A kind of synthetic method of phthalonitrile

A technology of phthalonitrile and synthesis method, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., and can solve no reports on pilot scale and industrialization , there are not many research reports, and the weight yield is high, which is conducive to large-scale production, a wide range of raw material sources, and good reaction selectivity.

Active Publication Date: 2022-01-11
ANSHAN HIFICHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In practical applications, even for catalysts with high selectivity, phthalimide may become the main product due to changes in process conditions. Therefore, it is difficult to develop catalysts for ammoxidation of o-xylene
So far, there are not many domestic research reports, and the highest weight yield is only 75%, and there has been no report on pilot test and industrialization

Method used

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  • A kind of synthetic method of phthalonitrile

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preparation example Construction

[0033] The synthesis method of phthalonitrile provided by the present invention uses o-xylene as a raw material to carry out hierarchical catalytic synthesis, which specifically includes the following steps.

[0034] Step 1, mixing o-xylene, ammonia and air to carry out a first-order catalytic reaction to obtain a mixed intermediate product.

[0035] In the present invention, the ortho-xylene is mixed with decompressed quantitative ammonia and air after being passed through a heat-retaining metering pump to form a mixed gas, and then enters a primary catalytic bed for a primary catalytic reaction to obtain a mixed intermediate product.

[0036] The first-stage catalysis is carried out in the presence of catalyst I, and the catalyst I is a V-Cr-Mo-M catalyst, wherein V is vanadium, Cr is chromium, Mo is molybdenum; M is an alkali metal element , selected from one or more of Li, Na, K, Rb and Cs, preferably one or more of Li, Rb and Cs, more preferably Li and / or Cs, such as Cs. ...

Embodiment 1

[0083] Slowly dissolve 10.0g of vanadium pentoxide in 200g of oxalic acid aqueous solution containing 30g, add 3.8g of chromium trioxide at 85°C, and after it dissolves, add 4.5g of ammonium orthomolybdate ((NH 4 ) 2 MoO 4 ) and 2.6 g cesium sulfate, stirred for 2 hours. 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 about 85°C in advance, stirred evenly, and allowed to stand at 20-30°C for 16 hours to obtain a catalyst precursor. Take it out and place it in a muffle furnace to gradually raise the temperature to 600°C and keep it warm for 12 hours. After cooling to room temperature, the catalyst I is obtained and bottled for future use. In the catalyst I, V:Cr:Mo:Cs:=1:0.35:0.21:0.13. Physical adsorption BET test was carried out on catalyst Ⅰ, and its BET specific surface area was 361.1m 2 / g.

Embodiment 2

[0085] Slowly dissolve 5.0g of vanadium pentoxide and 21.5g of phosphoric acid solution with a mass fraction of 85% in 100g of aqueous solution containing 40g of oxalic acid, and then add 2.5g of chromium trioxide and 2.0g of nickel chloride at 80°C, and wait for them to dissolve After that, add 3.0g ammonium orthomolybdate ((NH 4 ) 2 MoO 4 ) and 1.5g of cesium sulfate, stirred for 1 hour, the above solution was added to 50g of silica gel with a particle size of 80-120 mesh, the silica gel was preheated to 95°C in advance, stirred evenly, and stood at 20-30°C for 20 hours. Take it out and place it in a muffle furnace and gradually raise the temperature to 650°C, keep it warm for 12 hours, and after cooling to room temperature, the catalyst II is obtained, which is bottled for later use. V:Cr:P:Ni:Mo:Cs:=1:0.45:3.39:0.28:0.28:0.15 in catalyst II. Physical adsorption BET test was carried out on Catalyst II, and its BET specific surface area was 399.2m 2 / g.

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Abstract

The invention provides a new synthesis method of phthalonitrile. In the method, o-xylene is used as a raw material to carry out hierarchical catalytic synthesis in the presence of a catalyst. During the synthesis process, there are very few side reactions, the yield is high, and the amount of ammonia used is greatly reduced. The catalyst used in the invention has good selectivity, reduces the requirements for reaction conditions, reduces the generation of three wastes, and is beneficial to industrial production.

Description

technical field [0001] The invention belongs to the technical field of synthesis of organic intermediates, in particular to a synthesis process of phthalonitrile, in particular to a synthesis method for preparing phthalonitrile by ammoxidation. Background technique [0002] Phthalonitrile, also known as phthalonitrile, is an important organic intermediate widely used in the synthesis of phthalocyanine pigments and dyes, phthalosulfonamide drugs, high thermal resistance polyamide fibers, xylyl diisocyanate plastics and desulfurization catalysts. Phthalonitrile is widely used in the field of material science due to its semiconducting properties and nonlinearity, such as photosensitive coatings and light guiding films. In addition, the phthalocyanine polymer precursor made from phthalonitrile is an advanced composite material, which has wide application potential in aviation, aerospace, aircraft carrier, ship, machinery, electronics and other fields. Therefore, the synthesis t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/51C07C253/28B01J23/28B01J27/19
CPCC07C253/28B01J23/28B01J27/19C07C255/51
Inventor 权于高振聪于顺明
Owner ANSHAN HIFICHEM CO LTD
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