阅读说明：本技术 一种对甲砜基甲苯的制备方法以及设备 (Preparation method and equipment of p-methylsulfonyl toluene ) 是由 袁源 朱宏菲 杨华春 张云云 熊攀 于 2020-07-31 设计创作，主要内容包括：本发明涉及一种对甲砜基甲苯的制备方法以及设备,所述方法包括：将亚硫酸钠、碳酸氢钠、水配制成水溶液,将对甲苯磺酰氯升温至70-90℃；将亚硫酸钠、碳酸氢钠的水溶液和升温后的对甲苯磺酰氯通入一级反应器反应；将氯乙酸钠溶解于水中配制成水溶液,将一级反应后的物料和氯乙酸钠水溶液通入二级反应器反应；反应完成后,进行气液分离,将液体反应物料中加入盐酸调节PH值；将反应物料冷却至室温、抽滤、水洗、抽干,干燥得白色固体为对甲砜基甲苯；所述设备包括一级反应器、二级反应器、配制釜、中间槽、缓冲槽以及氯乙酸钠配制釜。本发明所述方法连续稳定、易于操作,设备占地小,自动化程度高,单位时间产量大大增加。(The invention relates to a preparation method and equipment of p-methylsulfonyl toluene, wherein the method comprises the following steps: preparing sodium sulfite, sodium bicarbonate and water into an aqueous solution, and heating paratoluensulfonyl chloride to 70-90 ℃; introducing an aqueous solution of sodium sulfite, sodium bicarbonate and heated p-toluenesulfonyl chloride into a primary reactor for reaction; dissolving sodium chloroacetate in water to prepare an aqueous solution, and introducing the material subjected to the first-stage reaction and the aqueous solution of sodium chloroacetate into a second-stage reactor for reaction; after the reaction is finished, carrying out gas-liquid separation, and adding hydrochloric acid into the liquid reaction material to adjust the pH value; cooling the reaction material to room temperature, carrying out suction filtration, washing with water, carrying out suction drying, and drying to obtain a white solid, namely p-methylsulfonyl toluene; the equipment comprises a primary reactor, a secondary reactor, a preparation kettle, a middle tank, a buffer tank and a sodium chloroacetate preparation kettle. The method of the invention has the advantages of continuous and stable operation, easy operation, small occupied area of equipment, high automation degree and greatly increased yield in unit time.)

1. A preparation method of p-methylsulfonyl toluene is characterized in that: the method comprises the following steps:

the first step is as follows: preparing sodium sulfite, sodium bicarbonate and water into an aqueous solution, and heating paratoluensulfonyl chloride to 70-90 ℃;

the second step is that: introducing an aqueous solution of sodium sulfite, sodium bicarbonate and heated p-toluenesulfonyl chloride into a primary reactor for reaction;

the third step: dissolving sodium chloroacetate in water to prepare an aqueous solution, and introducing the material subjected to the first-stage reaction and the aqueous solution of sodium chloroacetate into a second-stage reactor for reaction;

the fourth step: after the reaction is finished, carrying out gas-liquid separation, and adding hydrochloric acid into the liquid reaction material to adjust the pH value;

the fifth step: and cooling the reaction material to room temperature, carrying out suction filtration, washing with water, carrying out suction drying, and drying to obtain a white solid, namely the p-methylsulfonyl toluene.

2. The method for preparing p-methylsulfonyltoluene according to claim 1, wherein: in the first step, 70-90g of sodium sulfite, 60-90g of sodium bicarbonate and 250-350g of water are prepared into an aqueous solution.

3. The method for preparing p-methylsulfonyltoluene according to claim 1, wherein: in the second step, the reaction time is 1.5-4 h.

4. The method for preparing p-methylsulfonyltoluene according to claim 1, wherein: in the third step, 70-80g of sodium chloroacetate is dissolved in 45-60g of water to prepare an aqueous solution.

5. The method for preparing p-methylsulfonyltoluene according to claim 1, wherein: in the third step, the sodium chloroacetate aqueous solution reacts with the material obtained after the reaction in the first-stage reactor for 5-6 hours at the temperature of 90-100 ℃ in the second-stage reactor.

6. The preparation equipment of the p-methylsulfonyl toluene is characterized by comprising a primary reactor (1), a secondary reactor (2), a preparation kettle (3), an intermediate tank (4), a buffer tank (5) and a sodium chloroacetate preparation kettle (6), wherein two material inlets of the primary reactor (1) are respectively connected with the preparation kettle (3) and the intermediate tank (4) through a pipeline and a pump body, and the preparation kettle (3) is used for preparing sodium sulfite and a sodium bicarbonate water solution; the middle tank (4) is used for containing tosyl chloride; the material exit linkage of first order reactor (1) has buffer slot (5), during material after first order reactor (1) reaction flowed into buffer slot (5), still include sodium chloroacetate and prepare cauldron (6), the material export that cauldron (6) were prepared to buffer slot (5) and sodium chloroacetate is through pump body and tube coupling to second order reactor (2), the exit linkage of second order reactor (2) has vapour and liquid separator (7), the exit linkage of vapour and liquid separator (7) has acidizing cauldron (8), the exit linkage of acidizing cauldron (8) has filter (9).

