CN211636445U - Thiodicarb synthesis reaction serialization apparatus for producing - Google Patents
Thiodicarb synthesis reaction serialization apparatus for producing Download PDFInfo
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- CN211636445U CN211636445U CN201922126046.9U CN201922126046U CN211636445U CN 211636445 U CN211636445 U CN 211636445U CN 201922126046 U CN201922126046 U CN 201922126046U CN 211636445 U CN211636445 U CN 211636445U
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Abstract
The utility model relates to a thiodicarb synthetic reaction continuous production device, which comprises a catalyst storage tank and a methomyl storage tank, wherein the lower part of the methomyl storage tank is connected with a methomyl feeder, the lower part of the catalyst storage tank is connected with a catalyst feeder, the upper part of a slurry tank is provided with a methomyl inlet, the device comprises a catalyst inlet and a salinization product inlet, wherein a hot water channel is arranged in a slurry tank, a mixture outlet is arranged at the bottom of the slurry tank, the mixture outlet is connected with the mixture inlet at the bottom of a synthesis reactor, a nitrogen inlet is also arranged at the bottom of the synthesis reactor, a gas distributor is arranged in the synthesis reactor, a gas collector and a nitrogen outlet are arranged at the upper part of the synthesis reactor, a product outlet is arranged at the side surface of the synthesis reactor, the nitrogen inlet is connected with a mixed nitrogen outlet of a nitrogen storage tank, the nitrogen outlet is connected with a top inlet of the nitrogen storage tank, and a fresh nitrogen inlet is; the utility model has the advantages of high reaction efficiency, environmental protection and high product quality.
Description
Technical Field
The utility model relates to a pesticide compound synthesis technical field, concretely relates to thiodicarb synthesis reaction serialization apparatus for producing.
Background
Thiocarb is a second-generation carbamate pesticide, is a low-toxicity derivative of methomyl, is formed into the dicarbamate by connecting two methomyl molecules through a thioether chain, has toxicity only about one tenth of that of methomyl, is a high-efficiency, broad-spectrum, low-toxicity and systemic stomach toxicity pesticide, has stomach toxicity as the main action on pests, almost has no contact poisoning effect, no fumigation and systemic action and strong selectivity, has short residual period in soil, has an action mechanism of nerve blocking action, namely blocks reactivation of conductive substances in nerve fibers by inhibiting activity of ephthalocyanine acetate so as to cause poisoning death of the pests, can kill eggs, larvae and certain adults, is mainly used for non-direct edible crops (cotton), horticultural crops and seed treatment of cabbage, peanut and corn in the early period, and is mainly used for treating lepidoptera, The larvae of pests of homoptera, hymenoptera, diptera, coleoptera and the like are particularly effective, and are excellent varieties for preventing and controlling resistant cotton bollworms at present in China.
Thiodicarb is generally synthesized by the following route:
(1) and (3) salinization reaction:
(2) and (3) synthesis reaction:
the synthesis reaction is the second step of producing thiodicarb, and the domestic existing thiodicarb synthesis reaction process adopts an intermittent reaction kettle operation process: the dipyridyl thioether hydrochloride, the methomyl and the catalyst after the salinization reaction are put into a reaction kettle at a certain temperature, and the heat preservation reaction is carried out for 4 to 6 hours, so that the following problems mainly exist: firstly, the reaction process is a full-mixing operation, and a large amount of products generated by reaction and unreacted raw materials are mixed together and cannot be separated, so that the required retention time is long, and side reactions are caused to affect the yield; secondly, the raw materials are difficult to stir uniformly by depending on the shearing force of the stirring paddle in the reaction, so that the contact specific surface area among the raw materials is small, the dissolution is slow, and the dissolution is not uniform; thirdly, frequent starting and stopping are needed, and processes such as heating, cooling, cleaning and the like are carried out, so that the operation is complicated, the energy consumption is high, and unsafe factors are increased; fourthly, the organic solvent is emitted to the environment along with the start and stop of the vehicle, thus harming the health of workers; fifthly, the quality fluctuation of different batches of products is large, and the quality is difficult to ensure; therefore, it is necessary to provide a continuous thiodicarb synthesis reaction production apparatus with high reaction efficiency, environmental friendliness, and high product quality.
SUMMERY OF THE UTILITY MODEL
The utility model aims at overcoming the defects of the prior art and providing a thiodicarb synthesis reaction continuous production device with high reaction efficiency, environmental protection and high product quality.
