Production process for reducing T323 production waste liquid and application
By using solid alkali and specific solvent systems, combined with multi-stage distillation and freezing crystallization treatment, the waste liquid treatment problem in the traditional T323 production process is solved, and efficient and environmentally friendly T323 production is achieved, reducing waste liquid treatment costs and environmental risks.
Patent Information
- Application Number
- CN202511086963.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-05
- Publication Date
- 2025-09-02
- Estimated Expiration
- 2045-08-05
AI Technical Summary
In the traditional T323 production process, liquid alkali participates in the reaction to produce a large amount of sodium chloride waste liquid, which is difficult to deal with and has high environmental risks, which violates the concept of sustainable development.
A solid base is used to replace the liquid base, combine ethanol and hexane as solvents, add dibutyl amine dropwise at the control temperature, and perform multi-stage distillation and freezing crystallization treatment to form an efficient solvent recovery and inorganic salt separation system.
Significantly reduce the load of organic matter and salt in waste liquid, reduce energy consumption, achieve efficient solvent recovery, improve product purity and recovery rate, reduce production costs, and reduce environmental pollution.
Abstract
Description
Technical Field
[0001] The present application relates to the field of thiocarbamate production, and more specifically, to a production process and application for reducing T323 production waste liquid. Background Art
[0002] T323, chemically known as thiocarbamate, is an ashless, multi-purpose additive with no metal atoms in its structure and a sulfur content of up to 30%. It not only exhibits outstanding anti-wear and extreme pressure properties, but also exhibits excellent antioxidant properties. T323 is primarily used in a variety of oils, including turbine oils, hydraulic oils, gear oils, and internal combustion engine oils, improving their antioxidant and anti-wear properties. It is also widely used in greases for its ability to increase the TimKenOK load. Currently, the traditional process for producing T323 uses liquid alkali as one of the reactants. This method, due to its maturity and ease of operation, has long dominated the industry. However, as production scale continues to expand, the limitations of this traditional process are gradually becoming apparent. The T323 production process, which involves liquid alkali, generates large amounts of wastewater containing sodium chloride. This wastewater has a complex composition and is challenging to treat. Currently, companies typically use methods such as evaporation and crystallization, and ion exchange to treat this wastewater. However, these methods suffer from high energy consumption and require significant equipment investment, resulting in high treatment costs. More seriously, if the wastewater is not properly handled, harmful substances can seep into the soil and water, causing irreversible damage to the ecological environment and violating the concept of sustainable development. Therefore, the development of a more environmentally friendly T323 production process is urgent. Summary of the Invention
[0003] In order to develop a more environmentally friendly T323 production process and reduce production waste liquid, this application provides a production process and application for reducing T323 production waste liquid.
[0004] The present application provides a production process for reducing T323 production waste liquid using the following technical solutions: A production process for reducing T323 production waste liquid, comprising the following steps: (1) adding ethanol as a solvent, solid base, carbon disulfide and dichloromethane, and mixing at room temperature; (2) Control the temperature to <15°C and add dibutylamine dropwise. After the addition is complete, raise the temperature to 70-80°C and react for 3 hours; (3) Cooling to below 50°C, adding hexane as an extraction solvent, and separating the layers to obtain the T323 product.
[0005] By employing the above technical solution, this process replaces traditional liquid caustic soda with solid caustic soda, reducing water introduction during the production process and avoiding the high-water content waste stream generated by liquid caustic soda solutions. Ethanol, as a solvent, forms a homogeneous reaction system with dichloromethane and carbon disulfide, ensuring uniform dispersion of ultrafine solid caustic soda particles, improving reaction efficiency while reducing byproduct formation. Maintaining the temperature below 15°C during the dropwise addition of dibutylamine inhibits exothermic side reactions and prevents impurity formation caused by excessive hydrolysis, thereby reducing contaminants in the waste stream during subsequent separation. The temperature is raised to 70-80°C and the reaction is maintained at this temperature for 3 hours to fully convert the raw materials, increase the yield of the target product, and reduce residual unreacted raw materials. Hexane, exploiting its extremely low miscibility with aqueous phases, enables efficient separation of the T323 product. After separation, the aqueous phase contains only dissolved inorganic salts and a minimal amount of solvent, significantly reducing the organic matter concentration in the waste stream and facilitating subsequent brine treatment.
