CN112624945B - Method and equipment for continuously synthesizing rubber vulcanization accelerator S - Google Patents
Method and equipment for continuously synthesizing rubber vulcanization accelerator S Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/14—Dithiocarbamic acids; Derivatives thereof
- C07C333/16—Salts of dithiocarbamic acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/14—Dithiocarbamic acids; Derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
Abstract
The invention belongs to the technical field of production of rubber vulcanization accelerators S, and relates to a method and equipment for continuously synthesizing the rubber vulcanization accelerators S. The invention can realize continuous production from feeding to discharging, and is convenient for realizing industrialized operation. The tubular reactor has small volume, high production efficiency, stable quality of the synthesized accelerator S, no peculiar smell and improved yield of the further synthesized accelerator S.
Description
Technical Field
The invention belongs to the technical field of production of rubber vulcanization accelerators S, and relates to a method and equipment for continuously synthesizing the rubber vulcanization accelerators S.
Background
Accelerator S, chemical name: sodium dimethyldithiocarbamate, amber to greenish or white scale crystals, or light yellow to orange colored liquids. The accelerator S is an overspeed vulcanization accelerator, is suitable for latex of natural rubber, styrene-butadiene rubber, chloroprene rubber and nitrile rubber, and is also an intermediate product of a terminator and accelerator TMTD for styrene-butadiene rubber polymerization.
At present, an industrial synthesis accelerator S generally adopts an intermittent reaction mode, and raw materials cannot be fully contacted in time, are volatile, and in a production operation site, volatile smell of the raw materials is scattered in the air, so that the waste of the raw materials is caused firstly; secondly, the field environment is poor, and environmental waste gas pollution is caused; thirdly, the quality batches of the synthesized accelerator S are uneven, and the stability of quality cannot be ensured; fourthly, after the reaction, a lot of incompletely reacted waste carbon exists, a carbon separation process is increased, and potential safety hazards and raw material waste exist; fifthly, batch reaction is usually kettle reaction, the number of reaction kettles is large, and the occupied area is large.
The tubular continuous reaction has simple equipment, high mixing speed and uniform reaction condition, is not influenced by the operation factors of personnel in the intermittent reaction process, and is favorable for improving the product yield, stabilizing the quality and ensuring the operation safety in the synthesis process. Solves some technical problems existing in batch reaction, and makes up for technical defects.
Disclosure of Invention
The invention provides a novel method and equipment for continuously synthesizing a rubber vulcanization accelerator S aiming at the problems existing in the production of the traditional rubber vulcanization accelerator S.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the equipment for continuously synthesizing the rubber vulcanization accelerator S comprises an equipment body, wherein the equipment body comprises a tubular reactor, the tubular reactor is horizontally arranged, a blast pipeline is arranged above the forefront end of an inlet of the reactor, vertically penetrates into the bottom of the reactor and is flatly paved at the inner bottom of the reactor, and air outlet holes (linear arrangement) are uniformly distributed on the blast pipe flatly paved at the bottom of the reactor; the inlet of the tubular reactor is sealed at the vertical foremost end, and a circular overflow port is arranged in the middle of the vertical end of the outlet; the upper end of the rear half part of the reactor is provided with a vent valve pipeline which is connected with a tail gas absorbing device; the reactor blast pipeline is connected with a blast blower; the inlet to outlet direction of the reactor is sequentially provided with a water inlet pipeline, a dimethylamine inlet pipeline, a carbon disulfide inlet pipeline and a liquid alkali inlet pipeline; the water inlet pipeline, the dimethylamine inlet pipeline, the carbon disulfide inlet pipeline and the liquid caustic soda inlet pipeline are respectively connected with the feed pump and the storage tank; the overflow outlet of the tubular reactor is connected with a transfer tank with a stirring device, the transfer tank is connected with a pressure reducing device, the outlet of the transfer tank is connected with a solid-liquid separation device, and the outlet of the solid-liquid separation device is connected with a standing groove; an opening above the transfer tank is communicated with a tail gas absorbing device; the outside of the tubular reactor is wrapped with a heating jacket, and a temperature sensor and a pressure sensor are arranged inside the tubular reactor.
