A wastewater recovery treatment device
By combining a neutralization vessel, a packing assembly, and a distillation column, the problem of low wastewater treatment efficiency in existing technologies is solved, achieving efficient wastewater and solvent recovery and reducing treatment costs.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SULI (NINGXIA) NEW MATERIAL TECH CO LTD
- Filing Date
- 2025-08-14
- Publication Date
- 2026-07-31
AI Technical Summary
In the existing technology, the wastewater generated during the production of N-methyl-N-isopropylaminosulfonyl chloride is difficult to treat effectively. Traditional methods such as activated sludge and chemical oxidation have problems such as low removal rate or high reagent consumption and high cost, which makes it difficult to effectively recover the solvent.
The device employs a combination of a neutralization vessel, a packed assembly, a distillation column, and a distillation column to achieve the recycling of materials in wastewater through mixing, separation, distillation, and distillation processes. The neutralization vessel is used to adjust the mixture, the packed assembly is used for material separation, the distillation column is used for material recovery, and the distillation column is used to extract and recover residues.
It improves the recovery rate of materials in wastewater, reduces treatment costs, achieves efficient wastewater treatment and solvent recovery, and meets the standards for the use of triethylamine raw materials.
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Figure CN224578112U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of wastewater treatment, and in particular to a wastewater recycling and treatment device. Background Technology
[0002] N-Methyl-N-isopropylaminosulfonyl chloride is an important chemical raw material and a key intermediate in the synthesis of the herbicide pyrimisulfuron. Its production usually involves a process of treating sulfonyl chloride with methyl isopropylamine, with triethylamine as an acid-binding agent. The process generates wastewater containing triethylamine hydrochloride, unreacted sulfonyl chloride, sulfides, and recalcitrant sulfonamide byproducts. The wastewater is contaminated with complex pollutants, including volatile chlorinated hydrocarbons, sulfides, and high COD (chemical oxygen demand). Furthermore, chlorinated organic matter has a strong inhibitory effect on microorganisms, making it difficult to apply directly using traditional biological methods.
[0003] Current technologies typically involve adding activated sludge or chemical agents to the equipment. However, activated sludge has a low COD removal rate (<50%) for recalcitrant organic matter, while chemical oxidation methods (such as the Fenton process) consume large amounts of chemicals and are prone to generating secondary pollution from iron sludge. These methods also lead to difficulties in effectively recovering the solvent, increasing treatment costs. Utility Model Content
[0004] The purpose of this invention is to address the shortcomings of existing technologies by proposing a wastewater recycling and treatment device.
[0005] To achieve the above objectives, the present invention adopts the following technical solution: a wastewater recycling and treatment device, comprising:
[0006] neutralization kettle;
[0007] The neutralization vessel receives wastewater and alkaline solution at its input end and mixes them to obtain a mixed solution.
[0008] The output end of the neutralization vessel is connected to the input end of the packing assembly;
[0009] The output end of the packing assembly is connected to a distillation column; the output end of the distillation column is connected to a storage tank to recover materials from the mixture.
[0010] As a further description of the above technical solution: the bottom of the distillation column is connected to the packing assembly to circulate and transport the mixture.
[0011] As a further description of the above technical solution: the bottom of the neutralization vessel is connected to a distillation column, and the output end of the distillation column is connected to the input end of the packing assembly to recover the material extracted by distillation.
[0012] As a further description of the above technical solution: the bottom of the distillation tower is connected to a wastewater tank for temporary storage of saline wastewater.
[0013] As a further description of the above technical solution: the packing assembly includes a first packed tower and a second packed tower.
[0014] As a further description of the above technical solution: the first packed tower and the second packed tower are connected in series.
[0015] As a further description of the above technical solution: the packing height in the first packed tower or the second packed tower is not less than 2 / 3 of the total length of the tower body.
[0016] As a further description of the above technical solution: a stirrer is provided on the neutralization vessel.
[0017] As a further description of the above technical solution: a heating jacket is provided on the outside of the neutralization vessel.
[0018] As a further description of the above technical solution: the packing assembly, the distillation column and the outer side of the distillation column are provided with heat insulation sleeves.
[0019] The above technical solution has the following advantages or beneficial effects:
[0020] By combining neutralization vessel, packed assembly, distillation column and distillation column, materials in wastewater can be recycled by distillation and extracted by distillation, thereby improving the material recovery rate. Attached Figure Description
[0021] Figure 1 This is a schematic diagram of the recycling and processing device proposed in this utility model.