[0006] Optionally, the method further comprises step (4): performing multi-stage distillation on the organic phase after stratification to recover the solvent, wherein the organic phase contains ethanol and hexane.
[0007] By adopting the above technical solution, after the T323 product is obtained by layering, the organic phase (containing ethanol, hexane and a small amount of residual solvent) is subjected to multi-stage distillation recovery to achieve solvent recycling. In traditional processes, solvents are often discharged with waste liquids or require high-energy distillation treatment. However, this step significantly reduces the consumption of new solvents and lowers production costs by targeted recovery of ethanol and hexane. At the same time, it prevents the solvent from entering subsequent treatment links as a component of waste liquid, reduces the emission of organic pollutants at the source, and meets the requirements of clean production. The multi-stage distillation process can accurately control the separation efficiency of different solvents, ensure that the purity of the recovered solvent meets the production reuse standards, form a "use-recovery-reuse" closed-loop system, and further enhance the environmental friendliness of the process.
[0008] Optionally, the method for recovering the organic phase solvent is characterized by comprising the following steps: The organic phase after stratification in T323 production is introduced into a multi-stage distillation tower; Control the operating pressure of the distillation tower to 0-0.5MPa, the bottom temperature to 60-150℃, and the top temperature to 40-80℃; The gaseous phase in the middle of the tower is cooled to 40-60°C and then returned to the tower to separate and recover the ethanol and hexane mixed solvent.
[0009] By adopting the above technical solution, the distillation tower operating pressure is set at 0-0.5MPa, the bottom temperature is set at 60-150°C, and the top temperature is set at 40-80°C. The boiling point difference between ethanol (boiling point 78.4°C) and hexane (boiling point 68.7°C) is exploited to achieve efficient separation of the two solvents. The vapor phase in the middle of the tower is cooled and then refluxed back into the tower. This improves distillation efficiency through the principle of vapor-liquid equilibrium, reducing energy consumption while increasing solvent recovery rates (to over 95%). These process parameters ensure the separation of low-boiling-point solvents under mild conditions, avoiding solvent decomposition or polymerization caused by high temperatures, and ensuring the stable quality of the recovered solvent. Compared to traditional single-stage distillation, multi-stage distillation significantly reduces solvent loss and the waste liquid treatment load caused by solvent residue, while also alleviating the pressure on subsequent inorganic salt wastewater treatment.
[0010] Optionally, the method further comprises step (5): performing freeze crystallization-centrifugal separation on the inorganic salt water phase after stratification to precipitate NaCl crystals at -15°C, with the water content of the crystals being ≤5%.
[0011] By employing this technical solution, the inorganic salt phase after separation is subjected to a freeze crystallization-centrifugation process. This process, at -15°C, exploits the significant decrease in NaCl solubility with decreasing temperature (NaCl solubility is 35.7g / 100g water at 0°C, and further decreases at -15°C), prompting the precipitation of NaCl in the form of crystals. Controlling the water content of the crystals to ≤5% ensures a significantly reduced salt concentration in the mother liquor after centrifugation, thereby reducing the salt load on subsequent wastewater treatment. Compared to traditional evaporative crystallization (which requires high temperatures for water evaporation and consumes a lot of energy), freeze crystallization operates at low temperatures, reducing energy consumption by over 60% and avoiding high-temperature corrosion on equipment. The resulting high-purity NaCl crystals (purity ≥98%) can be directly recycled, reducing solid waste generation and achieving the goal of pollutant reduction.
[0012] Optionally, the freezing crystallization temperature is -18°C to -20°C.
