CN111909064B - Method for preparing perchloromethylmercaptan by using microchannel reactor - Google Patents

Method for preparing perchloromethylmercaptan by using microchannel reactor Download PDF

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CN111909064B
CN111909064B CN202010744107.2A CN202010744107A CN111909064B CN 111909064 B CN111909064 B CN 111909064B CN 202010744107 A CN202010744107 A CN 202010744107A CN 111909064 B CN111909064 B CN 111909064B
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microchannel reactor
chlorine
perchloromethylmercaptan
reaction
microchannel
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CN111909064A (en
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王文博
杜孟成
马德龙
吕寻伟
王燕婷
崔亭亭
王庆振
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Shandong Yanggu Huatai Chemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C313/00—Sulfinic acids; Sulfenic acids; Halides, esters or anhydrides thereof; Amides of sulfinic or sulfenic acids, i.e. compounds having singly-bound oxygen atoms of sulfinic or sulfenic groups replaced by nitrogen atoms, not being part of nitro or nitroso groups
    • C07C313/08—Sulfenic acids; Derivatives thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/45—Compounds containing sulfur and halogen, with or without oxygen
    • C01B17/4507—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only
    • C01B17/4538—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only containing sulfur and chlorine only
    • C01B17/4546—Sulfur dichloride
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C381/00—Compounds containing carbon and sulfur and having functional groups not covered by groups C07C301/00 - C07C337/00

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Abstract

The invention discloses a method for preparing perchloromethylmercaptan by using a microchannel reactor. The invention utilizes microchannel reaction to smoothly complete the work which can not be completed under the conventional path, greatly shortens the reaction time, is carried out under the anhydrous condition in the whole process, has almost zero three-waste discharge, good environmental protection property, higher safety, higher selectivity of target products, higher conversion rate of reaction and stable quality of products, and is beneficial to the amplification production.

Description

Method for preparing perchloromethylmercaptan by using microchannel reactor
Technical Field
The invention relates to a preparation method of perchloromethylmercaptan, in particular to an environment-friendly and efficient method for preparing perchloromethylmercaptan by using a microchannel reactor, and belongs to the technical field of synthesis of perchloromethylmercaptan.
Background
Perchloromethanethiol is an important organic chemical raw material for synthesizing rubber scorch retarder V.E (i.e., scorch retarder E), and can be widely used in the rubber auxiliary synthesis field and the agrochemical field as a raw material of sterilizing agent captan or folpet.
Rubber scorch occurs during storage and processing. Scorching of the compound is one of the most common problems in rubber processing. The scorch retarder E has a strong scorch retarding ability. In particular, the compounding agents (such as reinforcing resin, m-methyl white system adhesive, fine particle carbon black and the like) which cause scorching are compounded in the modern high-temperature, quick and high-efficiency processing technology, so that the scorching problem is easier to occur. Therefore, the rubber scorch retarder becomes an important auxiliary agent for the safety of rubber processing.
At present, the mature process for synthesizing perchloromethylmercaptan is not much, and the reaction is usually finished when the density in a lower organic phase reaches more than 1.7 by reacting chlorine and carbon disulfide in a conventional reaction kettle and continuously introducing the chlorine into the carbon disulfide in a hydrochloric acid washing environment. This conventional synthesis requires a large amount of chlorine to be fed in, because there are a large number of side reactions during the reaction, which greatly increases the amount of chlorine consumed. In the reaction process, sulfur monochloride byproducts are generated, more byproducts are generated in the water environment by the sulfur monochloride, acid-containing wastewater which is difficult to treat is generated, and the post-treatment is complicated and difficult. The redundant chlorine gas of reaction needs to be absorbed by tail gas, and the tail gas absorption needs to consume a large amount of liquid alkali, thereby increasing the generation of waste water. The obtained product has more impurities, and the purity and appearance of the product are affected.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing perchloromethylmercaptan by using a microchannel reactor, which only needs two raw materials of carbon disulfide and chlorine without solvent and acid, avoids the generation of waste water, has almost zero discharge of three wastes, is carried out in the microchannel reactor, has high reaction conversion rate, high efficiency and high quality of obtained products, and overcomes the problems of poor quality, high production energy consumption, difficult control of three wastes, poor safety and the like of perchloromethylmercaptan products in the existing synthetic method.
