CN112279769A - Method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene and microchannel device - Google Patents
Method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene and microchannel device Download PDFInfo
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- C07C201/06—Preparation of nitro compounds
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Abstract
The invention provides a method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene, in particular to a synthetic method of 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene and a microchannel reaction device for producing the product. The method is characterized in that the method takes trichlorobenzene as a raw material, takes mixed acid of nitric acid and sulfuric acid as a nitrating agent, and continuously pumps the trichlorobenzene into a microchannel reactor for nitration, wherein the microchannel reactor comprises the following steps: stainless steel base, fixed pressure seal plate, micro-channel mixing preheating, nitrate, dinitrate and trinitrate reactor gradient heating templates, heat-conducting oil furnace connected with each stage of template jacket, raw material inlet and product outlet. Small reaction volume, easy amplification, high space-time yield and important significance for the safe production of the 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene.
Description
Technical Field
The invention relates to the technical field of fine organic chemical industry, in particular to a method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene, and also relates to a production method and a device for safely and efficiently synthesizing trinitrobenzene powder by controlling different temperatures through different modules through a micro-channel continuous flow reactor. The design and application of the microchannel reactor belong to the field of novel chemical reactors.
Technical Field
The 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene is also named trinitrobenzene powder, is an insecticide and a bactericide used in agriculture, and can also be used for organic synthesis intermediates, electrolytic depolarizers or fuel additives of military products.
At present, the domestic production method of trinitrotoluene is synthesized by kettle type batch reaction, and a continuous micro-channel synthesis method is not available. The kettle type reaction process has the defects of large waste acid, more waste water and certain difficulty brought to the operation by multi-step temperature rise in the nitration process, and most importantly, the kettle type reaction kettle has large capacity, poor heat and mass transfer effects, uneven temperature of kettle wall materials and kettle center materials and difficult control of reaction temperature in the kettle, and although three electron-withdrawing group chlorine atoms on a benzene ring cause high stability of trinitro dispersion, the production mode still brings certain potential safety hazard to production.
The micro chemical technology is a new technology which is developed in recent years and is used for preparing chemical intermediates such as pesticides, dyes and the like, the rapid, safe and efficient process strengthening is realized, and the reaction process is strengthened by changing the characteristics of fluid mass transfer, heat transfer and flow. The performance of the micro-reactor has great advantages in the aspects of safety control, temperature control and time control. The micro-reactor has the characteristics of small volume, green safety, less side reaction, large number increase and the like. That is, the mass production by adding the micro reaction unit has substantially no amplification effect.
The microchannel reactor is particularly suitable for dangerous chemical unit reactions in the chemical field. Including nitration, diazotization, alkylation, photooxidation, sulfonation and other unit reactions or other dangerous chemical reactions which are violent in reaction, flammable and explosive, such as azide, high-pressure addition, high-pressure cracking, cyclization and the like.
At present, most of the domestic and foreign literature publications on the production of the trinitrogenous ranges are production methods prepared by a kettle type reaction device. The technological process is that sym-trichlorobenzene is used as initial material and synthesized in mixed acid system of nitric acid and sulfuric acid at the temperature of 100-150 deg.c. After the reaction is finished, the product is obtained by acid separation, alkali washing, water washing and suction filtration. The reaction principle is as follows:
wherein the mol ratio of the trichlorobenzene to the nitric acid to the sulfuric acid is as follows: 1: 3.0-6.0: 15-50
The reaction temperature is 4 hours, the conversion rate of the sym-trichlorobenzene is 91 percent, the trinitrobenzene content is 95 percent, and the yield is 87 percent based on the sym-trichlorobenzene.
The process has the following unsafe factors:
the kettle type intermittent reaction has the defects of difficult temperature control, more side reactions, difficult uniform stirring and poor heat and mass transfer effects. The material in the kettle is many, the potential safety hazards such as burning and explosion are great, the reaction temperature is high, the operation cost is high, and the energy consumption is high. Therefore, there is a need to provide a new and higher safety device to address the above deficiencies. The microchannel device of the present invention solves the above problems.