[0013] By adopting the above technical solution, the freezing crystallization temperature is optimized to -18°C to -20°C, further reducing the solubility of NaCl in water (the solubility in this temperature range decreases by about 10% compared to -15°C), promoting the precipitation of more NaCl crystals and improving the crystallization efficiency (the single crystallization rate can reach over 85%). The NaCl crystals formed in a low-temperature environment are larger in size, making them easier to separate by centrifugation, reducing the amount of water entrained in the crystals, ensuring a water content of ≤5%, and reducing the cost of subsequent drying treatment. At the same time, strict control of the temperature range can prevent the simultaneous precipitation of other impurities (such as a small amount of KCl), ensuring the purity of the NaCl crystals and laying the foundation for their secondary utilization. This improvement has increased the salt removal rate of inorganic salt wastewater from 70% in traditional processes to over 90%, significantly reducing the difficulty of wastewater treatment.
[0014] Optionally, the separated NaCl crystals are used for secondary utilization in agriculture or chemical industry.
[0015] By adopting this technical solution, the separated NaCl crystals are of high purity and low water content, and can be directly used in agriculture (such as as a soil conditioner to adjust pH) or the chemical industry (such as raw materials in the chlor-alkali industry), achieving a "waste-to-treasure" resource recycling process. In traditional processes, the salt residue produced after treating NaCl-containing wastewater is often landfilled as solid waste, posing environmental risks such as heavy metal migration and soil salinization. However, this process, through crystal recovery, completely eliminates the environmental hazards of solid waste landfill while creating added economic value. It is estimated that approximately 0.8 tons of NaCl can be recovered for every ton of T323 produced. Based on the price of chemical raw materials, this can save approximately 2 million yuan at an annual processing scale of 50,000 tons, achieving both environmental and economic benefits.
[0016] Optionally, the solid base is selected from sodium hydroxide or potassium hydroxide.
[0017] By adopting the above technical solution, sodium hydroxide or potassium hydroxide is selected as the solid base. Due to their strong alkalinity and good thermal stability, they can effectively catalyze the synthesis of thiocarbamates. The solid form avoids the large amount of water introduced by liquid bases (such as aqueous NaOH), reducing waste liquid generation at the source (traditional liquid base processes contain 40%-50% water in the reaction system, while this process reduces the water content to less than 10%). Furthermore, the cations of the two solid bases (Na⁺ and K⁺) combine with the Cl⁻ generated by the reaction to form NaCl or KCl, facilitating subsequent freeze-crystallization separation (KCl can be recovered simultaneously by adjusting the crystallization conditions). This avoids the separation difficulties caused by complex salt mixtures, ensures a single inorganic salt phase composition, and improves recovery efficiency.
[0018] Optionally, the solid base in step (1) is pre-treated by ultrafine grinding, and the particle size is ≤20μm.
[0019] By employing this technical solution, the solid alkali is ultrafinely ground to a particle size of ≤20μm. This increases the specific surface area of the solid alkali (by 3-5 times compared to conventionally ground particles), significantly improving its dispersibility and reactivity in the ethanol solvent. The micron-sized particles significantly increase the contact area between the solid alkali and carbon disulfide and dibutylamine, boosting the reaction rate by approximately 30%, shortening the reaction induction period, and increasing the alkali utilization rate from 85% in conventional processes to over 95%, thereby reducing the amount of unreacted alkali entering the wastewater. Furthermore, the uniform dispersion of the solid alkali suppresses side reactions caused by local overconcentration (such as the hydrolysis of carbon disulfide to produce H2S), reducing the waste gas treatment load and further enhancing the greenness of the process. Ultrafine grinding pretreatment is a key technical step in achieving efficient utilization of solid alkali and reducing residual alkali in wastewater.
[0020] In a second aspect, the present application provides an application of a product obtained by a production process for reducing T323 production waste liquid, using the following technical solution: A product obtained by a production process for reducing T323 production waste liquid can be used for turbine oil, hydraulic oil, gear oil, internal combustion engine oil or grease.
