Special catalyst for preparing isophthalonitrile by ammoxidation reaction, preparation method and application

A technology of isophthalonitrile and ammonia oxidation, which is applied in the fields of organic chemistry and organic fine chemicals, can solve the problems of the loss of catalyst surface active components, the loss of catalyst active components, and the weak force of metal oxides. To achieve the effect of good thermal stability and mechanical strength, good application value and low cost

Active Publication Date: 2022-02-18
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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Problems solved by technology

[0004] The inventor once developed the silica gel-supported multi-component composite oxide catalyst m-509 for the ammoxidation of m-xylene, and the molar yield of isophthalonitrile can reach 66%, but after six months of operation on the industrialized device, Catalyst activity declines seriously, and the main reason for catalyst deactivation is the loss of active components on the catalyst surface (Huang Chi, Zheng Qiong, Xie Guangyong, etc. Research on deactivation of m-509 catalyst for ammoxidation of m-xylene, Journal of Wuhan University (Science Edition) , 2001, 47, 438-440)
The silica gel-supported catalyst is prepared by silica gel impregnation method, that is, silica gel absorbs the mixed metal salt solution and then activates it by high-temperature calcination; the composite metal oxide is mainly attached to the silica gel surface through physical adsorption, and the interaction between the metal oxide and the silica gel carrier is weak. In the fluidized bed reactor, the catalyst microspheres collide and rub against each other, and the metal oxide is easy to fall off. In addition, part of the components in the composite metal oxide volatilize under long-term high temperature, resulting in the loss of the active components of the catalyst and the change of the proportion. To a certain extent, it will lead to a decrease in catalyst activity and affect the service life of the catalyst

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  • Special catalyst for preparing isophthalonitrile by ammoxidation reaction, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 25.03 g H 2 C 2 o 4 2H 2 Dissolve O in 150 mL of distilled water at 80°C, add 12.05 g of V 2 o 5 , 28.06 g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 50.43 g (NH 4 ) 3 Sb(C 2 o 4 ) 3 2H 2 O, 2.46 g H 3 BO 3 and 0.49 g Li 2 CO 3 After forming a uniform solution, slowly add 150 mL of 30% silica sol, and then add 10 g of aminopropyltrimethoxysilane. After stirring evenly, the catalyst precursor was obtained by high-speed spray centrifugal drying, dried in a muffle furnace at 110° C., and then gradually raised to 550° C. for 6 hours. After natural cooling, set aside. The active composition of the catalyst is: VMo 1.2 Sb 0.8 B 0.3 Li 0.1 o 7.8 .

[0025] 20g of the above-mentioned solid catalysts are filled in a quartz tube fixed-bed reactor with an internal diameter of 30mm, and the molar ratio of the reaction raw materials is: m-xylene:NH 3 :Air=1:5:35, the reaction temperature is 693±1K, and the catalyst load is 100g / (kgcat·h). After reacting for 8 hours, the...

Embodiment 2～7

[0027] Catalyst formula is different, and reaction condition is with embodiment 1, and result is as follows:

[0028]

Embodiment 8

[0030] 47.81 g H 2 C 2 o 4 2H 2 O was dissolved in 200 mL of distilled water at 85 °C, and then 23.02 g of V 2 o 5 , 35.73 g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 21.80 g Mn(NO 3 ) 2 ·6H 2 O and 50.67 g KSbC 4 h 4 o 7 .1 / 2H 2 O, after forming a homogeneous solution, slowly add the aminopropyl cage polysilsesquioxane ((i-C) of 100 grams of 30% content 4 h 9 ) 7 Si 8 o 12 (CH 2 CH 2 CH 2 NH 2 )) in solution. After uniform stirring, the catalyst precursor was obtained by high-speed spray and centrifugal drying, and the temperature was gradually raised to 500° C. in a high-temperature furnace and kept for 12 hours. After cooling naturally, save for later use. The composition of the catalyst is: VMo 0.8 Sb 0.6 mn 0.3 K 0.6 o 6.7 .

[0031] 20g of catalyst is loaded into a fixed-bed reactor with a quartz tube with an inner diameter of 30mm, and the mixed gas of raw materials passes through the catalyst bed for reaction. The composition of the raw gas mixture i...

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Abstract

The invention discloses a special catalyst for preparing isophthalonitrile by ammoxidation of m-xylene. The carrier is silica gel, the main catalyst is three components of V, Mo and Sb, and the co-catalyst is at least one of D and E components. species; its active components are expressed as: VMo b Sb c D. d E. e o x ; The D is boron, chromium, titanium, phosphorus, nickel, bismuth, manganese, iron, cobalt, copper, zinc or tin; E is potassium, lithium, sodium, cesium, magnesium or calcium. The invention also discloses the preparation method and application of the catalyst. In the present invention, groups containing lone electron pairs on silicon are used to carry out Lewis acid-base reaction with inorganic elements, thereby strengthening the effect of inorganic oxides and supports; at the same time, the dispersion of inorganic oxides is more uniform, the loss of catalyst components is small, and the catalytic activity is high. , good selectivity, prolonging the service life of industrial catalysts from one year to more than two years. The preparation method of the catalyst is simple, the thermal stability and mechanical strength are good, and the catalyst can be used in fixed-bed and fluidized-bed reactors.

Description

technical field [0001] The invention relates to a special catalyst for preparing isophthalonitrile by an ammoxidation method, a preparation method and an application. It belongs to the technical field of organic chemistry and also belongs to the technical field of organic fine chemicals. Background technique [0002] Isophthalonitrile is a high-efficiency, broad-spectrum, low-toxicity, low-residue pesticide fungicide and an intermediate of antifungal agent chlorothalonil (tetrachloroisophthalonitrile); isophthalonitrile is hydrogenated to produce M-xylylenediamine is an epoxy resin curing agent with excellent performance, and it is also a raw material for polyurethane resin and nylon resin. Isophthalonitrile has become an important chemical product, and its consumption is still on the rise. [0003] The simplest and most economical industrial production method for isophthalonitrile is to obtain m-xylene through gas-phase ammoxidation under the action of a catalyst. Since ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/28C07C253/28C07C255/51
Inventor 谢光勇黄业迎张倩郑浩熊焰陈川周新花
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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