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System and process for continuously preparing 4-methyl-5-chlorobenzenesulfonic acid

Pending Publication Date: 2022-12-02
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The existing 4-methyl-5-chlorobenzenesulfonic acid production process at home and abroad generally adopts kettle type or tower type reaction device. This type of reactor has many obvious defects, such as poor gas-liquid mixing effect, low uniformity, The chlorine utilization rate is not high, the product yield is low, etc.
Chinese patent CN109369469A provides a method for preparing CLT acid chlorides by continuous reaction in a spray loop. Although the method utilizes an injector to mix chlorine gas with materials, the residence time of chlorine gas is short, and the reaction of chlorine gas is not complete, resulting in the generation of chlorine gas. waste
[0005] For traditional jet loop reactors, the aspect ratio of the loop reactor usually needs to be more than seven times during the industrial scale-up process. For large-scale loop reactors, too high aspect ratio will make the liquid level too high. High, the flow resistance is too large, the required mass transfer kinetic energy is large, so the energy consumption will increase accordingly, and the mass transfer effect will also be reduced, which will easily cause uneven distribution of the gas phase

Method used

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  • System and process for continuously preparing 4-methyl-5-chlorobenzenesulfonic acid
  • System and process for continuously preparing 4-methyl-5-chlorobenzenesulfonic acid
  • System and process for continuously preparing 4-methyl-5-chlorobenzenesulfonic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The volume flow rate of the raw material liquid (the volume ratio of p-toluenesulfonic acid and concentrated sulfuric acid is 1:1) entering the liquid phase inlet of injector 15 is v 0 =7.68m 3 / h, where the molar flow rate of p-toluenesulfonic acid F A0 is 1.39mol / s, the molar flow rate of the chlorine gas that enters injector 15 gas phase inlets is 1.45mol / s, the average temperature of the lower fully mixed reaction section is 78°C, and the average temperature of the upper circulation reaction section is 75°C, p-toluenesulfonic acid and Chlorine reaction rate-r A =3.65mol / m 3 s (the reaction rate when the reaction temperature is 78°C), the conversion rate X of the lower fully mixed reaction section is taken as 0.7, the inner diameter R of the cylinder 11 is taken as 0.5m, the number n of the guide tubes in the upper and lower regions is 4, and the lower The volume of the fully mixed reaction section is given by the formula, Calculate V=0.267m 3 , the calculated ...

Embodiment 2

[0048] The process parameters, operation method and structure size of the jet loop reactor 1 of the present embodiment are the same as those of the embodiment 1, except that the radius of the arc structure is 0.3 as the ratio r / R to the radius of the cylinder 11, such as Figure 5 As shown in b, through the simulated streamline diagram, it can be seen that there is almost no vortex at the edge of the arc, and a small-scale vortex appears at the bottom of the draft tube. According to the equation Obtain the dead zone volume fraction α = 1.46%

[0049] After the start-up of the entire process system is stable, sampling and analysis are carried out at the outlet of the top material, and analysis and detection are carried out by high-performance liquid chromatography. The conversion rate of p-toluenesulfonic acid is 98.1%, and the yield of the product 4-methyl-5-chlorobenzenesulfonic acid is was 96.1%.

Embodiment 3

[0051] The process parameters, operation method and structure size of the jet loop reactor 1 of the present embodiment are the same as those of the embodiment 1, except that the radius of the arc structure is 0.4 as the ratio r / R to the radius of the cylinder body 11, such as Figure 5 As shown in c, it can be seen from the simulated streamline diagram that almost no vortex can be seen near the partition, according to the equation A dead zone volume fraction α = 0.82% is obtained.

[0052] After the start-up of the whole process system is stable, sampling and analysis are carried out at the outlet of the top material, and analysis and detection are carried out by high-performance liquid chromatography. The conversion rate of p-toluenesulfonic acid is 98.8%, and the yield of product 4-methyl-5-chlorobenzenesulfonic acid is was 96.5%.

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Abstract

The invention discloses a system and a process for continuously preparing 4-methyl-5-chlorobenzenesulfonic acid, the system comprises a jet loop reactor, a circulating pump, a feed pump, a heat exchanger, a gas-liquid separator, a spray absorption tower, a liquid delivery pump and a crude product tank, a discharge port at the lower end of the jet loop reactor is sequentially connected with the circulating pump and the heat exchanger; an outlet of the heat exchanger is connected with a feed port of the jet loop reactor to form a circulation loop, a discharge port at the upper end of the jet loop reactor is connected with the gas-liquid separator through a pipeline, a discharge port at the lower end of the gas-liquid separator is connected with the crude product tank through a pipeline, and a side discharge port of the gas-liquid separator is connected with the spray absorption tower; the liquid delivery pump is connected with the spray absorption tower to form a circulating spray loop, and the barrel of the jet loop reactor is divided into an upper loop reaction section and a lower complete mixing reaction section through a partition plate. By optimizing the structural design of the jet loop reactor, the effects of fully mixing gas and liquid and controlling the chlorination depth are achieved, the product yield is high, and the selectivity is good.

Description

technical field [0001] The invention belongs to the technical field of preparation of 4-methyl-5-chlorobenzenesulfonic acid, and in particular relates to a system and a process for continuously preparing 4-methyl-5-chlorobenzenesulfonic acid. Background technique [0002] 4-Methyl-5-chlorobenzenesulfonic acid is an intermediate product of acid synthesis, and it is usually prepared industrially with p-toluenesulfonic acid and chlorine as raw materials and concentrated sulfuric acid as a medium. In this chlorination reaction, the methyl group and the sulfonic acid group have the same positioning effect, so the chlorination can only occur at the ortho position of the methyl group, so the formation of isomers is not considered. The chlorination of p-toluenesulfonic acid belongs to the substituting halogenation on the aromatic ring, and the most important factor affecting the formation of m-chloro-p-toluenesulfonic acid is the control of the chlorination depth and reaction temper...

Claims

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Application Information

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IPC IPC(8): B01J19/00B01J19/26B01J10/00B01D53/14B01D53/18C01B7/07C07C303/22C07C309/39
CPCB01J19/26B01J19/0053B01J19/0013B01J10/00B01D53/1418B01D53/145B01D53/1456B01D53/18C01B7/0706C07C303/22B01D2258/02B01D2257/2045C07C309/39Y02P20/10
Inventor 杨阿三邓家毅李琰君贾继宁屠美玲张建庭程榕郑燕萍
Owner ZHEJIANG UNIV OF TECH