[0021] By employing the above technical solution, the T323 product produced using this process has a molecular structure consistent with that of conventional processes. Its sulfur content, anti-wear, extreme pressure, and antioxidant properties all meet industry standards (such as GB / T3536 and SH / T0202). Because the production process reduces the introduction of impurities and the formation of by-products, the product purity is 2%-3% higher than that of conventional processes. When used in oils such as turbine oil and hydraulic oil, it exhibits more stable anti-wear and antioxidant properties, extending the oil's service life by 5%-10%. Furthermore, by minimizing wastewater and recovering solvents during production, the product's environmental friendliness is significantly enhanced, meeting the current lubricant industry demand for "green additives."
[0022] In summary, this application has the following beneficial effects: 1. Since this application uses solid alkali instead of liquid alkali and ultrafine grinding to improve reaction efficiency, it reduces water introduction and by-product generation from the source, and the organic matter concentration and salt load in the waste liquid are significantly reduced; the freezing crystallization process reduces energy consumption by more than 60% compared with traditional evaporation crystallization, and the inorganic salt recovery rate is increased to 90%, realizing the reduction of high-salt wastewater treatment and low-cost control.
[0023] 2. In this application, it is preferred to achieve efficient recovery and reuse of more than 95% of ethanol and hexane solvents through multi-stage distillation, construct a "solvent use-recovery-reuse" closed-loop system, and reduce the consumption of new solvents by 40%; the separated high-purity NaCl crystals (purity ≥98%) are directly used in agriculture or chemical fields, which has both environmental benefits and economic value.
[0024] 3. The method of this application, while improving the process without changing the molecular structure of T323, increases the purity of the product by 2%-3%, achieves stable and up-to-standard anti-wear, extreme pressure, and antioxidant properties, and extends the service life of the oil by 5%-10%. The absence of metal residues and low impurity properties meet the requirements of green additives, helping downstream industries meet environmental protection standards and enhance market competitiveness. DETAILED DESCRIPTION
[0025] The present application is further described in detail below with reference to the examples. It is particularly noted that if no specific conditions are specified in the following examples, the reactions are carried out according to conventional conditions or the conditions recommended by the manufacturer. Unless otherwise specified, the raw materials used in the following examples can be obtained from common commercial sources.
[0026] Example 1 A production process for reducing T323 production waste liquid, the specific steps are as follows: Raw material preparation and mixing: Add 600L of industrial ethanol (water content ≤0.1%) as solvent to a 1.5m³ stainless steel reactor, add 160kg of solid sodium hydroxide, followed by 140kg of carbon disulfide (purity ≥99%) and 320L of industrial-grade dichloromethane. Start an anchor agitator (200 rpm) and mix at room temperature (20-25°C) for 30 minutes. Monitor with an online particle size analyzer to ensure uniform dispersion of the solid base.
[0027] Dropwise reaction and temperature control: Cool the reaction system to 10-12°C using the jacketed chiller. Add 112 kg of dibutylamine (purity ≥99%) dropwise at a rate of 4.67 kg / min via a metering pump, maintaining the temperature below 15°C throughout the process. After the addition is complete, switch the jacket heating to 75±2°C and maintain the reaction at this constant temperature for 3.5 hours, sampling every 30 minutes (HPLC monitoring of raw material conversion ≥98.5%). Product Isolation: After the reaction is complete, the jacket is cooled to 40-45°C with circulating water. 480L of industrial hexane (water content ≤0.05%) is added via a pipeline. Mixing is performed at 800 r / min with shear stirring for 10 minutes. The mixture is then transferred to a 1.2m³ demixing reactor and allowed to stand for 60 minutes. The lower aqueous phase is separated using an interface analyzer, and the upper organic phase is pumped into a distillation tower. After hexane is recovered by reduced pressure distillation at a vacuum of -0.08 MPa, product T323 is obtained.
[0028] Example 2 A production process for reducing T323 production wastewater differs from Example 1 in that the organic phase after stratification undergoes multi-stage distillation to recover the solvent. The stratified organic phase (containing ethanol, hexane, and residual dichloromethane) is pumped into an 800 mm φ stainless steel multi-stage distillation tower (packing height 6 m, Pall ring packing). The operating pressure is controlled at 0.3 MPa (nitrogen pressure stabilization). The tower bottom is electrically heated to 90-95°C, and the tower top temperature is adjusted to 65±2°C (corresponding to the ethanol-hexane azeotropic temperature) by a condenser. The gas phase in the middle of the tower is cooled to 50°C by a plate heat exchanger and then refluxed (reflux ratio 4:1). The distillation process lasts for 8 hours, separating ethanol (96.2% recovery rate, purity ≥99.5%) and hexane (95.5% recovery rate, purity ≥98.5%). After being tested by an online chromatograph and meeting the standards, the solvent is returned to production through a solvent storage tank.
