Tetraethylthiuram disulfide production reaction device

Abstract

The utility model discloses a tetraethylthiuram disulfide production reaction device which comprises a reaction kettle, a stirring structure is arranged in the reaction kettle, a jacket is arranged outside the reaction kettle, and an ethanol solution adding pipeline, a diethylamine adding pipeline, a hydrogen peroxide adding pipeline and a carbon disulfide adding pipeline are arranged at the top end of the reaction kettle. The ethanol solution adding pipeline is connected with a liquid outlet of the ethanol solution static mixer, an ethanol inlet pipeline and a soft water inlet pipeline are arranged on the ethanol solution static mixer, and the carbon disulfide gas discharging pipeline is connected with a gas inlet of the condenser; a condensate outlet pipeline of the condenser is connected with a carbon disulfide receiving tank, a bottom outlet pipeline of the carbon disulfide receiving tank is connected with a carbon disulfide adding pipeline, the carbon disulfide adding pipeline is further connected with a carbon disulfide transfer pump, and a carbon disulfide metering pump is arranged on the carbon disulfide adding pipeline. One-step safe production of tetraethylthiuram disulfide can be realized, and the production efficiency is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to a chemical industry field, concretely is a tetraethylthiuram disulfide production reaction device. BACKGROUND

[0002] Vulcanization accelerator, can be simply called accelerator, is used to accelerate vulcanization speed, shorten vulcanization time, reduce vulcanization temperature, reduce vulcanization agent dosage when rubber vulcanization, and also can improve the physical and mechanical properties of vulcanized rubber. Tetraethylthiuram disulfide (TETD) is used as the super accelerator and vulcanizing agent of natural rubber, styrene butadiene rubber, nitrile rubber, butyl rubber, cis-butadiene rubber and latex.

[0003] Most of tetraethylthiuram disulfide currently adopts two-step method: condensation first, then oxidation. First, diethylamine, sodium hydroxide and carbon disulfide are condensed under the condition of 30-40 DEG C to generate sodium diethyl dithio carbamate, then the carbon residue is filtered, and the mother liquor is oxidized by chlorine gas or nitrous acid and air to generate tetraethylthiuram disulfide, which is prepared into finished product by cooling, filtering, drying and crushing, and the yield is only 86%. This production process is relatively mature, but has the disadvantages of serious three wastes, high product consumption quota, high physical labor intensity, poor operation environment and the like.

[0004] The applicant improves and adopts ethanol (recovered ethanol), water, diethylamine and carbon disulfide for condensation reaction, and directly adds hydrogen peroxide for oxidation after the reaction is finished. The conventional operation is to manually add diethylamine, carbon disulfide and the like into the reaction kettle. Among them, carbon disulfide has low boiling point (46.2 DEG C), ignition temperature is 90 DEG C, and is a colorless transparent liquid with a slight aromatic smell under normal temperature and pressure, has strong volatility, flammability and explosiveness. And has an unpleasant rotten radish smell, has great harm to the body, and manual feeding is undoubtedly to cause a large amount of labor input, low production efficiency, and is not conducive to environmental protection and safety production. CONTENT OF THE UTILITY MODEL

[0005] In view of the defects of the prior art, the utility model provides a tetraethylthiuram disulfide production reaction device, which can realize one-step safe production of tetraethylthiuram disulfide and improve production efficiency.

[0006] In order to achieve the above object, the utility model discloses a tetraethylthiuram disulfide production reaction device through the following technical scheme, which comprises a reaction kettle, characterized in that: a stirring structure is arranged in the reaction kettle, a jacket is arranged outside the reaction kettle, an ethanol solution adding pipeline, a diethylamine adding pipeline, a hydrogen peroxide adding pipeline, a carbon disulfide adding pipeline, a carbon disulfide gas discharge pipeline and a nitrogen gas pipeline are arranged at the top of the reaction kettle, the ethanol solution adding pipeline is connected with the liquid outlet of an ethanol solution static mixer, an ethanol inlet pipeline and a soft water inlet pipeline are arranged on the ethanol solution static mixer, the ethanol inlet pipeline and the soft water inlet pipeline are connected with an ethanol transfer metering pump and a soft water transfer metering pump respectively, the soft water transfer metering pump is connected with a soft water intermediate storage tank, the diethylamine adding pipeline is connected with a diethylamine storage tank through a diethylamine metering pump, the hydrogen peroxide adding pipeline is connected with a hydrogen peroxide storage tank through a hydrogen peroxide metering pump, the carbon disulfide gas discharge pipeline is connected with the gas inlet of a condenser, the condenser condensate outlet pipeline is connected with a carbon disulfide receiving tank, the bottom outlet pipeline of the carbon disulfide receiving tank is connected with the carbon disulfide adding pipeline, the carbon disulfide adding pipeline is also connected with a carbon disulfide transfer pump, and a carbon disulfide metering pump is arranged on the carbon disulfide adding pipeline.

