CN211497434U - Device for continuously preparing 5-amino-1, 2, 3-thiadiazole - Google Patents
Device for continuously preparing 5-amino-1, 2, 3-thiadiazole Download PDFInfo
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- CN211497434U CN211497434U CN201922364966.4U CN201922364966U CN211497434U CN 211497434 U CN211497434 U CN 211497434U CN 201922364966 U CN201922364966 U CN 201922364966U CN 211497434 U CN211497434 U CN 211497434U
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Abstract
The utility model discloses a device for continuously preparing 5-amino-1, 2, 3-thiadiazole, which comprises a preparation kettle, a diazotization tubular reactor, a diazoacetonitrile storage tank, a separator, a cyclization reactor and a flash tank; the diazotization tubular reactor comprises a front-end mixing section and a rear-end reaction section, and a heat exchanger is wound outside the diazotization tubular reactor; the front end mixing section is connected with a discharge port of the preparation kettle, and the upper part of the front end mixing section is provided with a plurality of feed ports; introducing the product of the rear-end reaction section into a diazoacetonitrile storage tank; the discharge hole of the diazoacetonitrile storage tank is connected with the feed inlet of the separator; the organic phase diazoacetonitrile solution of the continuous lower layer of the separator enters a cyclization reactor through a lower layer discharge hole of the separator for cyclization reaction, and the acid phase solution of the upper layer enters a flash tank through an upper layer discharge hole of the separator for concentration; the cyclization reactor is connected to a subsequent purification device for further purification to obtain a finished product of 5-amino-1, 2, 3-thiadiazole; the discharge hole of the flash tank is connected to the feed inlet of the diazotization tubular reactor, and the concentrated product is reused as reaction raw material.
Description
Technical Field
The utility model belongs to the technical field of the chemical industry, a preparation system of organic chemical industry midbody is related to, concretely relates to serialization preparation 5-amino-1, 2, 3-thiadiazole's device.
Background
The 5-amino-1, 2, 3-thiadiazole is an important organic chemical intermediate, is widely applied to synthesis of medicines and agrochemicals, and is a key intermediate for synthesizing lactam antibiotics and plant growth regulator thidiazuron.
In the traditional synthesis, a highly toxic and explosive raw material diazomethane is used, the reaction operation difficulty is high, the requirement on protective equipment is high, volatile diethyl ether is used as a solvent, a large amount of wastewater containing acid and diazonium salt is generated, and the three wastes are serious.
At present, the synthesis methods of 5-amino-1, 2, 3-thiadiazole have various types, generally have long routes, expensive and difficultly obtained raw materials, incapability of recycling mother liquor, more side reactions, low yield, difficult preparation, large discharge amount of three wastes and incapability of quickly forming mass production or industrialization.
Chinese patent CN103058956 adopts sodium nitrite or potassium nitrite solution to carry out diazotization reaction with hydrochloride to obtain diazo acetonitrile mixed solution, and Chinese patent CN 10139281 adopts sodium nitrite water solution to carry out diazotization reaction with aminoacetonitrile sulfate to obtain diazo acetonitrile mixed solution.
In the method, a large amount of salt-containing waste acid is generated, the treatment difficulty is very high, and the difficulty is brought to the model selection, use and maintenance of equipment.
SUMMERY OF THE UTILITY MODEL
The utility model discloses the purpose: the device for continuously preparing the 5-amino-1, 2, 3-thiadiazole is provided, so that diazotization and cyclization can be continuously carried out, no inorganic salt is generated in waste acid after diazotization, and water and organic matters in the waste acid are extracted by flash evaporation steam and then circularly used in a diazotization process.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
a device for continuously preparing 5-amino-1, 2, 3-thiadiazole comprises a preparation kettle, a diazotization tubular reactor, a diazoacetonitrile storage tank, a separator, a cyclization reactor and a flash tank;
the diazotization tubular reactor comprises a front-end mixing section and a rear-end reaction section, and a heat exchanger is wound outside the diazotization tubular reactor; the mixing section at the front end of the diazotization tubular reactor is connected with a discharge port of the preparation kettle, and the upper part of the mixing section is provided with a plurality of feed ports; introducing a reaction section product at the rear end of the diazotization tubular reactor into a diazoacetonitrile storage tank;
the discharge hole of the diazoacetonitrile storage tank is connected with the feed inlet of the separator, and the diazoacetonitrile mixed solution obtained by the reaction is fed into the separator for continuous separation;
the separator continuously separates out the organic phase diazoacetonitrile solution at the lower layer and the acid phase solution at the upper layer, the organic phase diazoacetonitrile solution at the lower layer enters the cyclization reactor through the lower layer discharge hole of the separator for cyclization reaction, and the acid phase solution at the upper layer enters the flash tank through the upper layer discharge hole of the separator for concentration;
the cyclization reactor is connected to a subsequent purification device, and the product is further purified to obtain a finished product of 5-amino-1, 2, 3-thiadiazole;
and a discharge hole of the flash tank is connected to a feed inlet of the diazotization tubular reactor, and a concentrated product is reused as a reaction raw material.
