阅读说明：本技术 苯磺酰氯粗品蒸馏制取苯磺酰氯和二苯砜的生产装置 (Production device for distilling crude benzenesulfonyl chloride to prepare benzenesulfonyl chloride and diphenyl sulfone ) 是由 朱雪松 张福祥 刘仕通 马龙 于海洋 于 2020-06-28 设计创作，主要内容包括：一种苯磺酰氯粗品蒸馏制取苯磺酰氯和二苯砜的生产装置,包括依次通过管道连接的蒸馏釜、精馏柱组、冷凝器组、物料接收体系和抽真空体系；精馏柱组包括大精馏柱和小精馏柱,小精馏柱顶端与头尾料储罐相连通；冷凝器组包括依次相互连通的第一预冷管、第二预冷管和冷凝器,物料接收体系包括苯磺酰氯接收罐和二苯砜接受罐；苯磺酰氯接收罐通过第一出料管与出料口相连通,二苯砜接收罐通过第二出料管连接在所述的第一出料管上；本发明通过在冷凝器前预设体积较小的第一冷凝管和第二冷凝管使得苯磺酰氯在经过大蒸馏柱分离后立即进入第一预冷管和第二预冷管,将温度较高的苯磺酰氯气体预冷,以减少苯磺酰氯的热分解,实现高效分馏,且提高了馏分的纯度。(A production device for preparing benzene sulfonyl chloride and diphenyl sulfone by distilling a crude benzene sulfonyl chloride product comprises a distillation still, a rectification column group, a condenser group, a material receiving system and a vacuum pumping system which are sequentially connected through pipelines; the rectification column group comprises a large rectification column and a small rectification column, and the top end of the small rectification column is communicated with the head and tail material storage tank; the condenser group comprises a first precooling pipe, a second precooling pipe and a condenser which are sequentially communicated with one another, and the material receiving system comprises a benzene sulfonyl chloride receiving tank and a diphenyl sulfone receiving tank; the benzene sulfonyl chloride receiving tank is communicated with the discharge hole through a first discharge pipe, and the diphenyl sulfone receiving tank is connected to the first discharge pipe through a second discharge pipe; according to the invention, the first condenser pipe and the second condenser pipe with smaller volume are preset in front of the condenser, so that benzene sulfonyl chloride immediately enters the first pre-cooling pipe and the second pre-cooling pipe after being separated by the large distillation column, and benzene sulfonyl chloride gas with higher temperature is pre-cooled, so that thermal decomposition of benzene sulfonyl chloride is reduced, efficient fractionation is realized, and the purity of fractions is improved.)

1. The production device for preparing the benzene sulfonyl chloride and the diphenyl sulfone by distilling the crude benzene sulfonyl chloride product is characterized by comprising a distillation still, a rectifying column group, a condenser group, a material receiving system and a vacuum pumping system which are sequentially connected through a pipeline; the rectification column group comprises a large rectification column and a small rectification column which are arranged side by side and are communicated with each other, and the top end of the small rectification column is communicated with the head and tail material storage tank;

the condenser group comprises a first precooling pipe, a second precooling pipe and a condenser which are sequentially communicated with each other, and the large rectification column is communicated with the first precooling pipe through a right-angle bent pipe; the bottom of the condenser is provided with a discharge hole, the side walls of one end of the first precooling pipe, the second precooling pipe and the condenser are provided with condensed water inlets, the side wall of the other end of the first precooling pipe is provided with a condensed water outlet, the condensed water inlet of the condenser is communicated with an external water source through a first water passing pipeline, and the condensed water outlet is connected to a water storage tank through a pipeline; a condensed water inlet of the second precooling pipe is communicated to the first water passing pipe through a second water passing pipe, and the condensed water inlet of the first precooling pipe is communicated with a condensed water outlet of the second precooling pipe; a condensed water outlet of the first pre-cooling pipe is connected to the water storage tank through a pipeline;

the material receiving system comprises a benzene sulfonyl chloride receiving tank and a diphenyl sulfone receiving tank; the benzene sulfonyl chloride receiving tank is communicated with the discharge hole through a first discharge pipe, and the diphenyl sulfone receiving tank is connected to the first discharge pipe through a second discharge pipe; the first discharging pipe and the second discharging pipe are respectively provided with a first valve;

the vacuum pumping system comprises a buffer tank and a vacuum pump which are communicated with each other; one end of the buffer tank is communicated with the air outlet of the benzene sulfonyl chloride receiving tank through a pipeline.

2. The apparatus for producing benzenesulfonyl chloride and diphenylsulfone by distilling crude benzenesulfonyl chloride as claimed in claim 1, wherein a stirring shaft is disposed in said distillation still, said stirring shaft extends upward and extends out of said distillation still, and a driving motor is connected to the upper end of said stirring shaft in a transmission manner.

