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Method for preparing unsaturated acid from unsaturated aldehyde

A technology of unsaturated and acrolein, applied in the field of unsaturated aldehydes to prepare unsaturated acids, can solve the problems of difficult and accurate control, and achieve the effects of difficult phase transition, high product selectivity and yield, and reasonable temperature distribution

Active Publication Date: 2015-05-27
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Tungsten bias on the surface side of the catalyst, and / or copper bias on the core side of the catalyst is difficult to accurately control

Method used

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  • Method for preparing unsaturated acid from unsaturated aldehyde
  • Method for preparing unsaturated acid from unsaturated aldehyde
  • Method for preparing unsaturated acid from unsaturated aldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1. Preparation of catalyst (I)

[0035] Under stirring conditions, take 180.1 grams of ammonium molybdate and 19.9 grams of ammonium metavanadate and dissolve them in 1000 ml of pure water (water temperature above 65°C) to obtain slurry (1), then take 98.9 grams of copper nitrate, 26.7 grams of strontium nitrate, 2.5 Dissolve one gram of zinc nitrate in 1000ml of purified water (water temperature above 65°C), stir well and mix evenly to obtain slurry (2). Then, the slurry (1) was mixed with the slurry (2) to obtain the slurry (3), and then 1.4 g of titanium dioxide and 64.4 g of antimony trioxide were added to obtain the active component slurry (a). Add 4.6 grams of silicon dioxide and 3.1 grams of graphite to the active component slurry (a), stir vigorously at 80°C for co-precipitation reaction, heat and dry, heat-treat at 160°C for 3 hours in nitrogen, and then extrude through an extruder It is a hollow columnar particle of φ4.5×5mm, which is dried at 110°C and then ...

Embodiment 2

[0043] Preparation of Catalyst 2

[0044] The preparation steps and main raw materials are the same as those of catalyst 1 in Example 1, and the catalyst (I) is obtained by calcining at 480° C. for 4 hours. Catalyst (I) is mainly composed of: Mo 12 V 6 Cu 0.6 Sb 0.5 Sr 1.9 Si 2.3 La 3 Zr 0.3 Ti 0.2 o x ,

[0045] Take 97 parts of catalyst (I), 3 parts of magnesium-based lanthanum hexaaluminate, add deionized water and knead in a kneader, extrude into hollow columnar particles of φ4.5×5mm, dry at 120°C, and dry at 500°C Calcined for 3.5 hours to obtain catalyst 2.

[0046] The inner diameter of the fixed-bed single-tube reactor is 25mm, and a thermocouple is installed inside. 45ml of the above-mentioned catalyst is loaded into the reactor bed along the feeding direction, and heated in a salt bath with a salt bath temperature of 255°C. From the entrance of the above reaction tube at a space velocity of 1700h -1 A mixed gas of 9 vol % of acrolein, 13 vol % of oxygen,...

Embodiment 3

[0048] The preparation steps and main raw materials are the same as those of catalyst 1 in Example 1, and the catalyst (I) is obtained by calcining at 500°C for 4 hours. Catalyst (I) is mainly composed of: Mo 12 V 4 Cu 3.5 Sb 3.5 Sr 0.1 Si 1.1 La 1.0 Zr 0.2 o x , take 94 parts of catalyst (Ⅰ), 6 parts of magnesium-based lanthanum hexaaluminate, add deionized water and knead in a kneader, extrude into hollow columnar particles of φ4.5×5mm, dry at 120°C, 500°C The catalyst 3 was obtained by lower calcining for 4 hours.

[0049] The internal diameter of the fixed-bed single-tube reactor is 25 mm, and a thermocouple is installed inside. The reactor bed layer is filled with 50 ml of the above-mentioned catalyst along the feeding direction, and heated in a salt bath with a temperature of 257 °C. From the entrance of the above reaction tube at a space velocity of 2000h -1 A mixed gas of 10% by volume of acrolein, 14% by volume of oxygen, 15% by volume of water vapor, and 61...

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Abstract

The invention relates to a method for preparing unsaturated acid from unsaturated aldehyde. A fixed bed reactor is employed in the method. Reaction raw materials are preheated through a pre-heater to higher than 160 DEG C and then are fed into the reactor, wherein a salt bath is employed for heating the raw materials at a salt bath temperature of 240-265 DEG C and at a space velocity of 800-2200 / h. The reaction raw materials comprise following components, by volume, 8-12% of acraldehyde or methyl acraldehyde, 11-17% of water steam, 9-17% of oxygen and 60-72% of nitrogen. The fixed bed reactor is filled with an oxidizing catalyst, which contains elements of molybdenum, vanadium, copper and antimony. Main composition of the catalyst is represented as the following general formula: MoVCu<c>Sb<d>Sr<e>Si<f>M<g>N<h>O<x> (I). The catalyst also contains magnesium-based lanthanum hexaaluminate. The catalyst is prepared by: mixing the compound represented containing the molybdenum and the vanadium as the formula (I) with the magnesium-based lanthanum hexaaluminate respectively according to mass percentage ratios of 91-98% and 0.5-10%; kneading the raw materials of the catalyst; moulding the catalyst; and drying and roasting the catalyst. The method can produce acrylic acid stably for a long period.

Description

technical field [0001] The invention relates to a method for preparing unsaturated acid from unsaturated aldehyde, especially a method for preparing acrylic acid or methacrylic acid by selective oxidation of acrolein or methacrolein. Background technique [0002] Industrially, the reaction device for the oxidation of acrolein or methacrolein to prepare the corresponding unsaturated acid is mainly composed of multiple reaction tubes. On the premise of ensuring that the catalyst is not sintered and has a long service life, the selectivity and the yield of the target product should be improved as much as possible. Raw materials are saved. If the conversion rate of raw materials and the yield of acrylic acid are increased by 0.1-0.5 percentage points, the amount of products obtained will increase by hundreds to thousands of tons, and the economic benefits will be considerable. [0003] The catalysts for the partial oxidation of propylene to acrolein and acrylic acid are mainly m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/25C07C57/055B01J23/887
CPCB01J23/8876B01J2523/17B01J2523/24B01J2523/27B01J2523/3706B01J2523/41B01J2523/47B01J2523/48B01J2523/53B01J2523/55B01J2523/64B01J2523/68C07C51/252C07C57/04
Inventor 翟月勤刘俊保吴毅范国宁李晓银魏玉丽陈跟平曹帅英王春龙张士玉王芳杨芳耿占杰高杜娟高冬梅
Owner PETROCHINA CO LTD
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