The purpose of the utility model is realized like this: a thiodicarb synthetic reaction continuous production device comprises a catalyst storage tank and a methomyl storage tank, wherein the lower portion of the methomyl storage tank is connected with a methomyl feeder, the lower portion of the catalyst storage tank is connected with a catalyst feeder, the other ends of the methomyl feeder and the catalyst feeder are connected with a slurry tank, the upper portion of the slurry tank is provided with a methomyl inlet, a catalyst inlet and a salinization inlet, a hot water channel is arranged inside the slurry tank, the bottom of the slurry tank is provided with a mixture outlet, the mixture outlet is connected with a mixture inlet at the bottom of a synthetic reactor, the bottom of the synthetic reactor is also provided with a nitrogen inlet, a gas distributor is arranged inside the synthetic reactor, the upper portion of the synthetic reactor is provided with a gas collector and a nitrogen outlet, the side surface of the synthetic reactor is provided with a product outlet, and the nitrogen inlet, the nitrogen outlet is connected with the top inlet of the nitrogen storage tank, and the upper part of the nitrogen storage tank is also provided with a fresh nitrogen inlet.
A slurry pump and a valve are arranged between the mixture outlet and the mixture inlet.
A product discharging pump is connected behind the product outlet.
And a cooling machine and a nitrogen compressor are arranged between the nitrogen inlet and the mixed nitrogen outlet, and the nitrogen compressor is also connected with a nitrogen storage tank.
The methomyl feeder and the catalyst feeder are solid feeders.
The synthesis reactor is a bubble column, a single-stage loop reactor or a multistage loop reactor.
The slurry pump can be a metering pump, a slurry pump and the like, and the slurry continuously enters the bottom of the synthesis reactor.
The gas distributor at the bottom of the reactor can be any type of gas distributor, preferably an aerator. The synthesis reactor overhead gas collector may be any form of gas collector, preferably a wire mesh demister gas collector.
The continuous thiodicarb synthesis reaction production process includes the following steps:
step 1): continuously adding the raw materials of methomyl and a catalyst into a slurry tank from a storage tank through a feeder respectively, uniformly stirring the materials and a salinized product, controlling the temperature to be 10-40 ℃, and continuously feeding the materials into a mixture inlet at the bottom of a synthesis reactor through a slurry pump;
step 2): the outside of the synthesis reactor is provided with a jacket, and the temperature in the reactor is controlled between 10 and 40 ℃;
step 3): the nitrogen enters a nitrogen storage tank and enters a nitrogen inlet of the synthesis reactor through a nitrogen compressor;
step 4): the bottom of the synthesis reactor is provided with a gas distributor, and nitrogen enters the synthesis reactor through the gas distributor;
step 5): the top of the synthesis reactor is provided with a gas collector, liquid foam separation and nitrogen collection are carried out, the mixture returns to a nitrogen storage tank and is circulated to the synthesis reactor through a nitrogen compressor;
step 6): the unreacted solid material in the synthesis reactor continuously reacts at the middle lower part of the reactor; the generated thiodicarb is floated to the middle upper part of the tower, and is collected from a product outlet at the side part to be used as a raw material for next water washing.
The utility model has the advantages that: the utility model realizes continuous operation, simple flow and less equipment investment, and by introducing nitrogen into the synthesis reactor, on one hand, a high gas content area and a low gas content area in the reactor generate larger density difference to promote the materials to form high-speed circulation inside, so that the materials are fully mixed and sheared and dissolved, the reaction is effectively promoted to the greatest extent, and the reaction rate is improved; on the other hand, by utilizing the properties of easy sedimentation of the methomyl and the salinized product and easy suspension of the thiodicarb, the products are enriched at the upper part of the reactor and are discharged in time, so that the side reaction caused by the retention of the thiodicarb generated in the original intermittent production process in the reaction kettle is avoided, and the yield is improved. The residence time required by the reaction is reduced to be within 3 hours from 6 hours, the reaction conversion rate is improved to be more than 99.0 percent from 96 percent, and the residue of the methomyl is reduced to be less than 1.0 percent from 4 percent; the utility model has the advantages of high reaction efficiency, environmental protection and high product quality.
Drawings
Fig. 1 is a schematic view of the apparatus and the flow structure of the present invention.
