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Method for co-producing n-butyl isocyanate from chloroformic acid-2-ethylhexyl ester

A technology of butyl isocyanate and ethyl hexyl ester is applied in the field of co-production of n-butyl isocyanate with 2-ethylhexyl chloroformate, which can solve problems such as unfavorable FNC phosgenation reaction, and achieve economical and environmental protection effects. Remarkably, reduce the treatment cost, and the effect of tail gas separation is good

Inactive Publication Date: 2021-02-23
NINGXIA RUITAI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, nitrogen is used as the solvent to extinguish the light, and more non-condensable gas is brought into the reaction system, which is not conducive to the phosgenation reaction of FNC.

Method used

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  • Method for co-producing n-butyl isocyanate from chloroformic acid-2-ethylhexyl ester
  • Method for co-producing n-butyl isocyanate from chloroformic acid-2-ethylhexyl ester
  • Method for co-producing n-butyl isocyanate from chloroformic acid-2-ethylhexyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Such as figure 1 As shown, (1) Add 50 mol of iso-octanol to the LDZ synthesis kettle, the mol ratio of phosgene to iso-octanol is 1.3:1, the reaction temperature is 10°C, and the reaction time is 3 hours. The reaction tail gas is condensed at -20°C, the non-condensable gas is dried by sulfuric acid, and the HCl of the tail gas is 45mol. The normalized content of LDZ is 98.1% and the yield is 97.2%.

[0027] (2) Add 40 mol of n-butylamine to the FNC synthesis kettle, and the mass ratio of n-butylamine to o-dichlorobenzene is 1:2. Pass in hydrogen chloride in step (1), the molar ratio of hydrogen chloride to n-butylamine is 1.12:1, and the salt-forming reaction temperature is 10°C. After salt formation, the temperature is raised to 80°C, phosgene is introduced in (1) and the light is supplemented until the material liquid is clarified. The light passage time is 5 hours, and the actual amount of phosgene used is 48mol. The amine molar ratio was 1.2:1. The FNC content o...

Embodiment 2

[0029] Such as figure 1 As shown, (1) Add 50 mol of iso-octanol to the LDZ synthesis kettle, the phosgene: iso-octanol mol ratio is 1.5:1, the reaction temperature is 10°C, and the reaction time is 3 hours. The tail gas of the reaction was condensed at -20°C, the non-condensable gas was dried with sulfuric acid, and the HCl in the tail gas was 46 mol. The normalized content of LDZ is 98.7% and the yield is 97.7%.

[0030] (2) Add 40 mol of n-butylamine to the FNC synthesis kettle, and the mass ratio of n-butylamine to o-dichlorobenzene is 1:3. Pass in hydrogen chloride in step (1), the molar ratio of hydrogen chloride to n-butylamine is 1.15:1, and the salt-forming reaction temperature is 10°C. After salt formation, raise the temperature to 90°C, pass through (1) phosgene and supplement light, and pass light for 7 hours. The actual amount of phosgene used is 52 mol, the supplementary phosgene in the process is 29.5 mol, and the molar ratio of phosgene to n-butylamine is 1.3...

Embodiment 3

[0032] Such as figure 1 As shown, (1) Add 50 mol of iso-octanol to the LDZ synthesis kettle, the phosgene:iso-octanol mol ratio is 1.7:1, the reaction temperature is 15°C, and the reaction time is 3 hours. The tail gas of the reaction was condensed at -20°C, the non-condensable gas was dried with sulfuric acid, and the HCl in the tail gas was 48mol. The normalized content of LDZ is 99.2% and the yield is 98.5%.

[0033] (2) Add 40 mol of n-butylamine to the FNC synthesis kettle, and the mass ratio of n-butylamine to o-dichlorobenzene is 1:5. Pass in hydrogen chloride in step (1), the molar ratio of hydrogen chloride to n-butylamine is 1.2:1, and the salt-forming reaction temperature is 15°C. After salt formation, raise the temperature to 90°C, pass through (1) phosgene and supplement light, and pass light for 5 hours. The actual amount of phosgene used is 50mol, the supplementary phosgene is 18.5mol in the process, and the molar ratio of phosgene to n-butylamine is 1.25:1. ...

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Abstract

The invention discloses a method for co-producing n-butyl isocyanate from chloroformic acid-2-ethylhexyl ester, wherein the method comprises the steps: preparing LDZ from phosgene and isooctanol as raw materials, wherein the tail gas composition is byproduct hydrogen chloride and excessive phosgene; introducing inert gas into the LDZ synthetic liquid, and performing a gas driving process to obtaina finished product LDZ and synthetic tail gas; condensing the LDZ synthetic tail gas by a condenser to obtain condensate, and enabling the condensate to be liquid phosgene containing LDZ and uncondensed gas to be HCl, wherein HCl is used for n-butylamine salifying after passing through a concentrated sulfuric acid scrubbing device, and liquid phosgene is used as a phosgene source for FNC synthesis after being washed with sulfuric acid; and introducing HCl for gas washing into an o-dichlorobenzene solution containing n-butylamine, carrying out a salifying reaction until n-butylamine in o-dichlorobenzene is not detected and salifying is finished, introducing phosgene, carrying out FNC synthesis until the synthesis solution is clear, and carrying out light driving and rectification on the synthesis solution to obtain an FNC finished product. According to the co-production scheme provided by the invention, the discharge amount of tail gas is greatly reduced, the waste gas is reduced by 85% or more, and the economic effect is remarkable.

Description

technical field [0001] The invention relates to a chemical production process, in particular to a method for co-producing n-butyl isocyanate from 2-ethylhexyl chloroformate. Background technique [0002] 2-Ethylhexyl chloroformate, referred to as chloroester (LDZ), is mainly used to prepare di(2-ethyl)hexyl peroxydicarbonate (EHP). EHP is a highly active initiator and is often used as a general-purpose plastic It can also be used as a polymerization initiator for rubber materials, and can also be used to produce bleaching agents, oxidation accelerators, flame retardants, etc. The current industrial process is to prepare LDZ by reacting isooctyl alcohol with phosgene. Since LDZ is unstable, it will decompose during the heating and refining process, posing a safety hazard. The content of the reaction solution should be more than 98% after being exhausted, and it will be sold as a product. Therefore, the amount of phosgene is required to be high, and the by-product hydrogen c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/10C07C263/20C07C265/04C07C68/02C07C68/08C07C69/96C01B7/01
CPCC07C263/10C07C263/20C07C68/02C07C68/08C01B7/01C07C265/04C07C69/96
Inventor 严绘石苏洋林洋摆永明孟海娟韩小文
Owner NINGXIA RUITAI TECH
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