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Chemical synthesis method for octadecyl isocyanic ester

An octadecyl isocyanate, chemical synthesis technology, applied in chemical instruments and methods, preparation of isocyanic acid derivatives, organic chemistry and other directions, can solve the high sealing requirements of reaction equipment, inconvenient and accurate measurement, safety hazards, etc. problems, to achieve the effect of large implementation value and social and economic benefits, elimination of hidden safety hazards, and no three wastes

Inactive Publication Date: 2008-08-20
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that it uses highly toxic gases that are strictly controlled and restricted internationally. Whether it is laboratory work or industrial production, the sealing of the reaction equipment is very high, the investment is also large, and the phosgene in the tail gas From the perspective of environmental protection, it will bring a lot of trouble. In production, there must be an additional set of equipment for producing and storing phosgene, and there are great safety hazards in the process.
At the same time, phosgene as a gas is not convenient for accurate measurement, especially when a small amount of accurate quantitative phosgene is required in the laboratory, excessive use may easily cause side reactions

Method used

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  • Chemical synthesis method for octadecyl isocyanic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The molar ratio of octadecylamine to bis(trichloromethyl)carbonate is 1:1 / 3, the solvent is n-hexane, and the amount used is 2 mL / g based on the mass of octadecylamine.

[0021] Add 29.7 g (0.1 mol) of bis(trichloromethyl) carbonate and n-hexane (70 mL) into a four-neck flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel, and a reflux condenser, start stirring, and cool to 0-5°C. Add 80.7g (0.3mol) of n-hexane (90mL) solution of octadecylamine dropwise into the reaction system through a constant pressure dropping funnel at a rate of about 1.5ml / min. After the dropwise addition, stir at room temperature for 0.5h before Raise the temperature to 70°C, and react at 70-80°C for about 2.5h. After the reaction was completed, nitrogen was blown to drive away the hydrogen chloride gas, n-hexane was recovered by vacuum distillation, and 69.4 g of the product octadecyl isocyanate was distilled out, with a yield of 78.2%. The purity of the...

Embodiment 2

[0023] The molar ratio of octadecylamine to bis(trichloromethyl)carbonate is 1:0.35, and the amount of solvent used is 3 times the mass of octadecylamine. Other operations were the same as in Example 1, the product octadecyl isocyanate was 70.5 g, the yield was 79.5%, and the product purity was 98.2% as determined by gas chromatography.

Embodiment 3

[0025] The molar ratio of octadecylamine to bis(trichloromethyl)carbonate is 1:0.35, the solvent is n-hexane, and the dosage is 3mL / g based on the mass of octadecylamine. Add 31.2 g (0.105 mol) of bis(trichloromethyl) carbonate and n-hexane (90 mL) into a four-neck flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel, and a reflux condenser, start stirring, and cool to 0-5°C. A n-hexane (150mL) solution with an octadecylamine dosage of 80.7g (0.3mol) was dropped into the reaction system at a rate of about 1.5ml / min through a constant pressure dropping funnel. After the addition was complete, stir at room temperature for 2h. Then heat up to 70°C, and react at 70-80°C for about 2h. After the reaction was completed, nitrogen gas was used to drive away the hydrogen chloride gas, and 70.7 g of the product octadecyl isocyanate was evaporated after recovering n-hexane by vacuum distillation, with a yield of 79.7%. The purity of the product det...

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Abstract

The invention discloses a chemical synthesis method of octadecyl isocyanate; wherein, the method adopts octadecyl amine and bi(trichloromethyl) carbonate as raw materials, organic solvents are used for dissolving the octadecyl amine solution to be slowly dropped into the solution of the bi(trichloromethyl) carbonate dissolved by the same organic solvent, the temperature of a reaction system is kept from 0 to 5 DEG C, and after the dropping is finished, the solution is stirred for 0.5 hour to 5 hours at room temperature, then the temperature is increased to 35 to 150 DEG C and the solution is reacted at the temperature of 35 to 150 DEG C for 0.5 hour to 10 hours and then the octadecyl isocyanate is obtained after the reaction solution is post treated. The chemical synthesis method is advanced in technical route, reasonable in technical condition and eliminates potential safety hazard from headstream; the used raw materials are cheap and easy to be obtained; the use of highly toxic gas phosgene controlled internationally is abolished and the problems of big potential safety hazard and severe three wastes, etc. of traditional technologies are eliminated; the chemical synthesis method is simple and safe in operation, high in reaction yield, low in production cost and basically has no three wastes and has greater implement value and social economic benefits.

Description

(1) Technical field [0001] The invention relates to a chemical synthesis method of octadecyl isocyanate. (2) Background technology [0002] Before the present invention was made, the chemical synthesis method of prior art octadecyl isocyanate was based on octadecylamine and phosgene (COCl 2 ) is synthesized from raw materials. For example, GB761590 proposes to react octadecyl isocyanate with 26.9g of octadecylamine and 12g of phosgene. The disadvantage of this process is that it uses highly toxic gases that are strictly controlled and restricted internationally. Whether it is laboratory work or industrial production, the sealing of the reaction equipment is very high, the investment is also large, and the phosgene in the tail gas Considering from an environmental protection point of view, it will bring great troubles. In production, there must be an additional set of equipment for producing and storing phosgene, and there are great potential safety hazards in the process. ...

Claims

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Application Information

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IPC IPC(8): C07C263/10C07C265/04
Inventor 吴华悦陈久喜刘妙昌
Owner WENZHOU UNIVERSITY
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