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Iron cobalt composite carbon copper catalyst for continuous production of 4,4-diaminodiphenyl ether as well as method

A technology of diaminodiphenyl ether and copper catalyst, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of high cost, low reaction pressure, and time Long-term problems, to ensure the reaction temperature, maintain the reaction temperature, good thermal conductivity effect

Inactive Publication Date: 2020-01-03
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the existing post-treatment process of 4,4-dinitrodiphenyl ether is precipitation by adding water, resulting in a large amount of waste water
[0003] Chinese patent 201810861785.X discloses a method for synthesizing 4,4-diaminodiphenyl ether. The method uses alcohols as solvents and diphenyl ether as the initial raw material to form nitroso intermediates through nitration reaction, and then Catalytic hydrogenation greatly reduces the amount of hydrogen used and the difficulty of the catalytic reaction, but due to the intermittent tank technology, there are still problems of incomplete conversion and low yield at high temperature and pressure
Chinese patent 201711478222.4 discloses a preparation method of 4,4-diaminodiphenyl ether, the method adopts kettle technology, the reaction pressure is low, but the temperature is high, and the yield of product 4,4-diaminodiphenyl ether More than 99%, the catalyst is 5% Pd / C, the cost of the catalyst is high, and the time required for the catalytic reaction to reach a conversion rate of more than 99% is long
At present, the industry still adopts the still-type process to produce 4,4-diaminodiphenyl ether, which has low efficiency and high cost. Therefore, it is necessary to improve production efficiency and reduce production costs. Fixed-bed continuous technology can realize the energy saving and reduction of catalytic hydrogenation reaction. Consumption, improve product quality, save production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Preparation of catalyst

[0026] (1) After washing and drying 200g of 10-20 mesh granular copper foam, place it in a muffle furnace and bake it at 400°C for 1h.

[0027] (2) After 200g of dry corn granules are ground into powder, stir and mix evenly with 100g of polyethylene glycol 2000 powder and 1000g of aluminum sol with a solid content of 20%, then place the foamed aluminum after roasting in 100g of step (1) Immerse in the obtained mixed solution for 1 hour, take it out, place it in a tube furnace, raise the temperature to 400°C at a rate of 1°C / min under the protection of nitrogen, treat at a constant temperature for 2 hours, and then add water vapor in nitrogen to control water vapor and The volume ratio of nitrogen was 13:87, and at the same time, the temperature was raised to 800 °C at a rate of 1 °C / min, the treatment was continued for 2 h, and the temperature was lowered to obtain a carbon-coated copper foam support (C@Cu).

[0028] (3) 2.89g ferric nitrat...

Embodiment 2

[0034] 1. Preparation of catalyst

[0035] (1) After washing and drying 200g of 10-20 mesh granular copper foam, place it in a muffle furnace and bake it at 400°C for 1h.

[0036] (2) After 200g of dry corn granules are ground into powder, stir and mix evenly with 100g of polyethylene glycol 2000 powder and 1100g of aluminum sol with a solid content of 20%, then place the foamed aluminum after roasting in 100g of step (1) Immerse in the obtained mixed solution for 3 hours, take it out, put it in a tube furnace, raise the temperature to 400°C at a rate of 2°C / min under the protection of nitrogen, and treat it at a constant temperature for 3 hours, then add water vapor in nitrogen to control water vapor and The volume ratio of nitrogen is 10:90, and at the same time, the temperature is raised to 800°C at a rate of 2°C / min, and the treatment is continued for 3 hours, and the temperature is lowered to obtain a carbon-coated copper foam carrier.

[0037] (3) Dissolve 2.89g of ferr...

Embodiment 3

[0043] 1. Preparation of catalyst

[0044] (1) After washing and drying 200g of 10-20 mesh granular copper foam, place it in a muffle furnace and bake it at 400°C for 1h.

[0045] (2) After 200g of dry corn granules are ground into powder, stir and mix evenly with 100g of polyethylene glycol 2000 powder and 1200g of aluminum sol with a solid content of 20%, then place the foamed aluminum after roasting in 100g of step (1) Immerse in the obtained mixed solution for 3 hours, take it out, put it in a tube furnace, raise the temperature to 400°C at a rate of 3°C / min under the protection of nitrogen, and treat it at a constant temperature for 4 hours, then add water vapor in nitrogen to control the relationship between water vapor and The volume ratio of nitrogen is 15:85, and at the same time, the temperature is raised to 800°C at a rate of 3°C / min, and the treatment is continued for 4h, and the temperature is lowered to obtain a carbon-coated copper foam carrier.

[0046] (3) 2....

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PUM

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Abstract

The invention discloses an iron cobalt composite carbon copper catalyst for continuous production of 4,4-diaminodiphenyl ether as well as a method. The catalyst takes carbon coated foam copper as a carrier and loads Fe, Co and noble metal; and the mass contents of the Fe, the Co and the noble metal in the catalyst are sequentially 0.1 to 1.0 percent, 0.1 to 0.8 percent and 0.1 to 0.9 percent. The4,4-diaminodiphenyl ether is continuously produced by adopting the iron cobalt composite carbon copper catalyst, by taking 4,4-dinitrodiphenyl ether as a raw material and by performing nitro hydrogenation reaction on a catalyst bed by a trickle bed, the catalytic reaction efficiency is high, the reaction heat is concentrated, the carbon coated foam copper carrier can disperse the active componentsof the catalyst well, also can rapidly remove reaction heat and guarantees that the reaction is conducted within the proper temperature range rapidly and stably, the raw material conversion rate is 100 percent, the selectivity of target products is more than 99.9 percent, the catalyst property is stable, the catalytic reaction is too simple the catalytic reaction heat is recoverable, the heat energy utilization efficiency is high, and environmental friendliness is realized.

Description

technical field [0001] The invention belongs to the technical field of catalytic hydrogenation, and in particular relates to an iron-cobalt composite carbon-copper catalyst and a method for continuously producing 4,4-diaminodiphenyl ether by using the catalyst. Background technique [0002] 4,4-Dinitrodiphenyl ether is a high value-added fine chemical intermediate. Its reduction product 4,4-diaminodiphenyl ether is the main monomer for the synthesis of heat-resistant plastics such as polyimide and polymaleimide, among which polyimide has high temperature resistance, radiation resistance and high mechanical strength. Advantages, used in films, coatings, fibers, foam plastics and photoresists, etc., widely used in aviation, navigation, atomic energy, electronic and electrical industries and other fields. 4,4-diaminodiphenyl ether is one of the main raw materials of polyimide. At the same time, 4,4-diaminodiphenyl ether can also be used to produce crosslinking agents, and is w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89C07C213/02C07C217/90
CPCB01J23/8926C07C213/02C07C217/90
Inventor 林涛程杰张炳亮张力高明明赵茁然万克柔曾永康张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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