Synthesis method of 1,3-dimethyl isocyanate cyclohexane

A technology of dimethyl isocyanate and synthetic method, which is applied in the preparation of isocyanic acid derivatives, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of large solvent consumption, many side reactions, and low conversion rate, etc. Achieve the effect of short reaction time, easy operation and reduction of by-products

Inactive Publication Date: 2018-11-06
JIANGSU KUAIDA AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In order to solve the above problems, the present invention provides a synthetic method of 1,3-dimethylisocyanate cyclohexane, which solves the problem that 1,3-cyclohexanedimethylamine has high viscosity, easy agglomeration and side effects in the process of passing through phosgene. Many reactions, low conversion rate, and large solvent consumption

Method used

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  • Synthesis method of 1,3-dimethyl isocyanate cyclohexane

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 150ml o-dichlorobenzene into a 1000ml flask, start the stirring device, turn on the refrigeration device to cool down the flask, and when the temperature reaches 0°C, open the phosgene valve to start feeding phosgene, adjust the flow rate of phosgene at 12g / h, pre-pass Phosgene 0.5h. Mix 550ml of o-dichlorobenzene and 70g of 1,3-cyclohexanedimethylamine evenly, add to the dropping funnel, pre-flow phosgene for 0.5h, continue to pass phosgene, open the dropping valve at the same time, start to add o- For the mixed solution of dichlorobenzene and 1,3-cyclohexanedimethylamine, the dropping temperature was kept at 0°C. After 4 hours of dropping, the solution was in the form of white slurry, and the reaction was kept for 0.5 hours. Remove the freezing device, slowly raise the temperature to 130°C for 1 hour, and keep the reaction for 5 hours. During the reaction process, the slurry liquid gradually becomes thinner, and the color of the solution gradually changes from wh...

Embodiment 2

[0024] Add 150ml of monochlorobenzene into a 1000ml flask, start the stirring device, turn on the refrigeration device to cool down the flask, and when the temperature reaches 0°C, open the phosgene valve to start feeding phosgene, adjust the flow rate of phosgene at 12g / h, pre-pass Phosgene 0.5h. Mix 550ml of monochlorobenzene and 70g of 1,3-cyclohexanedimethylamine evenly, add to the dropping funnel, pre-flow phosgene for 0.5h, then continue to pass phosgene, and open the dropping valve of the funnel at the same time, start to drop to the reaction system Add a mixed solution of chlorobenzene and 1,3-cyclohexanedimethylamine, and keep the dropping temperature at 0°C. After 4 hours of dropping, the solution is in the form of white slurry, and keep warm for 0.5 hours. Remove the freezing device, slowly raise the temperature to 130°C for 1 hour, and keep the reaction for 5 hours. During the reaction process, the slurry liquid gradually becomes thinner, and the color of the solu...

Embodiment 3

[0027] Add 150ml of toluene into a 1000ml flask, start the stirring device, turn on the refrigeration device to cool down the flask, and when the temperature reaches 0°C, open the phosgene valve to start feeding phosgene, adjust the flow rate of phosgene at 12g / h, and pre-pass phosgene at 0.5 h. Mix 550ml of toluene and 70g of 1,3-cyclohexanedimethylamine evenly, add to the dropping funnel, pre-pass phosgene for 0.5h, continue to pass through phosgene, open the dropping valve of the funnel at the same time, start to drop toluene and For the mixed solution of 1,3-cyclohexanedimethylamine, the dropping temperature was kept at 0°C. After 4 hours of dropping, the solution was in the form of white slurry, and the reaction was kept for 0.5 hours. Remove the freezing device, slowly raise the temperature to 120°C for 1 hour, and keep the reaction for 5 hours. During the reaction process, the slurry liquid gradually becomes thinner, and the color of the solution gradually changes from...

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Abstract

The invention discloses a synthesis method of 1,3-dimethyl isocyanate cyclohexane. The method comprises the steps of pumping a metered inert solvent into reactor capable of performing stirring and with phosgene ingress pipe for bedding, performing cooling, beginning to continuously supply metered phosgene, dropwise adding a metered mixed solution of 1,3-hexamethylene dimethylamine and the inert solvent into a reaction system to form a mixture of 1,3-hexanaphthene dimethylamine hydrochloride and 1,3-hexanaphthene dimethylcarbamoyl chloride (a material in the reactor is slurry and the process isa cold photochemical reaction), after dropwise adding, heating to a reaction temperature (the process is a heat photochemical reaction), after the reaction, removing excessive phosgene and hydrogen chloride through nitrogen, and performing high vacuum rectification to form high-purity 1,3-dimethyl isocyanate cyclohexane. The method has the advantages that raw materials are easy to obtain, the solvent can be recycled, and the method is simple in technology, easy and simple to operate, higher in yield, mild in reaction condition and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of isocyanate preparation, in particular to a method for synthesizing 1,3-dimethylisocyanate cyclohexane. Background technique [0002] 1,3-Dimethylisocyanate cyclohexane (referred to as H6XDI) is an aliphatic primary diisocyanate containing cyclohexane, which has the properties of hexamethylene diisocyanate (HDI) and isophorone diisocyanate (IPDI). advantage. H6XDI has excellent weather resistance and stable color, and is an important raw material that can be widely used in the preparation of cured coatings, artificial leather, paints, polyurethane elastomers, adhesives and sealing materials. Its chemical structural formula is: [0003] [0004] h 6 XDI is a cis-trans isomer mixture, a colorless transparent liquid at room temperature, with a relative molecular weight of 194.23, a density of 1.101g / mL (25°C), and a boiling point of 294.4°C (760mmHg). [0005] The phosgene method is commonly used to pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/10C07C265/14
CPCC07C263/10C07C2601/14C07C265/14
Inventor 韩邦友李炜钱圣利李强夏小峰李海燕曹卫东吴春辉
Owner JIANGSU KUAIDA AGROCHEM
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