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Method for preparing heteropolyacid catalyst and method for producing methacrylic acid

Inactive Publication Date: 2001-10-11
SUMITOMO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0032] According to the invention, a heteropolyacid catalyst excelling in performance, life and strength can be prepared, and by using this heteropolyacid catalyst, methacrylic acid can be produced at high yield.EXAMPLES
[0033] Hereinafter the present invention is explained more specifically, referring to working Examples, it being understood that the invention is not limited thereto. In the following Examples and Comparative Examples, the conversion, selectivity and one-pass yield have the following definitions.Conversion (mol %)=(mol number of reacted methacrolein) / (mol number of supplied methacrolein).times.100Selectivity (mol %)=(mol number of formed methacrylic acid) / (mol number of reacted methacrolein).times.100One-pass yield (mol %)=(mol number of formed methacrylic acid) / (mol number of supplied methacrolein).times.100

Problems solved by technology

Those heteropolyacid catalysts which are prepared in the presence of a nitrogen-containing heterocyclic compound, however, are inferior in selectivity and activity for reaction and in catalytic life, compared to oxidation catalysts conventionally used for making acrylic acid from acrolein, where they are used, for example, in production of methacrylic acid from methacrolein, isobutyl aldehyde and / or isobutyric acid.
In consequence, those heteropolyacid catalysts must be used in large quantities and brings about rise in production costs.
Where no ammonium ion is contained, moldability is objectionably impaired.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0034] To 2,800 ml of 60.degree. C. water, 900 g of ammonium paramolybdate, 273 g of molybdenum trioxide and 68.2 g of ammonium matavanadate were added and stirred, followed by further addition of 280 g of pyridine and 87.4 g of phosphoric acid (85% by weight), and a solution of 400 g of nitric acid (65% by weight), 136.4 g of cesium nitrate and 14.1 g of copper nitrate as dissolved in 1,000 ml of water, by the order stated, under continual stirring. Whereby an aqueous mixture containing pyridine, nitrate anions and ammonium ions was obtained, the ammonium ions / nitrate anions (molar ratio) being 1.00 and the ammonium ions / 12 molybdenum atoms (molar ratio) being 8.49. This aqueous mixture was concentrated under heating and stirring, and the resulting clay-like substance was molded into a columns of each 5 mm in diameter and 6 mm in height, which were dried at 250.degree. C. and calcined in a gaseous nitrogen stream at 430.degree. C. for 4 hours, and then in an air stream at 400.degre...

example 2

[0038] Example 1 was repeated except that the amount of the ammonium paramolybdate was changed to 600 g and that of the molybdenum trioxide, to 518 g. The results are shown in Table 1.

example 3

Example 1 was repeated except that the amount of the ammonium paramolybdate was changed to 150 g, and that of the molybdenum trioxide, to 884 g. The results are shown in Table 1.

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PUM

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Abstract

A novel method for preparing a heteropolyacid catalyst containing a heteropolyacid composed of molybdophosphoric acid and / or molybdovanadophosphoric acid, or a salt of the heteropolyacid, is provided. The method comprises preparing an aqueous solution or aqueous dispersion which (1) contains the nitrogen-containing heterocyclic compound, nitrate anions and ammonium ions, (2) the ammonium ion content not exceeding 1.7 mols per mol of the nitrate anion content, and (3) the ammonium ion content not exceeding 10 mols per 12 mols of the molybdenum atom content by mixing raw materials containing the catalyst-constituting elements with the nitrogen-containing heterocyclic compound in the presence of water, drying and calcining the same. This heteropolyacid catalyst excels over conventional catalysts in performance, life and strength.

Description

TECHNICAL FIELD TO WHICH THE INVENTION BELONGS[0001] This invention relates to a method for preparing heteropolyacid catalyst and method for producing methacrylic acid. More particularly, the invention relates to a method for preparing heteropolyacid catalyst containing heteropolyacid formed of molybdophosphoric acid and / or molybdovanadophosphoric acid, or a salt of the heteropolyacid, which is suitable for use in preparation of unsaturated carboxylic acid through vapor phase oxidation of unsaturated aldehyde; and also to a method for producing methacrylic acid through vapor phase oxidation or vapor phase oxydehydrogenation of methacrolein, isobutyl aldehyde and / or isobutyric acid in the presence of said heteropolyacid catalyst.PRIOR ART[0002] It is well known to use heteropolyacid catalyst whose chief component is a heteropolyacid composed of phosphorus-molybdenum or phosphorus-molybdenum-vanadium, or a salt thereof, for producing methacrylic acid through vapor phase oxidation of m...

Claims

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Application Information

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IPC IPC(8): B01J27/188B01J27/19B01J27/198B01J27/199B01J27/25B01J31/02C07B61/00C07C51/235C07C51/25C07C51/377C07C57/04C07C57/055
CPCB01J23/002B01J27/188B01J27/19B01J27/199B01J2523/00C07C51/252C07C57/04B01J2523/15B01J2523/17B01J2523/51B01J2523/55B01J2523/68B01J31/02B01J27/25
Inventor KASUGA, HIROTONAKATANI, KAORISHIRAISHI, EIICHI
Owner SUMITOMO CHEM CO LTD
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