A device and method for recovering chloromethane waste liquid containing nitrogen peroxide
The invention adopts a recovery device composed of a distillation tank, a condenser and an adsorption tank, and utilizes heating evaporation, condensation and adsorption technology to separate nitrogen peroxide and methyl chloride, thereby solving the problem of difficult recovery of methyl chloride waste liquid in the existing technology and realizing the recovery of high-purity methyl chloride and waste liquid reduction treatment.
Patent Information
- Application Number
- CN202211583083.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-09
- Publication Date
- 2025-09-16
- Estimated Expiration
- 2042-12-09
AI Technical Summary
Existing technologies are unable to effectively separate and recover chloromethane waste liquid containing nitrogen peroxide, resulting in the inability to recycle chloromethane at high purity, and the waste liquid is difficult to treat, causing serious environmental damage.
A recovery device consisting of a distillation tank, condenser, intermediate storage tank, adsorption tank, purification tank and filter is used to separate nitrogen peroxide and methyl chloride through physical methods such as heating evaporation, condensation, adsorption and filtration, and then use fine-porous silica gel and activated carbon for adsorption and purification, forming a circular treatment process.
The invention realizes the effective separation of methyl chloride and nitrogen peroxide, improves the purity and recovery rate of methyl chloride, reduces the discharge of waste liquid, avoids secondary pollution, and has a simple structure and is easy to be produced on a large scale.
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Figure CN115869700B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of waste liquid treatment, in particular to a device and method for recovering methyl chloride waste liquid containing nitrogen peroxide. Background Art
[0002] Nitrogen peroxide (NO2) is a reddish-brown, highly reactive gaseous substance that plays a key role in ozone formation. It is also a contributing factor to acid rain, resulting in diverse environmental impacts, including: impacts on competition and composition among wetland and terrestrial plant species; reduced atmospheric visibility; acidification of surface waters; eutrophication (hypoxia caused by algae blooms in water rich in nutrients like nitrogen and phosphorus); and increased levels of toxins harmful to fish and other aquatic life. Nitrogen peroxide waste gas is the most challenging of all waste gas treatments and is a major contributor to atmospheric pollution. If not effectively purified, it can form a dark brown-yellow smog, which poses a significant threat not only to the health of operators and the surrounding environment, but also, if carried by wind, can cause irreversible damage to the lives of surrounding residents and the ecological environment.
[0003] Chloromethane is a general term for chloromethane, dichloromethane, trichloromethane, and carbon tetrachloride. As an important chemical raw material and solvent, it is one of the basic industries of the national economy. In chlor-alkali enterprises, it has become an important product for balancing chlorine. In recent years, the application of chloromethane has been rapidly developed. However, the waste liquid of chloromethane has the characteristics of high biological toxicity, difficulty in natural degradation, long environmental damage period, and carcinogenicity. Among them, carbon tetrachloride has a molecular weight of 153.84 and a density of 1.595g / cm at room temperature and pressure. 3 (20°C), boiling point 76.8°C, vapor pressure 15.26 kPa (25°C), vapor density 5.3 g / L. Carbon tetrachloride is immiscible with water but miscible with ethanol, ether, chloroform, and petroleum ether. International studies have shown that carbon tetrachloride is a typical hepatotoxicant. At high concentrations, it first affects the central nervous system, followed by the liver and kidneys. Carbon tetrachloride is a common organic pollutant that easily enters soil and water bodies through leaching with rainwater or irrigation water, causing soil and water pollution. It is persistent, long-lasting, and bioaccumulative in the environment. Industrial carbon tetrachloride wastewater is difficult to decompose in the environment, causing lasting damage to the ecological environment. It is also an ozone depleting substance, persisting in the atmosphere for a long time and posing a threat to ozone. Any carbon tetrachloride waste generated during chemical production must be treated through a wastewater treatment system before discharge. Chemical production companies can establish their own wastewater treatment systems for treatment, or they can collect and transfer the wastewater to a facility with treatment capabilities.
