Post-treatment device for production of tetraethylthiuram disulfide
The post-processing unit, which combines a centrifuge with an ethanol distillation column, solves the problems of severe waste and high water treatment costs in the production of tetraethylthiuram disulfide, achieving solid-liquid separation and ethanol recovery, thus achieving energy conservation and emission reduction.
Patent Information
- Application Number
- CN202520158974.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-23
- Publication Date
- 2026-01-27
- Estimated Expiration
- 2035-01-23
AI Technical Summary
The existing tetraethyl thiuram disulfide production process suffers from serious problems such as waste, high product consumption quotas, poor operating environment, and high water treatment costs.
A post-treatment device combining a centrifuge and an ethanol distillation column is used to achieve solid-liquid separation and classification through centrifugal separation and ethanol recovery, thereby reducing wastewater discharge and recovering ethanol and organic phases.
This has achieved the goals of reducing wastewater discharge, lowering water treatment costs, improving operational safety, and achieving energy conservation and emission reduction.
Smart Images
Figure CN223831971U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of chemical technology, specifically to a post-processing device for the production of tetraethylthiuram disulfide. Background Technology
[0002] Vulcanization accelerators, often simply called accelerators, are used in rubber vulcanization to speed up the process, shorten vulcanization time, lower vulcanization temperature, and reduce the amount of vulcanizing agent required. They can also improve the physical and mechanical properties of the vulcanized rubber. Tetraethyl thiuram disulfide (TETD) is used as a super-accelerator and vulcanizing agent for natural rubber, styrene-butadiene rubber, nitrile rubber, butyl rubber, cis-butadiene rubber, and latex.
[0003] Currently, most tetraethylthiuram disulfide production processes employ a two-step method: condensation followed by oxidation. First, diethylamine, sodium hydroxide, and carbon disulfide are condensed at 30-40°C to produce sodium diethyldithiocarbamate. Then, the carbon residue is filtered, and the mother liquor is oxidized with chlorine or nitrous acid and air to produce tetraethylthiuram disulfide. After cooling, filtration, drying, and pulverization, the final product is obtained, with a yield of only 86%. While this production process is relatively mature, it suffers from significant waste, high product consumption quotas, high manual labor intensity, and a poor operating environment.
[0004] The applicant improved the process by using ethanol (with recovered ethanol), water, diethylamine, and carbon disulfide for a condensation reaction, followed by direct addition of hydrogen peroxide for oxidation after the reaction. Currently, the conventional procedure involves artificially adding diethylamine and carbon disulfide to the reaction vessel. Carbon disulfide, for example, has a low boiling point (46.2℃) and an ignition temperature of 90℃. At room temperature and pressure, it is a colorless, transparent, slightly aromatic, fat-soluble liquid with extremely high volatility, flammability, and explosiveness. It also has an unpleasant rotten radish odor and poses a significant health hazard.
[0005] Currently, after the reaction is complete, the reaction liquid is centrifuged, the solid is the product, which is washed with soft water and then dried. The mother liquor and washing liquid are discharged as wastewater, which increases the burden of wastewater treatment in the workshop and leads to high water treatment costs. Utility Model Content
[0006] To address the shortcomings of existing technologies, this invention provides a post-processing device for the production of tetraethylthiuram disulfide, which enables the recovery and classification of ethanol, thereby reducing processing costs.