[0022] Legend:
[0023] 1. Neutralization vessel; 11. Stirrer; 2. Packing assembly; 21. First packed tower; 22. Second packed tower; 3. Distillation tower; 4. Storage tank; 5. Distillation tower; 6. Wastewater tank; 7. Heating jacket. Detailed Implementation
[0024] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.
[0025] Reference Figure 1The present invention provides an embodiment of a wastewater recycling and treatment device, comprising: a neutralization vessel 1; the input end of the neutralization vessel 1 receives wastewater and alkaline solution and mixes them to obtain a mixed liquid; the output end of the neutralization vessel 1 is connected to the input end of a packing assembly 2; the output end of the packing assembly 2 is connected to a distillation column 3; the output end of the distillation column 3 is connected to a storage tank 4 to recover materials from the mixed liquid; the bottom of the distillation column 3 is connected to the packing assembly 2 to circulate and transport the mixed liquid.
[0026] In this embodiment, the neutralization vessel 1 is used to contain treated wastewater and liquid alkali, adjusting the pH of the wastewater. One end of the packing assembly 2 is connected to the neutralization vessel 1, and the other end is connected to the distillation column 3 for material separation in the mixture. The distillation column 3 performs distillation treatment on the wastewater to recover triethylamine material, which is then fed into the storage tank 4. The storage tank 4 is equipped with an exhaust port. The distillation column 3 reduces the water content in the recovered triethylamine, meeting the standards for use as triethylamine raw material, thus improving recovery efficiency and reducing the cost of triethylamine raw material. Through the cooperation of the neutralization vessel 1, the packing assembly 2, and the distillation column 3, the materials in the wastewater can be recycled and recovered through distillation, improving the material recovery rate.
[0027] The bottom of the neutralization vessel 1 is connected to the distillation column 5, and the output end of the distillation column 5 is connected to the input end of the packing assembly 2 to recover the material extracted by distillation; the bottom of the distillation column 5 is connected to the wastewater tank 6 for temporary storage of saline wastewater.
[0028] In this embodiment, the distillation tower 5 is connected to the bottom of the neutralization vessel 1, and the residual recyclable triethylamine is separated by heating and evaporation. After steam condensation, it is sent to the packing assembly 2 to improve the overall recovery rate. The saline wastewater after the triethylamine recovery treatment is sent to the distillation tower 5, where the aqueous triethylamine is distilled off and then sent to the wastewater tank 6 for storage. After the recovery is completed, the saline wastewater can be desalinated by MVR / triple-effect evaporation and then biochemically treated.
[0029] The packing assembly 2 includes a first packed tower 21 and a second packed tower 22, which are connected in series.
[0030] In this embodiment, one end of the first packed tower 21 is connected to the neutralization vessel 1, and the other end of the first packed tower 21 is connected to the second packed tower 22. The other end of the second packed tower 22 is connected to the distillation column. The first packed tower 21 and the second packed tower 22 are connected in series through a pipeline to form a two-stage filtration and separation process. Optionally, a circulating pump for conveying the material is installed on the pipeline between the first packed tower 21 and the second packed tower 22. The aqueous triethylamine after passing through the first packed tower 21 and the second packed tower 22 is transferred to the distillation column 3. The water content of the triethylamine is monitored during distillation. If it meets the requirements, it is transferred to the storage tank 4; otherwise, the triethylamine is returned to the first packed tower 21 for reprocessing.
[0031] The packing height in the first packed tower 21 or the second packed tower 22 shall not be less than 2 / 3 of the total length of the tower.
[0032] In this embodiment, the packing height is not less than 2 / 3 of the total length of the storage tank to ensure that the mixture is in full contact with the packing, improve the purity of the material entering the distillation column, reduce the distillation load, and improve the recovery rate of triethylamine. The packing can be one or more of ceramic packing and glass packing.
[0033] A stirrer 11 is installed on the neutralization vessel 1.
[0034] In this embodiment, the stirrer 11 is preferably a stirring paddle, which stirs and mixes the wastewater and alkaline solution received by the neutralization vessel 1 to obtain a mixture.
[0035] A heating jacket 7 is provided on the outside of the neutralization vessel 1.
