Production system and production method for continuously producing rubber vulcanization accelerator TBSI

Abstract

The present invention discloses a production system and a production method for continuously producing rubber vulcanization accelerator TBSI. In the present invention, the MBT powder feeding system and the water slurry feeding system are fixedly connected to a powder mixing pump. The powder mixing pump, the tert-butylamine feeding system, and the catalyst feeding system are respectively fixedly connected to a mixing pipeline device. The mixing pipeline device is fixedly connected to a first-stage reaction kettle through a pipeline. The first-stage reaction kettle is connected to a second-stage reaction kettle through a pumping system, and the second-stage reaction kettle is connected to a third-stage reaction kettle through a pumping system. The first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle are respectively fixedly connected to an oxygen inlet system, and the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle are also respectively fixedly connected to a pressure regulation system. The oxygen inlet system is fixedly connected to the pressure regulation system. The third-stage reaction kettle is also sequentially connected with a slurry buffer tank, a filtration system, and a drying system through pipelines. The present invention is applicable to the continuous production of vulcanization accelerator TBSI.

Description

Technical Field

[0001] The present invention belongs to the technical field of rubber vulcanization accelerator TBSI production, and particularly relates to a production system and a production method for continuously producing rubber vulcanization accelerator TBSI. Background Art

[0002] Rubber vulcanization accelerators are the main auxiliaries for promoting rubber vulcanization. Their function is to activate the vulcanizing agent when added to the rubber compound, thereby accelerating the cross-linking reaction between the vulcanizing agent and rubber molecules, achieving the effects of shortening the vulcanization time and reducing the vulcanization temperature. Rubber vulcanization accelerators are mainly classified into six types according to their chemical structures, namely sulfenamides, thiazoles, thiurams, guanidines, thioureas, and dithiocarbamates. Among them, sulfenamide accelerators account for more than 30% of the total amount of accelerators. However, with the increasingly severe national environmental protection situation, during the processing of tires and other rubber products, the generation of toxic nitrosamines will affect human physical and mental health, and the generation of nitrosamines is the result of using sulfenamide accelerators containing secondary amine groups. Therefore, the research and development of new environmentally friendly auxiliaries and the research and optimization of their preparation processes have become an inevitable trend. N-tert-butyl-bis(2-benzothiazolyl) sulfenimide (TBSI) is a general-purpose primary amine sulfenamide rubber vulcanization accelerator, which has good scorch resistance and operating stability, and can replace the widely used accelerators NOBS, DCBS, and TBBS combined with the anti-scorch agent CTP.

[0003] At present, there are five routes for the synthesis process of TBSI, namely sulfenimide chloride method, acid method, acid anhydride method, catalytic oxidation method, and hydrogen peroxide oxidation method. Chinese patent document CN106916117A discloses a process for preparing TBSI by catalytic oxidation. In this method, accelerator M is dissolved in an excessive amount of tert-butylamine to form a solution, and a catalyst is added for high-pressure reaction. However, it can be seen from the patent that the product yield of this process is only about 65%, and it belongs to batch reaction, with relatively low production efficiency. Subsequently, acetic anhydride is required for recrystallization, increasing the production cost. Summary of the Invention

[0004] In order to make up for the deficiencies of the existing process and solve the problems of batch production, low production efficiency, and poor product quality uniformity among batches in the existing process, the present invention provides a production system and a process method for continuously producing rubber vulcanization accelerator TBSI.

[0005] The present invention is realized by the following technical solutions:

[0006] A production system for continuously producing rubber vulcanization accelerator TBSI, comprising an MBT powder feeding system, a pulping water feeding system, a tert-butylamine feeding system, and a catalyst feeding system. The MBT powder feeding system and the pulping water feeding system are fixedly connected to a powder mixing pump. The powder mixing pump is fixedly connected to a mixing pipeline device through a pipeline. The tert-butylamine feeding system and the catalyst feeding system are also respectively fixedly connected to the mixing pipeline device. The mixing pipeline device is fixedly connected to a first-stage reaction kettle through a pipeline. The first-stage reaction kettle is connected to a second-stage reaction kettle through a pumping system. The second-stage reaction kettle is connected to a third-stage reaction kettle through a pumping system. The first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle are respectively fixedly connected to an oxygen inlet system. The first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle are also respectively fixedly connected to a pressure regulation system. The oxygen inlet system is fixedly connected to the pressure regulation system. The third-stage reaction kettle is also sequentially connected with a slurry buffer tank, a filtration system, and a drying system through pipelines.

[0007] Preferably, the oxygen inlet system includes three oxygen inlet pipes respectively fixedly connected to the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle. Oxygen flow regulating valve groups are provided on all three oxygen inlet pipes. The other ends of the three oxygen inlet pipes are fixedly connected to an oxygen buffer tank through pipelines. The oxygen buffer tank is connected to a liquid oxygen storage tank.

[0008] Preferably, the pressure regulation system includes three return air pipes respectively fixedly connected to the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle. Pressure regulating valve groups are provided on all three return air pipes. The other ends of the three return air pipes are fixedly connected to a gas buffer tank through another pipeline. The gas buffer tank is fixedly connected to an oxygen compressor through a pipeline. The oxygen compressor is fixedly connected to the oxygen buffer tank through a pipeline.