[0007] To achieve the above objectives, this utility model provides the following technical solution: a post-processing device for tetraethylthiuram disulfide production, comprising a centrifuge. The centrifuge's top cover is equipped with a feed pipe, a soft water inlet pipe, a nitrogen pipeline, an exhaust pipe, and a centrifugal liquid discharge pipe. The feed pipe is connected to the discharge pipeline of the reaction vessel; the soft water inlet pipe is connected to a soft water metering tank; the centrifugal liquid discharge pipe branches into three branches, respectively connected to a centrifugal mother liquor receiving tank, a secondary wash water receiving tank, and a tertiary wash water receiving tank; each of the three branches is equipped with an independently controlled valve; and the outlet pipes of the centrifugal mother liquor receiving tank, the secondary wash water receiving tank, and the tertiary wash water receiving tank are respectively connected to… The basket filter of the centrifugal mother liquor receiving tank is connected to the centrifugal mother liquor temporary storage tank via a centrifugal mother liquor transfer pump. The basket filters of the secondary wash water receiving tank and the tertiary wash water receiving tank are connected to the soft water inlet pipe via their respective transfer pumps. The centrifugal mother liquor temporary storage tank is connected to the cold side inlet of the feed preheater of the ethanol distillation column via a distillation mother liquor transfer pump. The hot side outlet of the feed preheater is connected to the material inlet in the middle of the ethanol distillation column. The hot side inlet of the feed preheater is connected to the top vapor outlet of the ethanol distillation column. The cold side outlet of the feed preheater is connected to the ethanol condenser. The condensed ethanol outlet pipeline of the ethanol condenser is connected to the ethanol receiving tank.
[0008] In the above scheme, the bottom of the ethanol distillation column is equipped with a bottom residue discharge pipeline. This pipeline is connected to the top inlet of the distillation residue stratification tank via a bottom residue transfer pump. The top of the stratification tank is equipped with a waste gas discharge pipeline connected to the workshop's main waste gas pipeline. The distillation residue is stratified in the stratification tank, separating the organic and aqueous layers for separate treatment. The oil phase is treated as hazardous waste by a qualified treatment facility, while the aqueous phase is treated as wastewater by the company's wastewater treatment plant.
[0009] In the above scheme, the lower part of the distillation residue stratification tank is wrapped with a cooling coil to cool the components inside the tank.
[0010] In the above scheme, the bottom of the distillation residue stratification tank is equipped with a funnel-shaped discharge section, and the cooling coil is located above the discharge section. The bottom of the discharge section is equipped with a bottom liquid discharge pipe, which branches into two branches, one of which is connected to a distillation wastewater temporary storage tank. After stratification, the aqueous phase enters the distillation wastewater temporary storage tank through one of the branches and is sent to the company's wastewater treatment plant for processing. The oil phase, as hazardous waste, is sent to a qualified treatment unit for separate treatment.
[0011] In the above scheme: a reboiler outlet pipeline is provided on the lower part of the side wall of the distillation residue stratification tank and connected to the reboiler, and the outlet pipeline of the reboiler is connected to the bottom reflux pipeline of the distillation residue stratification tank.
[0012] This utility model's post-processing device for tetraethylthiuram disulfide production utilizes a closed centrifugation system to reduce the volatilization of organic matter into the air and environmental pollution. Waste gas generated during centrifugation is discharged into the workshop's main exhaust pipe for centralized treatment. The centrifuged solid material is received in a solid material receiving tank, dried, and packaged to obtain the finished TETD product. The centrifugal mother liquor enters a centrifugal mother liquor receiving tank, while the wash water initially enters secondary and tertiary wash water receiving tanks. The soft water entering these tanks is further filtered through a basket filter to remove residue before being pumped back to the centrifuge for recycling. This significantly reduces water discharge.
[0013] The centrifuged mother liquor is further filtered through a basket filter before entering an ethanol distillation column for rectification. The light components at the top of the column are condensed and cooled to obtain recovered ethanol, which is reused in the next batch of reaction. Lost ethanol is replenished with fresh ethanol. The vapor exiting the top of the ethanol distillation column is first preheated by a feed preheater to reduce energy consumption. After cooling, the ethanol is recovered.
[0014] The device of this utility model is reasonably designed and achieves the effect of energy saving and emission reduction. Attached Figure Description
[0015] Figure 1 This is a schematic diagram of the structure of this utility model (excluding the distillation part).
[0016] Figure 2 This is a schematic diagram of the structure of this utility model (distillation section). Detailed Implementation
[0017] The present invention will be further described below with reference to the accompanying drawings and embodiments.