Preferably, a sampling port and a feed valve are arranged between the tubular reactor and the transfer tank; the inner wall of the transfer tank is coated with glass paint, the transfer tank is provided with a plurality of glass paint, the outer wall of the transfer tank is wrapped with a jacket, and a temperature sensor and a radar liquid level gauge are arranged in the transfer tank.
Preferably, the tubular reactor is horizontally arranged, the equipment body further comprises a controller, the input end of the controller is connected with a radar liquid level gauge, each temperature sensor and each pressure sensor, the output end of the controller is connected with each feed valve switch, each feed pump and a heat source switch of a heating jacket, and the water inlet pipeline, the dimethylamine inlet pipeline, the carbon disulfide inlet pipeline and the liquid alkali inlet pipeline are respectively connected with the feed pumps in a linkage control mode.
Preferably, the regulating valves of the four raw materials of water, dimethylamine, carbon disulfide and liquid caustic soda and the regulating valve of the air blower are automatically interlocked, and when one material stops dripping or blowing, the valves of the rest materials are immediately cut off.
The method for continuously synthesizing the rubber vulcanization accelerator S adjusts the reaction temperature in the tubular reactor to 30-45 ℃ and the temperature in the transfer tank to 30-45 ℃; after the four raw materials of water, dimethylamine, carbon disulfide and liquid alkali are arranged in the order from an inlet to an outlet of the tubular reactor, firstly starting a water feeding pump switch, and then sequentially starting the dimethylamine, carbon disulfide and liquid alkali feeding pump switch, wherein the four raw materials are started at intervals of 1s respectively through linkage control; the residence time of water, dimethylamine, carbon disulfide and liquid caustic soda in the tubular reactor is 3-6 seconds; the flow ratio of water, dimethylamine, carbon disulfide and liquid alkali is (7-8): (25-30): (10-15): (15-20); after the reaction is finished, the materials flow into a transfer kettle to be collected, then the materials are decompressed and concentrated at 30-45 ℃ to separate out crystals, the crystals stand for 20-24 hours, and the green or off-white crystals are obtained through suction filtration, so that the finished product accelerator S is obtained.
Preferably, the liquid alkali is sodium hydroxide solution with the mass fraction of 30-35%, the dimethylamine is aqueous solution with the mass fraction of 40-42%, and the mass fraction of carbon disulfide is not less than 98%.
Preferably, water with mass fraction lower than 2% is added into the carbon disulfide material.
The traditional batch reaction equation is:
the invention adopts a tubular reactor, and the reaction equation is as follows:
the advantages are that: the invention strictly controls the feeding sequence of each raw material in the tubular reactor, ensures that each step of reaction is clear and the reaction is carried out in sequence, ensures that the synthesis process of the next step is carried out after each step of synthesis is full, and ensures that the reaction can be continuously and rapidly carried out.
Compared with the prior art, the invention has the advantages and positive effects that:
the invention can realize continuous production from feeding to discharging, and is convenient for realizing industrialized operation. The tubular reactor has small volume, high production efficiency, stable quality of the synthesized accelerator S, no peculiar smell and improved yield of the further synthesized accelerator S.
Drawings
Fig. 1 is a schematic view of the lower part structure of the air duct.
FIG. 2 is a flow chart of the present invention.
Detailed Description
In order that the above objects, features and advantages of the invention will be more clearly understood, a further description of the invention will be provided with reference to specific examples. It should be noted that, in the case of no conflict, the embodiments of the present application and the features in the embodiments may be combined with each other.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as described herein, and therefore the present invention is not limited to the specific embodiments of the disclosure that follow.
Example 1
This example provides the structure of a continuous reaction apparatus.