[0009] Preferably, the lower discharge port of the first-stage reaction kettle is connected to the upper feed port of the second-stage reaction kettle through a pumping system. The lower discharge port of the second-stage reaction kettle is connected to the upper feed port of the third-stage reaction kettle through a pumping system.

[0010] Preferably, the MBT powder feeding system includes a powder bin. A bin anti-bridging device is fixedly connected to the inner side wall of the powder bin. The lower opening end of the powder bin is fixedly connected to a screw conveyor. The discharge port of the screw conveyor is fixedly connected to a loss-in-weight feeder. Among them, the loss-in-weight feeder is a prior art. The loss-in-weight feeder includes a weighing bin, an anti-arching device, and a screw feeder. The anti-arching device is fixedly connected to the weighing bin. The lower end of the weighing bin is fixedly connected to the feed port of the screw feeder. The discharge port of the screw feeder is fixedly connected to the powder mixing pump. The discharge port of the screw conveyor is fixedly connected to the weighing bin of the loss-in-weight feeder.

[0011] Preferably, the tert-butylamine feeding system includes a delivery pump and a pipeline fixedly connected to the delivery pump. The pipeline is fixedly connected to a mixing pipeline device, and a tert-butylamine flow regulating valve group is also fixedly connected to the pipeline.

[0012] Preferably, the catalyst feeding system includes a delivery pump and a pipeline fixedly connected to the delivery pump. The pipeline is fixedly connected to a mixing pipeline device, and a catalyst flow regulating valve group is also fixedly connected to the pipeline.

[0013] Preferably, the sizing water feeding system includes a delivery pump and a pipeline fixedly connected to the delivery pump. The pipeline is fixedly connected to a powder mixing pump, and a sizing water flow regulating valve group is also fixedly connected to the pipeline.

[0014] Preferably, the pumping system connecting the first-stage reactor and the second-stage reactor includes a pipeline and a transfer pump. The first-stage reactor is fixedly connected to the pipeline, the pipeline is fixedly connected to the transfer pump, and the transfer pump is fixedly connected to the second-stage reactor through another pipeline. A liquid level regulating valve group is fixedly connected to the pipeline connecting the first-stage reactor.

[0015] Preferably, the pumping system connecting the second-stage reactor and the third-stage reactor includes a pipeline and a transfer pump. The second-stage reactor is fixedly connected to the pipeline, the pipeline is fixedly connected to the transfer pump, and the transfer pump is fixedly connected to the third-stage reactor through another pipeline. A liquid level regulating valve group is fixedly connected to the pipeline connecting the second-stage reactor.

[0016] Preferably, at least one pressure-reducing buffer tank is further connected between the third-stage reactor and the slurry buffer tank through a pipeline, and a liquid level regulating valve group is also fixedly arranged on the pipeline connecting the third-stage reactor. In the above setting, the pressure-reducing buffer tank can gradually reduce the pressure to reduce the volatilization of tert-butylamine in the slurry buffer tank and improve the purity of the product.

[0017] Preferably, the number of the pressure-reducing buffer tanks is two.

[0018] Preferably, the slurry buffer tank is also fixedly connected to a gas condenser. The purpose of the above setting is to facilitate the subsequent recovery of the tert-butylamine gas entrained in the tail gas, further reduce the consumption of tert-butylamine, and ensure the quality of the product.

[0019] Preferably, a liquid level regulating valve group is arranged on the pipeline connecting the slurry buffer tank and the filtration system.

[0020] Preferably, the filtration system is a pressure filter; the drying system is a tray drying system.

[0021] A continuous production method using the production system for continuously producing rubber vulcanization accelerator TBSI, including the above-mentioned production system for continuously producing rubber vulcanization accelerator TBSI. The continuous production method includes the following steps:

[0022] 1) The raw material MBT powder enters the weighing bin through the buffer of the powder bin. The MBT powder is continuously transported to the powder-liquid mixing pump by metering. At the same time, the pulping water is continuously transported to the powder-liquid mixing pump by adjusting the flow through the transfer pump and the flow regulating valve group. The MBT powder and the pulping water are mixed in the powder-liquid mixing pump to form a slurry;

[0023] 2) The MBT slurry is transported to the first-stage reaction kettle through a pipeline mixer, and then sequentially transported to the second-stage reaction kettle and the third-stage reaction kettle through a transfer pump and a liquid level regulating valve group. The tert-butylamine solution and the catalyst solution are pumped into the pipeline mixer, and oxygen is transported into the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle; the MBT weighing and pulping water flow regulating valve group adjusts the ratio of the MBT flow to the pulping water flow, the tert-butylamine flow regulating valve group adjusts the tert-butylamine flow ratio, and the catalyst flow regulating valve group adjusts the catalyst flow ratio. The oxygen flow in the first-stage reaction kettle is adjusted by the first-stage oxygen flow regulating valve group, the oxygen flow in the second-stage reaction kettle is adjusted by the second-stage oxygen flow regulating valve group, and the oxygen flow in the third-stage reaction kettle is adjusted by the third-stage oxygen flow regulating valve group; the pressure in the first-stage reaction kettle is controlled by adjusting through the first-stage pressure regulating valve group, the pressure in the second-stage reaction kettle is controlled by the second-stage pressure regulating valve group, and the pressure in the third-stage reaction kettle is controlled by the third-stage pressure regulating valve group;

[0024] 3) The discharge from the lower part of the third-stage reaction kettle enters the slurry buffer tank; the materials in the slurry buffer tank are transported through a pipeline to the continuous filtration and water washing device, and after filtration and water washing, they are transferred to the continuous drying device for drying to obtain the finished product.