[0036] In this embodiment, the heating jacket 7 heats the neutralization vessel 1. The neutralization vessel can be heated by water bath heating or steam heating, with water bath heating being preferred to accelerate the reaction rate.
[0037] The packing assembly 2, the distillation column 3, and the distillation column 5 are all equipped with heat insulation sleeves.
[0038] In this embodiment, the outer sides of the packing assembly 2, the distillation column 3, and the distillation column 5 are also covered with insulation sleeves, which include, but are not limited to, insulation cotton, to reduce heat loss, maintain stable internal temperature, and reduce energy consumption.
[0039] This invention relates to the treatment of wastewater from the synthesis of N-methyl-N-isopropylaminosulfonyl chloride and the acquisition of triethylamine with high recovery rate. The specific preparation process and principle are as follows:
[0040] A total of 882g of waste acid aqueous phase was added to neutralization vessel 1, along with 568g of 32% liquid alkali. The pH was adjusted to 13-14, and the mixture was heated to approximately 80℃. After settling, the layers separated, with the upper layer being triethylamine. This was then separated by first packed column 21 and second packed column 22, using glass packed columns. 221.2g of triethylamine with a moisture content of 2.48% was obtained and transferred to distillation column 3. Atmospheric pressure distillation was used to remove the fraction with a top temperature below 80℃ (which was returned to first packed column 21 for recycling). When the top temperature reached 80℃, a sample was taken from distillation column 3 to test the moisture content of the undistilled triethylamine. The moisture content was 0.07%, meeting the requirements. This treatment method can achieve a triethylamine recovery rate of over 90%.
[0041] After the triethylamine is recovered and treated, the wastewater phase is transferred from the neutralization vessel 1 to the distillation tower 5, where a small amount of triethylamine / water is distilled off (returned to the first packed tower 21 for recycling). The remaining saline wastewater is desalinated by MVR / triple-effect evaporation, and the desalinated wastewater phase is then subjected to biochemical treatment.
[0042] After treatment by the recycling and treatment device, the N-methyl-N-isopropylaminosulfonyl chloride synthesis wastewater before treatment was tested for ammonia nitrogen (5240 mg / L), COD (443750 mg / L), and total nitrogen (35620 mg / L); after treatment, the wastewater was tested for COD (522.1 ppm), chloride ions (48.7%), sulfate ions (8.82%), and TOC (71.67 ppm).
[0043] Finally, it should be noted that the above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.
Claims
1. A wastewater recovery treatment device, characterized by, include: Neutralization kettle(1); The neutralization vessel (1) receives wastewater and alkaline solution at its input end and mixes them to obtain a mixed solution; The output end of the neutralization vessel (1) is connected to the input end of the packing assembly (2); The output end of the packing assembly (2) is connected to the distillation column (3); the output end of the distillation column (3) is connected to the storage tank (4) to recover the material in the mixture.
2. The recycling processing apparatus according to claim 1, characterized by: The bottom of the distillation column (3) is connected to the packing assembly (2) to circulate and transport the mixture.
3. The recycling processing apparatus according to claim 1, characterized by: The bottom of the neutralization vessel (1) is connected to the distillation column (5), and the output end of the distillation column (5) is connected to the input end of the packing assembly (2) to recover the material extracted by distillation.
4. The recycling processing apparatus according to claim 3, characterized by: The bottom of the distillation tower (5) is connected to a wastewater tank (6) for temporarily storing saline wastewater.
5. The recycling processing apparatus according to claim 1, characterized by: The packing assembly (2) includes a first packed tower (21) and a second packed tower (22).
6. The recycling processing apparatus according to claim 5, characterized by: The first packed tower (21) and the second packed tower (22) are connected in series.
7. The recycling processing apparatus according to claim 5, characterized by: The packing height in the first packed tower (21) or the second packed tower (22) is not less than 2 / 3 of the total length of the tower body.
8. The recycling processing apparatus according to claim 1, characterized by: A stirrer (11) is provided on the neutralization vessel (1).
9. The recycling processing apparatus according to claim 1, characterized by: A heating jacket (7) is provided on the outside of the neutralization vessel (1).
10. The recycling processing apparatus according to claim 3, characterized by: The packing assembly (2), the distillation column (3), and the distillation column (5) are provided with heat insulation sleeves on their outer sides.