Furthermore, more than one diazotization mature device which is connected in sequence is arranged between the diazotization tubular reactor and the diazoacetonitrile storage tank, and a heat exchanger with a tubular structure is arranged outside the diazotization mature device; the diazotization mature device has the function of ensuring that the diazotization reaction can have sufficient reaction time and ensuring the complete diazotization reaction.
Furthermore, the rear part of the cyclization reactor is connected with more than one cyclization mature kettle which are connected in sequence, and the function of the cyclization mature kettle is to ensure sufficient cyclization reaction time.
Preferably, the cyclization reactor and the cyclization mature kettle are of a vertical structure and are provided with a stirrer, the outer wall of the reactor is provided with a jacket, the discharge port is formed in the side surface of the reactor, and the cyclization reactor and the cyclization mature kettle which are sequentially connected are arranged in a step shape from top to bottom.
Furthermore, more than one cooler connected in sequence is arranged between the discharge hole of the flash tank and the feed inlet of the diazotization tubular reactor and is used for cooling the concentrated product.
Specifically, the heat exchanger wound outside the mixing section at the front end of the diazotization tubular reactor is of a sleeve type structure, the inner pipe is used for conveying materials, and the outer pipe is used for conveying frozen brine.
The heat exchanger wound outside the reaction section at the rear end of the diazotization tubular reactor is of a tubular structure, materials are fed on the tube side, and frozen brine is fed on the shell side.
Has the advantages that:
the utility model discloses a pipeline formula diazotization reactor, continuous type separator and cyclization reactor adopt the stair structure to arrange with the cyclization mature cauldron, realize whole production process serialization, the investment has been practiced thrift greatly, can realize long-range distributed control simultaneously, the essential safety degree of apparatus for producing has been improved, adopt aminoacetonitrile sulfate and nitrosyl sulfuric acid to carry out diazotization reaction, the inorganic salt in the spent acid has been eliminated, the spent acid can retrieval and utilization or other usefulness after the flash distillation concentration treatment, the spent acid pollution difficult problem in the diazoacetonitrile production has thoroughly been solved.
Drawings
These and/or other advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings and the following detailed description.
FIG. 1 is a schematic block diagram of the apparatus for continuously preparing 5-amino-1, 2, 3-thiadiazole.
FIG. 2 is a schematic view of a process for continuously preparing 5-amino-1, 2, 3-thiadiazole.
Wherein each reference numeral represents:
1 preparing a kettle; 2 diazotizing a tubular reactor; 3 a first diazotization mature device; 4 a second nitridation mature device; 5 a third nitridation mature device; 6, a diazoacetonitrile storage tank; 7 circulating pump; 8, a separator; 9 ring closure reactor; 10 a first cyclization maturation kettle; 11, a second ring synthesis cooked kettle; 12 flash tank; 13 a sulfuric acid pump; 14 a first cooler; 15 second cooler.
Detailed Description
The invention will be better understood from the following examples.
The drawings in the specification show the structure, ratio, size, etc. only for the purpose of matching with the content disclosed in the specification, so as to be known and read by those skilled in the art, and not for the purpose of limiting the present invention, so the present invention does not have the essential meaning in the art, and any structure modification, ratio relationship change or size adjustment should still fall within the scope covered by the technical content disclosed in the present invention without affecting the function and achievable purpose of the present invention. Meanwhile, the terms "upper", "lower", "front", "rear", "middle", and the like used in the present specification are for the sake of clarity only, and are not intended to limit the scope of the present invention, and changes or adjustments of the relative relationship thereof are also considered to be the scope of the present invention without substantial changes in the technical content.
