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Catalyst for preparing isophthalodinitrile and preparation method and use thereof

A technology of isophthalonitrile and catalyst, applied in the field of catalyst for preparing isophthalonitrile and its preparation and application, can solve the problems of poor catalyst activity, poor selectivity, low conversion rate, etc., and reduce the cost of raw materials , less ammonia consumption and strong adsorption capacity

Active Publication Date: 2009-10-14
SHANGHAI TAIHE INT TRADE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The present invention is to solve the above problems, overcome the problems of poor catalyst activity, poor selectivity, low conversion rate and high cost, and provide a catalyst for preparing isophthalonitrile and its preparation method and use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Catalyst preparation

[0044] First put 2.8g of V 2 o 5 and 1.05gCrO 3 Add them together to 250ml distilled water containing 20g oxalic acid, heat and dissolve at about 343K to make a dark blue solution. Then add 0.15g of KCl, 1.25g of P 2 o 5 , 1.00g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 2.00g NiCl 2 ·6H 2O and other substances, stirred to make a transparent solution of the active substance. Add 100 g of dried 120-mesh spherical silica gel to the above solution, stir evenly, dry at 373K, and then activate at 813K for 6 hours to obtain the required catalyst.

[0045] Ammoxidation of m-xylene

[0046] In a steel pipe with an internal diameter of 40mm, add 90g of catalyst prepared by the method described in this example, heat up to 643K, and press m-xylene: ammonia: oxygen (converted by air) = 1: 2.5: 10 in the amount of substance ratio The reaction mixture is sent into the reactor, the conversion rate of m-xylene is 99.6%, and the mass yield of isophthalonitrile is 9...

Embodiment 2

[0048] Catalyst preparation

[0049] Put 2.80g of V 2 o 5 and 1.05g of CrO 3 Add them together to 250ml distilled water containing 20g oxalic acid, heat and dissolve at about 343K to make a dark blue solution, then add 0.16g NaCl, 1.10g P 2 o 5 , 1.04g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 2.10 g NiCl 2 ·6H 2 O, dissolve evenly and make a transparent solution. Add 100 g of dried 80-mesh spherical silica gel (same example 1) into the transparent solution, stir evenly, dry at 373K, and activate at 813K for 6 hours to obtain the desired catalyst.

[0050] Ammoxidation of m-xylene

[0051] In the reactor described in Example 1, add 90 g of catalysts prepared by the method described in this example, maintain the temperature of the catalyst bed at 643K, press m-xylene: ammonia: oxygen (converted by air)=1: 6: 16 The amount ratio of the substance is to send the reaction mixture into the reactor, the conversion rate of m-xylene is 98.9%, and the mass yield of isophthalonitrile is 9...

Embodiment 3

[0053] Catalyst preparation

[0054] Put 2.80g of V 2 o 5 and 1.16g of CrO 3 Add them together to 250ml distilled water containing 20g oxalic acid, heat and dissolve at about 343K to make a dark blue solution, then add 0.17g NaCl, 1.18g P 2 o 5 , 0.85g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 2.46g NiCl 2 ·6H 2 O, dissolve evenly and make a transparent solution. Add 100 g of dried 40-mesh spherical silica gel (same example 1) into the transparent solution, stir evenly, dry at 373K, and activate at 813K for 6 hours to obtain the desired catalyst.

[0055] Ammoxidation of m-xylene

[0056] In the reactor described in Example 1, add 90 g of the catalyst prepared by the method described in this example, maintain the temperature of the catalyst bed at 643K, press m-xylene: ammonia: oxygen (converted by air)=1: 1.2: 4 The amount ratio of the substance is to send the reaction mixture into the reactor, the conversion rate of m-xylene is 98.7%, and the mass yield of isophthalonitrile i...

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Abstract

A catalyst for preparing isophthalodinitrile uses spherical silica gel or gamma-Al2O3 of 40 to 120 meshes as carrier; the main active substances are V2O5, MoO3 and CrO3; the auxiliary active substances are oxides of Ni and P and at least one oxide of Na, K and Cs; and the contents of the active components are in the range of 1.05% to 28%, preferably 3% to 20%. A preparation method is as follows: the oxides or salts of the component elements are respectively dissolved; the calcined carrier is poured in the solution to be exactly immersed, and is aged and dried to activate for 6 to 7 hours at 773K to 823 K to obtain the required catalyst. The catalyst in the invention is used for synthesizing isophthalodinitrile by gas phase ammonia oxidation process. The invention has the advantages of wide material selection, simple preparation method and high yield.

Description

technical field [0001] The present invention relates to a kind of catalyst for preparing isophthalonitrile and its preparation method and application Background technique [0002] Isophthalonitrile (abbreviated as IPN) is an important organic raw material for organic synthesis. Tetrachloroisophthalonitrile synthesized by chlorination is an efficient and low-toxic fungicide; m-xylylenediamine obtained by hydrogenation is a superior performance It is an excellent curing agent for epoxy resin, and it is also a raw material for polyurethane resin and nylon resin. [0003] The simplest and most economical production method of isophthalonitrile is obtained by gas-phase ammoxidation of m-xylene under the action of a catalyst, and its core technology is the catalyst. [0004] In the 1950s, Japan’s Showa Denko developed the production technology of m-xylene ammoxidation in a fixed bed to synthesize isophthalonitrile. In the 1970s, Japan’s Mitsubishi Gas Co., Ltd. and the US Badger C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/199B01J21/08B01J21/04C07C253/28C07C255/51
Inventor 王海波李强田晓宏
Owner SHANGHAI TAIHE INT TRADE CO LTD