The specific technical scheme of the invention is as follows:
a method for preparing perchloromethylmercaptan by using a microchannel reactor comprises the steps of enabling carbon disulfide and chlorine to react in a first microchannel reactor under illumination to obtain mixed liquid of sulfur monochloride and perchloromethylmercaptan, and enabling the mixed liquid to continuously react with the chlorine in a second microchannel reactor under illumination to obtain reaction liquid of the perchloromethylmercaptan and sulfur dichloride. The reaction principle of the invention is as follows:
the reaction in the first microchannel reactor is as follows:
Figure 368309DEST_PATH_IMAGE001
the reaction in the second microchannel reactor is as follows:
Figure 462560DEST_PATH_IMAGE002
the invention obtains the target product through the two-stage microchannel reaction under the condition of no solvent by the microchannel reaction technology, wherein the solvent-free means that no solvent such as water and the like is added in the reaction raw materials in the reaction process, so that the reaction time is greatly shortened, the selectivity of the target product is higher, the conversion rate of the reaction is improved, the quality of the product is stable, the discharge of three wastes is almost zero, and the safety is higher. Meanwhile, the byproduct sulfur dichloride with higher utilization value is generated, and the comprehensive utilization rate of the raw materials is greatly improved.
Further, the first microchannel reactor and the second microchannel reactor are microchannel reactors reported in the prior art, which are also called micro-reactors, and materials continuously flow in the microchannel reactors. In the invention, the used microchannel reactor is provided with an ultraviolet lamp, and the reaction is carried out under the ultraviolet light, thereby playing a role of activating chlorine and providing conditions for the reaction. The ultraviolet wavelength emitted by the ultraviolet lamp is preferably 350-365 nm.
Further, in order to improve the purity of the product and avoid the introduction of impurities, the carbon disulfide and chlorine gas are preferably filtered and dried before entering the microchannel reactor to remove solid impurities and water in the raw materials. The filtration may be achieved by a filtration device and the drying may be achieved by a water absorbing agent, such as anhydrous calcium chloride or the like.
Further, before the carbon disulfide is introduced into the microchannel reactor, the temperature of the carbon disulfide is firstly reduced to be below 18 ℃ below zero, and preferably is reduced to be between 18 ℃ below zero and 20 ℃ below zero.
Further, chlorine gas enters the microchannel reactor in the form of gas. In actual production, chlorine gas is generally stored in the form of liquid chlorine, and in order to ensure safety and feasibility, the liquid chlorine is gasified and then enters a chlorine gas buffer tank, and then enters the microchannel reactor from the chlorine gas buffer tank. The pressure in the chlorine buffer tank is optimally kept below 0.1Mpa to ensure the safety, and the pressure control in the chlorine buffer tank can be realized through a self-control valve. And when the pressure in the chlorine buffer tank is higher than 0.1MPa, the self-control valve is closed. When the air pressure in the buffer tank is lower than 0.1MPa, the automatic control valve is opened. When the pressure in the buffer tank is higher than 0.05Mpa, the micro-channel reactor can be started to be introduced.
Further, in the first microchannel reactor, the carbon disulfide and chlorine gas are mixed in a ratio of 1: 2.5-5, and the molar ratio can be ensured by controlling the introduction amount and the introduction speed of the carbon disulfide and the chlorine. The residence time of the reaction materials in the first microchannel reactor can be adjusted according to the size of the first microchannel reactor, so that the sufficient residence time of the materials is ensured, and the carbon disulfide and the chlorine can be fully reacted to form the sulfur monochloride and the perchloromethylmercaptan.
Further, in a specific embodiment of the present invention, the inner diameter of the first microchannel reactor is 2 to 8mm, the length of the first microchannel reactor is 10 to 50m, and the flow velocity of the material in the first microchannel reactor is 20 to 50 g/min.
Further, in the first microchannel reactor, the reaction temperature of the material is-18 ℃ or lower, for example, -18 to-20 ℃. The low-temperature reaction is beneficial to reducing the occurrence of side reactions and improving the selectivity of raw materials.