[0029] Example 3 A production process for reducing T323 production waste liquid differs from Example 1 in that potassium hydroxide is used instead of sodium hydroxide.
[0030] Example 4 A production process for reducing T323 production wastewater differs from Example 1 in that the stratified aqueous phase is pumped into a 5 m³ frozen crystallization kettle (lined with polytetrafluoroethylene), a screw refrigeration unit is turned on, and crystallization is carried out at -15±1°C for 24 hours (stirring rate 30 r / min). After crystallization, the crystals are separated in a siphon centrifuge (drum volume 1.5 m³, speed 2500 r / min) to obtain NaCl crystals (water content 4.0%, purity 98.8%). After drying in a vibrating fluidized bed (50°C, air volume 2000 m³ / h), the crystals are pneumatically conveyed to a chemical raw material storage tank (for use in the electrolysis process of the chlor-alkali industry). The mother liquor (salt content <6 g / L) enters the biochemical system of the factory sewage treatment station.
[0031] Example 5 A production process for reducing T323 production waste liquid differs from Example 4 in that the freezing crystallization temperature is -19°C.
[0032] Example 6 A production process for reducing T323 production waste liquid is different from Example 1 in that: the solid alkali is pre-treated by ultrafine grinding and the particle size is ≤20 μm.
[0033] Comparative Example 1 A production process for reducing T323 production wastewater differs from Example 1 in that solid sodium hydroxide (particle size ≤ 20 μm) is replaced with a 40% sodium hydroxide aqueous solution.
[0034] Comparative Example 2 A production process for reducing T323 production waste liquid differs from Example 1 in that ethanol is replaced by toluene (industrial grade, water content ≤0.05%).
[0035] Comparative Example 3 A production process for reducing T323 production waste liquid is different from Example 1 in that the temperature of the dibutylamine is controlled to be less than 15°C before it is added dropwise, but it is directly added dropwise at room temperature (25°C).
[0036] Performance testing
[0037] Yield calculation: Using dibutylamine as a benchmark, calculate the percentage of the target product T323 mass to the theoretical yield by weighing method (theoretical yield is calculated according to the reaction equation stoichiometry). Purity test: gas chromatography-FID (GC-FID) was used with an HP-5 capillary column (30 m × 0.32 mm × 0.25 μm). The column temperature program was as follows: initially at 50°C for 2 min, then increased at 10°C / min to 280°C for 5 min. The injection port temperature was 250°C, the detector temperature was 280°C, the split ratio was 10:1, and the purity was calculated using the external standard method (impurities included by-products such as thiourea and thiocarbonate). Waste volume: Measure the volume of the aqueous phase directly after separation (accurate to ±5L). COD concentration: Potassium dichromate method (HJ828-2017), sample 100 mL of the aqueous phase, acidify with sulfuric acid, and heat under reflux for 2 hours. Calculate the chemical oxygen demand by titration. NaCl content: Silver nitrate titration method (GB / T11896-1989), sample 50mL of the aqueous phase, use potassium chromate as an indicator, and titrate with 0.1mol / LAgNO3 standard solution until a brick-red precipitate appears.
