Dye intermediate waste acid treatment device

By designing a waste acid treatment device for dye intermediates and using a combination of components such as a concentration kettle, the problem of waste acid treatment was solved, achieving low-cost and high-efficiency waste acid concentration and solid-liquid separation, reducing production costs and improving enterprise efficiency.

CN223464433UActive Publication Date: 2025-10-24NANJING GUANSHAN CHEM TECH
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Patent Information

Application Number
CN202422975967.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-12-04
Publication Date
2025-10-24
Estimated Expiration
2034-12-04

AI Technical Summary

Technical Problem

The treatment of waste acid generated during the production of dye intermediates is a challenge. Traditional alkali neutralization treatment technology requires a large amount of alkali to generate solid waste, and vacuum concentration technology has high investment and cost, which is difficult for enterprises to bear.

Method used

Design a waste acid treatment device for dye intermediates. The device uses components such as a concentration kettle, steam washing tower, circulating pump, condenser, condensate tank, condensate transfer pump, acid-acid heat exchanger, recooler, intermediate tank, centrifuge and acid storage tank. Through evaporation concentration, solid-liquid separation, acid-acid heat exchange and interlock control, the waste acid is concentrated to 45% and reused.

Benefits of technology

It achieves low-cost and efficient waste acid treatment, reduces solid waste, lowers production costs, and improves enterprise efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to a dye intermediate waste acid treatment device. A first feed port on a concentration kettle is connected with a raw material acid outlet of an acid-acid heat exchanger, and a discharge port at the lower part of the concentration kettle is connected with a concentrated acid inlet of the acid-acid heat exchanger; a second feeding port in the upper portion of the concentration kettle is connected with a first discharging pipe at the bottom of the steam washing tower, a second discharging pipe at the bottom of the steam washing tower is connected with an inlet of the circulating pump, a liquid outlet of the circulating pump is connected to a feeding port in the upper portion of the steam washing tower, and an outlet in the bottom of the condenser is connected with an inlet in the upper portion of the condensate water tank. An outlet in the bottom of the condensate water tank is connected with an inlet of the condensate water conveying pump, and a discharging opening of the recooler is connected to a feeding opening of the intermediate tank; a discharge hole in the bottom of the intermediate tank is connected with a feed hole in the top of the centrifugal machine through a slurry delivery pump; and a liquid outlet of the centrifugal machine is connected with the concentrated acid storage tank. According to the device, the in-situ application requirement can be met, meanwhile, most of boric acid and salt impurities are removed, and concentrated sulfuric acid is returned to an acid using station to be continuously used.
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Description

TECHNICAL FIELD

[0001] The utility model relates to the field of medicine chemical industry and environmental protection, concretely relates to a dye intermediate waste acid treatment device. BACKGROUND

[0002] A waste acid liquid is produced in the dye intermediate production process, the waste liquid contains about 15% sulfuric acid, and contains boric acid and salt impurities, how to handle becomes a problem in the production process. The traditional alkali neutralization treatment technology needs a large amount of alkali, and also produces secondary pollution such as solid waste, increases the production cost, and reduces the enterprise benefit. The newly developed vacuum concentration technology is difficult for enterprises to bear due to large investment and high cost. A waste acid liquid treatment device produced in the dye intermediate production process needs to be designed. SUMMARY

[0003] To solve the above problems, the present application discloses a dye intermediate waste acid treatment device, which is suitable for waste sulfuric acid liquid containing boric acid and a small amount of salt impurities produced in the dye intermediate production process. The device can concentrate sulfuric acid in the waste liquid from 10-15% content to about 45%, meet the in-situ reuse requirements, remove most of the boric acid and salt impurities, and return the concentrated sulfuric acid to the acid post for continuous use.

[0004] A dye intermediate waste acid treatment device, comprising a concentration kettle, a washing tower, a circulating pump, a condenser, a condensate tank, a condensate delivery pump, and an acid- acid heat exchanger, a re-cooler, an intermediate tank, a centrifugal machine and an acid storage tank. A heater is arranged in the concentration kettle. A first feed port on the concentration kettle is connected with a raw material acid outlet of the acid- acid heat exchanger, and a lower discharge port is connected with a concentrated acid inlet of the acid- acid heat exchanger. A steam outlet on the upper part of the concentration kettle is connected with a steam inlet on the lower part of the washing tower. A second feed port on the upper part of the concentration kettle is connected with a first discharge pipe on the bottom of the washing tower. A second discharge pipe on the bottom of the washing tower is connected with an inlet of the circulating pump. An outlet of the circulating pump is connected with a feed inlet on the upper part of the washing tower. A top discharge port of the washing tower is connected with a top gas inlet of the condenser. A bottom outlet of the condenser is connected with an upper inlet of the condensate tank. A bottom outlet of the condensate tank is connected with an inlet of the condensate delivery pump. A concentrated acid outlet of the acid- acid heat exchanger is connected with a feed inlet of the re-cooler. A discharge port of the re-cooler is connected with a feed inlet of the intermediate tank. A bottom discharge port of the intermediate tank is connected with a top feed inlet of the centrifugal machine through a slurry delivery pump. An outlet of the centrifugal machine is connected with the concentrated acid storage tank.