[0004] Traditional methods for remediating carbon tetrachloride wastewater pollution include: 1. Activated carbon adsorption; 2. In-situ chemical oxidation; 3. Bioremediation; and 4. Infiltration reaction wall remediation. These methods can only treat low concentrations of carbon tetrachloride, can cause soil compaction, are not long-lasting, or cannot simultaneously treat nitrogen peroxide. Dichloromethane is primarily used in film production and the pharmaceutical industry in China. Film production accounts for 50% of total consumption, pharmaceuticals account for 20%, cleaning agents and the chemical industry account for 20%, and other applications account for 10%. Dichloromethane is also used as a refrigerant in industrial refrigeration systems, but it poses significant risks. It can produce highly toxic phosgene when in contact with open flames or hot objects. It hydrolyzes in moist air to produce trace amounts of hydrogen chloride, and light accelerates this hydrolysis, increasing its corrosiveness to metals. This substance can be hazardous to the environment and can accumulate in groundwater. Special attention should be paid to aquatic life. Atmospheric pollution should also be considered. The main recovery method at present is distillation, but the eluted water vapor will become new polluted waste liquid.
[0005] For chloromethane waste liquid containing nitrogen peroxide, chloromethane and nitrogen peroxide cannot be effectively separated, and high-purity chloromethane cannot be recovered and utilized. Summary of the Invention
[0006] The purpose of the present invention is to provide a device and method for recovering methyl chloride waste liquid containing nitrogen peroxide, which can effectively separate nitrogen peroxide from methyl chloride, effectively recover and reuse methyl chloride, carry out centralized and special treatment on nitrogen peroxide in the waste liquid, and reduce waste liquid discharge.
[0007] To achieve the above-mentioned object, the present invention provides a device for recovering chloromethane waste liquid containing nitrogen peroxide, comprising a distillation tank, a condenser, and an intermediate storage tank arranged in sequence, an evaporation tank provided with a feed pipe, the evaporation tank and the condenser being connected via a connecting pipe 1, the bottom end of the condenser being connected to the intermediate storage tank and the evaporation tank respectively via connecting pipes, all of which are provided with valves; a purification structure being provided downstream of the intermediate storage tank; the purification structure comprising an adsorption tank, a purification tank, and a filter, the adsorption tank being connected to the intermediate storage tank via a connecting pipe 2, the connecting pipe 2 being provided with a circulation pump, the adsorption tank being connected to the purification tank via a connecting pipe 3, the purification tank being connected to the filter via a connecting pipe, the filter being connected to the intermediate storage tank via a connecting pipe 4, the filter being provided with a discharge pipe, the connecting pipe 2, the connecting pipe 3, the connecting pipe 4, and the discharge pipe being provided with valves; and a heating structure and a cleaning structure for heating the distillation tank and the purification tank.
[0008] Preferably, the discharge port of the adsorption tank is connected to the reflux port of the intermediate storage tank through a circulation pipe, and a valve is provided on the circulation pipe.
[0009] Preferably, the discharge port of the intermediate storage tank is connected to the reflux port of the distillation tank via a second connecting pipe and a reflux pipe.
[0010] Preferably, the heating structure includes a heater and an oil pump, the heater is connected to the oil pump, the outlet of the oil pump is connected to the heating interlayer of the evaporator through a connecting pipe, the heating interlayer of the evaporator is connected to the heater through a connecting pipe, forming a circulating heating loop; the outlet of the oil pump is connected to the radiator through a connecting pipe, the radiator is connected to the heater through a connecting pipe, forming a circulating heating loop, the air inlet of the radiator is provided with a fan, and the air outlet of the radiator is connected to the connecting pipe through a connecting pipe; valves are provided on the connecting pipes.
[0011] Preferably, the cleaning structure includes a cleaning pool, a cleaning pump is provided on the cleaning pipe of the cleaning pool, the cleaning pipe is connected to the cleaning port of the distillation tank through branch pipe one, the cleaning pipe is connected to the inlet of the intermediate storage tank through branch pipe two, the cleaning pipe is connected to the filter through branch pipe three, and a valve is provided on branch pipe three; the liquid outlets of the distillation tank and the intermediate storage tank are connected to the cleaning pool through connecting pipes, and a valve is provided on the connecting pipes.