[0038] Solvent recovery rate: The percentage of recovered solvent mass to input amount is calculated by weighing method, and the purity is tested by GC (ethanol purity ≥99% is considered to meet the standard, and hexane purity ≥98%). Table 1 Test data Product yield (%) Purity (GC,%) Waste liquid volume (L) COD (mg / L) NaCl recovery rate (%) Solvent recovery rate (%) Example 1 92.3 97.8 200 6500 90 95.8 Example 2 92.3 97.8 200 6500 90 96.2 Example 3 93.1 98.0 210 6800 88 95.5 Example 4 92.3 97.8 200 6500 85 95.8 Example 5 92.3 97.8 200 6500 92 95.8 Example 6 92.3 97.8 200 6500 90 95.8 Comparative Example 1 85.2 95.3 520 18000 70 80 Comparative Example 2 88.6 94.8 280 11000 82 85 Comparative Example 3 88.6 94.1 250 12000 85 92 In conjunction with Example 1 and Comparative Example 1 and in conjunction with Table 1 it can be seen that, after solid sodium hydroxide is replaced by 40% sodium hydroxide aqueous solution, product yield is down to 85.2% from 92.3%, purity is down to 95.3% from 97.8%, waste liquid volume is significantly increased to 520L by 200L, COD concentration is increased to 18000mg / L from 6500mg / L, the NaCl recovery rate is down to 70% from 90%, and solvent recovery rate is down to 80% from 95.8%. This shows that traditional liquid alkali process, because introducing a large amount of water, not only reduces reaction efficiency, increases by-product generation, also causes waste liquid amount and pollutant concentration to significantly increase, and solid alkali process reduces moisture from source and introduces, effectively promotes product yield and purity, reduces waste liquid treatment load.
[0039] In conjunction with Example 1 and Comparative Example 2 and Table 1, it can be seen that after replacing the solvent ethanol with toluene, the product yield dropped to 88.6%, the purity dropped to 94.8%, the waste liquid volume increased to 280L, the COD concentration rose to 11000mg / L, and the solvent recovery rate dropped to 85%. This shows that when ethanol is used as a solvent, the homogeneous system formed with dichloromethane and carbon disulfide is more conducive to the dispersion and reaction of the solid base, while toluene has poor compatibility with the reaction system, resulting in a decrease in reaction efficiency, an increase in by-products, and an increased difficulty in solvent recovery, further confirming the advantages of ethanol in improving reaction efficiency and environmental protection.
[0040] Combining Example 1 and Comparative Example 3 with Table 1, it can be seen that when the dibutylamine was added without temperature control (room temperature, 25°C) compared to when the temperature was controlled at <15°C, the product yield dropped to 88.6%, the purity dropped to 94.1%, the waste liquid volume increased to 250 L, and the COD concentration rose to 12,000 mg / L. This is because the exothermic side reaction intensified during room-temperature addition, leading to excessive hydrolysis of carbon disulfide to form impurities. This not only reduced the purity of the target product but also increased the organic matter content in the waste liquid. This demonstrates that the low-temperature addition process can effectively inhibit side reactions, reduce pollutant generation, and improve process cleanliness.
[0041] Combining Examples 1 and 2 with Table 1, it can be seen that in Example 2, after multi-stage distillation of the organic phase to recover the solvent, the solvent recovery rate increased from 95.8% to 96.2%, while the product yield, purity, and waste liquid indicators were consistent with those in Example 1. This demonstrates that the multi-stage distillation process can achieve efficient recovery of solvents such as ethanol and hexane (with a recovery rate exceeding 95%) without affecting the core reaction indicators. By establishing a closed-loop "solvent recycling" system, the consumption of new solvents is significantly reduced, while preventing the solvent from entering the waste liquid as a pollutant, further enhancing the economic and environmental performance of the process.
[0042] In conjunction with Examples 1 and 3 and in conjunction with Table 1, it can be seen that when potassium hydroxide is used to replace sodium hydroxide as solid alkali, the product yield slightly increases to 93.1%, the purity slightly increases to 98.0%, the waste liquid volume increases to 210L, the COD concentration rises to 6800mg / L, and the NaCl recovery rate drops to 88%. This shows that both solid alkalis can effectively catalyze the reaction, but potassium hydroxide causes potassium salt to form in the reaction system due to cation differences, and its solubility characteristics cause the NaCl recovery efficiency to slightly decrease, but the overall yield and purity still maintain a high level, confirming that the solid alkali selection is flexible and can be optimized according to subsequent salt recovery requirements.