Disclosure of Invention
The invention aims to provide a method for solving the problems of blasting danger, poor heat and mass transfer effects, low conversion rate of trichlorobenzene and low yield of trinitrobenzene in the prior art for producing trinitrobenzene.
The invention also provides a microchannel device of the gradient heating module, and the device can ensure that after the materials such as the sym-trichlorobenzene, the mixed acid and the like are fed, the materials are mixed and preheated by the mixing preheater and then react in the microchannel reactor to prepare the trinitro powder.
The technical scheme adopted is as follows:
a method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene comprises the following steps: the method comprises the following steps:
1) simultaneously pumping the heated and melted sym-trichlorobenzene, the mixed nitric acid and the mixed sulfuric acid into a micro-channel reactor mixing preheater module by a pump;
2) sending the mixed liquid from the 1) micro-channel mixing preheater module into each stage of nitration reactor module of the micro-channel reactor for nitration reaction;
3) and nitrifying liquid discharged from the trinitrotoluene reactor module enters an acid separating tank, an acid layer is separated for treatment and recycling, and a finished product is separated, sent to a cooling kettle for cooling, washed by alkali, washed by water and filtered by suction to obtain the finished product.
In the step 1), the mol ratio of the trichlorobenzene to the nitric acid to the sulfuric acid is preferably 1: 4.0-4.5: 30.
the sym-trichlorobenzene is in industrial grade, and the content is more than 98 percent; the concentrations of the nitric acid and the sulfuric acid are industrial grade concentrated nitric acid and concentrated sulfuric acid, and the mass fractions of the nitric acid and the sulfuric acid are more than 98%.
The temperature of the mixture can be controlled by the micro-channel mixing preheater module in the step 1), the preheating temperature of the micro-channel preheater module is 40-80 ℃, and the preheating temperature can be set according to the oil temperature of a heat-conducting oil furnace connected with the upper jacket layer of the module.
The temperature of the mononitration in the step 2) is between 80 and 90 ℃, the temperature of the dinitration is between 90 and 110 ℃, and the temperature of the trinitration is between 110 and 130 ℃. Can be set according to the oil temperature of the heat-conducting oil furnace connected with different upper jacket layers of the modules.
The residence time of the materials in the micro-channel is 20-200s, the pump flow rate is 100-2000ml/min, the flow pressure of the materials in the micro-channel is 0-8.0MPa, and the reaction temperature is 80-150 ℃.
The invention discloses a device for synthesizing trinitrogenous powder by a microchannel reactor, which comprises the following steps: mainly comprises a micro-channel mixing preheater, a nitrate reactor, a dinitrate reactor and a trinitrate reactor which are sequentially connected in series; the whole micro-channel consists of 6 modules, wherein a mixing preheater is provided with one module, a single nitrate reactor is provided with one module, a dinitrate reactor is provided with two modules, and a trinitrate reactor is provided with two modules; the inner diameter of the channel is 0.3-0.8 mm, the total length of the channel is 200-1000cm, the whole device consists of a stainless steel base, a pressure seal strip and modules, and different modules are respectively connected with different heat-conducting oil furnaces to realize gradient temperature rise of different nitration modules.
The advantages and the characteristics of the invention are as follows:
1) the reaction raw materials are continuously fed, are fully contacted and uniformly mixed, can realize the accurate control of the reaction, provides a good environment for the nitration of the sym-trichlorobenzene, and has high sym-trichlorobenzene conversion rate, high trinitrobenzene yield and less side reactions
2) Large specific surface area, high mass transfer rate, short contact time and less side reaction. The burning and explosion danger is greatly reduced, and the safety coefficient is extremely high.
3) The liquid holdup of the reaction liquid in the micro-channel is low, and the total amount is 4.8 kilograms; after different temperature control of different modules is carried out, the storage amount of the trinitro powder of the final product is 0.15 kg, the safety risk of a reaction zone is greatly reduced, and the production safety is guaranteed.
4) The method has the advantages of quick and direct amplification, no need of scale amplification of the microreactor, only need of adding a module for micro reaction, small occupied area, less investment, high efficiency and direct amplification for industrial production.