[0005] Further, the condensate delivery pump has two outlets, one of which is connected to a sewage treatment station outside the device, and the other is connected to a circulating liquid inlet pipe of the washing tower.

[0006] Further, a flow regulating valve is installed on the circulating liquid inlet pipeline, and the opening of the flow regulating valve is controlled by the top temperature of the washing tower.

[0007] 2. The temperature of the gas out of the tower is controlled by the flow regulating valve, the lower the temperature, the lower the sulfuric acid partial pressure, and the less the sulfuric acid loss. The temperature at the top of the washing tower is generally controlled at 102-106 DEG C.

[0008] Further, a break pipe is installed on the pipeline of the second feeding interface to ensure the stability of the liquid level in the washing tower.

[0009] Further, the washing tower is a packed tower, the packing is ceramic structured packing, and a demister is further installed on the upper part of the packing of the washing tower.

[0010] Further, a stirrer is installed on the intermediate tank to prevent solid particles from depositing in the intermediate tank or causing the pipeline to be blocked.

[0011] The raw material acid is preheated to 80-90 DEG C. after being exchanged with concentrated acid in the acid-acid heat exchanger, enters the concentration kettle, is heated and vaporized by a heater, and the rising acid gas enters the washing tower, the sulfuric acid is absorbed into the circulating liquid, the circulating liquid enters the concentration kettle for further heating and evaporation, the break pipe ensures the stability of the liquid level in the washing tower, the water vapor enters the condenser and is condensed into condensate and is sent to a sewage treatment station, the raw material acid in the concentration kettle is concentrated to 45% (temperature 119 DEG C.) and then enters the acid-acid heat exchanger, is cooled by the raw material acid and then enters the re-cooler for further cooling to normal temperature (below 40 DEG C.) and enters the intermediate tank with a stirrer, is sent to the centrifuge for solid-liquid separation by a slurry delivery pump, the liquid is 45% recovered sulfuric acid and enters the acid storage tank, and the solid is boracic acid and sulfate for solid waste treatment. The concentration part of the device is a continuous production process, and the solid-liquid separation part is an intermittent production process.

[0012] The concentrated sulfuric acid is returned to the acid post for continuous use. The production device built by adopting the technologies of evaporation concentration, solid-liquid separation, acid-acid heat exchange and interlocking control has the advantages of low investment, low energy consumption, high automation degree and less solid waste. BRIEF DESCRIPTION OF DRAWINGS

[0013] Figure 1 The device structure schematic diagram of the utility model.

[0014] LIST OF REFERENCE NUMERALS

[0015] 1. Concentrator; 2. Steam scrubber; 3. Circulating pump; 4. Condenser; 5. Condensate tank; 6. Condensate transfer pump; 7. Acid-acid heat exchanger; 8. Subcooler; 9. Intermediate tank; 10. Slurry transfer pump; 11. Centrifuge; 12. Acid storage tank; 21. Circulating liquid inlet pipe; 22. Flow control valve; 23. Siphon breaker; 91. Agitator. DETAILED DESCRIPTION

[0016] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. It should be noted that the terms "front," "rear," "left," "right," "up," and "down" used in the following description refer to directions in the accompanying drawings, and the terms "inward" and "outward" refer to directions toward or away from the geometric center of a particular component, respectively.

[0017] like Figure 1 As shown, a dye intermediate waste acid treatment device includes a concentration kettle 1, a steam scrubber 2, a circulation pump 3, a condenser 4, a condensate tank 5, a condensate delivery pump 6, an acid-acid heat exchanger 7, a subcooler 8, an intermediate tank 9, a centrifuge 11 and an acid storage tank 12; a heater is provided in the concentration kettle 1, a first feed interface on the concentration kettle 1 is connected to the raw acid (shell side) outlet of the acid-acid heat exchanger 7, and a lower discharge port is connected to the concentrated acid (tube side) inlet of the acid-acid heat exchanger 7; an upper steam riser of the concentration kettle 1 is connected to a lower steam inlet of the steam scrubber 2.

[0018] The second feed port at the top of the concentration kettle 1 is connected to the first discharge pipe at the bottom of the steam scrubber 2 , and a siphon breaker 23 is installed on the pipe of the second feed port.

[0019] The second discharge pipe at the bottom of the steam scrubber 2 is connected to the inlet of the circulation pump 3, the water outlet of the circulation pump 3 is connected to the feed port at the top of the steam scrubber 2, and the top discharge port of the steam scrubber 2 is connected to the top air inlet of the condenser 4; the bottom outlet of the condenser 4 is connected to the upper inlet of the condensate tank 5, the bottom outlet of the condensate tank 5 is connected to the inlet of the condensate delivery pump 6, the concentrated acid outlet of the acid-acid heat exchanger 7 is connected to the feed port of the subcooler 8, and the discharge port of the subcooler 8 is connected to the feed port of the intermediate tank 9; the intermediate tank 9 is equipped with an agitator 91; the bottom discharge port of the intermediate tank 9 is connected to the top feed port of the centrifuge 11 through the slurry delivery pump 10; the liquid outlet of the centrifuge 11 is connected to the concentrated acid storage tank 12.

