Production device for synthesizing TBTD in one step

Abstract

The utility model provides a production device for synthesizing TBTD in one step, which comprises a reaction kettle, a di-n-butylamine adding pipeline, a hydrogen peroxide adding pipeline, a carbon disulfide adding pipeline, a soft water adding pipeline, a carbon disulfide gas discharging pipeline and a nitrogen pipeline are arranged at the top end of the reaction kettle, and the carbon disulfide gas discharging pipeline is connected with a gas inlet of a 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, and the carbon disulfide adding pipeline is further connected with a carbon disulfide transfer pump; hydrogen peroxide is adopted as an oxidizing agent, so that high-salinity wastewater discharge is reduced; the reaction liquid is washed with water for many times to remove residual alkali liquor and byproducts, water is used as a solvent to replace a traditional methanol / ethanol system, and emission of VOCs is reduced; the metering pump is used for dropwise adding materials, so that automatic sealing feeding is realized, and harm to bodies of workers is reduced; carbon disulfide is recycled for next reaction, so that the material loss is reduced, and the pollution problem in the subsequent treatment process is reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to the related technical field of chemical production, especially to a production device of one-step synthesis TBTD. BACKGROUND

[0002] Di (thioperoxyl dimethyl formyl) tetrabutyl diamine (TBTD), di (thioperoxyl dimethyl formyl) tetrabutyl diamine is an organic compound. Colorless to light yellow solid. Solubility is good in nonpolar solvents, such as ethanol, acetone etc. Di (thioperoxyl dimethyl formyl) tetrabutyl diamine (TBTD) is a strong oxidant, can be used as active oxidizing reagent in organic synthesis reaction. It is often used in oxidation embrittlement reaction, heterocyclic synthesis reaction, olefin anion polymerization etc. Also be applied to explosive preparation aspect, have certain use in the field of explosives, also can be used as the super accelerator of natural rubber and synthetic rubber, also can be used as vulcanizing agent.

[0003] The current synthesis method is complex, generally needs high-purity raw materials and special synthesis operation. Such as including the following steps:

[0004] (1) the preparation of sodium dibutyl carbamate: first dibutylamine and water are stirred and dissolved, then carbon disulfide and sodium carbonate are added, and sodium dibutyl dithiocarbamate is generated by reaction.

[0005] (2) preparation of accelerator TBTD: first, potassium ferricyanide is added to the prepared sodium dibutyl dithiocarbamate, and then the reaction is carried out under stirring, and then the reaction product is washed with water and filtered, and accelerator TBTD is obtained.

[0006] The reaction method is complex. The applicant optimizes the reaction, uses di-n-butylamine and carbon disulfide as main raw materials, carries out condensation reaction in alkaline aqueous environment, uses hydrogen peroxide (H2O2) as oxidant, replaces traditional chlorine or sodium hypochlorite or potassium ferricyanide, and reduces high-salt wastewater discharge. The reaction liquid is separated by standing, and the water phase and the oil phase are removed, and the oil phase is washed with water for several times to remove residual lye and unreacted raw materials. The utility model uses water as solvent to replace traditional methanol / ethanol system, reduces VOCs emission. Therefore, the applicant also hopes to develop a device for automatic production of TBTD. UTILITY MODEL CONTENT

[0007] The utility model aims at providing a production device of one-step synthesis TBTD, which can realize safe production of TBTD, reduce VOCs emission and improve production efficiency.

[0008] To this end, the utility model adopts technical scheme, a kind of production device of one-step synthesis TBTD, including reaction kettle, be provided with stirring structure in the reaction kettle, the reaction kettle outside is provided with jacket, it is characterized by: the top of the reaction kettle is provided with di-n-butylamine addition pipeline, hydrogen peroxide addition pipeline, carbon disulfide addition pipeline, soft water addition pipeline, carbon disulfide gas discharge pipeline and nitrogen gas pipeline, the carbon disulfide gas discharge pipeline is connected with the gas inlet of condenser, the condenser condensate outlet pipeline is connected with carbon disulfide receiving tank, the bottom outlet pipeline of carbon disulfide receiving tank is connected with carbon disulfide addition pipeline, carbon disulfide addition pipeline is also connected with carbon disulfide transfer pump, carbon disulfide addition pipeline is provided with carbon disulfide metering pump, the bottom of the reaction kettle is provided with water phase discharge pipeline and oil phase discharge pipeline, the water phase discharge pipeline is connected with waste water collection tank, the oil phase discharge pipeline is connected with washing kettle, the top of the washing kettle is provided with soft water addition pipeline, the bottom of the washing kettle is provided with water phase outlet pipeline and washing water temporary storage tank connection, and oil phase outlet pipeline goes to drying device;The washing water temporary storage tank is connected with waste water treatment tank and the soft water addition pipeline of reaction kettle by washing water transfer pump.