5) The operability is good, and the safety is high. The liquid holdup in the micro-reaction system is small, a large amount of heat can be taken away in time, and the possibility of safety accidents can be avoided to the greatest extent.
6) And the reaction liquid is fully contacted in the microchannel, so that the proportion of the input nitric acid and the input sulfuric acid is small, the waste acid is reduced, and the production cost is saved.
7) In the microchannel reactor, procedures such as feeding, mixing, preheating, reacting and the like are carried out in a closed and continuous manner, so that leakage in a device which needs to be additionally configured and in transfer in the conventional kettle type batch reaction process is avoided, safety and environmental protection are realized, and production efficiency is high.
Drawings
FIG. 1 is a schematic view of the structure of the device
FIG. 2 is a view of a preheating template
FIG. 3 is a diagram of a reaction template.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the accompanying drawings, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The parts not described in the present invention are all the prior art or standard products, and are not described again.
In the description of the present invention, it should be noted that unless otherwise explicitly stated or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected, mechanically connected, electrically connected, directly connected, or indirectly connected through an intermediate medium, and communicate between two elements. The specific meaning of the terms in the present invention can be understood in a specific case to those skilled in the art. In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
Example 1
1) The device comprises the following components: a continuous flow microchannel reactor (microchannel reactor connection mode identified with reference to the figures).
2) The raw material tank 1 is an enamel tank with a steam heating device, the pipeline connected with the micro-channel mixing template is a hot water heat-insulating sleeve, and the infusion pressure pump 3 is also a heat-insulating pump. The raw material tank 2 is a mixed acid tank, and is also an enamel tank as the tank 1. Nitric acid and sulfuric acid in a certain proportion are uniformly mixed and then are pumped into a mixing module 5 through a pressure pump 4 at a certain speed, the feed liquid which is uniformly mixed with the sym-trichlorobenzene and is preheated can sequentially pass through the 6, 7 and 8 times of nitration modules under the pressure of the pump, and the reaction temperature of the feed liquid in each module is respectively regulated by different heat-conducting oil furnaces corresponding to a, b, c and d. The residence time of the feed liquid in the microchannel reactor was 77 s. The product after the reaction continuously flows into a heat-preserving acid-separating tank 9 for acid-separating treatment. The waste acid liquid is separated out and put into a tank 11, and is recycled into the 2 acid preparation kettle after being treated. Separating the product liquid to 10 for alkali washing and water washing, and then performing suction filtration to obtain a finished product.
3) And putting 182 kg of the weighed trichlorobenzene into the raw material tank 1, and heating to about 60 ℃ for standby. 252 kg of fuming nitric acid and 2940 kg of concentrated sulfuric acid are put into the raw material tank 2 and mixed uniformly for standby.
4) And preheating different module combinations according to different set temperatures. The temperature of each module group reaches the corresponding temperature respectively, wherein the temperature of the mixing preheating module reaches 60-80 ℃, the temperature of the first nitrate reaction is 80-90 ℃, the temperature of the second nitrate reaction is 90-110 ℃, and the temperature of the third nitrate reaction is 110-130 ℃, and after preheating for 10 minutes, the modules reach the temperature, and then feeding is started.
5) The flow of the metering pump 3 and the pump 4 is adjusted to be trichlorobenzene: mixed acid (weight ratio) = 1: 17.75, the mixture is fed at a uniform speed, the feeding speed of a pump 3 (trichlorobenzene) is 0.2kg/min, and the feeding speed of a pump 4 (mixed acid) is 3.55kg/min, the mixture is continuously fed into the micro-channel, the temperature of a mixing and preheating module is 73 ℃, the temperature of mononitrate reaction is 85 ℃, the temperature of dinitrate reaction is 105 ℃, and the temperature of trinitrobenzene reaction is 128 ℃. The residence time of the materials in the whole micro-channel is 1.28min, the total amount of the materials in the whole micro-channel system is 4.8 kg, and the amount of the trinitrogen powder as a final product is 0.15 kg. Finally, the outlet of the template flows out to an acid separating tank 9 in a high-dispersion continuous flow state.