[0025] Preferably, the flow rate of MBT powder input from the MBT powder feeding system into the powder mixing pump is 8 - 25 kg / min; the flow rate of beating water in the beating water feeding system is 16 - 100 kg / min; the flow rate of tert-butylamine in the tert-butylamine feeding system is 16 - 95 kg / min, and the mass concentration of tert-butylamine is 50% - 66%; the flow rate of the catalyst in the catalyst feeding system is 0.08 - 2.00 kg / min; the oxygen input flow rates into the first-stage reactor, the second-stage reactor, and the third-stage reactor are 5 - 50 kg / min, and the oxygen input flow rate from the oxygen inlet system into the first-stage reactor is less than that into the second-stage reactor; the oxygen input flow rate into the second-stage reactor is less than that into the third-stage reactor; the reaction pressures in the first-stage reactor, the second-stage reactor, and the third-stage reactor are 0.2 - 0.8 MPa, and under the regulation of the pressure control system, the pressure of the first-stage reactor is less than that of the second-stage reactor, and the pressure of the second-stage reactor is less than that of the third-stage reactor; the reaction temperatures in the first-stage reactor, the second-stage reactor, and the third-stage reactor are 30 - 50 °C.

[0026] Preferably, the catalyst is an aqueous solution catalyst with a mass concentration of 1% prepared by adding water to a solid catalyst; the solid catalyst is a water-soluble transition metal salt.

[0027] Preferably, the solid catalyst is one of copper chloride, copper acetate hydrate, copper acetate hydrate, copper sulfate, and copper nitrate.

[0028] Preferably, the oxygen input flow rate from the oxygen inlet system into the first-stage reactor is 25 - 33 kg / min; the oxygen input flow rate from the oxygen inlet system into the second-stage reactor is 29 - 38 kg / min; the oxygen input flow rate from the oxygen inlet system into the third-stage reactor is 32 - 43 kg / min.

[0029] Preferably, the internal liquid levels in the first-stage reactor, the second-stage reactor, and the third-stage reactor are controlled at 60% - 80% of the reactor volume.

[0030] Preferably, the liquid level of the slurry buffer tank is controlled at 30% - 50% of the slurry buffer tank volume.

[0031] Preferably, gas distributors are also provided inside the first-stage reactor, the second-stage reactor, and the third-stage reactor, and the gas distributors are fixedly connected to the pipelines extending into the first-stage reactor, the second-stage reactor, and the third-stage reactor. The above setting is beneficial to the contact between oxygen and liquid materials, making the reaction more complete.

[0032] The technical effects of the present invention:

[0033] The present invention uses a closed continuous autoclave production equipment to prepare vulcanization accelerator TBSI, realizing automatic control and continuous production of products; the pressurized closed reaction avoids the volatilization of materials, protects the environment and reduces consumption.

[0034] In this application, through the dual control of the oxygen flow regulating valve group and the in-kettle pressure control regulating valve group at the upper part of each stage of the reaction kettle, while maintaining the stability of the pressure in each stage of the kettle, by setting an oxygen flow rate far higher than the theoretical requirement, the oxygen released by the pressure control regulating valve group is compressed by a compressor and then recycled into the reaction system, increasing the circulation of oxygen in each stage of the reaction kettle, improving the contact ratio of gas and liquid, and enhancing the reaction efficiency. In this application, the oxygen flow rate of each stage of the reaction kettle is set by first calculating the theoretical oxygen amount required for a specific pressure of each stage of the reaction kettle according to the ideal gas state equation, and then inputting oxygen into each stage of the reaction kettle by adjusting the oxygen flow regulating valve group according to 1 to 5 times of the theoretical oxygen amount.

[0035] In addition, in this application, a gas distributor is also used to solve the problems of poor fluidity of oxygen in the kettle and small gas-liquid ratio, increasing the contact probability between the oxidant and the reaction materials, and enhancing the reaction efficiency. Pressure regulating valve groups are connected to the pipelines connecting the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle. The pressure regulating valve groups are used to maintain the pressure of each kettle. When the pressure in the kettle exceeds the set value, the regulating valve opens to release the oxygen pressure to the oxygen buffer tank, and then after being pressurized by the oxygen compressor, it returns to the system again, realizing the recycling of oxygen; due to the multiple supply of oxygen and the pressure regulating effect of the pressure regulating system in this application, when all mechanical equipment operates normally, it can effectively ensure the reaction time of the entire reaction, realizing continuous production, improving the equipment utilization rate and production efficiency, solving the defect that there are differences in the quality of products between batches, and avoiding the strong labor intensity of workers in intermittent production. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] The present invention will be further described below with reference to the drawings.

[0037] Figure 1 It is a structural schematic diagram of the present invention.

