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Method of preparing diisocyanate composition

A technology of diisocyanate and composition, applied in the field of triphosgene composition, can solve the problems of reduced yield, increased purity of final product, difficulty in storage and management, etc., and achieves high yield, excellent handling convenience and excellent processability. Effect

Active Publication Date: 2021-06-08
SKC CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the amine is dissolved in aqueous hydrochloric acid solution, the yield is significantly reduced to 50%, making it difficult for practical application
The difficulty is that amines with low water and impurity content should be used as raw materials in order to increase the purity of the final product
In addition, the phosgene gas used in the conventional phosgene process is highly toxic and a substance regulated by environmental regulations
Difficulties in storage and management as a separate cooling device is required to store it

Method used

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  • Method of preparing diisocyanate composition
  • Method of preparing diisocyanate composition
  • Method of preparing diisocyanate composition

Examples

Experimental program
Comparison scheme
Effect test

example A1

[0226] Into a 5-liter 4-neck reactor, 963.5 g (9.25 moles) of 35% aqueous hydrochloric acid was charged, and then the internal temperature of the reactor was lowered to 15°C while stirring. While maintaining the temperature of the reactor at 50° C., 600.0 g (4.4 moles) of m-xylylenediamine (m-XDA) was introduced for 1 hour. After the introduction was completed, the internal temperature of the reactor was lowered to 10° C., and it was stirred for 1 hour. Thereafter, 1,200.0 g of diethyl ether (Et 2 O) as an organic solvent, and the internal temperature of the reactor was lowered to -5°C, followed by stirring for 1 hour. After the reaction was completed, it was vacuum filtered using a filter, and the filtered diethyl ether was recovered for reuse. The recovery of diethyl ether was 73%. After vacuum filtration, m-xylylenediamine (m-XDA) hydrochloride composition was obtained. In order to remove the residual organic solvent and water, the reactor was dried under the conditions...

example A2

[0228] Into a 5-liter 4-neck reactor, 986.5 g (9.47 moles) of 35% aqueous hydrochloric acid was charged, and then the internal temperature of the reactor was lowered to 15° C. while stirring. While maintaining the temperature of the reactor at 50°C, 600.0 g (4.4 moles) of m-XDA was introduced for 1 hour. After the introduction was completed, the internal temperature of the reactor was lowered to 10° C., and it was stirred for 1 hour. Thereafter, 1,260 g of isopropanol (i-PrOH) was introduced as an organic solvent, and the internal temperature of the reactor was lowered to -5° C., followed by stirring for 1 hour. After the reaction was completed, it was vacuum filtered using a filter, and the filtered isopropanol was recovered for reuse. Here, the recovery rate of isopropanol was 75%. After vacuum filtration, the m-XDA hydrochloride composition was obtained. In order to remove the residual organic solvent and water, drying was carried out under the condition that the externa...

example A3

[0230]Into a 5-liter 4-neck reactor was charged 1,009.4 g (9.69 moles) of a 35% aqueous hydrochloric acid solution, and then the internal temperature of the reactor was lowered to 15° C. with stirring. While maintaining the temperature of the reactor at 50°C, 600.0 g (4.4 moles) of m-XDA was introduced for 1 hour. After the introduction was completed, the internal temperature of the reactor was lowered to 10° C., and it was stirred for 1 hour. Thereafter, 1,320 g of tetrahydrofuran was introduced, and the internal temperature of the reactor was lowered to -5° C., followed by stirring for 1 hour. After the reaction was finished, it was vacuum filtered using a filter, and the filtered tetrahydrofuran was recovered for reuse. The recovery of tetrahydrofuran was 82%. After vacuum filtration, the m-XDA hydrochloride composition was obtained. In order to remove the residual solvent and water, drying was carried out under the condition that the external temperature of the reactor ...

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Abstract

The embodiments provide processes for preparing a diisocyanate composition and an optical lens, which are excellent in yield and quality with mitigated environmental problems by using a solid triphosgene composition instead of phosgene gas in the process of preparing a diisocyanate from a diamine through a hydrochloride thereof and by controlling the content of a decomposition product in a triphosgene composition, the b* value according to CIE color coordinate of the triphosgene composition in an organic solvent, or the content of water in the triphosgene.

Description

technical field [0001] Embodiments relate to methods of making diisocyanate compositions. More specifically, the embodiments relate to a method for producing a diisocyanate composition by diamine hydrochloride, a method for producing an optical lens using the thus-prepared diisocyanate composition, and a Sanko lens having a specific component content and used in the above production gas composition. Background technique [0002] Isocyanates used as raw materials for plastic optical lenses are produced by a phosgene method, a non-phosgene method, a pyrolysis method, and the like. [0003] In the phosgene method, amines are used as raw materials and phosgene (COCl 2 ) gases react to synthesize isocyanates. In addition, in the non-phosgene method, dibromomethylbenzene is reacted with sodium cyanate in the presence of a catalyst to synthesize isocyanate. In the pyrolysis method, an amine is reacted with an alkyl chloroformate to prepare a carbamate, which is pyrolyzed at hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/76C08G18/75C08G18/73C08G18/38G02B1/04
CPCC08G18/7642C08G18/757C08G18/73C08G18/755C08G18/3876G02B1/04Y02P20/582C07C263/10C07C265/08C07C265/14C07C263/20
Inventor 裵栽荣金正武明正焕韩赫熙
Owner SKC CO LTD