6) After the reaction, the feed liquid flows into an acid separating tank 9, is subjected to acid separation by 9, then is subjected to alkali washing by a washing tank 10, and then is subjected to washing by water and filtering, so that 316.8 kg of finished trinitro powder is obtained, the content is 96.1%, and the yield is 96.2%.
Example 2
1) The used raw material tank, the used feed pump, the used microchannel reactor, the used heat-preservation acid-separating tank and the like are the same as those in the embodiment 1
2) The retention time of the feed liquid in the microchannel reactor is 87 s. After the reaction, the continuous flow of the products flows into a heat-preserving and acid-separating tank for post-treatment.
3) And putting 182 kg of the weighed trichlorobenzene into the raw material tank 1, and heating to about 60 ℃ for standby. 240 kg of fuming nitric acid and 1897 kg of concentrated sulfuric acid are put into a raw material tank 2 and mixed uniformly for standby.
4) And preheating different module combinations according to different set temperatures. The temperature of each module group reaches the corresponding temperature respectively, wherein the temperature of the mixing preheating module reaches 70-80 ℃, the temperature of the first nitrate reaction is 85-95 ℃, the temperature of the second nitrate reaction is 95-115 ℃, and the temperature of the third nitrate reaction is 120-140 ℃, and after preheating for 10 minutes, the modules start to feed after reaching the temperature.
5) Adjusting the flow of a metering pump 3 and a pump 4, and mixing the components in a mixture of trichlorobenzene: mixed acid (weight ratio) = 1: the materials are fed at the uniform speed of the proportion of 11.67, the feeding speed of a pump 3 (trichlorobenzene) is 0.2kg/min, the pump 4 (mixed acid) continuously feeds materials into the micro-channel at the speed of 2.33kg/min, the temperature of a mixing and preheating module is 70 ℃, the temperature of mononitrate reaction is 87 ℃, the temperature of dinitrate reaction is 109 ℃ and the temperature of trinitrate reaction is 135 ℃. The residence time of the materials in the whole micro-channel is 1.45min, the total amount of the materials in the whole micro-channel system is 3.67 kg, and the amount of the trinitrogen powder as a final product is 0.17 kg. Finally, the outlet of the template flows out to an acid separating tank 9 in a high-dispersion continuous flow state.
6) After the liquid after the reaction flows into a heat-preservation and acid-separation tank, 313.8 kg of finished trinitrotoluene powder with the content of 95.8 percent and the yield of 95.0 percent is obtained by acid separation, alkali washing and water washing and then filtering.
Example 3
1) The feed tank, feed pump, microchannel reactor, thermal insulation acid-separating tank and the like used were the same as in example 1.
2) The residence time in the microchannel reactor was 72 s. After the reaction, the continuous flow of the products flows into a heat-preserving and acid-separating tank for post-treatment.
3) And putting 182 kg of the weighed trichlorobenzene into the raw material tank 1, and heating to about 60 ℃ for standby. 285 kg of fuming nitric acid and 3390 kg of concentrated sulfuric acid are put into a raw material tank 2 and mixed evenly for standby.
4) And preheating different module combinations according to different set temperatures. The temperature of each module group reaches the corresponding temperature respectively, wherein the temperature of the mixing preheating module reaches 70-80 ℃, the temperature of the first nitrate reaction is 85-90 ℃, the temperature of the second nitrate reaction is 90-115 ℃, and the temperature of the third nitrate reaction is 115-130 ℃, and after preheating for 10 minutes, the modules reach the temperature, and then feeding is started.
5) Adjusting the flow of a metering pump 3 and a pump 4, and mixing the components in a mixture of trichlorobenzene: mixed acid (weight ratio) = 1: 20.17, the feeding speed is 0.2kg/min for the pump 3 (trichlorobenzene) and 4.03kg/min for the pump 4 (mixed acid), the temperature of the mixing and preheating module is 65 ℃, 76 ℃ for the mononitration, 102 ℃ for the dinitration and 125 ℃ for the trinitration. The residence time of the materials in the whole micro-channel is 1.2min, the total amount of the materials in the whole micro-channel system is 5.08 kg, and the amount of the trinitrogen powder as a final product is 0.14 kg. Finally, the outlet of the template flows out to an acid separating tank 9 in a high-dispersion continuous flow state.