As shown in figure 1, the device for continuously preparing 5-amino-1, 2, 3-thiadiazole comprises a preparation kettle 1, a diazotization tubular reactor 2, a diazoacetonitrile storage tank 6, a separator 8, a cyclization reactor 9 and a flash tank 12.
Wherein, the preparation kettle 1 is used for preparing the aminoacetonitrile sulfate into the aminoacetonitrile sulfate aqueous solution with the required concentration.
The diazotization tubular reactor 2 comprises a front-end mixing section (with the model number of DN50-1000) and a rear-end reaction section (with the model number of DN200-5000), and a heat exchanger is wound outside; the mixing section at the front end of the diazotization tubular reactor 2 is connected with a discharge port of the preparation kettle 1, and the upper part of the mixing section is provided with an organic solvent feed port, a nitrosyl sulfuric acid feed port and a sulfuric acid aqueous solution feed port; the product of the rear reaction section of the diazotization tubular reactor 2 is introduced into a diazoacetonitrile storage tank 6. The heat exchanger wound outside the mixing section at the front end of the diazotization tubular reactor 2 is of a sleeve type structure, the inner pipe is used for conveying materials, and the outer pipe is used for conveying frozen brine; the heat exchanger wound outside the rear-end reaction section is of a tube type structure, materials are fed on a tube side, and frozen brine is fed on a shell side; so that the temperature in the diazotization tubular reactor is controlled at-5 ℃ to 5 ℃. A first diazotization mature device 3, a second diazotization mature device 4 and a third diazotization mature device 5 (models are DN200-5000) which are connected in sequence are arranged between the diazotization tubular reactor 2 and the diazoacetonitrile storage tank 6; the first, second and third nitriding maturers are externally provided with a heat exchanger with a tube type structure, the tube side is used for feeding materials, and the shell side is used for feeding frozen brine.
The discharge hole of the diazoacetonitrile storage tank 6 is connected with the feed inlet of the separator 8, the connecting pipeline is provided with a circulating pump 7, and the diazoacetonitrile mixed solution obtained by the reaction is sent into the separator 8 for continuous separation.
The separator 8 is of a continuous separation structure, the length, the width and the height of the separator are 2400mm, 1200mm and 800mm respectively, a feed inlet and a discharge outlet are arranged on the same side of the width of the separator, the feed inlet and the discharge outlet are separated by a partition plate, the residence time of materials in the separator is increased to ensure that the materials are fully separated, and the partition plate is 2000mm long and 780mm high; the center line of the upper layer discharge port is 200mm away from the top end of the separator, the lower layer discharge port is connected with the inner side cofferdam of the separator, the length and the width of the cofferdam are 250mm, the upper opening of the cofferdam is 60mm away from the top end of the separator, the bottom end of the cofferdam is 10mm lower than the position of the lower opening of the discharge pipe, the middle of the bottom plate of the cofferdam is vertically inserted into the open pipelines at two ends, the upper opening of the pipeline is connected with a threaded sleeve pipe with the height being adjusted up and down, the upper opening of the pipeline is 100mm away from the bottom plate of the. The center of the top end of the separator is provided with a gas outlet, and the bottom end of the separator is provided with a sewage outlet opposite to the feed inlet. Continuously separating out organic phase diazoacetonitrile solution at the lower layer and acid phase solution at the upper layer through the separator, allowing the organic phase diazoacetonitrile solution at the lower layer to enter the cyclization reactor 9 through the lower layer discharge port of the separator 8 for cyclization reaction, and allowing the acid phase solution at the upper layer to enter the flash tank 12 through the upper layer discharge port of the separator 8 for concentration.
The ring closure reactor 9(200L enamel kettle, with stirring and jacket) is connected to a first ring closure mature kettle 10 and a second ring closure mature kettle 11(200L enamel kettle, with stirring and jacket) at the rear, the ring closure reactor and the ring closure mature kettle are both of vertical structures and are provided with stirrers, the outer wall of the ring closure reactor is provided with the jacket, a discharge port is arranged at the side surface of the reactor, and the ring closure reactor and the ring closure mature kettle which are sequentially connected are in a step shape and are arranged from top to bottom. The second ring synthesis mature kettle 11 is connected to a subsequent existing purification device, and the product is further purified to obtain a finished product of the 5-amino-1, 2, 3-thiadiazole.