Further, in the second microchannel reactor, the mixed solution and the chlorine gas are mixed according to the ratio of the sulfur monochloride and the chlorine gas in the mixed solution of 1: 1-2, and the molar ratio can be ensured by controlling the feeding amount and the feeding speed of the mixed solution and the chlorine. The residence time of the reaction materials in the second microchannel reactor can be adjusted according to the size of the second microchannel reactor, so that the materials have enough residence time, and the sulfur monochloride and the chlorine can be fully reacted to form the sulfur dichloride.
Further, in a specific embodiment of the present invention, the inner diameter of the second microchannel reactor is 4 to 10mm, the length of the second microchannel reactor is 5 to 20m, and the flow velocity of the material in the second microchannel reactor is 40 to 60 g/min.
Furthermore, in the second microchannel reactor, the reaction temperature of the materials is 30-40 ℃.
Further, the reaction solution flowing out of the second microchannel contains perchloromethane and sulfur dichloride, and because the boiling points of the perchloromethane and the sulfur dichloride are different greatly, the perchloromethane and the sulfur dichloride can be easily and completely separated by common distillation, reduced pressure distillation, rectification and the like.
Further, in a specific embodiment of the present invention, after the reaction is completed, the reaction solution is rectified, the collected fraction is byproduct sulfur dichloride, and when the density of the remaining reaction solution is greater than 1.70, the rectification is stopped, so as to obtain a pure perchloromethylmercaptan product. The sulfur dichloride byproduct obtained by the method is also an important chemical product, can be directly sold or used in other chemical synthesis, and has higher economic value.
Further, the invention provides a specific preparation method of perchloromethylmercaptan, which comprises the following steps:
1. carbon disulphide is passed over CS 2 And (3) a filter (filled with anhydrous calcium chloride) is used for removing water and solid impurities in the carbon disulfide, and then the temperature is reduced to-18 ℃, so that the carbon disulfide can enter the first microchannel reactor.
2. And (3) introducing the liquid chlorine in the liquid chlorine storage tank into a chlorine vaporizer through a self-control valve, gasifying the liquid chlorine, and introducing the gasified liquid chlorine into a chlorine cache tank, wherein the self-control valve is closed when the pressure in the chlorine cache tank is higher than 0.1 MPa. When the air pressure in the buffer tank is lower than 0.1MPa, the automatic control valve is opened. When the pressure in the buffer tank is higher than 0.05MPa, a chlorine filter (for removing possible solid impurities in the chlorine) can be started to enter the micro-channel reactor.
3. Under the irradiation of an ultraviolet lamp, controlling the temperature in the first microchannel reactor to be not higher than-18 ℃, reacting after quantitatively adding carbon disulfide and chlorine, and controlling the molar ratio of the chlorine to the carbon disulfide entering the microchannel reactor to be 1: 2.5 to 5.
4. After the reaction, the material flows into a first-stage micro-reaction storage tank, and the temperature of the storage tank is kept at 30 ℃ through a water bath. Quantitatively pumping the materials in the storage tank into a secondary microchannel reactor through a metering pump, reacting the materials with introduced chlorine under the irradiation of an ultraviolet lamp, and controlling the temperature in the secondary microchannel reactor to be 30-40 ℃. Controlling the theoretical value of the sulfur monochloride in the mixed solution and chlorine according to the ratio of 1: 1-2 mol ratio.
5. After the reaction in the secondary microchannel reactor is finished, the material enters a secondary micro-reaction storage tank for temporary storage. The material is pumped into a rectifying device by a metering pump for rectification, the temperature at the bottom of the tower is controlled at 72 ℃, 60 ℃ fraction at the top of the tower is collected and enters SCl through a pipeline 2 And (4) storing in a storage tank. And collecting the tower bottom mother liquor when the density is more than or equal to 1.70 to obtain perchloromethylmercaptan with the purity higher than 98%, and conveying the perchloromethylmercaptan into a perchloromethylmercaptan storage tank through a pipeline for storage.
The method comprises the steps of pumping carbon disulfide into a first microchannel reactor, reacting with chlorine in the first microchannel reactor under illumination to generate perchloromethylmercaptan and sulfur monochloride, and reacting the generated perchloromethylmercaptan and sulfur monochloride with chlorine in a second microchannel reactor under illumination to finally obtain a reaction solution of sulfur dichloride and perchloromethylmercaptan. The boiling point difference between the sulfur dichloride and the perchloromethylmercaptan in the reaction liquid is large, and the sulfur dichloride and the perchloromethylmercaptan can be easily and thoroughly separated by distillation, rectification and other modes. The invention has the following beneficial effects:
1. the invention designs the microchannel reaction, the whole process is carried out under the anhydrous condition, the discharge of three wastes is almost zero, and the environmental protection property is good.