3. The apparatus for producing benzenesulfonyl chloride and diphenylsulfone by distillation of crude benzenesulfonyl chloride as claimed in claim 1, wherein said first water passing pipeline is provided with a second valve, and said second water passing pipeline is provided with a metering pump.

4. The apparatus for producing benzenesulfonyl chloride and diphenylsulfone by distillation of crude benzenesulfonyl chloride as claimed in claim 1, wherein said distillation still is an enamel still.

5. The apparatus for producing benzenesulfonyl chloride and diphenylsulfone by distillation of crude benzenesulfonyl chloride as claimed in claim 1, wherein said distillation still is equipped with a jacket, and an electric heating tube is disposed in said jacket.

Technical Field

The invention relates to the technical field of benzene sulfonyl chloride production, and particularly relates to a production device for preparing benzene sulfonyl chloride and diphenyl sulfone by distilling a crude benzene sulfonyl chloride product.

Background

Benzenesulfonyl chloride is a dye and a medical intermediate, distillation is a key process for producing high-quality benzenesulfonyl chloride, and the following problems often occur in the distillation operation. Firstly, the distillation temperature is mainly determined by the absolute pressure in the distillation kettle, and in the case of the absolute pressure being too high, if the substances are absolutely separated, the heating temperature is often too high, so that the benzene sulfonyl chloride is easy to be locally decomposed at high temperature, and some impurities with high boiling point are gasified, so that the produced benzene sulfonyl chloride is impure, and even the color of the product turns yellow, and the expected distillation effect cannot be achieved.

Disclosure of Invention

The invention aims to solve the defects of the prior art and provides a production device for preparing benzene sulfonyl chloride and diphenyl sulfone by distilling a crude benzene sulfonyl chloride product.

The production device for preparing the benzene sulfonyl chloride and the diphenyl sulfone by distilling the crude benzene sulfonyl chloride product is characterized by comprising a distillation still, a rectifying column group, a condenser group, a material receiving system and a vacuum pumping system which are sequentially connected through a pipeline; the rectification column group comprises a large rectification column and a small rectification column which are arranged side by side and are communicated with each other, and the top end of the small rectification column is communicated with the head and tail material storage tank;

the condenser group comprises a first precooling pipe, a second precooling pipe and a condenser which are sequentially communicated with each other, and the large rectification column is communicated with the first precooling pipe through a right-angle bent pipe; the bottom of the condenser is provided with a discharge hole, the side walls of one end of the first precooling pipe, the second precooling pipe and the condenser are provided with condensed water inlets, the side wall of the other end of the first precooling pipe is provided with a condensed water outlet, the condensed water inlet of the condenser is communicated with an external water source through a first water passing pipeline, and the condensed water outlet is connected to a water storage tank through a pipeline; a condensed water inlet of the second precooling pipe is communicated to the first water passing pipe through a second water passing pipe, and the condensed water inlet of the first precooling pipe is communicated with a condensed water outlet of the second precooling pipe; a condensed water outlet of the first pre-cooling pipe is connected to the water storage tank through a pipeline;

the material receiving system comprises a benzene sulfonyl chloride receiving tank and a diphenyl sulfone receiving tank; the benzene sulfonyl chloride receiving tank is communicated with the discharge hole through a first discharge pipe, and the diphenyl sulfone receiving tank is connected to the first discharge pipe through a second discharge pipe; the first discharging pipe and the second discharging pipe are respectively provided with a first valve;

the vacuum pumping system comprises a buffer tank and a vacuum pump which are communicated with each other; one end of the buffer tank is communicated with the air outlet of the benzene sulfonyl chloride receiving tank through a pipeline.

Preferably, a stirring shaft is arranged in the distillation kettle, the stirring shaft extends upwards and extends out of the distillation kettle, and the upper end of the stirring shaft is connected with a driving motor in a transmission manner.

Preferably, the first water passing pipeline is provided with a second valve, and the second water passing pipeline is provided with a metering pump.

Preferably, the distillation kettle shell is an enamel kettle.

Preferably, the distillation kettle is provided with a jacket, and an electric heating pipe is arranged in the jacket.

Has the advantages that:

(1) the invention relates to a benzene sulfonyl chloride distillation device, which is characterized in that a first condenser pipe and a second condenser pipe with small volumes are preset in front of a condenser, so that benzene sulfonyl chloride immediately enters a first precooling pipe and a second precooling pipe after being separated by a large distillation column, benzene sulfonyl chloride gas with high temperature is precooled, thermal decomposition of benzene sulfonyl chloride is reduced, efficient fractionation is realized, and the purity of fractions is improved;

(2) by arranging a vacuum system, the distillation temperature can be obviously reduced, the thermal decomposition of benzene sulfonyl chloride is further reduced, and a high-purity product can be separated, so that the economic benefit of the process is improved.