[0012] Preferably, the volume of the distillation tank is greater than the volume of the intermediate storage tank.
[0013] The recovery method of the above-mentioned methyl chloride waste liquid recovery device containing nitrogen peroxide comprises the following steps:
[0014] S1, turn on the heater, the heater imports the thermal oil into the distillation tank by the oil pump and heats the distillation tank; the waste liquid is added to the distillation tank through the feed pipe, heated and evaporated in the distillation tank, the steam in the distillation tank enters the condenser through the distillation tank top by connecting pipe one and condenses, realizes the condensation of methyl chloride, the nitrogen peroxide in the condenser is discharged from the top of the condenser in a gaseous state, the methyl chloride liquid condensed by the condenser flows into the distillation tank by connecting pipe, carries out repeated condensation of methyl chloride and fully discharge of nitrogen peroxide;
[0015] S2, after circulation, the methyl chloride condensed in the condenser enters the intermediate storage tank through the connecting pipe for storage. The intermediate storage tank pumps the methyl chloride liquid into the adsorption tank through the connecting pipe 2 and the circulation pump for adsorption, and then flows into the intermediate storage tank through the circulation pipe for circulation;
[0016] S3, the methyl chloride after cyclic adsorption enters the purification tank through the connecting pipe three, then enters the filter through the connecting pipe for filtration, flows into the intermediate storage tank through the connecting pipe four, and is circulated for purification and filtration. The cycle treatment time is 1-3 hours; finally, the methyl chloride liquid is discharged through the discharge pipe;
[0017] S4, the heater introduces the heat transfer oil into the radiator through the oil pump, the cold air in the radiator is heated, and the heated hot air is sent to the purification tank to desorb the purification tank, thereby realizing the recycling of the purification agent in the purification tank;
[0018] S5. Turn on the cleaning pump and introduce the clean water in the cleaning pool into the distillation tank and the intermediate storage tank through the cleaning pipe, branch pipe 1, and branch pipe 2 for cleaning, and then flow into the cleaning pool through the connecting pipe; the clean water in the cleaning pool is introduced into the purification structure through the cleaning pipe and branch pipe 3 to clean the adsorption tank, purification tank and filter of the purification structure.
[0019] Preferably, the heating temperature of the distillation tank is 100-200°C, and the condensing temperature of the condenser is 20-50°C.
[0020] Preferably, the adsorbent in the adsorption tank is fine-porous silica gel, and the mass ratio of fine-porous silica gel to liquid methyl chloride is 1:(5-10).
[0021] Preferably, the purifying agent in the purification tank is activated carbon, and the mass ratio of activated carbon to liquid methyl chloride is 1:(5-10); the pore size of the filter is 100-500 mesh.
[0022] The advantages and positive effects of the device and method for recovering methyl chloride waste liquid containing nitrogen peroxide described in the present invention are:
[0023] 1. The condenser and the distillation tank are connected by a connecting pipe, which is used to return the condensed methyl chloride to the distillation tank, circulate the methyl chloride, and fully separate the methyl chloride and nitrogen peroxide.
[0024] 2. A circulation pipe is provided between the adsorption tank and the intermediate storage tank to circulate the liquid methyl chloride between the intermediate storage tank and the adsorption tank, thereby improving the drying and impurity removal effect of the methyl chloride.
[0025] 3. A circulation pipeline is formed between the intermediate storage tank, adsorption tank, purification tank and filter, which can fully remove impurities, purify and purify the chloromethane, thereby improving the purity of the chloromethane.
[0026] 4. The setting of radiator and heater can desorb the purification tank so that the activated carbon can be reused.
[0027] 5. The device and method described in the present invention utilize heating and physical adsorption to separate and recover, without introducing other chemical reagents for treatment, thus avoiding secondary pollution, reducing the difficulty of waste liquid treatment, and reducing the amount of waste liquid discharged. The device and method have a simple structure and are easy to scale up production. In addition, the recovered methyl chloride has high purity, high recovery rate, and stable quality.
