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Improved method for treatment of isophoronenitrile reaction solution

A technology of isophorone nitrile and isophorone, which is applied in the process field of secondary neutralization and treatment, can solve the problems of increased side reactions, etc., achieve stable operation of the device, reduce equipment and safety costs, and reduce high polymer The effect of equal solid waste

Active Publication Date: 2014-12-24
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the method of the present invention solves the problem of increased side reactions, solid salt problem and residual acid problem that are inevitably brought about after the current process handles the reaction neutralization liquid

Method used

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  • Improved method for treatment of isophoronenitrile reaction solution
  • Improved method for treatment of isophoronenitrile reaction solution
  • Improved method for treatment of isophoronenitrile reaction solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The acidic cation exchange resin is AMBERLITE IR120H. If the resin leaves the factory in sodium form, it needs to be washed or backwashed several times with hydrochloric acid or sulfuric acid solution to convert it into hydrogen form, and then washed with soft water. AMBERLITE IR120H has a pore size between 80-100nm and a total mass exchange capacity of 4.5mmol / g. It is filled in a tubular container with a filling capacity of 87kg.

[0047] (1) Add 5.5g of ethylenediamine and 32.5g of phenylenediamine (the total molar weight is about 0.1% of the molar weight of the hydrogen ion of the sulfonic acid group in the resin) to 380kg of isophorone to make a mass content of about 0.01% IP solution of the diamine at 10 °C. The solution was transported into a tubular container filled with resin, and flowed through the entire resin layer for a residence time of 5 minutes to modify the strongly acidic cation exchange resin.

[0048] (2) Under 150 ℃, 1350kg isophorone and 135kg hyd...

Embodiment 2

[0054] The strongly acidic cation exchange resin is selected from German Bayer Lewatit Monoplus S100. If it is in the sodium form at the factory, it will be converted to the hydrogen form by referring to the method of Example 1. In the tube container, the filling quantity is 250kg.

[0055] (1) Add 1740g of diethylenetriamine (the total molar weight is about 1.5% of the hydrogen ion molar weight in the sulfonic acid group in the resin) to 1740kg of isophorone to make diethylenetriamine with a mass content of about 0.1%. Amine solution in isophorone at 30°C. The solution is transported into a tubular container filled with resin, flows through the entire resin layer, and stays for 10 minutes to modify the strongly acidic cation exchange resin.

[0056] (2) At 80°C, 1.35t of isophorone reacted with 145kg of hydrocyanic acid under the action of the alkaline catalyst sodium ethoxide, of which 18.2kg of the alkaline catalyst sodium ethoxide, and 1506kg of the reaction solution was ...

Embodiment 3

[0063] Jiangsu Suqing 001×7 is selected as the strongly acidic cation exchange resin. If it leaves the factory as sodium form, refer to the method of Example 1 to convert it into hydrogen form. Jiangsu Suqing 001×7 has a pore size between 100-200nm and a total mass exchange capacity of 4.5mmol. / g, filled in a tube container, the filling amount is 34kg.

[0064] (1) 670g triethylenetetramine (total molar weight is about 3% of sulfonic acid group molar weight in resin) is added in 67kg isophorone, is made into the isophorone solution of 1% triethylene tetramine, temperature is 20°C. The solution is transported into a tubular container filled with resin, flows through the entire resin layer, and stays for 20 minutes to modify the strongly acidic cation exchange resin.

[0065] (2) At 180°C, 1350 kg of isophorone reacted with 135 kg of hydrocyanic acid under the action of the basic catalyst calcium hydroxide, wherein 375 g of the basic catalyst calcium hydroxide obtained 1480 kg...

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Abstract

The invention provides a method for treatment of a reaction solution obtained in preparation of isophoronenitrile from raw materials, namely isophorone and hydrocyanic acid under the catalysis of an alkaline catalyst. By adopting a two-step neutralization method, the reaction solution of isophoronenitrile is relatively stable, the influence of a salt produced in a neutralization process on a subsequent separation system is avoided and the stability in operation of a device is increased; furthermore, decomposition and polymerization reactions of isophoronenitrile and the reaction speed of polymerization of isophorone in the neutralization process and subsequent rectification separation of the reaction solution of isophoronenitrile are greatly reduced, the product yield is further improved, the unit consumption of materials is reduced by above 5%, the solid and waste content in a high polymer is reduced by above 80%, and a series of production, safety, environmental production and other problems caused by production of hydrocyanic acid in a rectification system are avoided.

Description

technical field [0001] The invention relates to a method for treating isophorone nitrile reaction liquid, more specifically a process for treating by secondary neutralization before rectification and separation. technical background [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): C07C255/46C07C253/32
Inventor 丛鑫何光文朱发明董岩峰王爱发陈海波黎源华卫琦王文薛莹姜庆梅曹善健宋锦宏杨在刚
Owner WANHUA CHEM GRP CO LTD
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