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Preparation method of chlorinated special pentane

A technology of chlorpentane and phosphorus trichloride, which is applied in the field of preparation of chlorpentane, can solve the problems of low production efficiency, large amount of hydrochloric acid added, difficult post-treatment, etc., and achieves shortened reaction time, high content The effect of improving and reducing the difficulty of absorption

Inactive Publication Date: 2014-01-15
ZHANGJIAGANG CITY ZHENFANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1) The amount of hydrochloric acid added is too large, and a large amount of waste acid is produced, resulting in difficult post-processing and a large environmental burden
[0007] 2) The production efficiency is not high, and each reactor produces 3.5 to 4 batches per day, and each batch can produce 759±10Kg of chloropentane

Method used

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  • Preparation method of chlorinated special pentane
  • Preparation method of chlorinated special pentane
  • Preparation method of chlorinated special pentane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0022] Phosphorus trichloride is added to the reaction kettle equipped with 5±2Wt.% hydrochloric acid aqueous solution, and the reaction temperature is controlled at 5°C±2°C to generate hydrogen chloride gas, and the flow rate of hydrogen chloride gas is controlled to be 150m 3 / h, by controlling the gauge pressure -0.005~-0.01MPa, the generated hydrogen chloride gas is introduced into the packed tower. The gas is convected with the pre-cooled isopentene spray liquid, the flow rate of the isopentene spray liquid is 680L / h, the contact reaction time of isopentene and hydrogen chloride gas is 20-30s, and the direct gas-liquid reaction can produce chlorinated Pentane.

[0023] Gauge pressure -0.005~-0.01MPa draws unreacted hydrogen chloride gas, which is absorbed by the hydrochloric acid absorption tower. After absorbing the hydrochloric acid content of 5±2Wt.%, it can be recycled for the reaction raw material.

[0024] Table 1: Effect of temperature on product content and yield...

Embodiment 6-10

[0028] Phosphorus trichloride is added in the reactor that is equipped with 5 ± 2Wt.% hydrochloric acid aqueous solution, control reaction temperature 5 ± 2 ℃, generate hydrogen chloride gas, control the flow rate of hydrogen chloride gas, by controlling gauge pressure -0.005~-0.01MPa, will produce The hydrogen chloride gas is introduced into the packed tower. The packed tower body used is 10m high, the packing layer height is 8m, and the tower diameter is 60cm. The contact reaction time between alkenes and hydrogen chloride gas is 20-30s, and the direct gas-liquid reaction can produce chloropentane; during the whole reaction process, the temperature at the bottom of the tower is controlled at 10±2°C.

[0029] Gauge pressure -0.005~-0.01MPa draws unreacted hydrogen chloride gas, which is absorbed by the hydrochloric acid absorption tower. After absorbing the hydrochloric acid content of 5±2Wt.%, it can be recycled for the reaction raw material.

[0030] Table 2: Effects of the...

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Abstract

The invention discloses a preparation method of chlorinated special pentane, which includes the following steps: adding phosphorus trichloride into a reaction kettle filled with hydrochloric acid water solution of 5+ / -2Wt.%, controlling reaction temperature to be 5+ / -2 DEG C to generate hydrogen chloride gas, controlling flowing speed of the hydrogen chloride gas to be 150+ / -10m<3> / h, introducing generated hydrogen chloride gas into a packed tower by controlling gauge pressure to be -0.005 to -0.01MPa, enabling the hydrogen chloride gas to form convection with isoamylene spraying liquid which is pre-cooled to 5+ / -2 DEGC and has the flowing speed of 680+ / -10L / h, enabling reaction time of the isoamylene and the hydrogen chloride gas to be 20s-30s and conducting direct gas liquid reaction to obtain the chlorinated special pentane. In the whole reaction process, the tower bottom temperature is controlled to be 10+ / 2 DEG C. By means of the preparation method of the chlorinated special pentane, the problem of recycling of hydrogen chloride gas generated in phosphorous acid production is resolved, and sodium hydroxide water solution consumption is reduced. Product content is increased from prior 92Wt.%-93Wt.% to 97.5Wt.%-98.5Wt.%, the yield is correspondingly increased by 3%-4%, and the method improves production efficiency and saves production cost.

Description

technical field [0001] The invention relates to a preparation method of chloropentane, which belongs to the field of organic synthesis. Background technique [0002] Chloropentane is mainly used as an intermediate in the production of pinacolone, which is the main raw material for pesticides, medicines, and spices. [0003] Literature: 1) Synthesis of pinacolone in "Pesticides"; Volume 31, Issue 2, 1992, Du Jingxing, Ying Taosheng; 2) Synthesis method of pinacolone in "World Pesticides", Issue 06, 1983, Daoxing. The disclosed preparation method of chloropentane is summarized as follows: isopentene reacts with 31% hydrochloric acid at 5° C.±2° C. to generate chloropentane. [0004] Add quantitative isopentene to the reaction kettle and cool down to 5°C±2°C, then drop excess hydrochloric acid into the kettle, the molar ratio is 1:2.5, the dropping time is 2.5 to 3 hours, and the temperature is 5°C±2°C after the addition is completed. Keeping it warm for 2 hours under low tem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/01C07C17/08
Inventor 葛鹏圣曹爱春钱志强
Owner ZHANGJIAGANG CITY ZHENFANG CHEM
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