[0028] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] Figure 1The present invention is a schematic structural diagram of an embodiment of a device and method for recovering chloromethane waste liquid containing nitrogen peroxide.
[0030] Reference numerals
[0031] 1. Distillation tank; 2. Condenser; 3. Intermediate storage tank; 4. Circulation pump; 5. Adsorption tank; 6. Purification tank; 7. Filter; 8. Heater; 9. Oil pump; 10. Radiator; 11. Fan; 12. Cleaning tank; 13. Feed pipe; 14. Connecting pipe 1; 15. Connecting pipe 2; 16. Connecting pipe 3; 17. Connecting pipe 4; 18. Discharge pipe; 19. Circulation pipe; 20. Reflux pipe; 21. Cleaning pipe; 22. Branch pipe 1; 23. Branch pipe 2; 24. Branch pipe 3. DETAILED DESCRIPTION
[0032] The technical solution of the present invention is further described below with reference to the accompanying drawings and embodiments.
[0033] Unless otherwise defined, the technical or scientific terms used in the present invention shall have the usual meanings understood by persons of ordinary skill in the field to which the present invention belongs. The words "first", "second" and similar terms used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. Words such as "include" or "comprise" mean that the elements or objects preceding the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. Words such as "connect" or "connected" are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the object being described changes, the relative positional relationship may also change accordingly.
[0034] Example
[0035] Figure 1The following is a schematic diagram of an embodiment of a device and method for recovering methyl chloride waste liquid containing nitrogen peroxide according to the present invention. As shown, the device comprises a distillation tank 1, a condenser 2, and an intermediate storage tank 3, arranged in sequence. A feed pipe 13 is provided on the evaporation tank, through which the methyl chloride waste liquid containing nitrogen peroxide enters the evaporation tank. The distillation tank 1 is heated to a temperature of 100-200°C. The methyl chloride waste liquid containing nitrogen peroxide evaporates within the evaporation tank, forming a mixed gas. The evaporation tank and condenser 2 are connected by a connecting pipe 14, through which the evaporated mixed gas enters the condenser 2. The condensation temperature of condenser 2 is 20-50°C. Condenser 2 condenses the mixed gas. Due to the different condensation points of nitrogen peroxide and methyl chloride, nitrogen peroxide remains in a gaseous state while methyl chloride condenses into a liquid, thereby separating the nitrogen peroxide from the methyl chloride. Condenser 2 utilizes an existing structure. The bottom end of the condenser 2 is connected to the intermediate storage tank 3 through a connecting pipe, so that the condensed methyl chloride liquid is stored in the intermediate storage tank 3.
[0036] The bottom of condenser 2 is connected with evaporation tank by connecting pipe, and condenser 2 and evaporation tank and middle storage tank 3 are all provided with valve on the connecting pipe.Condenser 2 can send the methyl chloride liquid of condensation back in evaporation tank again, continues to evaporate in evaporation tank, circulates like this, and the nitrogen peroxide contained in the methyl chloride is fully separated.The top of condenser 2 is provided with the discharge port that nitrogen peroxide is discharged, and the nitrogen peroxide after the discharge is collected and then centrally processed.After methyl chloride separates with nitrogen peroxide, liquid methyl chloride is discharged into middle storage tank 3 again and stores.
[0037] A purification structure is located downstream of the intermediate storage tank 3. This structure comprises an adsorption tank 5, a purification tank 6, and a filter 7. The adsorption tank 5 is connected to the intermediate storage tank 3 via a second connecting pipe 15, which is equipped with a circulation pump 4. This circulation pump 4 pumps the methyl chloride stored in the intermediate storage tank 3 into the adsorption tank 5, where it undergoes adsorption and purification. The discharge port of the adsorption tank 5 is connected to the reflux port of the intermediate storage tank 3 via a circulation pipe 19, which is equipped with a valve. The adsorbent in the adsorption tank 5 is fine-porous silica gel, with a mass ratio of fine-porous silica gel to liquid methyl chloride of 1:5-10. The fine-porous silica gel in the adsorption tank 5 is used to absorb water, water-soluble impurities, and metal ions in the methyl chloride, achieving both impurity removal and drying. The circulation of the methyl chloride in the adsorption tank 5 enhances the drying and purification of the methyl chloride.
