Method for synthesizing terephthalonitrile

A technology of terephthalonitrile and synthesis method, applied in chemical instruments and methods, ammonia-carboxylic acid reaction preparation, carboxylic acid amide dehydration preparation and other directions, can solve the problems of difficulty in further improvement, great influence, and high production, etc., Achieve the effect of improving yield, reducing oxidation and reducing usage

Active Publication Date: 2021-06-15
ANSHAN HIFICHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The ammoxidation of terephthalonitrile is carried out under high temperature conditions, and side reactions such as deep oxidation and ammoxidative decomposition are prone to occur. The product selectivity and yield are affected by the catalyst and reaction conditions. The impact is relatively large, and the yield of the product needs to be further improved. The product contains a certain amount of impurities and needs to be purified. Even so, the quality is difficult to further improve, the production cost is high, and a large amount of three wastes will be generated.

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  • Method for synthesizing terephthalonitrile

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preparation example Construction

[0056] The present invention also provides the preparation method of the vanadium-chromium-phosphorus catalyst and the vanadium-chromium-phosphorus alkali metal catalyst, the method is that after the vanadium source is reduced, it is mixed with the chromium source, the phosphorus source and other metal sources to form a mixed solution II. On the carrier, the catalyst is obtained by calcining. Described concretely comprises the following steps:

[0057] Step a, dissolving the vanadium source in the reducing liquid, stirring and dissolving to obtain the mixed solution I.

[0058] The vanadium source is selected from pentavalent vanadium compounds, preferably selected from V 2 o 5 Or ammonium metavanadate, more preferably V 2 o 5 . The reducing liquid is oxalic acid aqueous solution, methanol or isobutanol, preferably oxalic acid.

[0059] The molar ratio of the vanadium source to the reducing liquid is 1:(1.1-14), preferably 1:(1.5-10), more preferably 1:(2-6). Wherein, t...

Embodiment 1

[0087] At room temperature, slowly dissolve 12.0 g of vanadium pentoxide in 220 g of oxalic acid aqueous solution containing 60 g, and stir to react. Heat above-mentioned solution to 80 ℃, add 3.0g chromium trioxide again, after it dissolves, add the phosphoric acid solution of the 85% concentration of 28g and 3.5g ammonium orthomolybdate ((NH 4 ) 2 MoO 4 ), stirred for 1 hour.

[0088] The above solution was added to 110 g of silica gel with a particle size of 80-120 mesh. The silica gel was preheated to about 85°C in advance, stirred evenly, left to stand at room temperature for 24 hours, and filtered to obtain a catalyst precursor.

[0089] Place the catalyst precursor in a muffle furnace and gradually raise the temperature to 620°C and keep it warm for 10 hours. After cooling to room temperature, a vanadium-chromium-phosphorus catalyst is obtained, which is bottled for later use. In the vanadium chromium phosphorus catalyst, the molar ratio of each element is V:Cr:P:Mo=...

Embodiment 2

[0091] At room temperature, slowly dissolve 10.0 g of vanadium pentoxide in 200 g of aqueous solution containing 75 g of oxalic acid, and stir to react. Heat the above solution to 80°C, add 6.5g of chromium trioxide and 2.5g of nickel chloride hexahydrate in sequence, after they dissolve, add 2.2g of cesium sulfate, stir and mix, after completely dissolving, add 25g of 85% phosphoric acid solution , add 1.0 g of potassium chloride, and stir for 1 hour.

[0092] The above solution was added to 100 g of silica gel with a particle size of 80-120 mesh. The silica gel was preheated to 85°C in advance, stirred evenly, left standing at 20-30°C for 24 hours, and filtered to obtain a catalyst precursor.

[0093] Take it out and place it in a muffle furnace to gradually raise the temperature to 640° C. and keep it warm for 12 hours. After cooling to room temperature, a vanadium-chromium-phosphorus alkali metal catalyst is obtained, which is bottled for later use. In the vanadium chromi...

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Abstract

The invention provides a method for synthesizing terephthalonitrile. The method comprises the following steps: performing catalytic oxidation reaction on paraxylene serving as a raw material in the presence of a vanadium catalyst, and controlling the reaction of synthesizing an intermediate product to obtain the terephthalonitrile. The production of byproducts in the ammoxidation process can be effectively reduced in the reaction process, so that the yield of terephthalonitrile is greatly improved, the raw materials are effectively utilized, impurity products in the product are few, and the post-treatment process is simplified. And the method is beneficial to realization of green chemistry, and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of terephthalonitrile. Background technique [0002] Terephthalonitrile, also known as terephthalonitrile or 1,4-dicyanobenzene, is an important chemical product intermediate, which can be used to manufacture various organic products such as pesticides, medicines, dyes, and spices, and has a wide range of uses. For example, terephthalonitrile can be hydrolyzed to obtain terephthalic acid or methyl terephthalate, polyester resin, etc.; after chlorination, fluorination and hydrolysis and other reaction processes, pyrethroid pesticide products can be obtained; P-xylylenediamine is an excellent resin curing agent. [0003] At present, the methods for preparing terephthalonitrile mainly include: oxidizing p-xylene to acid, aldehyde, etc., and then ammonolysis to prepare nitrile; dipentene ammoxidation method to prepare terephthalonitrile; p-xyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/28C07C255/57C07C253/22C07C253/20C07C255/51C07C255/50B01J27/199
CPCC07C253/28B01J27/199C07C253/22C07C253/20C07C255/51C07C255/57C07C255/50Y02P20/52
Inventor 权于于顺明高振聪
Owner ANSHAN HIFICHEM CO LTD
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