In the figure, 1, a methomyl storage tank 2, a catalyst storage tank 3, a slurry tank 4, a nitrogen storage tank 5, a synthesis reactor 6, a methomyl feeder 7, a catalyst feeder 8, a gas collector 9, a nitrogen compressor 10, a gas distributor 11, a slurry pump 12, a product discharge pump 13, a salinate inlet 14, a methomyl inlet 15, a catalyst inlet 16, a hot water channel 17, a mixture outlet 18, a mixture inlet 19, a nitrogen outlet 20, a nitrogen inlet 21, a product outlet 22, a fresh nitrogen inlet 23, a top inlet 24, a mixed nitrogen outlet 25 and a cooler are arranged.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
Example 1
As shown in figure 1, raw material methomyl is continuously added into a slurry tank 3 by a methomyl feeder 6 in a certain proportion through a methomyl storage tank 1, catalyst is continuously added into the slurry tank 3 by a catalyst feeder 7 in a certain proportion through a catalyst storage tank 2, the mixture and salinized product are uniformly stirred, the mixture is heated to 10-40 ℃, the mixture is continuously conveyed into a mixture inlet at the bottom of a synthesis reactor 5 through a slurry pump 11, a jacket is arranged outside the synthesis reactor 5, and the temperature in the synthesis reactor 5 is controlled to be 10-40 ℃; nitrogen enters a nitrogen storage tank 4 and enters a gas distributor 10 at the bottom of a synthesis reactor 5 through a nitrogen compressor 9; the nitrogen gradually rises to the upper part of the synthesis reactor 5 along with the reactants, a gas collector 8 is arranged at the top of the synthesis reactor 5, the nitrogen is separated and collected at the top of the tower and returns to the nitrogen storage tank 4, and the nitrogen is circularly pumped back to the synthesis reactor 5 through a nitrogen compressor 9; the unreacted solid material continues to react at the middle lower part of the synthesis reactor 5; the generated thiodicarb is floated to the upper part of the synthesis reactor 5 and is collected by a product discharge pump 12 to be used as a raw material for next washing.
45kg of methomyl serving as a raw material is put into a methomyl storage tank 1, 1.0kg of catalyst is put into a catalyst storage tank 2, the methomyl is continuously added into a slurry tank 3 by a methomyl feeder 6 according to the proportion of 0.5kg/h, the catalyst is 0.01kg/h and the salinized product is 3kg/h, the mixture is uniformly stirred, the mixture is heated to 29 ℃, the mixture is continuously conveyed to a mixture inlet at the bottom of a synthesis reactor 5 according to the proportion of 3.51kg/h through a slurry pump connection 11, a jacket is arranged outside the synthesis reactor 5 by adopting a multistage circulating reactor, and the temperature in the reactor is controlled to be 20 ℃; nitrogen enters a nitrogen storage tank 4 and enters a gas distributor 10 at the bottom of a synthesis reactor 5 at 4Nm3/h through a nitrogen compressor 9; the nitrogen gradually rises to the upper part of the synthesis reactor 5 along with the reactants, a gas collector 8 is arranged at the top of the synthesis reactor 5, the nitrogen is separated and collected at the top of the tower and returns to the nitrogen storage tank 4, and the nitrogen is circularly pumped back to the synthesis reactor 5 through a nitrogen compressor 9; the unreacted solid material continues to react at the middle lower part of the synthesis reactor 5; the generated thiodicarb is floated to the upper part of a synthesis reactor 5, 3.51kg/h is continuously collected by a product discharge pump 12 to be used as a raw material for next washing, and after 3h of reaction, the content of methomyl is sampled and analyzed to be 0.797 percent, and the content of thiodicarb is 99.203 percent.
Example 2
45kg of methomyl serving as a raw material is put into a methomyl storage tank 1, 1.0kg of catalyst is put into a catalyst storage tank 2, the methomyl is continuously added into a slurry tank 3 by a methomyl feeder 6 according to the proportion of 1.5kg/h, the catalyst is 0.01kg/h and the salinized product is 8kg/h, the mixture is uniformly stirred, the mixture is heated to 29 ℃, the mixture is continuously conveyed to a mixture inlet at the bottom of a synthesis reactor 5 according to the proportion of 9.51kg/h through a slurry pump connection 11, a jacket is arranged outside the synthesis reactor 5 by adopting a multistage circulating reactor, and the temperature in the reactor is controlled to be 10 ℃; nitrogen enters a nitrogen storage tank 4 and enters a gas distributor 10 at the bottom of a synthesis reactor 5 at 2Nm3/h through a nitrogen compressor 9; the nitrogen gradually rises to the upper part of the synthesis reactor 5 along with the reactants, a gas collector 8 is arranged at the top of the synthesis reactor 5, the nitrogen is separated and collected at the top of the tower and returns to the nitrogen storage tank 4, and the nitrogen is circularly pumped back to the synthesis reactor 5 through a nitrogen compressor 9; the unreacted solid material continues to react at the middle lower part of the synthesis reactor 5; the generated thiodicarb is floated to the upper part of a synthesis reactor 5, 9.51kg/h is continuously extracted by a product discharge pump 12 to be used as a raw material for next washing, and after reaction for 3h, the content of the methomyl is sampled and analyzed to be 0.92 percent, and the content of the thiodicarb is 99.08 percent.