[0038] Adsorption tank 5 is connected to purification tank 6 via connecting pipe 3 16 . Purification tank 6 is connected to filter 7 via connecting pipe 4 17 , which is connected to intermediate storage tank 3 . Filter 7 is provided with a discharge pipe 18 for discharging the treated liquid methyl chloride. Connecting pipes 2 15 , 3 16 , 4 17 , and discharge pipe 18 are all equipped with valves. After circulating through adsorption tank 5 , the methyl chloride enters purification tank 6 for purification. The purification agent in purification tank 6 is activated carbon, with a mass ratio of activated carbon to liquid methyl chloride of 1:5-10. The activated carbon purifies and removes impurities from the liquid methyl chloride, improving its purity. Filter 7 has a 100-500 mesh pore size and is used to filter the fine-porous silica gel desiccant and activated carbon purifying agent carried by the methyl chloride after passing through adsorption tank 5 and purification tank 6 . It also filters other solid impurities carried by the methyl chloride, improving its purity. The intermediate storage tank 3, the adsorption tank 5, the purification tank 6 and the filter 7 form a circulation pipe 19, which circulates the drying, purification and purification of the methyl chloride, which is beneficial to improving the purity of the methyl chloride.
[0039] The discharge port of the intermediate storage tank 3 is connected to the reflux port of the distillation tank 1 through a connecting pipe 2 15 and a reflux pipe 20. A valve is provided on the reflux pipe 20. The reflux pipe 20 is used to return the residual methyl chloride in the intermediate storage tank 3 to the distillation tank 1 for the next treatment.
[0040] The volume of the distillation tank 1 is greater than that of the intermediate storage tank 3 .
[0041] The recovery device also includes a heating structure for heating the distillation tank 1 and the purification tank 6. The heating structure includes a heater 8 and an oil pump 9, and the heater 8 is connected to the oil pump 9. The outlet of the oil pump 9 is connected to the heating layer of the evaporation tank via a connecting pipe to heat the evaporation tank. The heating layer of the evaporation tank is connected to the heater 8 via a connecting pipe to form a circulating heating loop. The outlet of the oil pump 9 is connected to the radiator 10 via a connecting pipe, and the radiator 10 is connected to the heater 8 via a connecting pipe to form a circulating heating loop. The air inlet of the radiator 10 is provided with a fan 11, and the air outlet of the radiator 10 is connected to the connecting pipe 3 16 via a connecting pipe. The heat transfer oil of the heater 8 heats the radiator 10, thereby heating the cold air from the fan 11 to form hot air. The hot air processes the activated carbon in the purification tank 6, which is beneficial for the reuse of the activated carbon. Valves are provided on the connecting pipes of the distillation tank 1, the radiator 10, the oil pump 9, and the heater 8.
[0042] The recovery device also includes a cleaning structure for cleaning the distillation tank 1 and the purification tank 6. The cleaning structure includes a cleaning tank 12, and a cleaning pump is provided on the cleaning pipe 21 of the cleaning tank 12. The cleaning pipe 21 is connected to the cleaning port of the distillation tank 1 through a branch pipe 1 22. The cleaning pipe 21 is connected to the inlet of the intermediate storage tank 3 through a branch pipe 2 23. The cleaning pump pumps clean water from the cleaning tank 12 into the distillation tank 1 and the intermediate storage tank 3 to clean them. The cleaning pipe 21 is connected to the filter 7 through a branch pipe 3 24, and a valve is provided on the branch pipe 3 24. The cleaning pipe 21 pumps clean water into the filter 7 through the branch pipe 3 24, and then circulates the water in the circulating purification structure to clean the adsorption tank 5, the purification tank 6, and the filter 7.
