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Isophorone nitrile production method using acrylonitrile byproduct hydrocyanic acid continuous reaction

A technology of isophorone nitrile and isophorone, which is applied in the field of producing isophorone nitrile, can solve the problems of unrecoverable activity, increased production cost, energy consumption, etc.

Inactive Publication Date: 2013-04-24
YINGKOU YINGXIN CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The use of basic catalysts, whether organic bases (such as ammonium salts, etc.) After the end, neutralization with acidic substances is required to avoid the decomposition of isophoronenitrile during the distillation process. Neutralization with acidic substances requires filtration to remove the generated salt. During the production process, some auxiliary equipment needs to be added. Operation steps Complicated, increasing the cost of production
[0006] In order to avoid the above-mentioned dilemma, CN102199109A discloses a method for preparing IPN by reacting isophorone and hydrocyanic acid in the presence of a basic anion exchange resin, However, anion exchange resin has a shortcoming, the highest use temperature: hydrogen-oxygen type ≤ 60 ° C, chlorine type ≤ 80 ° C, and this reaction needs to be reacted at a temperature above 100 ° C, or even higher, so anion exchange resin is very fast It will lose its activity, and the activity cannot be restored, and it needs to consume a lot of resin, which increases the production cost
Regarding the above-mentioned defects of the resin, the 21st paragraph of the document description also clearly points out that "the catalytic ability of the basic anion exchange resin decreases after a period of use, and needs to be replaced or regenerated. However, the activity of the resin after the regenerated treatment is not high, and the regeneration causes Reduced energy consumption and increased production costs

Method used

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  • Isophorone nitrile production method using acrylonitrile byproduct hydrocyanic acid continuous reaction
  • Isophorone nitrile production method using acrylonitrile byproduct hydrocyanic acid continuous reaction
  • Isophorone nitrile production method using acrylonitrile byproduct hydrocyanic acid continuous reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Catalyst preparation:

[0036] In a 1000ml beaker, add 500ml of 10A molecular sieve, then add 500ml of pre-configured calcium chloride solution with a content of 25%, stir several times with a glass rod at intervals of ten minutes, soak for 2 hours, filter, and remove an appropriate amount Rinse with deionized water, then add 500ml of pre-configured saturated sodium bicarbonate solution, stir several times with a glass rod at intervals of ten minutes, soak for 2 hours, filter, rinse with appropriate amount of deionized water, and then put it in the oven After drying at 90°C for 4 hours to constant weight, transfer it to a muffle furnace, calcine at 900°C for more than 3 hours, take it out, and put it in a desiccator to cool down for later use.

Embodiment 2-8

[0038] Obtain method according to embodiment 1, change processing condition, prepare corresponding molecular sieve catalyst:

[0039]

[0040] Example 1:

[0041] Continuous reaction to prepare isophorone nitrile:

[0042]In the fixed-bed reactor, fill the catalyst of Example 1 made according to the above-mentioned process, turn on the isophorone pump, and adopt a larger flow rate to make the raw material isophorone fill the preheater, pipeline and fixed-bed reactor and circulate Return to the storage tank, adjust the flow rate of isophorone to 12ml / min at this time, open the heat transfer oil valve of the preheater, preheat the raw material of isophorone to the set temperature of 100°C, and open the heat transfer oil valve of the fixed bed reactor to make the fixed bed reactor The bed reached the set reaction temperature of 130°C. When the equipment is debugged and stabilized, turn on the hydrocyanic acid pipeline pump, adjust the flow rate of hydrocyanic acid to 1ml / min...

Embodiment 2

[0043] Example 2: In the fixed-bed reactor, fill the catalyst of Example 2 made according to the above-mentioned process, turn on the isophorone pump, and use a larger flow rate to make the raw material isophorone fill the preheater, pipeline and fixed bed The reactor is circulated back to the storage tank. At this time, adjust the flow rate of isophorone to 13ml / min, open the heat transfer oil valve of the preheater, preheat the isophorone raw material to the set temperature of 80°C, and turn on the heat transfer oil of the fixed bed reactor. valve to make the fixed bed reach the set reaction temperature of 180°C. When the equipment is debugged and stabilized, turn on the hydrocyanic acid pipeline pump, adjust the flow rate of hydrocyanic acid to 2ml / min, control the volume ratio of hydrocyanic acid to isophorone at 10:1, and the hydrocyanic acid and isophorone pass through the mixer Finally, stay in the preheater for a short time (10 seconds), preheat to the set temperature,...

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Abstract

The invention provides an isophorone nitrile production method using an acrylonitrile byproduct hydrocyanic acid continuous reaction. After raw materials of isophorone and acrylonitrile byproduct hydrocyanic acid are mixed, the materials continuously react through a fixed bed reactor, processed molecular sieves fill the interior of a fixed bed and are used as catalysts, and the isophorone not only is a reaction raw material but also serves as reaction solvent. Reaction liquid flowing from the fixed bed is decompressed and rectified, isophorone which does not react is recovered and returns to a raw material storage tank to continue reaction, and products of isophorone nitrile are rectified through a continuous tower to obtain qualified products.

Description

Technical field: [0001] The invention relates to a method for producing isophorone nitrile by using hydrocyanic acid and isophorone in the presence of a catalyst, and the catalyst used is an activated molecular sieve. Background technique: [0002] Isophoronenitrile, chemical name 3-cyano-3,5,5-trimethylcyclohexanone (IPN), is the production of various chemical products, such as aliphatic isocyanate isophorone diisocyanate (IPDI), The basic raw material of 3-nitromethyl-3,5,5-trimethylcyclohexylamine (isophorone diamine, IPDA), the current synthesis process is to use hydrocyanic acid and isophorone in the presence of a basic catalyst After ketone reaction and neutralization, unreacted raw material isophorone and product isophorone nitrile are separated through rectification. Concrete reaction formula is as follows: [0003] [0004] There are many patents on the production of isophoronenitrile at home and abroad, and the difference between these patents is mainly to cha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/46C07C253/10
Inventor 耿佃云于秀媛王明贤
Owner YINGKOU YINGXIN CHEM TECH CO LTD
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