The utility model provides a continuous synthetic rubber vulcanization accelerator S' S equipment, includes the equipment body, the equipment body includes tubular reactor, tubular reactor horizontal installation, reactor entry front end top is provided with the blast pipe, and the blast pipe is vertical to go deep into the reactor bottom to the tiling is in the reactor bottom, tiling evenly distributed air outlet on the blast pipe of reactor bottom, and the air outlet is arranged linearly, can set up one or more rows, according to actual feed rate design, this embodiment is one row. One end of the inlet of the tubular reactor is closed at the outermost side (the leftmost end of the reactor in fig. 2), and a circular overflow port is arranged in the middle of the outlet end (the rightmost end of the reactor in fig. 2); the upper end of the rear half part of the reactor is connected with a vent valve pipeline which is connected with a tail gas absorbing device; the reactor blast pipeline is connected with a blast blower; the inlet to outlet direction of the reactor is sequentially provided with a water inlet pipeline, a dimethylamine inlet pipeline, a carbon disulfide inlet pipeline and a liquid alkali inlet pipeline; the water inlet pipeline, the dimethylamine inlet pipeline, the carbon disulfide inlet pipeline and the liquid caustic soda inlet pipeline are respectively connected with the feed pump and the storage tank. In actual production, four raw materials of water, dimethylamine, carbon disulfide and liquid caustic soda can also be connected to the tubular reactor through a centrifugal pump, a flowmeter and a regulating valve. The feed pipes for the four raw materials were vertical and penetrated the inner wall of the reactor. The regulating valves for adding samples of four raw materials are automatically interlocked with the regulating valve of the air blower, and when one material stops dripping or blowing, the valves of the rest materials are immediately cut off. The four raw materials of water, dimethylamine, carbon disulfide and liquid alkali are uniformly distributed on the tubular reactor at the same distance, and an overflow port is arranged at the middle position of the outlet end of the tubular reactor, so that the residence time of the materials in the tubular reactor is kept at 3-6s, the materials can react more fully and rapidly, and the pipe diameter of the tubular reactor and the position of each material feed port can be calculated and specifically designed according to the residence time and the material consumption during actual production. Before raw materials are added dropwise, an air valve is opened; when raw materials are added dropwise, a water valve is firstly opened, pure water with the temperature of about 45 degrees is preferably added during production, after the water valve is opened, dimethylamine, carbon disulfide and liquid alkali valves are sequentially opened, and the opening time of the four raw materials is respectively 1s at intervals through linkage control. The reaction temperature is kept at 30-45 ℃, circulating water is introduced into the jacket of the tubular reactor for heat preservation reaction in the embodiment, and the circulating water inlet pipeline is connected to the inlet pipeline at the lower part of the jacket of the tubular reactor through a centrifugal pump and a regulating valve. The tubular reactor is provided with a temperature sensor, when the sensed temperature deviates from the reaction required temperature through linkage control, the temperature of the circulating water is changed, the valve opening degree of the regulating valve is regulated, the circulating speed of the circulating water is regulated, the reaction temperature is controlled within the reaction required temperature range, the temperature regulating mode is a common temperature control mode in chemical production, the embodiment is not repeated, other heating modes such as electric heating, coil heating and the like can be adopted, and the temperature regulating mode is within the protection range of the invention. The outlet of the tubular reactor is connected with a transfer tank with a stirring device, the transfer tank is connected with a pressure reducing device, the outlet of the transfer tank is connected with a solid-liquid separation device, and the outlet of the solid-liquid separation device is connected with a standing groove; an opening above the transfer tank is communicated with a tail gas absorbing device. The upper parts of the reactor and the transfer tank are connected with the tail gas absorbing device, the two pipelines can be designed independently, and the two pipelines can be connected to the tail gas absorbing device in parallel after being collected by the tail gas absorbing pipelines respectively, and the tail gas absorbing device is equipment adopted in the traditional S production. In this embodiment, several identical transfer tanks are connected in parallel at the outlet of the tubular reactor, and the transfer tanks can bear pressure and are provided with jackets. The circulating water in the jacket is used for preserving heat of materials in the transfer tank, the water inlet pipe orifice of the circulating water in the jacket is connected with the regulating valve, meanwhile, the transfer tank is internally provided with a temperature sensor, and the opening degree of the circulating water regulating valve is regulated by self control to keep the materials in the transfer tank stable within the process requirement range. The radar liquid level gauge is arranged in each transfer tank, automatic control is realized through the connection controller, after the materials in the transfer tanks rise to a certain liquid level, the transfer tank feeding valve is closed through automatic control, and the other transfer tank feeding valve is opened simultaneously, and the automatic control is sequentially performed. The junction of the tubular reactor and the transfer tank is provided with a sampling emptying valve. Each transfer tank is connected with a vacuum-pumping decompression device, and liquid materials are concentrated and crystallized at a certain temperature through the decompression device. And the outlets of the transfer tanks are connected with a set of continuous solid-liquid separation device, and are used for receiving crystals and residual liquid from each transfer tank and carrying out solid-liquid separation. The solid-liquid separation device may be a filtration device or a centrifugation device. The solid-liquid separation device is connected with the standing groove and is used for standing and drying the solid obtained by solid-liquid separation; and standing and drying to obtain the qualified accelerator S.