7. The p-methylsulfonyltoluene production apparatus according to claim 6, wherein the intermediate tank (4) is provided with a heating device and a temperature sensor.

8. The apparatus for preparing p-methylsulfonyltoluene according to claim 6, wherein the first stage reactor (1) and the second stage reactor (2) are pipeline reactors.

Technical Field

The invention relates to the technical field of pesticides, in particular to a preparation method and equipment of p-methylsulfonyl toluene.

Background

The p-methylsulfonyl toluene is an important organic medicine raw material. The crystal is light brown powdery crystal, has a melting point of 86-88 ℃, is insoluble in water and is soluble in common organic solvents. It is an important intermediate of novel broad-spectrum antibiotics thiamphenicol and thiamphenicol glycine ester hydrochloride. Because thiamphenicol and the derivative glycine ester hydrochloride have low toxicity and small side effect; has long curative effect, good antibacterial effect and antibacterial activity more than 6 times stronger than that of chloramphenicol. The use of antibiotics in immunosuppressive states and as food, feed additives and the like has been widely permitted abroad, and the demand has grown year by year.

The existing p-methylsulfonyl toluene adopts a kettle type batch reaction, namely sodium sulfite, sodium bicarbonate, sodium chloroacetate, water and the like are put into a reaction kettle, and after reacting for more than ten hours, the p-methylsulfonyl toluene is obtained by acidification and filtration.

The process has the advantages of long reaction time, small yield per unit time, large equipment quantity and complex operation, and the invention is provided for solving the problem.

Disclosure of Invention

The invention aims to provide a preparation method of p-methylsulfonyl toluene aiming at the defects in the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of p-methylsulfonyl toluene comprises the following steps:

the first step is as follows: preparing sodium sulfite, sodium bicarbonate and water into an aqueous solution, and heating paratoluensulfonyl chloride to 70-90 ℃;

the second step is that: introducing the aqueous solution in the first step and the p-toluenesulfonyl chloride heated in the second step into a first-stage reactor for reaction;

the third step: dissolving sodium chloroacetate in water to prepare an aqueous solution, and introducing a reaction solution obtained after the first-stage reaction and the aqueous solution of sodium chloroacetate into a second-stage reactor for reaction;

the fourth step: after the reaction is finished, carrying out gas-liquid separation, and adding hydrochloric acid into the liquid to adjust the pH value;

the fifth step: cooling to room temperature, carrying out suction filtration, washing with water, carrying out suction drying, and drying to obtain a white solid, namely the p-methylsulfonyl toluene.

Further, in the first step, 70-90g of sodium sulfite, 60-90g of sodium bicarbonate and 250-350g of water are prepared into an aqueous solution.

Furthermore, in the second step, the reaction time is 1.5-4 h.

Further, in the third step, 70-80g of sodium chloroacetate is dissolved in 45-60g of water to prepare an aqueous solution.

Furthermore, in the third step, the sodium chloroacetate aqueous solution reacts with the materials obtained after the reaction in the first-stage reactor for 5-6 hours at the temperature of 90-100 ℃ in the second-stage reactor.

The gas-liquid separation process separates CO generated in the reaction process₂And (5) discharging and collecting.

The invention aims to provide a preparation device of p-methylsulfonyl toluene.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation device of p-methylsulfonyl toluene comprises a primary reactor, a secondary reactor, a preparation kettle, an intermediate tank, a buffer tank, a sodium chloroacetate preparation kettle, a gas-liquid separator and a filter, wherein two material inlets of the primary reactor are respectively connected with the preparation kettle and the intermediate tank through a pipeline and a pump body, and the preparation kettle is used for preparing sodium sulfite and sodium bicarbonate water solution; the middle tank is used for containing tosyl chloride; the material exit linkage of first order reactor has the dashpot, during the material after the first order reactor reaction flowed into the dashpot, still includes sodium chloroacetate and prepares the cauldron, the material export that the cauldron was prepared to dashpot and sodium chloroacetate is through pump body and tube coupling to second order reactor, the exit linkage of second order reactor has vapour and liquid separator, vapour and liquid separator's exit linkage has the acidizing cauldron, the exit linkage of acidizing cauldron has the filter.

The gas-liquid separator separates CO generated in the reaction process₂And (4) a discharge device.

Further, the intermediate tank is provided with a heating device and a temperature sensor for heating the tosyl chloride and measuring the temperature thereof.

Further, the primary reactor and the secondary reactor are pipeline reactors.

Has the advantages that:

1. the method has the advantages of stable process, easy operation, small occupied area of equipment, high automation degree and greatly increased yield per unit time.

2. The equipment provided by the invention can realize stable and continuous reaction of the preparation method of the p-methylsulfonyl toluene, is easy to operate and takes less time.

Drawings

FIG. 1 is a schematic structural diagram of a preparation device of p-methylsulfonyltoluene.

In the figure: 1-a first stage reactor; 2-a secondary reactor; 3-preparing a kettle; 4-an intermediate tank; 5-a buffer tank; 6-sodium chloroacetate preparation kettle; 7-gas-liquid separator; 8-acidifying the kettle; 9-a filter.

Detailed Description

The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.