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Catalyst for synthetizing benzenetetracarboxylic anhydride and preparation method of catalyst

A technology of pyromellitic dianhydride and catalyst, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of low yield of pyromellitic dianhydride and low catalyst activity, and achieve The effect of rich source, good performance and low source

Inactive Publication Date: 2013-07-17
天津北洋国精科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the pyromellitic dianhydrides are prepared by using durene as a raw material by air gas-phase oxidation. Since this process is a complex heterogeneous catalytic process, the yield of pyromellitic dianhydride is very low.
The preparation of pyromellitic dianhydride by air gas-phase oxidation of durene mostly uses catalysts with vanadium as the main active component. According to the chemical reaction equation, the theoretical yield of pyromellitic dianhydride should reach 163%, but the traditional preparation The catalyst activity obtained by the method is relatively low, and the highest actual yield of pyromellitic dianhydride can only reach 56% of the theoretical yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 17.21 g of oxalic acid into 39 mL of deionized water, and stir the temperature to 70°C. After the oxalic acid is completely dissolved, add 8.605 g of ammonium metavanadate and stir at 70°C at a constant temperature. When there are no bubbles in the solution, transfer all the blue-black solution to the preparation container, install the condenser tube and pass the condensed water to reflux and stir for 1.5 hours. Add ammonium phosphate (P = 0.02), niobium pentoxide (Nb = 0.2), and antimony pentoxide (Sb = 0.02) in mass proportions, continue to reflux and stir for 15 minutes, remove the condensed water, stir at 70°C, and evaporate part The volume of the suspension is about 30 mL with water, 6.763 g of titanium dioxide is added after cooling to room temperature, so that the mass ratio of V:Ti is 0.45:0.55, and its total mass is 20% of the mass of the inert carrier, and it is aged overnight. Take 30mL of the inert ceramic ball carrier and heat it to 250℃ in a muffle fu...

Embodiment 2

[0020] Weigh 17.21 g of oxalic acid into 39 mL of deionized water, and stir the temperature to 90°C. After the oxalic acid is completely dissolved, add 8.605 g of ammonium metavanadate and stir at a constant temperature of 80°C. When there are no bubbles in the solution, transfer all the blue-black solution to a three-necked flask, install the condenser tube and pass the condensed water to reflux and stir for 1.5 hours. Add ammonium phosphate (P = 0.02), niobium pentoxide (Nb = 0.2), and antimony pentoxide (Sb = 0.02) in mass proportions, continue to reflux and stir for 15 minutes, remove the condensed water, stir at 80°C, and evaporate part The volume of the suspension is about 30 mL with water, 6.763 g of titanium dioxide is added after cooling to room temperature, so that the mass ratio of V:Ti is 0.45:0.55, and its total mass is 20% of the mass of the inert carrier, and it is aged overnight. Take 30mL ceramic ball carrier ( 4-6mm) Heat to 250℃ in a muffle furnace, stir the...

Embodiment 3

[0022] Weigh 17.21 g of oxalic acid into 39 mL of deionized water, and stir the temperature to 80°C. After the oxalic acid is completely dissolved, add 8.605 g of ammonium metavanadate and stir at a constant temperature of 90°C. When there are no bubbles in the solution, transfer all the blue-black solution to a three-necked flask, install the condenser tube and pass the condensed water to reflux and stir for 1.5 hours. Add ammonium phosphate (P is 0.02), niobium pentoxide (Nb is 0.2), and antimony pentoxide (Sb is 0.02) in mass proportions, continue to reflux and stir for 15 minutes, remove the condensed water, stir at 90°C, and evaporate part The volume of the suspension is about 30 mL with water, 6.763 g of titanium dioxide is added after cooling to room temperature, so that the mass ratio of V:Ti is 0.45:0.55, and its total mass is 20% of the mass of the inert carrier, and it is aged overnight. Take 30mL ceramic ball carrier ( 4-6mm) Heat to 250℃ in a muffle furnace, stir ...

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PUM

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Abstract

The invention discloses a catalyst capable of being used for synthetizing benzenetetracarboxylic anhydride and a preparation method of the catalyst, and belongs to a catalyst technology. The catalyst comprises the main catalytic active components V and Ti; the weight ratio is (0.9 to 0.1) to (0.1 to 0.9); the total mass is 10-50% of that of an inert carrier; the total mass reference of the main catalyst is 1; the component P of a cocatalyst is 0.01-0.3; Nb is 0.01-1; and Sb is 0.01-0.3. The method comprises the following steps of: adding proper ammonium metavanadate to reflux and react in an oxalate solution; adding different cocatalysts and titanium dioxide to steep over the night; spraying prepared turbid liquid to a high-temperature spherical inert carrier; and heating and baking in a muffle furnace to obtain the catalyst. The catalyst disclosed by the invention has the advantages that the prepared material is abundant in source; use of toxic vanadium metal is reduced; the catalyst is used for synthesizing the benzenetetracarboxylic anhydride from durene air in a gas phase oxidation manner, and is good in performance; and the yield of the benzenetetracarboxylic anhydride can be effectively improved.

Description

Technical field [0001] The invention relates to a catalyst for synthesizing pyromellitic dianhydride and a preparation method thereof, and belongs to the technical field of pyromellitic dianhydride synthesis catalysts. Background technique [0002] Pyromellitic dianhydride is an important organic chemical raw material, and its main purpose is to react with diaminodiphenyl ether to synthesize polyimide. Polyimide is a new type of synthetic material with high temperature resistance, radiation resistance, impact resistance and excellent electrical conductivity and mechanical properties. It is widely used in high-end technology sectors such as aerospace and electronics. In addition, pyromellitic dianhydride is also an important raw material for the production of high-quality plasticizers, curing agents and powder matting agents. With the development of the petrochemical industry, the output of C9 and C10 aromatic fractions has increased sharply, providing a large amount of high-qual...

Claims

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Application Information

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IPC IPC(8): B01J27/198B01J35/08C07D493/04
Inventor 李鑫钢贤晖姜斌李洪
Owner 天津北洋国精科技有限责任公司
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