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A kind of method for continuously producing stearyl chloride

A stearyl chloride, production equipment technology, applied in the direction of chemical instruments and methods, preparation of organic compounds, carboxylate preparation, etc., can solve the problems of harsh reaction conditions, low phosgene utilization rate, slow reaction speed, etc., to achieve accelerated Reaction speed, low tar content, and improved utilization

Inactive Publication Date: 2016-01-06
甘肃银光聚银化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In summary, most of the existing technologies for producing stearyl chloride are reacted in a stirred tank, the mass transfer efficiency is poor, the reaction speed is slow, or the reaction conditions are harsh, and the phosgene utilization rate is low

Method used

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  • A kind of method for continuously producing stearyl chloride
  • A kind of method for continuously producing stearyl chloride
  • A kind of method for continuously producing stearyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1, see figure 1 :

[0031] The size of No. 1 bubble tower and No. 3 bubble tower is φ325×800mm, the size of No. 2 bubble tower is φ457×800mm, and the No. 1 and No. 3 circulating pumps used are experimental metering pumps with a flow rate of 1m 3 / h, No. 2 circulating pump is a metering pump for experiments, with a flow rate of 2m 3 / h, the proportion of DMF in the molten stearic acid is 0.8%, placed in a high-level tank with a heat preservation device (temperature is 75 ° C), and continuously flows to the No. 1 bubble column, which is controlled by pipeline valves and flow meters The velocity is 0.035m 3 / h, continuously entering No. 1 bubble tower phosgene is 0.25m 3 / h, continuously entering No. 3 bubble tower phosgene is 0.3m 3 / h, No. 1 heat exchanger, No. 2 heat exchanger and No. 3 heat exchanger use warm water at 60°C. After phosgene is introduced for 0.5 hours, No. 1 bubble tower, No. 2 bubble tower and No. 3 bubble tower The temperature starts to ri...

Embodiment 2

[0032] Example 2, the equipment size is the same as that of Example 1, the operation process is the same as that of Example 1, the reaction temperature is controlled at 65°C, and the sample is taken from the discharge port after continuous operation for 1 hour, and the acid chloride content in the crude acid chloride is 92.63% by potentiometric titration . After 3.0 hours of continuous operation, the content of acid chloride was stabilized above 97.50%, but the color of the obtained crude product of acid chloride was slightly lighter than that of Example 1.

Embodiment 3

[0033] Example 3, the equipment size is the same as in Example 1, the operation process is the same as in Example 1, the reaction temperature is controlled at 85°C, and the sample is taken from the discharge port after continuous operation for 1 hour, and the acid chloride content in the crude acid chloride is 94.92% by potentiometric titration. . After 2.3 hours of continuous operation, the acid chloride content was stable above 97.50%, but the color of the obtained crude acid chloride was slightly darker than that of Examples 1 and 2.

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Abstract

The invention relates to a method for continuously producing stearoyl acid chloride. The method comprises steps as follows: a, stearic acid and a catalyst are continuously and proportionally fed from a liquid phase feeding port in the top of a first bubble tower and sequentially enter a second bubble tower and a third bubble tower in a streaming manner; through forced circulation of a first tower bottom pump, a second tower bottom pump and a third tower bottom pump, a crude productstearoyl acid chloride is finally discharged out of a discharging port in the third tower bottom pump and then enters an acyl chloride refining procedure; b, fresh phosgeneenters a gas phase feeding portand continuously bubbles through the first bubble tower and the third bubble tower, exhaust of the first bubble tower enters the middle of the second bubble tower, exhaust of the third bubble tower enters the bottom of the second bubble tower, unreacted phosgene in exhaust of the first bubble tower and the third bubble tower continuously participates in reaction in the second bubble tower, and exhaust from the top of the second bubble tower enters a follow-up hydrochloric acid absorption procedure. According to the method and the device, the quality of stearoyl acid chloride produced through reaction is good, the crude productstearoyl acid chloride can be higher than 97.5%, the tar content of the crude product is low, and the follow-up treatment is easy.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a production method for generating stearyl chloride by continuous bubbling reaction of gas-phase phosgene. Background technique [0002] Stearoylacidchloride (Stearoylacidchloride, also known as octadecanoyl chloride) is a pesticide intermediate and a raw material for the production of neutral sizing agent for papermaking - alkyl ketene dimer (AKD). Under the catalysis of dimethylformamide (DMF), it reacts with phosgene to generate acylated products. The reaction is mainly divided into two stages: [0003] 1. Catalyst activation stage [0004] [0005] Phosgene reacts with dimethylformamide to generate active group (1), which is very unstable and releases a molecule of CO soon 2 , and generate active group(2) [0006] [0007] 2. The active group (2) reacts with stearic acid to generate stearyl chloride, regenerates dimethylformamide, and releases a molecule...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/42C07C51/60
CPCC07C51/60C07C53/42
Inventor 韩胜兵蒙鸿飞齐国栋李小利沈精平李晓明陈玫君孟柱乔鼎何玉姣
Owner 甘肃银光聚银化工有限公司
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