[0018] Example 1: As Figure 1 and 2 As shown, due to limited paper, Figure 1 and 2The following diagram shows two parts of this utility model. The post-processing device for tetraethylthiuram disulfide production includes a centrifuge 1. The centrifuge's top cover is equipped with a feed pipe 101, a soft water inlet pipe 102, a nitrogen line 103, an exhaust pipe 104, and a centrifugal liquid discharge pipe 105. The structure of the centrifuge 1 itself is prior art and will not be described in detail here. The feed pipe 101 is connected to the discharge line of the reaction vessel. The material from the tetraethylthiuram disulfide reaction vessel enters the centrifuge through the feed pipe 101 via a transfer pump for centrifugation. The soft water inlet pipe 102 is connected to a soft water metering tank 2, which is equipped with a soft water inlet pipe connected to a soft water pump. The centrifugal liquid discharge pipe 105 branches into three branches, which are respectively connected to the centrifugal mother liquor receiving tank 3, the secondary wash water receiving tank 4, and the tertiary wash water receiving tank 5. Each of the three branches is equipped with an independently controlled valve. The tops of the centrifugal mother liquor receiving tank 3, the secondary wash water receiving tank 4, and the tertiary wash water receiving tank 5 are all equipped with exhaust pipes connected to the workshop's main exhaust pipe. The outlet pipes of the centrifugal mother liquor receiving tank 3, the secondary wash water receiving tank 4, and the tertiary wash water receiving tank 5 are respectively connected to basket filters 6. The structure of the basket filters 6 is existing technology and will not be described in detail here. The outlet pipe of the basket filter 6 of the centrifugal mother liquor receiving tank 3 is connected to the centrifugal mother liquor temporary storage tank 8 via the centrifugal mother liquor transfer pump 7. The basket filters 6 of the secondary wash water receiving tank 4 and the tertiary wash water receiving tank 5 are connected to the soft water inlet pipe 102 via their respective transfer pumps. The centrifugal mother liquor storage tank 8 is connected to the cold-side inlet of the feed preheater 11 of the ethanol distillation column 10 via a distillation mother liquor transfer pump 9. The top cover of the centrifugal mother liquor storage tank 8 is equipped with an exhaust pipe connected to the workshop's main exhaust pipe. The structure of the ethanol distillation column 10 is existing technology and will not be described in detail here. The structure of the feed preheater 11 is also existing technology, consisting of a tube side and a shell side. (The text abruptly ends here.) Figure 2 The mother liquor flows through the tubular layer, while the top vapor flows through the shell layer. Specifically, the hot-side outlet of the feed preheater 11 is connected to the material inlet in the middle of the ethanol distillation column 10. The hot-side inlet of the feed preheater 11 is connected to the top vapor outlet of the ethanol distillation column 10, and the cold-side outlet of the feed preheater 11 is connected to the ethanol condenser 12. The condensed ethanol outlet pipeline of the ethanol condenser 12 is connected to the ethanol receiving tank 13. The top of the ethanol receiving tank 13 is also equipped with an exhaust pipe connected to the workshop exhaust main pipeline. A branch pipe from the condensed ethanol outlet pipeline of the ethanol condenser 12 is connected to the ethanol reflux pipeline at the top of the ethanol distillation column 10. Figure 2 As shown, the ethanol condenser 12 is a prior art technology, including a shell and a tube layer. Cooling water is introduced into the shell to cool the ethanol gas in the tube layer, and the ethanol vapor flows through the tube layer.
[0019] The bottom of the ethanol distillation column 10 is equipped with a bottom residue discharge line, which is connected to the top inlet of the distillation residue stratification tank 15 via a bottom residue transfer pump 14. The top of the stratification tank 15 (top cover) is equipped with a waste gas discharge line 1501 connected to the workshop's main waste gas pipe. A cooling coil 1503 is wound around the lower part of the distillation residue stratification tank 15. A condensate inlet line 15031 and a condensate outlet line 15032 are installed on the cooling coil 1503.