In the embodiment, a sampling port and a feed valve are arranged between the tubular reactor and the transfer tank; the inner wall of the transfer tank is coated with glass paint, the transfer tank is provided with a plurality of glass paint, the outer wall of the transfer tank is wrapped with a jacket, and a temperature sensor and a radar liquid level gauge are arranged in the transfer tank.
In this embodiment, the tubular reactor is horizontally installed, a row of blast pipes are arranged inside the tubular reactor, a blow-down pipe is arranged on the upper portion of the tubular reactor and is connected with a tail gas absorbing device, an overflow outlet is arranged at the tail end of the tubular reactor, the device body further comprises a controller, the input end of the controller is connected with a radar liquid level gauge, each temperature sensor and each pressure sensor, the output end of the controller is connected with a feed valve switch, a feed pump and a heat source switch of a heating jacket, and a water inlet pipeline, a dimethylamine inlet pipeline, a carbon disulfide inlet pipeline and a liquid alkali inlet pipeline are respectively connected with the feed pumps in a linkage control manner.
In the embodiment, the anticorrosive paint is lined in the tubular reactor, and is horizontally placed and installed at the same time, a row of blast pipes are arranged at the bottom of the inside of the tubular reactor, the upper part of the tubular reactor is provided with a blow-down pipe connected with a tail gas absorbing device, the inlet of the tubular reactor is vertically sealed at the forefront end, and the tail end of the tubular reactor is provided with an overflow outlet. The materials enter the tubular reactor through the feed inlet, firstly: the blast pipe is used for carrying out micro air quantity, so that various raw materials are uniformly mixed, the reaction is quick and sufficient, the burdensome of speed reduction stirring is reduced, and the equipment is simple and portable and occupies a small area; secondly, it is: the material flows into the next working procedure while reacting through the overflow port; thirdly, the method comprises the following steps: ensures that the reaction residence time of the materials in the tubular reactor is kept between 3 and 6 seconds.
According to the advancing direction of the materials, sequentially designing water, dimethylamine, carbon disulfide and liquid alkali storage tanks, wherein each material storage tank is connected with a peristaltic pump and a tubular reactor through a silica gel pipeline, or a stainless steel pipeline lined with anticorrosive paint is used for connecting a centrifugal pump and a flowmeter in production, and continuously entering the tubular reactor according to the designed flow rate.
The outlet of the tubular reactor is connected with the transfer tank, and a sampling port is reserved at the joint of the tubular reactor and the transfer tank for sampling and detecting. Transfer pot requirements: and (3) a step of: the inner wall of the transfer tank is lined with glass smooth paint, so that the synthesized material is prevented from being stuck to the inner wall; and II: the transfer tank can be internally provided with deceleration stirring, so that the materials can uniformly and stably enter the next working procedure; thirdly,: the transfer tank is required to be pressure-bearing, and an opening is required to be connected with a pipeline to the tail gas absorbing device.
Example 2
This example provides a method of continuously synthesizing a rubber vulcanization accelerator S.
