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Method for continuous production of isophorone nitrile

A technology of isophorone nitrile and isophorone, which is applied in the field of continuous preparation of isophorone nitrile, can solve the problems of increasing the cost of isophorone nitrile, increasing energy consumption, and high equipment requirements, and achieves safety in the production process Stable and reliable, improved stability and safety, and mild reaction conditions

Active Publication Date: 2017-07-25
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Formamide is the method for preparing hydrocyanic acid as a raw material, the reaction temperature is higher, and it is carried out under negative pressure conditions, the operation energy consumption is large, the process conditions are harsh, and the equipment requirements are also high; It needs to be liquefied at low temperature, which increases energy consumption and indirectly increases the cost of isophorone nitrile
[0009] So far, the prior art does not disclose the method for producing isophorone nitrile with other raw materials instead of raw material hydrocyanic acid, nor does it disclose the method for the integrated production of isophorone nitrile with liquid formamide as raw material

Method used

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  • Method for continuous production of isophorone nitrile
  • Method for continuous production of isophorone nitrile
  • Method for continuous production of isophorone nitrile

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Experimental program
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Effect test

Embodiment 1

[0055] The flow rate of isophorone is 13.8kg / h, preheated to 160°C, the preheating residence time is 40s, and the flow rate is 2.94kg / h formamide, the flow rate is 1468kg / h circulating fluid, the flow rate is 0.1kg / h tetramethylammonium bromide alkaline After the co-catalysts are mixed, they enter into the tubular reactor together, and the solid catalyst is filled in the tubular reactor. Part of the solid catalyst is Cr 2 o 3 load Al 2 o 3 The porous material of the catalyst, the Cr element content of the catalyst accounts for 2.5% of the mass of the catalyst, and the other part is the stainless steel packing made of 022Cr17Ni12Mo2 material, the volume ratio of the two is 2.5:1, uniformly mixed, and the total volume of the catalyst is 12.2L. Reaction temperature 160°C, absolute pressure 0.3MPa, liquid volume space velocity 30s -1 , the circulating liquid at the outlet of the reactor accounts for 98.9wt% of the total effluent. Add flow rate 0.026kg / h phosphoric acid neutra...

Embodiment 2

[0057] The flow rate of isophorone is 13.8kg / h, preheating to 220°C, the preheating residence time is 30s, and the flow rate is 4.06kg / h formamide, the flow rate is 996.83kg / h circulating fluid, the flow rate is 0.013kg / h triethylamine and tetramethyl The basic cocatalyst composed of ammonium hydroxide equimolar ratio mixture enters into the tubular reactor together after being mixed, and the solid catalyst is filled in the tubular reactor. Part of the solid catalyst is V 2 o 5 load Al 2 o 3 The porous material of the catalyst, the V element content of the catalyst accounts for 0.1% of the mass of the catalyst, and the other part is the stainless steel filler made of 022Cr17Ni12Mo2 material, the volume ratio of the two is 1:1, uniformly mixed, the total volume of the catalyst is 0.28L. Reaction temperature 220°C, absolute pressure 0.5MPa, liquid volume space velocity 1s -1 , the circulating liquid at the outlet of the reactor accounts for 98.2wt% of the total effluent, and...

Embodiment 3

[0059] The flow rate of isophorone is 13.8kg / h, preheated to 180°C, the preheating residence time is 35s, mixed with the flow rate of 3.63kg / h formamide, the flow rate of 1193.07kg / h circulating fluid, and the flow rate of 0.022kg / h sodium methoxide alkaline cocatalyst Then enter into the tubular reactor together, and the solid catalyst is filled in the tubular reactor. Part of the solid catalyst is V 2 o 5 Loaded Al 2 o 3 Porous material, partly Mn 2 o 3 and MoO 3 load SiO 2 The porous material of the catalyst, the total content of Mn and Mo elements in the catalyst accounts for 5% of the mass of the catalyst, and the other part is the stainless steel filler made of 022Cr17Ni12Mo2 material, the volume ratio of the two is 5:1, uniformly mixed, and the total volume of the catalyst is 5.04L. Reaction temperature 180°C, absolute pressure 0.4MPa, liquid volume space velocity 15s -1 , the circulating liquid at the outlet of the reactor accounts for 98.6wt% of the total effl...

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Abstract

The present invention provides a method for continuous production of isophorone nitrile, raw material formamide, an alkaline cocatalyst, preheated warm isophorone and a circulation reaction liquid are mixed in a certain proportion and sent into a reactor filled with a solid catalyst for reaction to obtain a reaction liquid containing the isophorone nitrile, and an isophorone nitrile productis obtained after separation. Compared with the traditional method for production of the isophorone nitrile from hydrocyanic acid as a raw material, on one hand, the raw material is more easily to obtain, hypertoxic cyanide as a reaction intermediate in the reaction system has a low concentration, security is greatly improved; on the other hand, energy consumption for production of liquid hydrocyanic acid is saved, production cost of the isophorone nitrile is reduced, and the molar yield of the isophorone nitrile (calculated on the basis of methanamide) is greater than 96%.

Description

technical field [0001] The invention relates to a method for continuously producing isophorone nitrile, in particular to a method for continuously preparing isophorone nitrile with formamide as a raw material. Background technique [0002] 3-cyano-3,5,5-trimethylcyclohexanone, commonly known as isophorone nitrile (IPN), is an important industrial intermediate, which can be converted into isophorone di Amine (IPDA). IPDA can be used as a curing agent and crosslinking agent for epoxy resin coatings; it can also be used to prepare isophorone diisocyanate (IPDI) in the polyurethane industry, and IPDI is used as a crosslinking agent, coupling agent, hydroxyl stabilizer and Special monomer use. [0003] Isophorone nitrile is generally obtained by the addition reaction of isophorone (IP) and hydrocyanic acid under basic catalyst conditions, and then neutralized, rectified or crystallized to obtain pure isophorone nitrile. The reaction equation is as follows Shown: [0004] ...

Claims

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Application Information

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IPC IPC(8): C07C253/06C07C255/46
CPCC07C253/06C07C255/46
Inventor 丛鑫何光文黎源初乃波华卫琦刘超崔乾王鹏董科郑超宋锦宏姜庆梅曹善健
Owner WANHUA CHEM GRP