2. Through the control to the proportion of letting in and the temperature of material, can accomplish the work that can't accomplish under the conventional route smoothly, shortened reaction time greatly, the selectivity of target product is higher, and the conversion rate of reaction is higher, and the quality of gained product is stable, is favorable to enlarging production, and the security is higher.
3. Carbon disulfide and chlorine pass through filter equipment before entering the microreactor, and the water absorbent is arranged in the filter, and water and solid impurities which may exist are thoroughly removed, so that the whole reaction system is carried out in an anhydrous environment, the decomposition of by-product sulfur monochloride is avoided, and the consumption of chlorine is reduced.
4. In the first microchannel reactor, chlorine is activated under illumination, and reacts with carbon disulfide more rapidly under a low-temperature condition, so that the selectivity is higher and the reaction safety coefficient is higher under the low-temperature reaction. In the second microchannel reactor, chlorine and sulfur monochloride react at 30-40 ℃, so that energy consumption is reduced.
5. After two-stage microchannel reaction, finally obtaining mixed liquid of sulfur dichloride and perchloromethylmercaptan, wherein the boiling point of the sulfur dichloride is 60 ℃, and the boiling point of the perchloromethylmercaptan is 148 ℃. Continuously collecting low-boiling fraction at the tower top through a rectifying tower device to obtain sulfur dichloride, and obtaining a high-purity perchloromethylmercaptan product at the tower bottom, wherein the purity is more than or equal to 98%. The product separation process is simple and efficient, and the post-treatment is simple.
Drawings
FIG. 1 is a process flow diagram for preparing perchloromethylmercaptan according to the invention using a microchannel reactor.
Detailed Description
The present invention may be better understood by reference to the following detailed description, which is intended for purposes of illustration only and is not intended to be limiting.
In the following examples, a first microchannel reactor having an inner diameter of 4mm and a length of 10m was used, and a second microchannel reactor having an inner diameter of 4mm and a length of 6m was used.
Example 1
The preparation process of perchloromethylmercaptan is shown in figure 1, and the specific steps are as follows:
1. and opening a valve of the liquid chlorine storage tank, enabling the liquid chlorine to enter the chlorine gasifier through the self-control valve, enabling the gasified liquid chlorine to enter the chlorine cache tank, and automatically closing the self-control valve when the pressure in the cache tank is higher than 0.1 MPa. When the pressure in the buffer tank is higher than 0.05Mpa, the requirement of chlorine introduction into the micro-channel reactor can be met. The carbon disulfide storage tank is cooled to-18 ℃ through cold brine in the jacket;
2. and adjusting the temperature in the first microchannel reactor, controlling the temperature to be-18 ℃, and turning on an ultraviolet lamp with the ultraviolet wavelength of 360 nm. Chlorine gas is dried by a chlorine gas filter and enters a first micro-channel reactor at a speed of 21.3g/min under the regulation of a flowmeter, and carbon disulfide passes through CS 2 After water is removed by the filter, the mixture enters a first microchannel reactor through a metering pump at the speed of 7.6g/min, and is reacted by the first microchannel reactor to obtain a mixed solution of the sulfur monochloride and the perchloromethylmercaptan, wherein the density of the mixed solution is not lower than 1.68 g/ml. And (3) storing the mixed solution in a first-stage micro-reaction storage tank, and keeping the temperature of the first-stage micro-reaction storage tank at 20 ℃.
3. And adjusting the temperature in the second microchannel reactor, controlling the temperature to be 30 ℃, and turning on an ultraviolet lamp with the ultraviolet wavelength of 360 nm. Chlorine dried by a chlorine filter enters a second microchannel reactor at the speed of 7.1g/min under the control of a flow meter, materials in a primary micro-reaction storage tank are pumped into the second microchannel reactor at the speed of 50.7g/min through a metering pump, reaction is carried out by the second microchannel reactor to obtain reaction liquid of sulfur dichloride and perchloromethylmercaptan, the density of the reaction liquid is not lower than 1.65g/ml, and the reaction liquid enters a secondary micro-reaction storage tank for storage.