[0020] The bottom of the distillation residue stratification tank 15 is equipped with a funnel-shaped discharge section 1502. A cooling coil 1503 is located above the discharge section 1502. The bottom of the discharge section 1502 is equipped with a bottom liquid discharge pipe 1504, which branches into two branches. One branch is connected to the distillation wastewater temporary storage tank 16. The other branch collects the bottom residue (organic phase), which is then barrelled and sent to a qualified treatment facility. The top of the distillation wastewater temporary storage tank 16 is equipped with a waste gas pipe connected to the workshop's main waste gas pipe. The bottom of the distillation wastewater temporary storage tank 16 is equipped with a discharge pipe connected to the distillation wastewater transfer pump 18. A reboiler outlet line is located on the lower side wall of the distillation residue stratification tank 15 and connected to the reboiler 17. The reboiler outlet line is connected to the bottom reflux line of the distillation residue stratification tank 15. The reboiler 17 is heated by steam.
[0021] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A post-processing device for tetraethylthiuram disulfide production, comprising a centrifuge (1), wherein the top cover of the centrifuge (1) is provided with a feed pipe (101), a soft water inlet pipe (102), a nitrogen pipeline (103), an exhaust pipe (104), and a centrifugal liquid discharge pipe (105), characterized in that: The feed pipe (101) is connected to the discharge pipe of the reactor. The soft water inlet pipe (102) is connected to the soft water metering tank (2). The centrifugal liquid discharge pipe (105) branches into three branches, which are respectively connected to the centrifugal mother liquor receiving tank (3), the secondary wash water receiving tank (4), and the tertiary wash water receiving tank (5). Each of the three branches is equipped with an independently controlled valve. The outlet pipes of the centrifugal mother liquor receiving tank (3), the secondary wash water receiving tank (4), and the tertiary wash water receiving tank (5) are respectively connected to the basket filter (6). The outlet pipe of the basket filter (6) of the centrifugal mother liquor receiving tank (3) is connected to the centrifugal mother liquor temporary storage tank (8) through the centrifugal mother liquor transfer pump (7). The basket filters (6) of the receiving tank (4) and the tertiary wash water receiving tank (5) are connected to the soft water inlet pipe (102) through their respective transfer pumps; the centrifugal mother liquor temporary storage tank (8) is connected to the cold side inlet of the feed preheater (11) of the ethanol distillation column (10) through the distillation mother liquor transfer pump (9); the hot side outlet of the feed preheater (11) is connected to the material inlet in the middle of the ethanol distillation column (10); the hot side inlet of the feed preheater (11) is connected to the top vapor outlet of the ethanol distillation column (10); the cold side outlet of the feed preheater (11) is connected to the ethanol condenser (12); and the condensed ethanol outlet pipeline of the ethanol condenser (12) is connected to the ethanol receiving tank (13).
2. The post-processing apparatus for tetraethylthiuram disulfide production according to claim 1, characterized in that: The bottom of the ethanol distillation column (10) is provided with a bottom residue discharge pipeline, which is connected to the top inlet of the distillation residue stratification tank (15) via a bottom residue transfer pump (14). The top of the distillation residue stratification tank (15) is provided with a waste gas discharge pipeline (1501) which is connected to the workshop waste gas main pipe.
3. The post-processing apparatus for tetraethylthiuram disulfide production according to claim 2, characterized in that: The lower part of the distillation residue stratification tank (15) is wrapped with a cooling coil (1503).
4. The post-processing apparatus for tetraethylthiuram disulfide production according to claim 3, characterized in that: The bottom end of the distillation residue stratification tank (15) is provided with a funnel-shaped discharge section (1502), the cooling coil (1503) is located above the discharge section (1502), the bottom end of the discharge section (1502) is provided with a bottom liquid discharge pipe (1504), the bottom liquid discharge pipe (1504) branches into two branches, one of which is connected to the distillation wastewater temporary storage tank (16).
5. The post-processing apparatus for tetraethylthiuram disulfide production according to claim 4, characterized in that: The lower side wall of the distillation residue stratification tank (15) is provided with a reboiler outlet pipeline connected to the reboiler (17), and the outlet pipeline of the reboiler is connected to the bottom reflux pipeline of the distillation residue stratification tank (15).