[0038] Figure 1 In the figure, powder bin 1, weighing bin 2, powder-liquid mixing pump 3, pulping water transfer pump 4, tert-butylamine solution transfer pump 5, catalyst transfer pump 6, pipeline mixer 7, first-stage reaction kettle 8, second-stage reaction kettle 9, third-stage reaction kettle 10, first-stage decompression buffer tank 11, second-stage decompression buffer tank 12, slurry buffer tank 13, pressure filter 14, drying system 15, gas buffer tank 16, oxygen compressor 17, oxygen buffer tank 18, liquid oxygen storage tank 19;

[0039] Bunker anti-bridging device 1-1, screw conveyor 1-2, arch-breaking device 2-1, screw feeder 2-2, flow regulating valve group for beating water 4-1, flow regulating valve group for tert-butylamine 5-1, flow regulating valve group for catalyst 6-1, primary oxygen flow regulating valve group 8-1, primary autoclave pressure regulating valve group 8-2, primary autoclave transfer pump 8-3, primary liquid level regulating valve group 8-4, secondary oxygen flow regulating valve group 9-1, secondary autoclave pressure regulating valve group 9-2, secondary autoclave transfer pump 9-3, secondary liquid level regulating valve group 9-4, tertiary oxygen flow regulating valve group 10-1, tertiary autoclave pressure regulating valve group 10-2, tertiary liquid level regulating valve group 10-3, tertiary liquid level regulating valve group 10-4, gas condenser 13-1, buffer tank liquid level regulating valve group 13-2. Detailed implementation mode

[0040] The detailed implementation example of the production system for continuously producing rubber vulcanization accelerator TBSI is as shown in Example 1:

[0041] Example 1:

[0042] A production system for continuously producing rubber vulcanization accelerator TBSI includes an MBT powder feeding system and a beating water feeding system.

[0043] Among them, the MBT powder feeding system includes a powder bunker 1. The inner side wall of the powder bunker 1 is fixedly connected with a bunker anti-bridging device 1-1. The bunker anti-bridging device 1-1 is a prior art. The lower opening end of the powder bunker 1 is fixedly connected with a screw conveyor 1-2. The discharge port of the screw conveyor 1-2 is fixedly connected with a loss-in-weight feeder. Among them, the loss-in-weight feeder is a prior art. The loss-in-weight feeder includes a weighing bunker 2, an arch-breaking device 2-1 and a screw feeder 2-2. The arch-breaking device 2-1 is fixedly connected with the weighing bunker 2. The lower end of the weighing bunker 2 is fixedly connected with the feed inlet of the screw feeder 2-2. The discharge port of the screw feeder 2-2 is fixedly connected with a powder mixing pump 3. The discharge port of the screw conveyor 1-2 is fixedly connected with the weighing bunker 2 of the loss-in-weight feeder.

[0044] The beating water feeding system includes a beating water transfer pump 4 and a pipeline fixedly connected with the beating water transfer pump 4. The pipeline is fixedly connected with the powder mixing pump 3. The pipeline is also fixedly connected with a flow regulating valve group for beating water 4-1.

[0045] The powder mixing pump 3 is fixedly connected with a mixing pipeline device 7 through a pipeline.

[0046] This application also includes a tert-butylamine feeding system and a catalyst feeding system. Among them:

[0047] The tert-butylamine feeding system includes a tert-butylamine solution delivery pump 5 and a pipeline fixedly connected to the tert-butylamine solution delivery pump 5. The pipeline is fixedly connected to a mixing pipeline device 7, and a tert-butylamine flow regulating valve group 5-1 is also fixedly connected to the pipeline.

[0048] The catalyst feeding system includes a catalyst delivery pump 6 and a pipeline fixedly connected to the catalyst delivery pump 6. The pipeline is fixedly connected to a mixing pipeline device 7, and a catalyst flow regulating valve group 6-1 is also fixedly connected to the pipeline.

[0049] The mixing pipeline device 7 is fixedly connected to a primary reaction kettle 8 through a pipeline. The primary reaction kettle 8 is connected to a secondary reaction kettle 9 through a pumping system, which consists of a primary kettle transfer pump 8-3 and a primary liquid level regulating valve group 8-4. The primary kettle transfer pump 8-3 and the primary liquid level regulating valve group 8-4 are fixedly installed on the pipeline connecting the primary reaction kettle 8 and the secondary reaction kettle 9.

[0050] The secondary reaction kettle 9 is connected to a tertiary reaction kettle 10 through a pumping system, which consists of a secondary kettle transfer pump 9-3 and a secondary liquid level regulating valve group 9-4. The secondary kettle transfer pump 9-3 and the secondary liquid level regulating valve group 9-4 are fixedly installed on the pipeline connecting the secondary reaction kettle 9 and the tertiary reaction kettle 10.

[0051] The primary reaction kettle 8, the secondary reaction kettle 9, and the tertiary reaction kettle 10 are also respectively fixedly connected with an oxygen inlet pipe. An primary oxygen flow regulating valve group 8-1, a secondary oxygen flow regulating valve group 9-1, and a tertiary oxygen flow regulating valve group 10-1 are respectively fixedly provided on the three oxygen inlet pipes. The other ends of the primary oxygen flow regulating valve group 8-1, the secondary oxygen flow regulating valve group 9-1, and the tertiary oxygen flow regulating valve group 10-1 are all fixedly connected to an oxygen buffer tank 18 through pipelines. The oxygen buffer tank 18 is fixedly connected to a liquid oxygen storage tank 19 through a pipeline.