A discharge port of a flash tank 12(200L enamel kettle with stirring and jacket) is connected to a feed port of the diazotization tubular reactor 2, a sulfuric acid pump 13, a first cooler 14 and a second cooler 15 (models are DN200-5000) which are sequentially connected are arranged on a connecting pipeline, the former cooler is used for cooling hot sulfuric acid aqueous solution, cooling water is used as a heat exchange medium for the cooler, the latter cooler is used for further cooling the sulfuric acid aqueous solution cooled by the former cooler to-5 ℃, and chilled brine is used as the heat exchange medium. The concentrated product is cooled and then returned to the diazotization tubular reactor 2 as a reaction raw material for utilization.
The process flow for preparing 5-amino-1, 2, 3-thiadiazole of the utility model is shown in figure 2, and comprises the following steps:
(1) diazotization reaction: continuously adding nitrosyl sulfuric acid, an aminoacetonitrile sulfate aqueous solution, an organic solvent and a dilute sulfuric acid aqueous solution into a diazotization tubular reactor with a heat exchanger at the same time, maintaining the temperature at-5 ℃, and controlling the pH value of the materials to be 1-2 to react to generate a diazoacetonitrile mixed solution;
(2) separation: enabling the diazoacetonitrile mixed solution flowing out in the step (1) to enter a separator, continuously separating out an organic phase diazoacetonitrile solution on the lower layer, performing flash evaporation concentration on an acid phase solution on the upper layer, recycling the acid phase solution as a dilute sulfuric acid aqueous solution of the reaction raw material in the step (1), and sending the wastewater to a wastewater treatment device;
(3) and (3) cyclization reaction: and (3) putting the diazoacetonitrile solution obtained by separation in the step (2) into a cyclization reactor, cooling to-15 to-5 ℃, adding a catalyst triethylamine under stirring, slowly introducing hydrogen sulfide gas, reacting with the diazoacetonitrile to generate 5-amino-1, 2, 3-thiadiazole, and performing post-treatment after the reaction to obtain the finished product of the 5-amino-1, 2, 3-thiadiazole.
Example 1:
210 g of aminoacetonitrile sulfate is added with water to prepare an aminoacetonitrile sulfate aqueous solution with the mass concentration of 45 percent,
uniformly and continuously adding 610 g of nitrosyl sulfuric acid with the mass concentration of 50% and ethylene glycol dimethyl ether into a diazotization tubular reactor, wherein the flow rate of nitrosyl sulfuric acid is controlled to be between 7.5 and 10ml/min, the flow rate of aminoacetonitrile sulfate aqueous solution is controlled to be between 5.5 and 7.5ml/min, the flow rate of ethylene glycol dimethyl ether is controlled to be between 55 and 75ml/min, meanwhile, dilute sulfuric acid with the mass concentration of 28% is introduced at the flow rate of 6.5 to 8ml/min to adjust the pH value of the material to be between 1 and 2, so that diazoacetonitrile mixed solution is generated by reaction, the effluent diazoacetonitrile mixed solution enters a separator, the separated acid phase solution at the upper layer is recycled or used after flash evaporation concentration at the vacuum degree of 0.05 to 0.085MPa and the temperature of 180 to 190 ℃, the organic phase diazoacetonitrile solution at the lower layer is removed from the cyclization reactor, and triethylamine catalyst is added under the temperature condition of-15 to-5 ℃ and stirring, and chlorine sulfide gas is slowly introduced to react to generate a crude product of the 5-amino-1, 2, 3-thiadiazole, and after the reaction is finished, 153.38 g of a finished product of the 5-amino-1, 2, 3-thiadiazole with the purity of 99.3 percent is obtained through post-treatment, and the yield is 75.4 percent.
Examples 2 to 30:
according to the method and apparatus described in example 1, the amount of nitrosyl sulfuric acid dosed at the time of diazotization is the ratio of the amount of nitrosyl sulfuric acid dosed to the amount of aminoacetonitrile sulfate species dosed at the time of diazotization, and the dosing for examples 2-30 is shown below:
TABLE 1
The utility model provides a thought and method of device of serialization preparation 5-amino-1, 2, 3-thiadiazole, the method and the way that specifically realize this technical scheme are many, above only the preferred embodiment of the utility model discloses should point out, to ordinary skilled person in this technical field, do not deviate from the utility model discloses under the prerequisite of principle, can also make a plurality of improvements and moist decorations, these improvements and moist decorations should also regard as the utility model discloses a protection scope. All the components not specified in the present embodiment can be realized by the prior art.