Drawings

FIG. 1 is a schematic structural diagram of a production apparatus for distilling crude benzenesulfonyl chloride to prepare benzenesulfonyl chloride and diphenylsulfone;

1-distillation still, 11-stirring shaft, 12-driving motor, 13-jacket, 2-rectification column group, 21-large rectification column, 22-small rectification column, 23-head tailing storage tank, 3-condenser group, 31-first precooling pipe, 32-second precooling pipe, 33-condenser, 34-first water passing pipe, 341-second valve, 35-second water passing pipe, 351-metering pump, 4-material receiving system, 41-benzenesulfonyl chloride receiving tank, 42-diphenylsulfone receiving tank, 43-first discharging pipe, 44-second discharging pipe, 45-first valve, 5-vacuumizing system, 51-buffer tank, 52-vacuum pump and 6-water storage tank.

Detailed Description

For the purpose of enhancing the understanding of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.

Referring to fig. 1, the invention provides a production device for preparing benzenesulfonyl chloride and diphenylsulfone by distilling a benzenesulfonyl chloride crude product, which comprises a distillation still 1, a rectification column group 2, a condenser group 3, a material receiving system 4 and a vacuum pumping system 5 which are sequentially connected through a pipeline; the rectifying column group 2 comprises a large rectifying column 21 and a small rectifying column 22 which are arranged side by side and are communicated with each other, and the top end of the small rectifying column 22 is communicated with a head tailing material storage tank 23;

the condenser group 3 comprises a first precooling pipe 31, a second precooling pipe 32 and a condenser 33 which are communicated with each other in sequence, and the large rectifying column 21 is communicated with the first precooling pipe 31 through a straight-angle bent pipe; a discharge hole is formed in the bottom of the condenser 33, a condensed water inlet is formed in each of the side walls of one end of the first pre-cooling pipe 31, the second pre-cooling pipe 32 and the condenser 33, a condensed water outlet is formed in the side wall of the other end of the first pre-cooling pipe 33, the condensed water inlet of the condenser 33 is communicated with an external water source through a first water passing pipe 34, and the condensed water outlet is connected to the water storage tank 6 through a pipeline; the condensed water inlet of the second precooling pipe 32 is communicated to the first water passing pipe 34 through a second water passing pipe 35, and the condensed water inlet of the first precooling pipe 31 is communicated with the condensed water outlet of the second precooling pipe; the condensed water outlet of the first pre-cooling pipe 31 is connected to the water storage tank 6 through a pipeline;

the material receiving system 4 comprises a benzene sulfonyl chloride receiving tank 41 and a diphenyl sulfone receiving tank 42; the benzene sulfonyl chloride receiving tank 41 is communicated with the discharge port through a first discharge pipe 43, and the diphenyl sulfone receiving tank 42 is connected to the first discharge pipe 43 through a second discharge pipe 44; the first discharging pipe 43 and the second discharging pipe 44 are both provided with a first valve 45;

the vacuumizing system 5 comprises a buffer tank 51 and a vacuum pump 52 which are communicated with each other; one end of the buffer tank 51 is communicated with the air outlet of the benzene sulfonyl chloride receiving tank 41 through a pipeline.

In the above technical scheme, a stirring shaft 11 is arranged in the distillation still 1, the stirring shaft 11 extends upwards and extends out of the distillation still 1, and the upper end of the stirring shaft 11 is connected with a driving motor 12 in a transmission manner.

In the above technical solution, the first water passing pipe 34 is provided with a second valve 341, and the second water passing pipe 35 is provided with a metering pump 351.

In the technical scheme, the shell of the distillation kettle 1 is an enamel kettle.

In the above technical scheme, the distillation still is provided with a jacket 13, and an electric heating pipe is arranged in the jacket 13.

During the use, add crude benzene sulfonyl chloride to the stills casing through the feed inlet, press from both sides the cover type heater and heat crude benzene sulfonyl chloride with coil type heater together for the distillation time shortens, has improved efficiency, and the agitator begins work simultaneously, makes crude benzene sulfonyl chloride be heated more evenly. The impurity mainly contained in the crude benzene sulfonyl chloride is phenyl sulfone, the boiling point of the phenyl sulfone is higher than that of the benzene sulfonyl chloride, when the temperature reaches about 220 ℃, the benzene sulfonyl chloride is gasified and enters a condensing device from a gas outlet, the phenyl sulfone at the bottom of a distillation kettle shell is discharged from a discharge port, and the distillation of the benzene sulfonyl chloride is finished.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.