[0020] The condensate delivery pump 6 has two outlets, one of which is connected to a sewage treatment station outside the device, and the other is connected to the circulating liquid inlet pipe 21 of the steam scrubber 2.

[0021] The flow regulating valve 22 is installed on the circulating liquid inlet pipeline 21, and the opening degree of the flow regulating valve 22 is controlled by the overhead temperature of the washing tower 2.

[0022] The washing tower 2 is a packed tower, the packing is ceramic structured packing, and a defoaming device is further installed on the upper part of the packing of the washing tower 2.

[0023] The raw material acid is continuously sent into the acid inlet (the shell inlet) of the acid-heat exchanger 7 at a stable flow, the inlet and outlet steam valves of the concentration kettle heater are opened, the temperature in the kettle rises until steam enters the washing tower 2 (the overhead temperature rises), the circulating pump 3 is started, the circulating liquid is sprayed in the washing tower 2 to wash the rising steam, the water vapor of the sulfuric acid is washed away and enters the condenser to be condensed into condensate and enters the condensate tank, the condensate conveying pump 6 and the flow regulating valve on the condensate pipeline entering the inlet of the washing tower 2 are started, the flow controller temperature is set to 102 DEG C, and the overhead temperature is kept stable at 102 DEG C ± 1 DEG C. The stable heating steam pressure is 0.4 MPa, the raw material acid feeding flow is stable at 1000 kg / h, the temperature in the concentration kettle is 119 DEG C to 121 DEG C, and the concentration system enters the stable operation. The concentrated acid flowing out from the lower outlet of the concentrator passes through the acid-heat exchanger 7 and the re-cooler 8, the temperature is reduced to below 40 DEG C, enters the intermediate tank 9, the stirrer 91 of the intermediate tank 9 is started, when the liquid level rises to about 50%, the centrifuge 11 and the slurry conveying pump 10 are started to carry out solid-liquid separation, the obtained solid is treated as solid waste, and the obtained concentrated acid with a sulfuric acid content of 45% enters the acid storage tank 12 for collection and utilization.

[0024] The technical means disclosed in the scheme of the present application is not only limited to the technical means disclosed in the above-mentioned embodiments, but also includes the technical scheme composed of any combination of the above technical features.

Claims

1. A dye intermediate waste acid treatment apparatus comprising a concentration still (1) and a steam scrubber (2), characterized by: The circulating pump (3), the condenser (4), the condensate tank (5), the condensate delivery pump (6), and the acid- acid heat exchanger (7), the subcooler (8), the intermediate tank (9), the centrifuge (11) and the acid storage tank (12); the condensation kettle (1) is provided with a heater, the first feed port on the condensation kettle (1) is connected with the raw material acid outlet of the acid- acid heat exchanger (7), and the lower discharge port is connected with the concentrated acid inlet of the acid- acid heat exchanger (7); the upper steam outlet of the condensation kettle (1) is connected with the lower steam inlet of the scrubber (2); the second feed port of the upper part of the condensation kettle (1) is connected with the first discharge pipe at the bottom of the scrubber (2), the second discharge pipe at the bottom of the scrubber (2) is connected with the inlet of the circulating pump (3), the liquid outlet of the circulating pump (3) is connected with the feed inlet of the upper part of the scrubber (2), and the top discharge port of the scrubber (2) is connected with the top gas inlet of the condenser (4); the bottom outlet of the condenser (4) is connected with the upper inlet of the condensate tank (5), the bottom outlet of the condensate tank (5) is connected with the inlet of the condensate delivery pump (6), the concentrated acid outlet of the acid- acid heat exchanger (7) is connected with the feed inlet of the subcooler (8), and the discharge port of the subcooler (8) is connected with the feed inlet of the intermediate tank (9); the bottom discharge port of the intermediate tank (9) is connected with the top feed inlet of the centrifuge (11) through the slurry delivery pump (10); the liquid outlet of the centrifuge (11) is connected with the concentrated acid storage tank (12).

2. A dye intermediate waste acid treatment apparatus according to claim 1, characterized by: The condensate delivery pump (6) has two outlets, one of which is connected to a sewage treatment station outside the device, and the other is connected to the circulating liquid inlet pipe (21) of the scrubber (2).

3. A dye intermediate waste acid treatment apparatus according to claim 2, characterized by: A flow regulating valve (22) is installed on the circulating liquid inlet pipe (21), and the opening degree of the flow regulating valve (22) is controlled by the top temperature of the scrubber (2).

4. The dye intermediate waste acid treatment apparatus according to claim 1, characterized by: A broken rainbow pipe (23) is installed on the pipeline of the second feed port.

5. The dye intermediate waste acid treatment apparatus according to claim 1, characterized by: The scrubber (2) is a packed tower, and the packing is ceramic structured packing; the upper part of the packing of the scrubber (2) is also provided with a demister.

6. A dye intermediate waste acid treatment apparatus according to claim 1, characterized by: The intermediate tank (9) is provided with a stirrer (91).