Example 3
45kg of methomyl serving as a raw material is put into a methomyl storage tank 1, 1.0kg of catalyst is put into a catalyst storage tank 2, the methomyl is continuously added into a slurry tank 3 by a methomyl feeder 6 according to the proportion of 0.4kg/h, the catalyst is 0.01kg/h and the salinized product is 3kg/h, the mixture is uniformly stirred, the mixture is heated to 40 ℃, the mixture is continuously conveyed to a mixture inlet at the bottom of a synthesis reactor 5 according to the proportion of 2.91kg/h through a slurry pump connection 11, a jacket is arranged outside the synthesis reactor 5 by adopting a multistage circulating reactor, and the temperature in the reactor is controlled to be 40 ℃; nitrogen enters a nitrogen storage tank 4 and enters a gas distributor 10 at the bottom of a synthesis reactor 5 at the speed of 7Nm3/h through a nitrogen compressor 9; the nitrogen gradually rises to the upper part of the synthesis reactor 5 along with the reactants, a gas collector 8 is arranged at the top of the synthesis reactor 5, the nitrogen is separated and collected at the top of the tower and returns to the nitrogen storage tank 4, and the nitrogen is circularly pumped back to the synthesis reactor 5 through a nitrogen compressor 9; the unreacted solid material continues to react at the middle lower part of the synthesis reactor 5; the generated thiodicarb is floated to the upper part of a synthesis reactor 5, 3.91kg/h is continuously collected by a product discharge pump 12 to be used as a raw material for next washing, and after 3h of reaction, the content of the methomyl is sampled and analyzed to be 0.67 percent, and the content of the thiodicarb is 99.33 percent.
The utility model realizes continuous operation, simple flow and less equipment investment, and by introducing nitrogen into the synthesis reactor, on one hand, a high gas content area and a low gas content area in the reactor generate larger density difference to promote the materials to form high-speed circulation inside, so that the materials are fully mixed and sheared and dissolved, the reaction is effectively promoted to the greatest extent, and the reaction rate is improved; on the other hand, by utilizing the properties of easy sedimentation of the methomyl and the salinized product and easy suspension of the thiodicarb, the products are enriched at the upper part of the reactor and are discharged in time, so that the side reaction caused by the retention of the thiodicarb generated in the original intermittent production process in the reaction kettle is avoided, and the yield is improved. The residence time required by the reaction is reduced to be within 3 hours from 6 hours, the reaction conversion rate is improved to be more than 99.0 percent from 96 percent, and the residue of the methomyl is reduced to be less than 1.0 percent from 4 percent; the utility model has the advantages of high reaction efficiency, environmental protection and high product quality.
Claims (6)
1. The utility model provides a thiodicarb synthetic reaction serialization apparatus for producing, it includes catalyst storage tank and methomyl storage tank, its characterized in that: the device comprises a methomyl storage tank, a methomyl feeder, a catalyst feeder, a slurry tank, a methomyl inlet, a catalyst inlet and a salinization inlet, wherein the lower part of the methomyl storage tank is connected with the catalyst feeder, the other ends of the methomyl feeder and the catalyst feeder are connected with the slurry tank, the upper part of the slurry tank is provided with the methomyl inlet, the catalyst inlet and the salinization inlet, a hot water channel is arranged in the slurry tank, the bottom of the slurry tank is provided with a mixture outlet, the mixture outlet is connected with the mixture inlet at the bottom of a synthesis reactor, the bottom of the synthesis reactor is also provided with a nitrogen inlet, a gas distributor is arranged in the synthesis reactor, the upper part of the synthesis reactor is provided with a gas collector and a nitrogen outlet, the side surface of the synthesis, and the upper part of the nitrogen storage tank is also provided with a fresh nitrogen inlet.
2. The thiodicarb synthesis reaction continuous production apparatus according to claim 1, wherein: and a slurry pump and a valve are arranged between the mixture outlet and the mixture inlet.
3. The thiodicarb synthesis reaction continuous production apparatus according to claim 1, wherein: and a product discharging pump is connected behind the product outlet.
4. The thiodicarb synthesis reaction continuous production apparatus according to claim 1, wherein: and a cooling machine and a nitrogen compressor are arranged between the nitrogen inlet and the mixed nitrogen outlet, and the nitrogen compressor is also connected with a nitrogen storage tank.
5. The thiodicarb synthesis reaction continuous production apparatus according to claim 1, wherein: the methomyl feeder and the catalyst feeder are solid feeders.
6. The thiodicarb synthesis reaction continuous production apparatus according to claim 1, wherein: the synthesis reactor is a bubble column, a single-stage loop reactor or a multi-stage loop reactor.
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| CN111054278A (en) * | 2019-12-02 | 2020-04-24 | 河南金鹏化工有限公司 | Continuous production process and device for thiodicarb synthesis reaction |
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