Catalyst for continuously preparing N-isopropyl-4-fluoroanilines, and preparation method and application of catalyst

A technology of catalyst and fluoroaniline, which is applied in the field of catalyst and preparation for continuous preparation of N-isopropyl-4-fluoroaniline, can solve the problems of difficult post-processing, lack of market competitiveness in technology and economy, and high reaction requirements, and achieve High catalytic activity and stability, good market promotion prospects, mild reaction conditions

Active Publication Date: 2015-10-14
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is relatively mature, but the price of p-fluoroaniline is expensive, the yield is low, the production cycle is long, the cost is high, and the product quality is poor; the equipment is severely corroded, and the amount of three wastes is large, and post-processing is difficult, which does not meet the requirements of modern clean production
[0005] 2) Use p-fluoronitrobenzene, acetone, and hydrogen as raw materials to catalyze the alkylation process. The catalysts include copper chromite, modified zeolite, and loaded noble metal catalysts. Copper chromite and modified zeolite are used as catalysts. The reaction temperature is 300 ℃, the pressure is above 5MPa, the conversion rate is lower than 70%, the selectivity is 80%, the reaction requirements are high, the production cost is high, and it does not have market competitiveness i

Method used

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  • Catalyst for continuously preparing N-isopropyl-4-fluoroanilines, and preparation method and application of catalyst
  • Catalyst for continuously preparing N-isopropyl-4-fluoroanilines, and preparation method and application of catalyst
  • Catalyst for continuously preparing N-isopropyl-4-fluoroanilines, and preparation method and application of catalyst

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Experimental program
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Embodiment 1

[0037] The catalyst of the present embodiment includes activated carbon carrier, Pt, Fe and K loaded on the activated carbon carrier; the mass percentage of Pt in the catalyst is 0.3%, the mass percentage of Fe is 0.05%, and the mass percentage of K The content is 0.05%; the average particle diameter of the activated carbon carrier is 1.0mm, and the specific surface area is 920m 2 / g.

[0038] The preparation method of the catalyst of the present embodiment is:

[0039] Step 1, dissolving chloroplatinic acid containing 0.3g of platinum in dilute nitric acid with a mass concentration of 0.8%, to obtain solution A;

[0040] Step 2, dissolving ferric chloride containing 0.05g iron in dilute nitric acid with a mass concentration of 1%, to obtain solution B;

[0041] Step 3. Mix the solution A described in step 1 and the solution B described in step 2 evenly to obtain solution C. Soak 99.6g of activated carbon carrier in solution C, heat to 40°C, keep warm and ultrasonic for 2 ho...

Embodiment 2

[0047] The catalyst of the present embodiment includes activated carbon carrier, Pt, Sn and Ce loaded on the activated carbon carrier; the mass percentage of Pt in the catalyst is 0.5%, the mass percentage of Sn is 0.25%, and the mass percentage of Ce is The content is 0.25%; the average particle diameter of the activated carbon carrier is 0.5mm, and the specific surface area is 1180m 2 / g.

[0048] The preparation method of the catalyst of the present embodiment is:

[0049] Step 1, dissolving chloroplatinic acid containing 0.5g of platinum in dilute nitric acid with a mass concentration of 0.5%, to obtain solution A;

[0050] Step 2, dissolving stannous chloride containing 0.25g tin in dilute nitric acid with a mass concentration of 0.5%, to obtain solution B;

[0051] Step 3. Mix the solution A described in step 1 and the solution B described in step 2 evenly to obtain solution C. Soak 99g of activated carbon carrier in solution C, heat it to 35°C, keep it warm and ultras...

Embodiment 3

[0057] The catalyst of the present embodiment comprises activated carbon carrier, Pt, Cu and Ce loaded on the activated carbon carrier; the mass percent composition of Pt in the described catalyst is 1.0%, the mass percent composition of Cu is 0.5%, the mass percent composition of Ce The content is 0.5%; the average particle diameter of the activated carbon carrier is 1.5mm, and the specific surface area is 810m 2 / g.

[0058] The preparation method of the catalyst of the present embodiment is:

[0059] Step 1, dissolving chloroplatinic acid containing 1.0 g of platinum in dilute nitric acid with a mass concentration of 1.2%, to obtain solution A;

[0060] Step 2, dissolving copper nitrate containing 0.5g copper in dilute nitric acid with a mass concentration of 1.2%, to obtain solution B;

[0061] Step 3. Mix the solution A described in step 1 and the solution B described in step 2 evenly to obtain solution C. Soak 98g of activated carbon carrier in solution C, heat it to 4...

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Abstract

The invention discloses a catalyst for continuously preparing N-isopropyl-4-fluoroanilines. The catalyst comprises an activated carbon carrier, Pt, metal M1 and metal M2, wherein the Pt, metal M1 and metal M2 are loaded on the activated carbon carrier; the Pt accounts for 0.3-1.0wt% of the catalyst; the metal M1 accounts for 0.05-0.5wt% of the catalyst; the metal M2 accounts for 0.05-0.5wt% of the catalyst; the metal M1 is selected from Fe, Cu or Sn; the metal M2 is selected from K, Ce, or Ag. In addition, the invention also discloses a preparation method and application of the catalyst. The catalyst disclosed by the invention has the characteristics of being high in activity, high in selectivity and high in stability and can be used for preparing N-isopropyl-4-fluoroanilines in a high-efficiency catalyzing manner; the conversion ratio of a raw material, namely 4-fluoronitrobenzene, is 98% or more, the yield of a product, namely N-isopropyl-4-fluoroanilines, is 95% or more, and the yield of dehydrogenation by-products is not more than 0.1%.

Description

technical field [0001] The invention belongs to the technical field of catalytic hydrogenation anti-dehalogenation and ketone-amine condensation process, and specifically relates to a catalyst for continuously preparing N-isopropyl-4-fluoroaniline, a preparation method and application thereof. Background technique [0002] N-isopropyl-4-fluoroaniline is mainly used in the synthesis of pharmaceutical intermediates, the pesticide herbicide flufenacet, etc. Among them, flufenacet is a new type of aryloxyacetamide herbicide developed and listed by German Bayer company in 1998 , compared with difenacet, it has higher activity and is suitable for controlling weeds in more crops. The market of flufenacet is developing rapidly. It is currently one of the top 50 pesticides in the world, but there is no mature technology in my country And large-scale production, so the market prospect of N-isopropyl-4-fluoroaniline is very broad. [0003] At present, there are two synthetic methods of ...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J23/63B01J23/66C07C209/26C07C209/36C07C211/52
Inventor 万克柔林涛程杰曾永康曾利辉高武王鹏宝张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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