6) After the liquid after the reaction flows into a heat-preservation and acid-separation tank, 313.5 kg of finished trinitrotoluene powder with the content of 96.8 percent and the yield of 95.9 percent is obtained by acid separation, alkali washing and water washing and then filtering.
Example 4
1) The feed tank, feed pump, microchannel reactor, thermal insulation acid-separating tank and the like used were the same as in example 1.
2) The residence time in the microchannel reactor was 58 s. After the reaction, the continuous flow of the products flows into a heat-preserving and acid-separating tank for post-treatment.
3) And putting 182 kg of the weighed trichlorobenzene into the raw material tank 1, and heating to about 60 ℃ for standby. 285 kg of fuming nitric acid and 3390 kg of concentrated sulfuric acid are put into a raw material tank 2 and mixed evenly for standby.
4) And preheating different module combinations according to different set temperatures. The temperature of each module group reaches the corresponding temperature respectively, wherein the temperature of the mixing preheating module reaches 70-80 ℃, the temperature of the first nitrate reaction is 85-90 ℃, the temperature of the second nitrate reaction is 90-115 ℃, and the temperature of the third nitrate reaction is 115-130 ℃, and after preheating for 10 minutes, the modules reach the temperature, and then feeding is started.
5) Adjusting the flow of a metering pump 3 and a pump 4, and mixing the components in a mixture of trichlorobenzene: mixed acid (weight ratio) = 1: 20.17, the materials are fed at a uniform speed, the feeding speed of a pump 3 (trichlorobenzene) is 0.25kg/min, the pump 4 (mixed acid) continuously feeds the materials into the micro-channel at a speed of 5.04kg/min, the temperature of a mixing and preheating module is 67 ℃, the temperature of mononitration reaction is 75 ℃, the temperature of dinitrate reaction is 100 ℃, and the temperature of trinitration reaction is 127 ℃. The residence time of the materials in the whole micro-channel is 0.97min, the total amount of the materials in the whole micro-channel system is 5.08 kg, and the amount of the trinitrogen powder as a final product is 0.13 kg. Finally, the outlet of the template flows out to an acid separating tank 9 in a high-dispersion continuous flow state.
6) After the liquid after the reaction flows into a heat-preservation acid-separating tank, 312.8 kg of finished trinitrotoluene powder with the content of 95.2 percent and the yield of 94.1 percent is obtained by acid separation, alkali washing, water washing and filtering.
Example 5
1) The used raw material tank, the used feed pump, the microchannel reactor, the used receiving and acid-separating heat-preserving tank and the like are the same as those in the embodiment 1
2) The feed ratio, feed amount and feed rate were the same as those in example 1.
3) Only changing the temperature of the preheating module to 70-90 ℃, the temperature of the mononitration reaction to 90-100 ℃, the temperature of the dinitration reaction to 100-.
4) Other post-treatments were the same as in example 1
5) 318.1 kg of finished trinitrotoluene powder is obtained, the content is 94.6 percent, and the yield is 95.1 percent.
Example 6
1) The feed tank, feed pump, microchannel reactor, and acid-receiving holding tank used were the same as in example 1.
2) The feed ratio, feed amount and feed rate were the same as those in example 1
3) Only changing the temperature of the preheating module to 50-70 ℃, the temperature of the first nitrate reaction module to 70-80 ℃, the temperature of the second nitrate reaction module to 80-100 ℃ and the temperature of the third nitrate reaction module to 100-120 ℃, and starting feeding after the modules reach the temperature after preheating for about 10 minutes.
4) Other post-treatments were the same as in example 1
5) 322.2 kg of finished product trinitrotoluene powder is obtained, the content is 93.1 percent, and the yield is 94.8 percent.
The present invention and its embodiments have been described above, and the description is not intended to be limiting, and the drawings are only one embodiment of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should, without their teaching, appreciate that they can readily devise similar arrangements and embodiments without departing from the spirit and scope of the invention.