[0009] As the preferred of above-mentioned scheme, the di-n-butylamine addition pipeline is connected with di-n-butylamine storage tank by di-n-butylamine metering pump, and the hydrogen peroxide addition pipeline is connected with hydrogen peroxide storage tank by hydrogen peroxide metering pump.

[0010] Further preferably, the lower portion of the jacket of the reaction kettle is provided with a universal cold brine inlet pipe, and the upper portion is provided with a universal cold brine outlet pipe.

[0011] Further preferably, the reaction kettle is provided with a steam coil, and the steam coil is staggered with the position of the stirring structure.

[0012] Further preferably, the top of the carbon disulfide receiving tank is provided with a liquid seal water inlet pipe.

[0013] The present application uses hydrogen peroxide (H2O2) as an oxidizing agent, instead of traditional chlorine or sodium hypochlorite, to reduce high-salinity wastewater discharge; the reaction liquid is stratified after standing, and the oil phase is washed with water multiple times to remove residual alkali and byproducts, using water as a solvent instead of the traditional methanol / ethanol system to reduce VOCs emissions. The metering pump is used to add and drop the material, and each metering pump is connected with a respective storage tank to realize automatic sealed feeding and reduce the harm to workers' bodies; after the reaction is completed, the carbon disulfide is recovered for the next reaction, reducing material loss and reducing pollution in the subsequent processing process. The present application is a one-step reaction, the device is simple, and the operation is easy. BRIEF DESCRIPTION OF DRAWINGS

[0014] Figure 1 It is a structural schematic diagram of the utility model. DETAILED DESCRIPTION

[0015] The utility model will be further described below in combination with the drawings and examples.

[0016] As Figure 1 shown, a production device for one-step synthesis of TBTD includes a reaction kettle 1, the reaction kettle 1 is provided with a stirring structure 2, the reaction kettle 1 is provided with a jacket 3 outside, the lower part of the jacket 3 of the reaction kettle 1 is provided with a general cold brine inlet pipe, and the upper part is provided with a general cold brine outlet pipe. The materials in the reaction kettle 1 are cooled by brine. The reaction kettle 1 is provided with a steam coil 10, and the steam coil 10 is staggered with the position of the stirring structure 2. Steam is introduced into the steam coil 10 to vaporize and discharge carbon disulfide in the reaction kettle 1. The top end of the reaction kettle 1 is provided with a pressure relief valve. The pressure relief valve is connected with a waste gas treatment device. Valves are arranged on each pipeline of the utility model.

[0017] The top end of the reaction kettle 1 is provided with a di-n-butylamine adding pipeline 402, a hydrogen peroxide adding pipeline 502, a carbon disulfide adding pipeline 701, a soft water adding pipeline, a carbon disulfide gas discharge pipeline and a nitrogen pipeline, the di-n-butylamine adding pipeline 402 is connected with a di-n-butylamine storage tank 4 through a di-n-butylamine metering pump 401, the hydrogen peroxide adding pipeline 502 is connected with a hydrogen peroxide storage tank 5 through a hydrogen peroxide metering pump 501, the carbon disulfide gas discharge pipeline is connected with the gas inlet of a condenser 6, and the condenser 6 condensate outlet pipeline is branched into a pipeline connected with the reaction kettle 1. When an abnormality occurs in the reaction process, the uncondensed gas in the condensation reaction process can be used to return to the kettle.

[0018] The condenser 6 condensate outlet pipeline is connected with a carbon disulfide receiving tank 7, the bottom outlet pipeline of the carbon disulfide receiving tank 7 is connected with the carbon disulfide adding pipeline 701, the carbon disulfide adding pipeline 701 is also connected with a carbon disulfide transfer pump 702, a carbon disulfide metering pump is arranged on the carbon disulfide adding pipeline 701, and the top end of the carbon disulfide receiving tank 7 is provided with a liquid seal water inlet pipeline. Since the density of carbon disulfide is greater than that of water and carbon disulfide is insoluble in water, volatilization of carbon disulfide can be avoided through liquid sealing. The top end of the carbon disulfide receiving tank 7 is also provided with a waste gas pipeline connected with a workshop waste gas main pipeline. The condenser 6 is an existing condenser, including a shell layer and a tube layer, the shell layer is introduced into condensate water, the gas enters the tube layer from the upper end, and the gas in the tube layer is condensed by the condensate water in the shell layer and becomes condensate liquid which comes out from the bottom outlet pipeline.