[0007] In the above scheme, the kettle bottom of the reaction kettle is provided with a discharge pipeline.

[0008] In the above scheme, the lower part of the jacket of the reaction kettle is provided with a general cold brine inlet pipe, and the upper part is provided with a general cold brine outlet pipe.

[0009] In the above scheme, the reaction kettle is provided with a steam coil, and the position of the steam coil is staggered with the stirring structure.

[0010] In the above scheme, the top of the reaction kettle is provided with a pressure relief valve.

[0011] In the above scheme, the condenser condensate outlet pipeline is connected with the reaction kettle.

[0012] In the above scheme, the top of the carbon disulfide receiving tank is provided with a liquid seal water inlet pipeline.

[0013] In the above scheme, the top of the carbon disulfide receiving tank is also provided with a waste gas pipeline connected with a workshop waste gas main pipe.

[0014] In the above scheme, the static mixer for the ethanol solution is equipped with a mass flow meter and a hydrometer. This allows for online measurement of the mass flow rate and specific gravity of the ethanol solution.

[0015] Ethanol and water are mixed in real time using a static mixer. The homogeneously mixed ethanol and water are then added to the reaction vessel. Using a static mixer eliminates the need for a separate storage tank for the ethanol-water solution. A predetermined amount of diethylamine is then added to the reaction vessel via a metering pump. Stirring and cooling water are then activated. A measured amount of carbon disulfide is then added dropwise to the reaction vessel via a carbon disulfide metering pump to initiate the condensation reaction. During the addition of carbon disulfide, brine is used for cooling to control the reaction temperature. After the carbon disulfide addition is complete, the reaction proceeds for 3-4 hours. After the condensation and heat preservation are completed, hydrogen peroxide is added dropwise to the reaction vessel via a hydrogen peroxide metering pump to initiate the oxidation reaction. During the addition of hydrogen peroxide, brine is used for cooling. The reaction continues at this temperature after the hydrogen peroxide addition is complete. After the oxidation and heat preservation are completed, the material in the reaction vessel is heated to 40-60°C. Unreacted carbon disulfide is discharged from the vessel and condensed in a condenser before being recycled to a carbon disulfide receiving tank for reuse in the next condensation reaction process. After the carbon disulfide is completely removed, the material in the reactor is cooled to 0-5℃. Then, the material in the reactor that has been cooled to the specified temperature is placed into a centrifuge for centrifugal dehydration to obtain the product.

[0016] This invention uses metering pumps to add materials dropwise. Each metering pump is connected to its own storage tank to achieve automatic sealed feeding, reducing harm to workers' health. After the reaction is complete, carbon disulfide is recovered for the next reaction, reducing material loss and pollution problems in subsequent processing. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the structure of this utility model. Detailed Implementation

[0018] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0019] Example 1: As Figure 1 As shown, the tetraethylthiuram disulfide production reaction apparatus includes a reactor 1, a stirring structure 2 inside the reactor 1, and a jacket outside the reactor 1. A general-purpose brine inlet pipe is located at the lower part of the jacket, and a general-purpose brine outlet pipe is located at the upper part. The general-purpose brine inlet pipe is connected to the brine circulation main pipe, and the general-purpose brine outlet pipe is connected to the general-purpose brine workshop return water main pipe.

[0020] The top of reactor 1 is equipped with ethanol solution inlet lines, diethylamine inlet lines, hydrogen peroxide inlet lines, carbon disulfide inlet lines, carbon disulfide gas outlet lines, and nitrogen line 101. Each of these lines is equipped with a feeding valve, which is automatically controlled. The ethanol solution inlet line is connected to the outlet of the ethanol solution static mixer 3. The ethanol solution static mixer 3 is equipped with an ethanol inlet line 301 and a soft water inlet line 302. These lines are connected to an ethanol transfer metering pump and a soft water transfer metering pump 401, respectively. The soft water transfer metering pump is connected to a soft water intermediate storage tank 4, which is equipped with a soft water inlet line 402. An automatically controlled valve is installed on the soft water inlet line. The ethanol transfer metering pump 1201 is connected to the ethanol intermediate storage tank 12. The static mixer 3 for the ethanol solution is equipped with a mass flow meter and a hydrometer. These are used for online measurement of the specific gravity of the ethanol solution, etc., to detect whether the mixing of the ethanol solution meets the standards. Valves are installed on each pipeline of this invention.