30ml of water, 115ml of dimethylamine aqueous solution with the mass fraction of 40%, 57ml of carbon disulfide with the mass fraction of 98% (adding a small amount of water for liquid sealing, reducing volatilization) and 81ml of sodium hydroxide aqueous solution with the mass fraction of 32% are respectively measured by using a measuring cylinder, and are put into four customized glass beakers with glass outlets and switches at the bottoms, wherein a steam pipeline is introduced into the glass beakers for placing water, the water is heated and kept at the temperature of 40-45 ℃, and meanwhile, a thermometer is inserted for measurement. The rest raw materials are fed at normal temperature. Before raw materials are added dropwise, a blower is turned on; when the raw materials are added, firstly 30ml of water is added dropwise, the rotation speed of a peristaltic pump is 7.6 revolutions per minute, then 115ml of dimethylamine is added dropwise, the rotation speed of the peristaltic pump is 25.8 revolutions per minute, then 57ml of carbon disulfide is added dropwise, the rotation speed of the peristaltic pump is 13 revolutions per minute, and finally 81ml of liquid caustic soda is added dropwise, and the rotation speed of the peristaltic pump is 18.2 revolutions per minute. The four materials are added into the tubular reactor in a dripping way according to the above adding amount and peristaltic pump rotating speed and the set adding sequence at intervals of 1s. The tubular reactor in this example had a diameter of 2cm and a length of 30cm. The positions of the feed inlets of the four substances of water, dimethylamine, carbon disulfide and liquid alkali on the tubular reactor are as follows: the uppermost inlet of the tubular reactor is 2cm, the uppermost inlet of the tubular reactor is 4 cm, the uppermost inlet of the tubular reactor is 6 cm, the uppermost inlet of the tubular reactor is 8 cm, and the tubular reactor is horizontally arranged.
The temperature of raw material water is controlled at 45 ℃, so that the temperature of the whole reaction system can be controlled between 30 and 45 ℃, and other raw materials are normal-temperature raw materials. The temperature measuring port can be arranged beside the sampling port.
The same amount of material was used to synthesize 1 batch of material in a batch reaction requiring 90 minutes, the synthesized material was dark yellow in color, non-uniform in specific gravity, between 1.070 and 1.076g/ml, and the material had a sharp taste. By adopting the embodiment, 1 batch of material can be synthesized within 30 minutes. The appearance of the synthesized material is colorless or light yellow, the mixture is repeated for 3 times in parallel, the obtained product has uniform specific gravity and is stable at 1.070g/ml, and the material has almost no peculiar smell.
The obtained liquid accelerator S was concentrated under reduced pressure at 30-45℃for 30 minutes, and after crystals were completely precipitated, suction filtration was carried out to obtain 131gS (in this example, both the reduced pressure and suction filtration were the conventional steps in the batch reaction operation), with a yield of 99.8% and a purity of 99.9%.
Example 3
The feed reaction was carried out by increasing the feed rate of the raw materials based on the conditions in example 2.
When the temperature of the reaction system is 25-45 ℃, a blower is turned on, 57ml of water, the peristaltic pump rotating speed is 28.8 revolutions per minute, 218.5ml of dimethylamine, the peristaltic pump rotating speed is 98.0 revolutions per minute, 108.3ml of carbon disulfide, the peristaltic pump rotating speed is 49.4 revolutions per minute, 153.9ml of liquid alkali and the peristaltic pump rotating speed is 69.2 revolutions per minute are sequentially turned on, and the four materials are dripped into the tubular reactor according to the above adding amount and peristaltic pump rotating speed.
The liquid flowing out of the tubular reactor is accelerator S, the appearance is light yellow liquid, no peculiar smell exists, the specific gravity is 1.070g/ml, and no waste carbon exists. Concentrating the liquid accelerator S under reduced pressure at 30 ℃ for 45min, and filtering after crystals are completely separated out to obtain 248.9gS of the crystal accelerator, wherein the yield is 99.7% and the purity is 99.9%.
Example 4
This example differs from example 2 in that the raw materials for the entire reaction were expanded in equal proportions and continuously operated for 24 hours. After 30min, sampling is carried out at random, the sampling frequency is not less than 6 times, and the stability of the product is detected. The results are shown in Table 1.
TABLE 1 results of the sample measurements taken at various times after the start of the reaction
From the detection data, the continuous reaction product of the embodiment has very stable quality, stable specific gravity of 1.070g/ml, light yellow to colorless appearance and no peculiar smell.
The present invention is not limited to the above-mentioned embodiments, and any equivalent embodiments which can be changed or modified by the technical content disclosed above can be applied to other fields, but any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical substance of the present invention without departing from the technical content of the present invention still belong to the protection scope of the technical solution of the present invention.
