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A kind of preparation method of 1-naphthylacetic acid

A technology of naphthaleneacetic acid and chloroacetic acid, which is applied in the field of preparation of 1-naphthaleneacetic acid, can solve the problems of reducing production costs, achieve the effects of reducing production costs, solving recycling problems, and reducing production

Active Publication Date: 2022-06-24
浙江大鹏药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It greatly reduces the production of by-products, solves the problem of excessive chloroacetic acid recovery, is highly efficient and environmentally friendly, saves complicated separation steps, greatly reduces production costs, and is suitable for large-scale continuous production of 1-naphthylacetic acid

Method used

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  • A kind of preparation method of 1-naphthylacetic acid
  • A kind of preparation method of 1-naphthylacetic acid
  • A kind of preparation method of 1-naphthylacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: (molar ratio 1:1)

[0033] Feeding is carried out in the reactor 3 that is equipped with 100kg ZSM-5, temperature of reaction is 190 ℃, and the naphthalene feed rate is 95kg / h, and is uniformly dispersed in the reactor by spray head 2 after melting, and the chloroacetic acid feed rate is 70kg / h, after gasification, press into the reactor through the compressor, separate the 1-naphthalene acetic acid and the excess liquid chloroacetic acid mother liquor through the filter press, and the mother liquor circulates the mother liquor through the pipeline to the reactor 3 through the circulating pump; the mother liquor passes through the mother liquor The circulation pump is returned to the reactor. The yield of 1-naphthaleneacetic acid was 95.5%, and the product purity after drying was 98.8%. IR(cm -1 ): 3300-2500, 3065.1, 2915.2, 1699.0, 1414.0, 1220.5, 935.1, 781.2. H NMR spectroscopy (CDCl 3 )δ: 11.9(S, 1H), 7.98-8.00(d, 2H), 7.88-7.90(d, 2H), 7.82-7.84(d, ...

Embodiment 2

[0034] Example 2: (molar ratio 1:10)

[0035] Feeding is carried out in the reactor 3 that is equipped with 100kg ZSM-11, temperature of reaction is 215 DEG C, and naphthalene feed rate is 100kg / h, after melting, uniformly dispersed in reactor by spray head 2, chloroacetic acid feed rate is 734kg / h, after gasification, press into the reactor through the compressor, separate the 1-naphthalene acetic acid and the excess liquid chloroacetic acid mother liquor through the filter press, and the mother liquor circulates the mother liquor through the pipeline to the reactor 3 through the circulating pump; 1-naphthalene The yield of acetic acid was 95.5%, and the product purity after drying was 98.9%.

Embodiment 3

[0036] Example 3: (molar ratio 1:1.36)

[0037]Feeding is carried out in the reactor 3 that 85kg ZSM-11 is housed in, temperature of reaction is 200 ℃, and the naphthalene feed rate is 1000kg / h, and is uniformly dispersed in the reactor by spray head 2 after melting, and the chloroacetic acid feed rate is 734kg / h, after gasification, press into the reactor through the compressor, separate the 1-naphthalene acetic acid and the excess liquid chloroacetic acid mother liquor through the filter press, and the mother liquor circulates the mother liquor through the pipeline to the reactor 3 through the circulating pump; 1-naphthalene The yield of acetic acid was 96.5%, and the product purity after drying was 98.7%.

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Abstract

The invention belongs to the field of pesticide synthesis, and in particular relates to a preparation method of 1-naphthaleneacetic acid. The method specifically comprises: adding naphthalene and chloroacetic acid into a reactor for reaction to obtain a mixture containing 1-naphthaleneacetic acid and excess chloroacetic acid; performing solid-liquid separation on the mixture to obtain 1-naphthaleneacetic acid and a mother liquor; the mother liquor circulation To the above reaction; when the naphthalene is fed, it is in a molten liquid state, and the chloroacetic acid is in a gaseous state. The method for continuously producing 1-naphthaleneacetic acid of the present invention greatly reduces the generation of by-products, solves the problem of excessive chloroacetic acid recovery, is highly efficient and environmentally friendly, saves complicated separation steps, greatly reduces production costs, and is suitable for large-scale continuous production. Production of 1-naphthylacetic acid.

Description

technical field [0001] The invention belongs to the field of pesticide synthesis, in particular to a preparation method of 1-naphthaleneacetic acid. Background technique [0002] 1-Naphthylacetic acid is a broad-spectrum plant growth regulator, which can rapidly promote cell division and expansion (fruit swelling agent, expandin, induce the formation of adventitious roots (rooting agent), and can regulate growth, promote rooting, flowering, prevent Falling flowers and fruits, forming seedless fruit, promoting early maturity, increasing yield, etc., and at the same time, after use, it can also enhance the plant's ability to resist drought, cold, salinity, disease, and dry and hot wind. It is a broad-spectrum, high-efficiency, low- Toxic plant growth regulator. [0003] There are many synthetic methods of 1-naphthaleneacetic acid. The first method is the condensation of naphthalene with chloroacetic acid to obtain naphthaleneacetic acid (Ogata Y, Ishiguro J.Preparation ofα-N...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/353C07C57/40B01J29/40
CPCC07C51/353B01J29/40C07C57/40
Inventor 蒋成君徐学春徐大国
Owner 浙江大鹏药业股份有限公司
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