[0021] The diethylamine inlet pipeline is connected to the diethylamine storage tank 6 via the diethylamine metering pump 5; the hydrogen peroxide inlet pipeline is connected to the hydrogen peroxide storage tank 8 via the hydrogen peroxide metering pump 7; the carbon disulfide gas outlet pipeline is connected to the inlet of the condenser 9; and the condensate outlet pipeline of the condenser 9 is connected to the carbon disulfide receiving tank 10. Figure 1 As shown, condenser 9 is an existing condenser, including a shell and a tube layer. Cooling water flows through the shell layer, and gas enters the tube layer from the top. The gas in the tube layer is condensed by the cooling water in the shell layer, becoming condensate, which exits from the bottom outlet pipe. A branch pipe from the condensate outlet pipe of condenser 9 connects to reactor 1. The top of carbon disulfide receiving tank 10 is also equipped with an exhaust gas pipeline connected to the workshop's main exhaust gas pipe. A liquid seal water inlet pipe 1001 is installed at the top of carbon disulfide receiving tank 10 to liquid seal the temporarily stored carbon disulfide and prevent volatilization. An exhaust gas outlet pipe 1002 is installed at the top of carbon disulfide receiving tank 10, connected to the workshop's main exhaust gas pipe.

[0022] The bottom outlet pipeline of the carbon disulfide receiving tank 10 is connected to the carbon disulfide inlet pipeline, which is also connected to the carbon disulfide transfer pump 13. The carbon disulfide transfer pump 13 is connected to the intermediate carbon disulfide storage device, which includes a storage tank. The upper part of the storage tank is equipped with a water seal, and the lower part is the carbon disulfide storage area. A nitrogen seal can also be installed in addition to the water seal (details omitted here). A carbon disulfide metering pump 14 is installed on the carbon disulfide inlet pipeline. The metering pump 14 meterly adds carbon disulfide to the reaction vessel.

[0023] The bottom of the reaction kettle 1 is provided with a discharge pipeline 102. The reaction kettle 1 is provided with a steam coil 11, which is staggered with the position of the stirring structure to avoid interference with the stirring structure. The top end of the reaction kettle 1 is provided with a blow-off valve. The blow-off valve is connected with a workshop waste gas main pipe.

[0024] Although the embodiments of the present application have been shown and described, it is to be understood that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present application, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A tetraethylthiuram disulfide production reaction device comprising a reaction kettle (1), characterized in that: The reaction kettle (1) is provided with a stirring structure (2), the reaction kettle (1) is provided with a jacket, the top end of the reaction kettle (1) is provided with an ethanol solution adding pipeline, a diethylamine adding pipeline, a hydrogen peroxide adding pipeline, a carbon disulfide adding pipeline, a carbon disulfide gas discharge pipeline and a nitrogen pipeline, the ethanol solution adding pipeline is connected with the liquid outlet of an ethanol solution static mixer (3), the ethanol solution static mixer (3) is provided with an ethanol inlet pipeline (301) and a soft water inlet pipeline (302), the ethanol inlet pipeline and the soft water inlet pipeline are connected with an ethanol transfer metering pump and a soft water transfer metering pump respectively, the soft water transfer metering pump is connected with a soft water intermediate storage tank (4), the diethylamine adding pipeline is connected with a diethylamine storage tank (6) through a diethylamine metering pump (5), the hydrogen peroxide adding pipeline is connected with a hydrogen peroxide storage tank (8) through a hydrogen peroxide metering pump (7), the carbon disulfide gas discharge pipeline is connected with the gas inlet of a condenser (9), the condenser (9) is connected with a carbon disulfide receiving tank (10) through a condensate outlet pipeline, the bottom outlet pipeline of the carbon disulfide receiving tank (10) is connected with the carbon disulfide adding pipeline, the carbon disulfide adding pipeline is also connected with a carbon disulfide transfer pump, and the carbon disulfide adding pipeline is provided with a carbon disulfide metering pump.

2. The tetraethylthiuram disulfide production reaction apparatus according to claim 1, wherein: The kettle bottom of the reaction kettle (1) is provided with a discharge pipeline.

3. The tetraethylthiuram disulfide production reaction apparatus according to claim 1 or 2, characterized by: The lower part of the jacket of the reaction kettle (1) is provided with a general cold brine inlet pipeline, and the upper part is provided with a general cold brine outlet pipeline.

4. The reaction apparatus for producing tetraethylthiuram disulfide according to claim 3, wherein: The reaction kettle (1) is provided with a steam coil (11), and the steam coil (11) is staggered with the position of the stirring structure.

5. The reaction apparatus for producing tetraethylthiuram disulfide according to claim 4, wherein: The top end of the reaction kettle (1) is provided with a pressure relief valve.

6. The reaction apparatus for producing tetraethylthiuram disulfide according to claim 5, wherein: The condensate outlet pipeline of the condenser (9) is connected with the reaction kettle (1) through a branch pipeline.

7. The reaction apparatus for producing tetraethylthiuram disulfide according to claim 6, wherein: The top end of the carbon disulfide receiving tank (10) is provided with a liquid seal water inlet pipeline (1001).

8. The tetraethylthiuram disulfide production reaction apparatus according to claim 7, wherein: The top end of the carbon disulfide receiving tank (10) is also provided with a waste gas pipeline connected with a workshop waste gas main pipeline.

9. The reaction apparatus for producing tetraethylthiuram disulfide according to claim 1, wherein: The ethanol solution static mixer (3) is provided with a mass flow meter and a specific gravity meter.

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