[0052] The primary reaction kettle 8, the secondary reaction kettle 9, and the tertiary reaction kettle 10 are also respectively fixedly connected with a return air pipe. A primary kettle pressure regulating valve group 8-2, a secondary kettle pressure regulating valve group 9-2, and a tertiary kettle pressure regulating valve group 10-2 are respectively fixedly provided on the three return air pipes. The other ends of the primary kettle pressure regulating valve group 8-2, the secondary kettle pressure regulating valve group 9-2, and the tertiary kettle pressure regulating valve group 10-2 are all fixedly connected to a gas buffer tank 16 through another pipeline. The gas buffer tank 16 is fixedly connected to an oxygen compressor 17 through a pipeline. The oxygen compressor 17 is fixedly connected to the oxygen buffer tank 18 through a pipeline.

[0053] The tertiary reaction kettle 10 is also sequentially connected with a primary pressure reducing buffer tank 11, a secondary pressure reducing buffer tank 12, and a slurry buffer tank 13 through pipelines.

[0054] A three - stage liquid level regulating valve group 10 - 3 is also fixedly installed on the pipeline connecting the three - stage reaction kettle 10 and the first - stage decompression buffer tank 11. The slurry buffer tank 13 is also respectively connected to a gas condenser 13 - 1 and a pressure filter 14 through pipelines. Among them, a buffer tank liquid level regulating valve group 13 - 2 is also fixedly installed on the pipeline connecting the slurry buffer tank 13 and the pressure filter 14. The pressure filter 14 is a pressure filter purchased from the market. In this embodiment, the pressure filter used is a pressure rotary drum filter; the pressure filter 14 is fixedly connected to a disk drying system 15 through a pipeline, and this disk drying system 15 is also a prior art.

[0055] The method for continuously producing vulcanization accelerator TBSI using the continuous production system of rubber vulcanization accelerator TBSI is as shown in Examples 2 to 4:

[0056] Example 2

[0057] Adopt the method for continuously producing vulcanization accelerator TBSI using the equipment as shown in Figure 1 and include the steps:

[0058] 1) Feed the raw material MBT powder into the weighing bin 2 of the loss - of - weight feeder through the powder bin 1 in a buffered manner. The MBT powder is continuously conveyed into the powder - liquid mixing pump 3 at a flow rate of 15 kg / min. At the same time, the pulping water is continuously conveyed into the powder - liquid mixing pump through the pulping water delivery pump 4 and the pulping water flow regulating valve group 4 - 1 at a flow rate of 45 kg / min. The MBT powder and the pulping water are mixed in the powder - liquid mixing pump to form a slurry.

[0059] 2) The MBT slurry is conveyed to the first - stage reaction kettle through the pipeline mixer 7. The tert - butylamine solution and the catalyst solution are pumped into the pipeline mixer and then conveyed to the first - stage reaction kettle; and then conveyed to the second - stage reaction kettle and the third - stage reaction kettle in sequence through the transfer pump and the liquid level regulating valve group. The tert - butylamine solution and the catalyst solution are pumped into the pipeline mixer, and oxygen is conveyed into the first - stage reaction kettle, the second - stage reaction kettle, and the third - stage reaction kettle.

[0060] Among them, the MBT slurry is continuously conveyed into the pipeline mixer 7 at a flow rate of 60 kg / min; the tert - butylamine solution delivery pump 5 and the flow regulating valve group 5 - 1 continuously convey the tert - butylamine solution into the pipeline mixer 7 at a flow rate of 37.5 kg / min;

[0061] The catalyst delivery pump 6 and the catalyst flow regulating valve group 6 - 1 continuously convey the catalyst into the pipeline mixer 7 at a flow rate of 0.75 kg / min. The catalyst used is an aqueous solution catalyst with a mass concentration of 1% prepared by adding copper acetate hydrate solid catalyst to water.

[0062] Adjust the primary oxygen flow rate so that the oxygen flow rate in the primary reactor is 32 kg / min. Slowly increase the reactor pressure and set the pressure value of the primary reactor to 0.35 MPa. At the same time, turn on the jacket circulating water of the primary reactor and adjust the temperature of the primary reactor to be controlled at 40 °C. When the liquid level in the primary reactor reaches the set level, turn on the transfer pump and the primary liquid level regulating valve group connected to the primary reactor, and transfer materials to the secondary reactor;

[0063] Adjust the secondary oxygen flow rate so that the oxygen flow rate in the secondary reactor is 41 kg / min. Slowly increase the reactor pressure and set the pressure value of the secondary reactor to 0.45 MPa. At the same time, turn on the jacket circulating water of the secondary reactor and adjust the temperature of the secondary reactor to be controlled at 45 °C. When the liquid level in the secondary reactor reaches the set level, turn on the transfer pump and the secondary liquid level regulating valve group connected to the secondary reactor, and transfer materials to the tertiary reactor;