Claims (5)
1. The equipment for continuously synthesizing the rubber vulcanization accelerator S comprises an equipment body and is characterized in that the equipment body comprises a tubular reactor, the tubular reactor is horizontally arranged, a blast pipeline is arranged above the forefront end of an inlet of the reactor, vertically penetrates into the bottom of the reactor and is flatly paved at the inner bottom of the reactor, and air outlets are uniformly distributed on a blast pipe flatly paved at the bottom of the reactor; the inlet of the tubular reactor is sealed at the vertical foremost end, and a circular overflow port is arranged in the middle of the vertical end of the outlet; the upper end of the rear half part of the reactor is provided with a vent valve and a vent pipeline, and the vent pipeline is connected with a tail gas absorbing device; the reactor inlet to outlet direction are provided with water inlet pipeline, dimethylamine inlet pipeline, carbon disulfide inlet pipeline, liquid alkali inlet pipeline with the same interval distance in proper order, and the feed inlet position of four kinds of substances of water, dimethylamine, carbon disulfide, liquid alkali on the tubular reactor is in proper order: 2cm of the uppermost inlet of the tubular reactor, 4 cm of the uppermost inlet of the tubular reactor, 6 cm of the uppermost inlet of the tubular reactor and 8 cm of the uppermost inlet of the tubular reactor; the water inlet pipeline, the dimethylamine inlet pipeline, the carbon disulfide inlet pipeline and the liquid caustic soda inlet pipeline are respectively connected with the feed pump and the storage tank; the outlet of the overflow port is connected with a transfer tank with a stirring device, the transfer tank is connected with a pressure reducing device, the outlet of the transfer tank is connected with a solid-liquid separation device, and the outlet of the solid-liquid separation device is connected with a standing groove; an opening above the transfer tank is also communicated with a tail gas absorbing device; the outside of the tubular reactor is wrapped with a heating jacket, and a temperature sensor and a pressure sensor are arranged in the tubular reactor;
the method for continuously synthesizing the rubber vulcanization accelerator S comprises the following steps: adjusting the reaction temperature in the tubular reactor to 30-45 ℃, placing four raw materials of water, dimethylamine, carbon disulfide and liquid caustic soda in the order from the inlet end to the outlet end of the tubular reactor, and opening a blower before dropwise adding the raw materials; when raw materials are added dropwise, firstly starting a water feed pump switch, then sequentially starting dimethylamine, carbon disulfide and liquid alkali feed pump switches, and respectively starting the four raw materials at intervals of 1s by linkage control; the residence time of water, dimethylamine, carbon disulfide and liquid caustic soda in the tubular reactor is 3-6 seconds; the flow ratio of water, dimethylamine, carbon disulfide and liquid alkali is (7-8): (25-30): (10-15): (15-20); after the reaction is finished, the materials flow into a transfer kettle to be collected, then the materials are decompressed and concentrated at 30-45 ℃ to separate out crystals, the crystals stand for 20-24 hours, and the green or off-white crystals are obtained through suction filtration, so that the finished product accelerator S is obtained.
2. The apparatus for continuously synthesizing a rubber vulcanization accelerator S according to claim 1, wherein a sampling port and a feed valve are provided between the tubular reactor and the transfer tank; the inner wall of the transfer tank is coated with glass paint, the transfer tank is provided with a plurality of glass paint, the outer wall of the transfer tank is wrapped with a jacket, and a temperature sensor and a radar liquid level gauge are arranged in the transfer tank.
3. The apparatus for continuously synthesizing a rubber vulcanization accelerator S according to claim 2, wherein the apparatus body further comprises a controller, the input end of the controller is connected with the radar level gauge and each temperature sensor, the output end of the controller is connected with each feed valve switch, each feed pump and the heat source switch of the heating jacket, and the water inlet pipeline, the dimethylamine inlet pipeline, the carbon disulfide inlet pipeline and the liquid alkali inlet pipeline are respectively connected with the feed pumps for linkage control.
4. The apparatus for continuously synthesizing a rubber vulcanization accelerator S according to claim 1, wherein the liquid alkali is a sodium hydroxide solution with a mass fraction of 30-35%, the dimethylamine is an aqueous solution with a mass fraction of 40-42%, and the carbon disulfide mass fraction is not less than 98%.
5. The apparatus for continuously synthesizing a rubber vulcanization accelerator S according to claim 1, wherein less than 2% by mass of water is added to the carbon disulfide material.
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