Claims (7)
1. A method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene comprises the following steps: the method is characterized in that: the method comprises the following steps:
1) simultaneously pumping the heated and melted sym-trichlorobenzene, the mixed nitric acid and the mixed sulfuric acid into a micro-channel reactor by a pump;
2) after the mixture is mixed and preheated in the step 1), the homogeneous phase mixed liquid is sequentially sent into a microchannel reactor;
3) and (3) entering a heat-preservation acid-separating tank after coming out from the last-stage module, separating an acid layer to 11 for treatment and recycling, separating a finished product, sending the finished product to a washing kettle 10 for alkali washing, washing with water, and then performing suction filtration to obtain the finished product.
2. The method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene according to claim 1, characterized in that: in the step 1), the mol ratio of the trichlorobenzene to the nitric acid to the sulfuric acid is preferably 1: 4.0-4.5: 15-30.
3. The method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene according to claim 1, characterized in that: the sym-trichlorobenzene is in industrial grade, and the content is more than 98 percent; the concentrations of the nitric acid and the sulfuric acid are industrial grade concentrated nitric acid and concentrated sulfuric acid, and the mass fractions of the nitric acid and the sulfuric acid are more than 98%.
4. The method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene according to claim 1, characterized in that: the temperature of the mixture can be controlled by the micro-channel preheater in the step 2), and the preheating temperature of the micro-channel preheater is 40-80 ℃.
5. The method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene according to claim 1, characterized in that: the temperature of the mononitration reaction in the steps 3) and 4) is 80-90 ℃, the temperature of the dinitrate reaction is 90-110 ℃, and the temperature of the trinitration reaction is 110-130 ℃. Different nitration gradient temperature rises can be realized according to the set temperature of the heat-conducting oil furnace connected with different modules.
6. The method for safely producing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene according to claim 1, characterized in that: the residence time of the materials in the micro-channel is 20-200s, the pump flow rate is 100-2000ml/min, the flow pressure of the materials in the micro-channel is 0-8.0MPa, and the reaction temperature is 80-150 ℃.
7. A micro-channel reactor device for synthesizing 1, 3, 5-trichloro-2, 4, 6-trinitrobenzene is characterized in that: comprises a mixer and a preheater, a micro-channel nitrate reactor, a dinitrate reactor and a trinitrate reactor which are sequentially connected in series; the main device of the micro-channel is provided with 6 modules, wherein a mixing preheater is provided with one module, a single nitrate reactor is provided with one module, a dinitrate reactor is provided with two modules, a trinitrate reactor is provided with two modules, and the mixing preheater is provided with four corresponding heat-conducting oil furnaces with different set temperatures; and each template is provided with a temperature measuring hole and a heat conducting oil inlet and outlet hole. The inner diameter of the micro-channel is 0.3-0.8 mm, the total length of the channel is 200-1000cm, and the whole micro-channel reactor module is fixed on a stainless steel base and is fixed by a fixed pressure seal and a bolt.
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| CN114805078A (en) * | 2022-02-11 | 2022-07-29 | 上海农帆生物科技有限公司 | Method for preparing 2,3, 4-trichloronitrobenzene by micro-channel nitration reaction |
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| CN102432471A (en) * | 2011-11-07 | 2012-05-02 | 常州大学 | Method for undergoing chlorobenzene nitration reaction by using micro-channel reactor |
| CN106800513A (en) * | 2017-01-10 | 2017-06-06 | 中国工程物理研究院化工材料研究所 | The synthetic method of trinitrophloroglucinol |
| CN109824521A (en) * | 2019-03-07 | 2019-05-31 | 中国工程物理研究院化工材料研究所 | Between photoacoustic spectroscopy channel synthetic method |
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| CN114805078A (en) * | 2022-02-11 | 2022-07-29 | 上海农帆生物科技有限公司 | Method for preparing 2,3, 4-trichloronitrobenzene by micro-channel nitration reaction |
| CN114805078B (en) * | 2022-02-11 | 2023-09-29 | 上海农帆生物科技有限公司 | Method for preparing 2,3, 4-trichloronitrobenzene through microchannel nitration |
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