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Process for producing isocyanate

A manufacturing method and technology of isocyanate, applied in the field of isocyanate manufacturing, can solve problems such as isocyanate yield reduction

Active Publication Date: 2011-04-20
ASAHI KASEI KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that during the evaporation of methyl urethane, the non-evaporated components are removed from the bottom of the evaporator, but the yield of isocyanate is reduced because the removed components contain methyl urethane
In addition, since the vapor of methyl urethane is transported at high temperature, it tends to easily cause the thermal modification reaction of methyl urethane

Method used

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  • Process for producing isocyanate
  • Process for producing isocyanate
  • Process for producing isocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0340] The present invention will be specifically described below based on examples, but the scope of the present invention is not limited to these examples.

[0341]

[0342] 1) NMR analysis method

[0343] Device: JNM-A400 FT-NMR system manufactured by Japan Electronics Co., Ltd.

[0344] (1) 1 H and 13 Preparation of samples for C-NMR analysis

[0345] Weigh about 0.3 g of the sample solution, add about 0.7 g of deuterated chloroform (manufactured by Aldrich, USA, 99.8%) and 0.05 g of tetramethyltin as an internal standard substance (manufactured by Wako Pure Chemical Industries, Ltd., Wako Grade 1) , and the homogeneously mixed solution was used as a sample for NMR analysis.

[0346] (2) Quantitative analysis method

[0347] Analysis is performed on each standard substance, and quantitative analysis of the analysis sample solution is performed based on the prepared calibration curve.

[0348] 2) Liquid chromatography analysis method

[0349] Device: LC-10AT system...

reference example 1

[0376] [Reference Example 1] Production of bis(3-methylbutyl)carbonate

[0377] ・Step (I-1): Production of dialkyltin catalyst

[0378] Add 625g (2.7mol) of di-n-butyltin oxide (manufactured by Japan Sankyo Organic Synthetic Co., Ltd.) and 2020g (22.7mol) of 3-methyl-1-butanol (Japanese Wako Pure Chemical Industries, Ltd.) into an eggplant-shaped flask with a volume of 5000mL. industrial society). The flask was mounted on an evaporator (manufactured by Japan Shibata Corporation, R-144), which was connected with an oil bath with a temperature regulator (manufactured by Japan Masuda Physical and Chemical Industry Corporation, OBH-24), a vacuum pump (manufactured by Japan ULVAC Corporation, Manufactured, G-50A) and vacuum controller (manufactured by Okano Manufacturing Co., Ltd., VC-10S). The discharge valve outlet of the evaporator was connected to a pipeline of nitrogen flowing under normal pressure. Close the discharge valve of the evaporator to depressurize the system, the...

reference example 2

[0381] [Reference Example 2] Manufacture of dibutyl carbonate

[0382] ・Step (II-1): Production of dialkyltin catalyst

[0383] 692 g (2.78 mol) of di-n-butyltin oxide and 2001 g (27 mol) of 1-butanol (manufactured by Wako Pure Chemical Industries, Ltd.) were placed in an eggplant-shaped flask with a volume of 3000 mL. The flask charged with the white slurry-like mixture was installed on an evaporator connected to an oil bath with a temperature regulator, a vacuum pump, and a vacuum controller. The discharge valve outlet of the evaporator was connected to a pipeline of nitrogen flowing under normal pressure. Close the discharge valve of the evaporator to depressurize the system, then slowly open the discharge valve, flow nitrogen into the system, and return to normal pressure. The temperature of the oil bath was set to 126° C., the flask was immersed in the oil bath, and the rotation of the evaporator was started. After heating with rotary stirring at normal pressure for ab...

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Abstract

A process for producing an isocyanate without using phosgene. The process has none of various problems encountered in prior art techniques and enables an isocyanate to be stably produced in high yield for long. The process is for producing an isocyanate by subjecting a carbamic acid ester to pyrolytic reaction. The process includes: a step in which low-boiling ingredients are recovered as a gas-phase ingredient from a pyrolysis reactor where the pyrolytic reaction is conducted; a step in which a liquid-phase ingredient containing the carbamic acid ester is recovered through a bottom part of the pyrolysis reactor; and a step in which part or all of the liquid-phase ingredient is supplied to an upper part of the pyrolysis reactor.

Description

technical field [0001] The present invention relates to a method for producing isocyanates. Background technique [0002] Isocyanates are widely used as raw materials for the manufacture of polyurethane foams, coatings, and adhesives. The main industrial production method of isocyanate is the reaction of amine compounds and phosgene (phosgene method), and almost all of the world's production is produced by the phosgene method. However, the phosgene method has many problems. [0003] First, a large amount of phosgene is used as a raw material. Phosgene is extremely toxic and its handling requires special care in order to prevent worker exposure to phosgene, as well as special devices for rendering waste harmless. [0004] Second, in the phosgene method, since a large amount of highly corrosive by-product hydrogen chloride is produced, a treatment for detoxifying the hydrogen chloride is required, and the produced isocyanate often contains hydrolyzable chlorine. Therefore,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/18C07C263/04C07C265/14
CPCC07C2101/14C07C263/18C07C263/04C07C2601/14C07C265/14C07C263/00C07C265/00C07C265/02
Inventor 篠畑雅亮三宅信寿
Owner ASAHI KASEI KK
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