[0064] Adjust the tertiary oxygen flow rate so that the oxygen flow rate in the tertiary reactor is 36.5 kg / min. Slowly increase the reactor pressure and set the pressure value of the tertiary reactor to 0.40 MPa. At the same time, turn on the jacket circulating water of the tertiary reactor and adjust the temperature of the tertiary reactor to be controlled at 42 °C. When the liquid level in the tertiary reactor reaches the set level, turn on the transfer pump and the tertiary liquid level regulating valve group connected to the tertiary reactor, and transfer materials to the slurry buffer tank; Among them, the liquid levels of the primary reactor, secondary reactor, and tertiary reactor are all controlled at 80% of the reactor volume, and the liquid level of the slurry buffer tank is controlled at 45% of the slurry buffer tank volume;

[0065] The oxygen flow rate into the primary reactor is regulated by the primary oxygen flow rate regulating valve group 8-1, the pressure in the primary reactor is regulated by the primary reactor pressure regulating valve group 8-2, and the liquid level of the primary reactor is regulated by the primary liquid level regulating valve group 8-4; The oxygen flow rate into the secondary reactor is regulated by the secondary oxygen flow rate regulating valve group 9-1, the pressure in the secondary reactor is regulated by the secondary reactor pressure regulating valve group 9-2, and the liquid level of the secondary reactor is regulated by the secondary liquid level regulating valve group 9-4; The oxygen flow rate into the tertiary reactor is regulated by the tertiary oxygen flow rate regulating valve group 10-1, the pressure in the tertiary reactor is regulated by the tertiary reactor pressure regulating valve group 10-2, and the liquid level of the tertiary reactor is regulated by the tertiary liquid level regulating valve group 10-4;

[0066] 3) The material discharged from the lower part of the tertiary reactor enters the slurry buffer tank. Set the liquid level of the slurry in the slurry buffer tank and control it through the buffer tank liquid level regulating valve group 13-2. Transport the slurry to the continuous filtration and washing device 14 through the transfer pump, and after filtration and washing, transport it to the continuous drying device 15 for drying to obtain the TBSI finished product. The yield of the TBSI finished product is 94.5%, and the initial melting point is 130.5 °C.

[0067] Example Three

[0068] A method for continuously producing vulcanization accelerator TBSI using the equipment shown in Figure 1 comprises the steps:

[0069] 1) The raw material MBT powder is buffered through the powder silo 1 and enters the powder weighing silo 2. The MBT powder is continuously conveyed into the powder-liquid mixing pump 3 at a flow rate of 15 kg / min. At the same time, the pulping water is continuously conveyed into the powder-liquid mixing pump through the conveying pump 4 and the flow regulating valve group 4-1 at a flow rate of 37.5 kg / min. The MBT powder and the pulping water are mixed in the powder mixing pump to form a slurry.

[0070] 2) The MBT slurry is conveyed to the first-stage reaction kettle through the pipeline mixer 7. The tert-butylamine solution and the catalyst solution are pumped into the pipeline mixer and then conveyed to the first-stage reaction kettle; and then conveyed to the second-stage reaction kettle and the third-stage reaction kettle in sequence through the transfer pump and the liquid level regulating valve group. The tert-butylamine solution and the catalyst solution are pumped into the pipeline mixer, and oxygen is conveyed into the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle.

[0071] Among them, the MBT slurry is continuously conveyed into the pipeline mixer 7 at a flow rate of 52.5 kg / min; the tert-butylamine solution delivery pump 5 and the flow regulating valve group 5-1 are continuously conveyed into the pipeline mixer 7 at a flow rate of 30 kg / min;

[0072] The catalyst delivery pump 6 and the catalyst flow regulating valve group 6-1 are continuously conveyed into the pipeline mixer 7 at a flow rate of 0.5 kg / min; the catalyst used is an aqueous solution catalyst with a mass concentration of 1% prepared by adding copper chloride solid catalyst to water.

[0073] As shown in steps 2) and 3) of Example 2, the oxygen flow rate, the pressure in the kettle, the liquid level control, and the opening of the delivery pump are adjusted in sequence until the slurry is conveyed to the slurry buffer tank. The liquid level of the slurry buffer tank is set and controlled by the buffer tank liquid level regulating valve group 13-2. The slurry is conveyed to the continuous filtration and washing device 14 through the delivery pump, and after filtration and washing, it is conveyed to the continuous drying device 15 for drying to obtain the TBSI finished product. Among them, in this Example 2, the oxygen flow rate of the first-stage reaction kettle is 15.6 kg / min, the oxygen flow rate of the second-stage reaction kettle is 18.9 kg / min, and the oxygen flow rate of the third-stage reaction kettle is 21.3 kg / min; the pressure of the first-stage reaction kettle is 0.30 MPa, the pressure of the second-stage reaction kettle is 0.35 MPa, and the pressure of the third-stage reaction kettle is 0.35 MPa; the liquid levels of the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle are all controlled at 80% of the kettle volume, and the liquid level of the slurry buffer tank is controlled at 45% of the slurry buffer tank volume.

[0074] The temperatures of the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle are all controlled at 40 °C.

[0075] The product yield of the TBSI finished product prepared in Example 2 is 92.3%, and the initial melting point is 129.8 °C.

[0076] Example 4

[0077] A method for continuously producing vulcanization accelerator TBSI using the equipment as shown in Figure 1 includes the steps:

[0078] 1) The raw material MBT powder is buffered through the powder bin 1 and enters the powder weighing bin 2. The MBT powder is continuously transported into the powder-liquid mixing pump 3 at a flow rate of 15 kg / min. At the same time, the pulping water is continuously transported into the powder-liquid mixing pump through the transport pump 4 and the flow regulating valve group 4-1 at a flow rate of 37.5 kg / min. The MBT powder and the pulping water are mixed in the powder mixing pump to form a slurry.