Claims (7)
1. A device for continuously preparing 5-amino-1, 2, 3-thiadiazole is characterized by comprising a preparation kettle (1), a diazotization tubular reactor (2), a diazoacetonitrile storage tank (6), a separator (8), a cyclization reactor (9) and a flash tank (12);
the diazotization tubular reactor (2) comprises a front-end mixing section and a rear-end reaction section, and a heat exchanger is wound outside the diazotization tubular reactor; the mixing section at the front end of the diazotization tubular reactor (2) is connected with a discharge hole of the preparation kettle (1), and the upper part of the mixing section is provided with a plurality of feed inlets; introducing a product at the rear end reaction section of the diazotization tubular reactor (2) into a diazoacetonitrile storage tank (6);
the discharge hole of the diazoacetonitrile storage tank (6) is connected with the feed inlet of the separator (8), and the diazoacetonitrile mixed solution obtained by the reaction is sent into the separator (8) for continuous separation;
the separator (8) continuously separates out the organic phase diazoacetonitrile solution at the lower layer and the acid phase solution at the upper layer, the organic phase diazoacetonitrile solution at the lower layer enters the cyclization reactor (9) through the lower layer discharge hole of the separator (8) for cyclization reaction, and the acid phase solution at the upper layer enters the flash tank (12) through the upper layer discharge hole of the separator (8) for concentration;
the cyclization reactor (9) is connected to a subsequent purification device, and the product is further purified to obtain a finished product of 5-amino-1, 2, 3-thiadiazole;
the discharge hole of the flash tank (12) is connected to the feed inlet of the diazotization tubular reactor (2), and the concentrated product is reused as a reaction raw material.
2. The device for continuously preparing 5-amino-1, 2, 3-thiadiazole according to claim 1, wherein more than one diazotization mature device (3, 4, 5) connected in sequence is arranged between the diazotization tubular reactor (2) and the diazoacetonitrile storage tank (6); and a heat exchanger with a tube type structure is arranged outside the diazotization maturity device (3, 4, 5).
3. The device for continuously preparing 5-amino-1, 2, 3-thiadiazole according to claim 1, wherein more than one cyclization maturation kettle (10, 11) connected in sequence are connected behind the cyclization reactor (9).
4. The device for continuously preparing 5-amino-1, 2, 3-thiadiazole according to claim 3, wherein the cyclization reactor (9) and the cyclization kettles (10, 11) are both vertical structures and are provided with a stirrer, the outer wall of the cyclization reactor is provided with a jacket, the discharge port is arranged on the side surface of the reactor, and the cyclization reactor (9) and the cyclization kettles (10, 11) which are sequentially connected are arranged in a step shape from top to bottom.
5. The device for continuously preparing 5-amino-1, 2, 3-thiadiazole according to claim 1, wherein more than one cooler (14, 15) connected in sequence is arranged between the discharge port of the flash tank (12) and the feed port of the diazotization tubular reactor (2) and is used for cooling a concentrated product.
6. The device for continuously preparing 5-amino-1, 2, 3-thiadiazole according to claim 1, wherein the heat exchanger wound outside the mixing section at the front end of the diazotization tubular reactor (2) is of a double-pipe structure.
7. The device for continuously preparing 5-amino-1, 2, 3-thiadiazole according to claim 1, wherein the heat exchanger wound outside the reaction section at the rear end of the diazotization tubular reactor (2) is in a tubular structure.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111018806A (en) * | 2019-12-25 | 2020-04-17 | 安道麦安邦(江苏)有限公司 | Method and device for continuously preparing 5-amino-1, 2, 3-thiadiazole |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111018806A (en) * | 2019-12-25 | 2020-04-17 | 安道麦安邦(江苏)有限公司 | Method and device for continuously preparing 5-amino-1, 2, 3-thiadiazole |
| CN111018806B (en) * | 2019-12-25 | 2024-04-12 | 安道麦安邦(江苏)有限公司 | Method and device for continuously preparing 5-amino-1, 2, 3-thiadiazole |
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