrylate from methyl-acrolein and its production

A technology of methyl methacrylate and methacrolein, which is applied in the field of catalysts and its preparation, can solve the problems of long reaction time, poor selectivity of MAA, low mechanical strength, etc., and achieve reduction of preparation cost, increase of space-time yield, The effect of simple manufacturing process

Inactive Publication Date: 2007-11-21
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of catalyst has the problems of low activity and long reaction time. Pd is a noble metal, and the production cost of the catalyst is very high, which brings inconvenience to large-scale industrial development.
The latter class divides the oxidative esterification into two steps, and first oxidizes MAL to MAA. It is mainly composed of P, Mo and V as the catalyst of the Keggin type heteropoly compound, and its counterion is based on alkali metal ions, such as JP57-171443, CN1483014A and CN1273232A, but this solid catalyst has defects such as poor thermal stability, low mechanical strength, short service life, poor selectivity to generate MAA; MAA and methyl alcohol are then obtained under the effects of catalysts such as acidic cationic resins MMA , using acidic resin as catalyst, such as Japanese Patent Application No. 59-65041, 54-81213, 58-159442 and CN1052848A

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 50 g of PMo 11 V 1 o 40 31H 2 O was dissolved in 20 ml of water, and CsNO was added slowly 3 1.5g, KNO 3 0.50 g, Bi(NO 3 ) 3 ·5H 2 O0.50 g, Cu(NO 3 ) 2 ·3H 2 O1.00 g, As 2 o 5 0.50 grams, 10 grams of quinoline dissolved in 20 milliliters of dilute nitric acid solution, mixed with the above solution, stirred evenly, baked at 105 ° C for 5 hours, crushed, finely ground, and pressed into tablets to make 40-60 mesh particles , and then pass nitrogen gas at 400°C for 3 hours, cool down to 350°C, and pass air for 3 hours. The gas flow rate is 50ml / min. i.e. get H 2.4 PMo 11 VCs 0.33 K 0.23 Bi 0.05 Cu 0.19 As 0.1 o 40 catalyst.

[0014] Application: reaction raw materials: methanol, water, MAL, air molar ratio is 2:1:1:6; reaction conditions: take 3 grams of the above catalyst in a fixed bed reactor, reaction temperature 290 ° C, normal pressure, total Volumetric space velocity 200h -1 ;Reaction products: methanol, water, air, MMA, MAA, MAL and other ace...

Embodiment 2

[0016] 50 g of H 5 PMo 10 V 2 33H 2 O was dissolved in 20 ml of water, and CsNO was added slowly 3 2.00 g, add KNO 3 0.50 g, Cu(NO 3 ) 2 ·3H 2 O0.50 g, As 2 o 5 0.70 grams, 5 grams of quinoline dissolved in dilute nitric acid solution, mixed with the above solution, stirred evenly, baked at 80°C for 5 hours, pulverized, finely ground, and tableted to make 40-60 mesh particles. Then nitrogen gas was passed in at 380° C. for 5 hours, then the temperature was lowered to 350° C., and air was passed in for 5 hours. The gas flow rate was 50 ml / min. i.e. get H 3.2 PMo 10 V 2 Cs 0.47 K 0.23 Bi 0.05 Cu 0.10 As 0.13 o 40 catalyst.

[0017] Application situation: reaction raw materials: methanol, water, MAL, air molar ratio is 2:1:1:6; reaction conditions: take 3 grams of catalyst in a fixed bed reactor, temperature 280 ° C, normal pressure, total volume empty Speed ​​180h -1 , Reaction products: methanol, water, air, MMA, MAA, MAL and other acetic acid, CO, CO 2 ; ...

Embodiment 3

[0019] 50 g of H 4 PMo 11 V·31H 2 O was dissolved in 20 ml of water and NaNO was added slowly 3 0.40 g, CsNO 3 2.00 g, Fe(NO 3 ) 3 9H 2 O1.58g, AgNO 30.66 grams, 5 grams of quinoline was dissolved in dilute nitric acid solution, mixed with the above solution, stirred evenly, baked at 130°C for 5 hours, crushed, finely ground, and tableted to make 40-60 mesh particles. Nitrogen gas was then fed at 450°C for 8 hours, then the temperature was lowered to 350°C, and air was fed for 3 hours. The gas flow rate was 50ml / min. i.e. get H 2.58 PMo 11 VCs 0.48 Na 0.22 Fe 0.18 Ag 0.18 o 40 catalyst.

[0020] Application situation: reaction raw materials: methanol, water, MAL, air molar ratio is 3:1:1:6; reaction conditions: take 3 grams of catalyst in a fixed bed reactor, temperature 280 ° C, normal pressure, total volume empty Speed ​​300h -1 ;Reaction products: methanol, water, air, MMA, MAA, MAL and other acetic acids, CO, CO 2 ; Reaction results: MAL conversion rate 6...

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PUM

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Abstract

The invention is concerned with the activator of polymethyl methacrylate and the preparation method that makes by methyl propenal directly, which is heteropolyacids catalyst with Keggin structure character. The transforming rate of the activator MAL is over 95%, which can maintain the selection of MMA to be over 90%, the stability of the activator is good; the feedback rate is higher than the reaction that the activator is Pd, the activator is fit for fixing bed reactor, the touching time is 20 to 28second, but, the Pd activator is fit for batch reactor, the reacting time is several hours.

Description

Technical field: [0001] The invention relates to a catalyst for directly preparing methyl methacrylate from methacrolein and a preparation method thereof. Background technique: [0002] Methyl methacrylate (MMA) is an important organic chemical raw material, mainly used in the production of plexiglass (PMMA), also used in the manufacture of polyvinyl chloride additive ACR and as a second monomer in the production of acrylic fibers. In addition, it is also widely used in coatings, textiles, adhesives and other fields. As a chemical product, it can be directly applied to leather, textiles, papermaking, floor polishing, unsaturated resin modification, methacrylic acid advanced esters, and can also be used as wood impregnating agent, printing and dyeing auxiliary agent, plasticizer of plastic, etc. industry. [0003] In the past, the method for synthesizing MMA was mainly the acetone cyanohydrin method (ACH method). The raw materials used in the production process of this met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/186B01J27/185B01J27/18B01J27/182C07C69/653C07C67/39
Inventor 陈标华黄崇品郭晓俊
Owner BEIJING UNIV OF CHEM TECH
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