[0079] 2) The MBT slurry is transported to the first-stage reaction kettle through the pipe mixer 7. The tert-butylamine solution and the catalyst solution are pumped into the pipe mixer and then transported to the first-stage reaction kettle; and then transported to the second-stage reaction kettle and the third-stage reaction kettle in sequence through the transfer pump and the liquid level regulating valve group. The tert-butylamine solution and the catalyst solution are pumped into the pipe mixer, and oxygen is transported into the first-stage reaction kettle, the second-stage reaction kettle, and the third-stage reaction kettle;

[0080] Among them, the MBT slurry is continuously transported into the pipe mixer 7 at a flow rate of 52.5 kg / min; the tert-butylamine solution transport pump 5 and the flow regulating valve group 5-1 are continuously transported into the pipe mixer 7 at a flow rate of 30 kg / min;

[0081] The catalyst transport pump 6 and the catalyst flow regulating valve group 6-1 continuously transport the catalyst into the pipe mixer 7 at a flow rate of 1.0 kg / min; the catalyst used is an aqueous solution catalyst with a mass concentration of 0.75% prepared by adding hydrated copper acetate solid catalyst to water. As shown in steps 2) and 3) of Example 2, the oxygen flow rate, the pressure in the kettle, the liquid level control, and the opening of the transport pump in each stage of the reaction kettle are adjusted in sequence until the slurry is transported to the slurry buffer tank. The slurry buffer tank liquid level is set and controlled by the buffer tank liquid level regulating valve group 13-2. The slurry is transported to the continuous filtration and washing device 14 through the transport pump, and after filtration and washing, it is transported to the continuous drying device 15 for drying to obtain the TBSI finished product. Among them, the oxygen flow rate in the first-stage reaction kettle is 15.6 kg / min, the oxygen flow rate in the second-stage reaction kettle is 17 kg / min, and the oxygen flow rate in the third-stage reaction kettle is 18.2 kg / min; the pressure in the first-stage reaction kettle is 0.4 MPa, the pressure in the second-stage reaction kettle is 0.45 MPa, and the pressure in the third-stage reaction kettle is 0.50 MPa;

[0082] The liquid levels of the first-stage reactor, the second-stage reactor, and the third-stage reactor are all controlled at 70% of the reactor volume, and the liquid level of the slurry buffer tank is controlled at 35% of the slurry buffer tank volume.

[0083] The temperatures of the first-stage reactor, the second-stage reactor, and the third-stage reactor are all controlled at 43 °C.

[0084] The yield of the TBSI product prepared in Example 3 is 93.6%, and the initial melting point is 129.2 °C. The above examples are only for clearly illustrating the examples of the present invention and are not intended to limit the embodiments. For those of ordinary skill in the art, the obvious changes or variations made on the basis of the above description are still within the protection scope of the present invention.

Claims

1. A production system for continuously producing rubber vulcanization accelerator TBSI, characterized in that: It includes an MBT powder feeding system, a pulping water feeding system, a tert-butylamine feeding system, and a catalyst feeding system. The MBT powder feeding system and the pulping water feeding system are fixedly connected to a powder mixing pump. The powder mixing pump is fixedly connected to a mixing pipeline device through a pipeline. The tert-butylamine feeding system and the catalyst feeding system are also respectively fixedly connected to the mixing pipeline device. The mixing pipeline device is fixedly connected to a first-stage reactor through a pipeline. The first-stage reactor is connected to a second-stage reactor through a pumping system. The second-stage reactor is connected to a third-stage reactor through a pumping system. The first-stage reactor, the second-stage reactor, and the third-stage reactor are respectively fixedly connected to an oxygen inlet system. The first-stage reactor, the second-stage reactor, and the third-stage reactor are also respectively fixedly connected to a pressure regulation system. The oxygen inlet system is fixedly connected to the pressure regulation system. The third-stage reactor is also sequentially connected with a slurry buffer tank, a filtration system, and a drying system through pipelines; The oxygen inlet system includes three oxygen inlet pipes respectively fixedly connected to the first-stage reactor, the second-stage reactor, and the third-stage reactor. Oxygen flow regulating valve groups are provided on all three oxygen inlet pipes. The other ends of the three oxygen inlet pipes are fixedly connected to an oxygen buffer tank through pipelines. The oxygen buffer tank is connected to a liquid oxygen storage tank; The pressure regulation system includes three return pipes respectively fixedly connected to the first-stage reactor, the second-stage reactor, and the third-stage reactor. Pressure regulating valve groups are provided on all three return pipes. The other ends of the three return pipes are fixedly connected to a gas buffer tank through another pipeline. The gas buffer tank is fixedly connected to an oxygen compressor through a pipeline; The oxygen compressor is fixedly connected to the oxygen buffer tank through a pipeline.