[0019] The bottom of the reaction kettle 1 is provided with a water phase discharge pipeline and an oil phase discharge pipeline, the water phase discharge pipeline is connected with a wastewater collection tank, the oil phase discharge pipeline is connected with a washing kettle 8, the top end of the washing kettle 8 is provided with a soft water adding pipeline, the bottom end of the washing kettle 8 is provided with a water phase outlet pipeline connected with a washing water temporary storage tank 9 and an oil phase outlet pipeline connected with a drying device; the washing water temporary storage tank 9 is connected with a wastewater treatment tank and the soft water adding pipeline of the reaction kettle 1 through a washing water circulating pump 901. A specified amount of di-n-butylamine and soft water (a metering pump or a flow meter can also be arranged on the soft water adding pipeline) are added into the reaction kettle 1 through a metering pump, then stirring and cooling water are started, then a specified amount of carbon bisulfide is added into the reaction kettle 1 through a carbon bisulfide metering pump for condensation reaction, salt water is used for cooling during the process of adding carbon bisulfide, the reaction temperature is controlled, after the addition of carbon bisulfide is completed, the reaction is stirred until the reaction is completed. After the condensation heat preservation is completed, hydrogen peroxide is added into the reaction kettle 1 through a hydrogen peroxide metering pump 501 for oxidation reaction, salt water is used for cooling during the process of adding hydrogen peroxide, the reaction is carried out at this temperature after the addition of hydrogen peroxide is completed. After the oxidation heat preservation is completed, the material in the reaction kettle 1 is heated to 40-60 DEG C, the unreacted carbon bisulfide in the kettle is discharged, the discharged carbon bisulfide is condensed through a condenser 6 and then recovered into a carbon bisulfide receiving tank 7 for use in the next batch of condensation reaction process. After the carbon bisulfide is discharged, the reaction kettle 1 is placed and stratified, the water phase is discharged to the wastewater collection tank, the oil phase enters the washing kettle 8 and is washed with soft water for multiple times to remove residual lye and unreacted raw materials, the washed water phase enters the wastewater treatment tank or is connected to the soft water adding pipeline of the reaction kettle 1 and then enters the reaction kettle 1 for reaction, and the oil phase enters the drying device for next step treatment.

[0020] Although the embodiments of the present application have been shown and described, those skilled in the art can understand that various changes, modifications, replacements and variations can be made to the embodiments without departing from the principles and purposes of the present application, and the scope of the present application is defined by the claims and their equivalents.

Claims

1. A production device for one-step synthesis of TBTD, comprising a reaction kettle (1), wherein a stirring structure (2) is arranged in the reaction kettle (1), and a jacket (3) is arranged outside the reaction kettle (1), characterized in that: The top end of the reactor (1) is provided with di-n-butylamine adding pipeline (402), hydrogen peroxide adding pipeline (502), carbon disulfide adding pipeline (701), soft water adding pipeline, carbon disulfide gas discharge pipeline and nitrogen pipeline, the carbon disulfide gas discharge pipeline is connected with the gas inlet of condenser (6), the condenser (6) condensate outlet pipeline is connected with carbon disulfide receiving tank (7), the bottom outlet pipeline of carbon disulfide receiving tank (7) is connected with carbon disulfide adding pipeline (701), the carbon disulfide adding pipeline (701) is also connected with carbon disulfide transfer pump (702), the carbon disulfide adding pipeline (701) is provided with carbon disulfide metering pump (703), the bottom of the reactor (1) is provided with water phase discharge pipeline and oil phase discharge pipeline, the water phase discharge pipeline is connected with waste water collection tank, the oil phase discharge pipeline is connected with washing kettle (8), the top end of the washing kettle (8) is provided with soft water adding pipeline, the bottom end of the washing kettle (8) is provided with water phase outlet pipeline and washing water temporary storage tank (9), and the oil phase outlet pipeline goes to drying device; The washing water temporary storage tank (9) is connected with waste water treatment tank and the soft water adding pipeline of the reactor (1) through washing water transfer pump (901).

2. The apparatus for producing one-step synthesized TBTD according to claim 1, characterized by: The di-n-butylamine adding pipeline (402) is connected with di-n-butylamine storage tank (4) through di-n-butylamine metering pump (401), and the hydrogen peroxide adding pipeline (502) is connected with hydrogen peroxide storage tank (5) through hydrogen peroxide metering pump (501).

3. A one-step production apparatus for synthesizing TBTD according to claim 1 or 2, characterized in that: The lower part of the jacket (3) of the reactor (1) is provided with universal cold brine inlet pipe, and the upper part is provided with universal cold brine outlet pipe.

4. A one-step synthesis TBTD production apparatus according to claim 3, characterized in that: The reactor (1) is provided with steam coil (10), and the steam coil (10) is staggered with the position of stirring structure (2).

5. A one-step synthesis TBTD production apparatus according to claim 4, characterized in that: The top end of the carbon disulfide receiving tank (7) is provided with liquid seal water inlet pipeline (704).

Images