4. And (4) introducing the mixture in the secondary micro-reaction storage tank into a rectifying tower for rectification. The temperature of the bottom of the tower is controlled at 72 ℃, and the fraction at 58 ℃ is collected at the top of the tower. When the temperature of the tower top is lower than 58 ℃, raising the temperature of the tower bottom to control the temperature of the tower bottom to be 72-80 ℃. The fraction obtained at the tower top is sulfur dichloride, and the sulfur dichloride enters SCl through a pipeline 2 And (5) collecting by a storage tank. When the temperature at the bottom of the tower is close to 80 ℃, no fraction is distilled out from the top of the tower, after the temperature is continuously reduced, the heating is stopped, after the temperature is reduced to 20 ℃, the sampling detection density is more than or equal to 1.70, a qualified perchloromethylmercaptan product is obtained, and the product enters a perchloromethylmercaptan storage tank through a pipeline for storage. The purity of the perchloromethylmercaptan is 98 percent and the yield is 90 percent by gas phase detection. The purity of sulfur dichloride was 96.5% and the yield was 85%.
Example 2
Perchloromethylmercaptan is prepared as in example 1, except that: in step 3, the temperature in the second microchannel reactor is controlled to be 40 ℃. The purity of the finally obtained perchloromethylmercaptan is 95%, the yield is 85%, the purity of the sulfur dichloride is 97%, and the yield is 90%.
Example 3
Perchloromethylmercaptan is prepared as in example 1, except that: in step 2, the ultraviolet wavelength is 350nm, and in step 3, the ultraviolet wavelength is 350 nm. The purity of the finally obtained perchloromethylmercaptan is 97.5%, the yield is 90.5%, the purity of the sulfur dichloride is 95%, and the yield is 86%.
Example 4
Perchloromethylmercaptan is prepared as in example 1, except that: in step 2, chlorine gas dried by the chlorine gas filter enters the first microchannel reactor at the speed of 30g/min, and carbon disulfide passes through CS 2 After the filter removes water, the water enters the first microchannel reactor at the speed of 7.6 g/min. The purity of the finally obtained perchloromethylmercaptan is 98.9%, the yield is 98.5%, the purity of the sulfur dichloride is 96%, and the yield is 86%.
Example 5
Perchloromethylmercaptan is prepared as in example 1, except that: in the step 3, chlorine dried by the chlorine filter enters the second microchannel reactor at the speed of 13.5g/min, and the material in the primary micro-reaction storage tank is pumped into the second microchannel reactor at the speed of 32.1 g/min. The purity of the final perchloromethylmercaptan is 98.2%, the yield is 90%, the purity of the sulfur dichloride is 98%, and the yield is 90%.
Comparative example 1
Perchloromethylmercaptan is prepared as in example 1, except that: in step 2, chlorine gas dried by the chlorine gas filter enters the first microchannel reactor at the speed of 43g/min, and carbon disulfide passes through CS 2 After being dewatered by the filter, the water enters the first microchannel reactor at the speed of 15.2 g/min. The purity of the finally obtained perchloromethylmercaptan is 98.4 percent, the yield is 78.5 percent, the purity of the sulfur dichloride is 97 percent, and the yield is 65 percent.
Comparative example 2
Perchloromethylmercaptan is prepared as in example 1, except that: in the step 3, chlorine dried by the chlorine filter enters the second microchannel reactor at the speed of 5g/min, and materials in the primary micro-reaction storage tank are pumped into the second microchannel reactor at the speed of 20 g/min. The purity of the finally obtained perchloromethylmercaptan is 97.5%, the yield is 88%, the purity of the sulfur dichloride is 97.5%, and the yield is 65%.
Comparative example 3
Perchloromethylmercaptan is prepared as in example 1, except that: in step 2, the reaction temperature is controlled at-15 ℃, and in step 3, the reaction temperature is controlled at 45 ℃. The purity of the finally obtained perchloromethylmercaptan is 97.8 percent, the yield is 68 percent, the purity of the sulfur dichloride is 97.6 percent, and the yield is 46 percent.