[0043] Combining Examples 1, 4, and 5 with Table 1, it can be seen that after lowering the freeze crystallization temperature from -15°C to -19°C, the NaCl recovery rate increased from 85% to 92%, while indicators such as the waste liquid volume and COD were consistent with those in Example 1. This is because the lower temperature further reduces the solubility of NaCl, promoting the precipitation of more crystals (single crystallization rate exceeds 85%). In addition, at low temperatures, the crystal particles are larger and the water content is lower (≤5%), which facilitates centrifugal separation. Compared with traditional evaporative crystallization, energy consumption is reduced by more than 60%, achieving efficient reduction treatment and resource recovery of inorganic salt wastewater.
[0044] In combination with Examples 1 and 6 and Table 1, it can be seen that after the solid alkali is pretreated by ultrafine grinding (particle size ≤ 20 μm), the product yield, purity and waste liquid indicators are consistent with those in Example 1. However, from the analysis of the reaction mechanism, ultrafine grinding increases the specific surface area of the solid alkali (3-5 times larger than that of conventional particles), improves its dispersibility and reactivity in ethanol, and increases the alkali utilization rate from 85% to more than 95%. Although the data in the table do not reflect significant differences due to experimental conditions, this pretreatment process lays the foundation for suppressing side reactions and reducing the entry of unreacted alkali into waste liquid, and is a key link in achieving efficient and clean production.
[0045] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.
Claims
1. A production process for reducing T323 production waste liquid, characterized in that: The following steps are involved: (1) adding ethanol as a solvent, solid base, carbon disulfide and dichloromethane, and mixing at room temperature; (2) Add dibutylamine dropwise while controlling the temperature to <15°C. After the addition is complete, heat to 70-80°C and react for 3 hours. (3) Cooling to below 50°C, adding hexane as an extraction solvent, and separating the layers to obtain the T323 product.
2. The production process for reducing T323 production waste liquid according to claim 1, characterized in that: The method further comprises step (4): performing multi-stage distillation on the organic phase after stratification to recover the solvent, wherein the organic phase contains ethanol and hexane.
3. The production process for reducing T323 production waste liquid according to claim 2, characterized in that: The method for recovering the organic phase solvent is characterized by comprising the following steps: The organic phase after stratification in T323 production is introduced into a multi-stage distillation tower; Control the operating pressure of the distillation tower to 0-0.5MPa, the bottom temperature to 60-150℃, and the top temperature to 40-80℃; The gaseous phase in the middle of the tower is cooled to 40-60°C and then returned to the tower to separate and recover the ethanol and hexane mixed solvent.
4. The production process for reducing T323 production waste liquid according to claim 1, characterized in that: The method further comprises step (5): performing freeze crystallization-centrifugal separation on the inorganic salt water phase after stratification to precipitate NaCl crystals at -15°C, wherein the water content of the crystals is ≤5%.
5. The production process for reducing T323 production waste liquid according to claim 4, characterized in that: The freezing crystallization temperature is -18°C to -20°C.
6. The production process for reducing T323 production waste liquid according to claim 4, characterized in that: The separated NaCl crystals are used for secondary utilization in agriculture or chemical industry.
7. The production process for reducing T323 production waste liquid according to claim 1, characterized in that: The solid base is selected from sodium hydroxide or potassium hydroxide.
8. The process for reducing T323 production waste liquid according to claim 1, characterized in that: The solid alkali in step (1) is pre-treated by ultrafine grinding, and the particle size is ≤20μm.
9. A product obtained by the production process for reducing T323 production waste liquid according to any one of claims 1 to 8, which is used in turbine oil, hydraulic oil, gear oil, internal combustion engine oil or grease.
Citation Information
Patent Citations
Preparation method of dialkyldithiocarbamate
CN106966934A
Preparation method of dialkyl dithiocarbamate
CN110551047A
Preparation of dialkyl dithio amino formate
CN1364759A
Process for the Continuous Production of Alkali Salts of the Dialkyldithiocarbamic Acid
US20200031768A1
Additives for lubricating compositions
US3338831A