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Preparation method and preparation device of 1-naphthyl isocyanate

A technology of naphthyl isocyanate and preparation equipment, which is applied in the field of chemical equipment, can solve problems such as increasing difficulty, and achieve the effects of improving reaction stability, reducing purification temperature, and improving product quality and yield

Pending Publication Date: 2022-05-06
UPCHEM CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, catalysts such as triethylamine, pyridine, N-methylpyrrole or tetrabutylurea are used in the reaction process, which increases the difficulty of post-treatment.

Method used

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  • Preparation method and preparation device of 1-naphthyl isocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of preparation method of 1-naphthyl isocyanate, described preparation method mainly comprises the following steps:

[0029] 1) 2 / 5 of the menaphthylamine and xylene are mixed uniformly in the first mixing kettle 1 in a mass ratio of 1:6, and are made into the first menaphthylamine solution for use;

[0030] 2) 2 / 5 of the menaphthylamine and xylene are mixed uniformly in the second mixing kettle 3 in a mass ratio of 1:3, and the second menaphthylamine solution is prepared for use;

[0031] 3) Add solid phosgene and xylene with a mass ratio of 1:4 in the reactor 5, and heat up to dissolve; the molar ratio of menaphthylamine to solid phosgene is 1:0.5;

[0032]4) When the temperature in the reaction kettle 5 reaches 100-130°C, add dropwise the first methylnaphthylamine solution prepared in the above step 1) into the reaction kettle 5, and when the first methylnaphthylamine solution is dripped, continue Add dropwise the second menaphthylamine solution prepared in ab...

Embodiment 2

[0040] A kind of production method of 1-naphthyl isocyanate, in the first menaphthylamine solution, the mass ratio of menaphthylamine and xylene is 1:7; In the second menaphthylamine solution, the mass ratio of menaphthylamine and xylene is 1:4; the mass ratio of solid phosgene to xylene is 1:4, and the molar ratio of menaphthylamine to solid phosgene is 1:0.5. All the other are with embodiment 1. The production device is the same as in Example 1. The yield of the prepared 1-naphthyl isocyanate is 91%, and the product content is more than or equal to 99%.

Embodiment 3

[0042] A kind of production method of 1-naphthyl isocyanate, in the first menaphthylamine solution, the mass ratio of menaphthylamine and xylene is 1:8; In the second menaphthylamine solution, the mass ratio of menaphthylamine and xylene is 1:5; the mass ratio of solid phosgene to xylene is 1:4, and the molar ratio of menaphthylamine to solid phosgene is 1:0.5. All the other are with embodiment 1. The production device is the same as in Example 1. The yield of the prepared 1-naphthyl isocyanate is 90.3%, and the product content is more than or equal to 98.5%.

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Abstract

The invention discloses a preparation method and a preparation device of 1-naphthyl isocyanate. The preparation method comprises the following steps: respectively preparing methylnaphthylamine and a solvent into methylnaphthylamine solutions with different gradient concentrations, and adding triphosgene and the solvent into a reaction kettle; when the temperature in the reaction kettle reaches 100-130 DEG C, sequentially dropwise adding a low-concentration menaphthylamine solution and a high-concentration menaphthylamine solution; the total dripping time is 1-2 hours, and the reflux heat preservation time is 0.5-1.5 hours; the reaction process is monitored by a DCS (Distributed Control System); and purifying the reaction mixed solution in a high-vacuum distillation manner. The preparation device comprises a first mixing kettle, a second mixing kettle, a reaction kettle, a solvent reflux device, a rectifying tower, a first condenser, a second condenser, a product storage tank and a vacuum unit. According to the invention, green process preparation, one-step synthesis and gradient concentration dropwise addition reaction are adopted, so that the initial reaction is more moderate and sufficient, the reaction stability is improved, and the generation of side reaction is reduced; a high-vacuum distillation technology is adopted for product purification, so that the product quality and yield are improved.

Description

technical field [0001] The invention relates to a preparation method and a preparation device of 1-naphthyl isocyanate, belonging to the field of chemical equipment. Background technique [0002] 1-Naphthyl isocyanate is an important intermediate of medicine, pesticide and polymer material, widely used in the synthesis of new fluorescent dyes and medicine. The synthesis of 1-naphthyl isocyanate can be prepared by using menaphthylamine and phosgene in an inert solvent medium by a one-step reaction; using phosgene as an acylating agent, because phosgene is a highly toxic chemical substance, it is difficult to produce, transport, store and There are strict precautions and regulations in use, and the protection of operators during production is also very strict. [0003] In recent years, non-phosgenation of isocyanate synthesis is a new technology development trend. The reactivity of solid phosgene is similar to that of phosgene and diphosgene, and it can replace phosgene and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/04C07C263/20C07C265/12C07C269/00C07C271/04B01J19/24B01J19/00B01J4/02B01J4/00B01F33/81B01D3/14
CPCC07C263/04C07C263/20C07C269/00B01J19/24B01J19/0053B01J19/00B01J4/001B01J4/02B01D3/14C07C271/04C07C265/12
Inventor 夏剑锋夏晨东陈映波方庆良林上理练峰樊晓园
Owner UPCHEM CHINA
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