2. The production system for continuously producing rubber vulcanization accelerator TBSI according to claim 1, characterized in that: The MBT powder feeding system includes a powder silo. A bin anti-bridging device is fixedly connected to the inner side wall of the powder silo. The lower opening end of the powder silo is fixedly connected to a screw conveyor. The discharge port of the screw conveyor is fixedly connected to a loss-in-weight feeder; The loss-in-weight feeder includes a weighing bin, an anti-arching device, and a screw feeder. The anti-arching device is fixedly connected to the weighing bin. The lower end of the weighing bin is fixedly connected to the feed inlet of the screw feeder. The discharge port of the screw feeder is fixedly connected to the powder mixing pump; The discharge port of the screw conveyor is fixedly connected to the weighing bin of the loss-in-weight feeder.

3. A production system for continuously producing rubber vulcanization accelerator TBSI according to claim 1, characterized in that: At least one pressure-reducing buffer tank is also connected between the third-stage reactor and the slurry buffer tank through a pipeline. A liquid level regulating valve group is also fixedly provided on the pipeline connected to the third-stage reactor.

4. A continuous production method of a production system for continuously producing rubber vulcanization accelerator TBSI, characterized in that: It includes a production system for continuously producing rubber vulcanization accelerator TBSI as described in claim 2; The continuous production method includes the following steps: 1) Feed the raw material MBT powder into the loss-in-weight feeder through the buffer of the powder silo. The MBT powder is continuously metered and conveyed into the powder-liquid mixing pump. At the same time, the pulping water is continuously conveyed into the powder-liquid mixing pump by adjusting the flow rate through a transfer pump and a flow regulating valve group. The MBT powder and the pulping water are mixed in the powder mixing pump to form a slurry; 2) The MBT slurry is transported to the first-stage reactor through a pipeline mixer, and then successively transported to the second-stage reactor and the third-stage reactor through a transfer pump and a liquid level regulating valve group. A tert-butylamine solution and a catalyst solution are pumped into the pipeline mixer, and oxygen is transported into the first-stage reactor, the second-stage reactor, and the third-stage reactor; the MBT weighing and pulping water flow regulating valve group regulates the ratio of the MBT flow to the pulping water flow, the tert-butylamine flow regulating valve group regulates the tert-butylamine flow ratio, the catalyst flow regulating valve group regulates the catalyst flow ratio, the oxygen flow in the first-stage reactor is regulated by the first-stage oxygen flow regulating valve group, the oxygen flow in the second-stage reactor is regulated by the second-stage oxygen flow regulating valve group, and the oxygen flow in the third-stage reactor is regulated by the third-stage oxygen flow regulating valve group; the pressure in the first-stage reactor is regulated and controlled by the first-stage pressure regulating valve group, the pressure in the second-stage reactor is controlled by the second-stage pressure regulating valve group, and the pressure in the third-stage reactor is controlled by the third-stage pressure regulating valve group; 3) The discharge from the lower part of the third-stage reactor enters the slurry buffer tank; the materials in the slurry buffer tank are transported through a pipeline to a continuous filtration and washing device, and after filtration and washing, they are transferred to a continuous drying device to obtain the TBSI finished product.

5. The continuous production method of a production system for continuously producing rubber vulcanization accelerator TBSI according to claim 4, characterized in that: The flow rate of the MBT powder input from the MBT powder feeding system to the powder mixing pump is 8 - 25 kg / min; the flow rate of the pulping water in the pulping water feeding system is 16 - 100 kg / min; the flow rate of the tert-butylamine in the tert-butylamine feeding system is 16 - 95 kg / min, and the mass concentration of the tert-butylamine is 50% - 66%; the flow rate of the catalyst in the catalyst feeding system is 0.08 - 2.00 kg / min; the oxygen input flow rate into the first-stage reactor, the second-stage reactor, and the third-stage reactor is 5 - 50 kg / min, and the oxygen input flow rate into the first-stage reactor by the oxygen intake system is less than that into the second-stage reactor; The oxygen input flow rate into the second-stage reactor is less than that into the third-stage reactor; The reaction pressure in the first-stage reactor, the second-stage reactor, and the third-stage reactor is 0.2 - 0.8 MPa, and under the regulation of the pressure control system, the pressure in the first-stage reactor is less than that in the second-stage reactor, and the pressure in the second-stage reactor is less than that in the third-stage reactor; the reaction temperature in the first-stage reactor, the second-stage reactor, and the third-stage reactor is 30 - 50 °C.

6. The continuous production method of a production system for continuously producing rubber vulcanization accelerator TBSI according to claim 4, characterized in that: The catalyst is an aqueous solution catalyst with a mass concentration of 0.5 - 1.5% prepared by adding water to a solid catalyst; the solid catalyst is a water-soluble transition metal salt.

7. The continuous production method of a production system for continuously producing rubber vulcanization accelerator TBSI according to claim 5, characterized in that: The oxygen input flow rate into the first-stage reactor by the oxygen intake system is 25 - 33 kg / min; the oxygen input flow rate into the second-stage reactor by the oxygen intake system is 29 - 38 kg / min; the oxygen input flow rate into the third-stage reactor by the oxygen intake system is 32 - 43 kg / min.

8. The continuous production method of a production system for continuously producing rubber vulcanization accelerator TBSI according to claim 4, characterized in that: The liquid levels of the first-stage reactor, the second-stage reactor, and the third-stage reactor are controlled at 60% - 80% of the reactor volume.

Images