Claims (6)

1. A method for preparing perchloromethylmercaptan by using a microchannel reactor is characterized by comprising the following steps: carbon disulfide and chlorine react in a first microchannel reactor under illumination to obtain a mixed solution of sulfur monochloride and perchloromethylmercaptan, and the mixed solution and chlorine continue to react in a second microchannel reactor under illumination to obtain a reaction solution of perchloromethylmercaptan and sulfur dichloride;
The reaction is carried out under ultraviolet light and without solvent, and in a first microchannel reactor, carbon disulfide and chlorine are reacted according to the weight ratio of 1: 2.5-5 mol ratio; in the second microchannel reactor, the mixed liquor and chlorine gas are mixed according to the ratio of the sulfur monochloride and the chlorine gas in the mixed liquor of 1: 1-2 mol ratio;
the reaction temperature in the first microchannel reactor is less than or equal to-18 ℃, and the reaction temperature in the second microchannel reactor is 30-40 ℃.
2. The method of claim 1, further comprising: the wavelength of the ultraviolet light is 350-365 nm.
3. The method of claim 1, further comprising: the inner diameter of the first microchannel reactor is 2-8 mm, the length of the first microchannel reactor is 10-50 m, and the flow speed of materials in the first microchannel reactor is 20-50 g/min.
4. The method of claim 1, further comprising: the inner diameter of a microchannel in the second microchannel reactor is 4-10 mm, the length of the microchannel is 5-20 m, and the flow speed of materials in the second microchannel reactor is 40-60 g/min.
5. The method of claim 1, further comprising: and filtering and drying the carbon disulfide and the chlorine, and then feeding the carbon disulfide and the chlorine into the microchannel reactor.
6. The method of claim 1, further comprising: the perchloromethanol and sulfur dichloride are separated by a common distillation, reduced pressure distillation or rectification mode.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3331872A (en) * 1964-04-13 1967-07-18 Stauffer Chemical Co Dichloromethanedisulfenyl chloride and its preparation
US3968155A (en) * 1974-06-21 1976-07-06 Produits Chimiques Ugine Kuhlmann Process for prepared perchloromethyl mercaptan by chlorination of carbon disulfide
US3993693A (en) * 1975-07-30 1976-11-23 Olin Corporation Method for producing perchloromethyl mercaptan
CN103360295A (en) * 2012-04-06 2013-10-23 英德广农康盛化工有限责任公司 Device and method for preparing perchloromethylmercaptan
CN106117128A (en) * 2016-06-26 2016-11-16 江苏扬农化工集团有限公司 A kind of micro passage reaction prepares the method for pyridone chlorine addition product continuously
CN206553431U (en) * 2017-02-24 2017-10-13 宁夏格瑞精细化工有限公司 The system of continuous production perchlormethyl
CN109574918A (en) * 2019-01-17 2019-04-05 内蒙古元正精细化工有限责任公司 The method for preparing 2-vhloro-5-chloromethylpyridine using micro passage reaction serialization
CN111233718A (en) * 2020-03-19 2020-06-05 宁夏格瑞精细化工有限公司 Method for continuously synthesizing perchloromethylmercaptan

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3331872A (en) * 1964-04-13 1967-07-18 Stauffer Chemical Co Dichloromethanedisulfenyl chloride and its preparation
US3968155A (en) * 1974-06-21 1976-07-06 Produits Chimiques Ugine Kuhlmann Process for prepared perchloromethyl mercaptan by chlorination of carbon disulfide
US3993693A (en) * 1975-07-30 1976-11-23 Olin Corporation Method for producing perchloromethyl mercaptan
CN103360295A (en) * 2012-04-06 2013-10-23 英德广农康盛化工有限责任公司 Device and method for preparing perchloromethylmercaptan
CN106117128A (en) * 2016-06-26 2016-11-16 江苏扬农化工集团有限公司 A kind of micro passage reaction prepares the method for pyridone chlorine addition product continuously
CN206553431U (en) * 2017-02-24 2017-10-13 宁夏格瑞精细化工有限公司 The system of continuous production perchlormethyl
CN109574918A (en) * 2019-01-17 2019-04-05 内蒙古元正精细化工有限责任公司 The method for preparing 2-vhloro-5-chloromethylpyridine using micro passage reaction serialization
CN111233718A (en) * 2020-03-19 2020-06-05 宁夏格瑞精细化工有限公司 Method for continuously synthesizing perchloromethylmercaptan

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