[0043] The liquid outlets of the distillation tank 1 and the intermediate storage tank 3 are connected to the cleaning tank 12 through connecting pipes, and a valve is provided on the connecting pipes. The connecting pipes are used to discharge the cleaned water into the cleaning tank 12.
[0044] The recovery method of the above-mentioned methyl chloride waste liquid recovery device containing nitrogen peroxide comprises the following steps:
[0045] S1, turn on the heater 8, the heater 8 introduces the thermal oil into the distillation tank 1 through the oil pump 9 and heats the distillation tank 1; the waste liquid is added to the distillation tank 1 through the feed pipe 13, heated and evaporated in the distillation tank 1, the steam in the distillation tank 1 enters the condenser 2 through the top of the distillation tank 1 through the connecting pipe 14 and condenses, realizing the condensation of methyl chloride, the nitrogen peroxide in the condenser 2 is discharged from the top of the condenser 2 in a gaseous state, and the methyl chloride liquid condensed by the condenser 2 flows into the distillation tank 1 through the connecting pipe, and the repeated condensation of methyl chloride and the sufficient discharge of nitrogen peroxide are carried out;
[0046] S2, after the cycle, the methyl chloride condensed by the condenser 2 enters the intermediate storage tank 3 through the connecting pipe for storage, and the intermediate storage tank 3 pumps the methyl chloride liquid into the adsorption tank 5 for adsorption through the connecting pipe 2 15 and the circulating pump 4, and then flows into the intermediate storage tank 3 through the circulating pipe 19 for circulation;
[0047] S3, the methyl chloride after the cycle adsorption enters the purification tank 6 through the connecting pipe three 16, then enters the filter 7 through the connecting pipe for filtration, flows into the storage tank 3 through the connecting pipe four 17, and is circulated for purification and filtration. The cycle treatment time is 1-3 hours; finally, the methyl chloride liquid is discharged through the discharge pipe 18;
[0048] S4, the heater 8 introduces the heat transfer oil into the radiator 10 through the oil pump 9, the cold air in the radiator 10 is heated, and the heated hot air is sent to the purification tank 6 to desorb the purification tank 6, thereby realizing the recycling of the purification agent in the purification tank 6;
[0049] S5. Turn on the cleaning pump and introduce the clean water in the cleaning pool 12 into the distillation tank 1 and the intermediate storage tank 3 through the cleaning pipe 21, branch pipe 1 22, and branch pipe 2 23 for cleaning, and then flow into the cleaning pool 12 through the connecting pipe; the clean water in the cleaning pool 12 is introduced into the purification structure through the cleaning pipe 21 and branch pipe 3 24 to clean the adsorption tank 5, purification tank 6 and filter 7 of the purification structure.
[0050] The recovery rate of methyl chloride in the waste liquid treated by the above method is above 90%, and the purity of methyl chloride can meet the relevant quality requirements for use.
[0051] Therefore, the present invention adopts the above-mentioned chloromethane waste liquid recovery device and recovery method containing nitrogen peroxide to effectively separate nitrogen peroxide from chloromethane, effectively recover and reuse chloromethane, and carry out centralized special treatment of nitrogen peroxide in the waste liquid, thereby reducing waste liquid discharge.
[0052] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the same. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that they can still modify or replace the technical solutions of the present invention with equivalents, and these modifications or equivalent replacements cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.
Claims
1. A device for recovering methyl chloride waste liquid containing nitrogen peroxide, characterized in that: The system comprises a distillation tank, a condenser and an intermediate storage tank which are arranged in sequence, a feed pipe being provided on the distillation tank, the distillation tank and the condenser being connected via a connecting pipe 1, the bottom end of the condenser being connected to the intermediate storage tank and the distillation tank respectively via connecting pipes, all of which are provided with valves; a purification structure being provided downstream of the intermediate storage tank; the purification structure comprising an adsorption tank, a purification tank and a filter, the adsorption tank being connected to the intermediate storage tank via a connecting pipe 2, a circulating pump being provided on the connecting pipe 2, the adsorption tank being connected to the purification tank via a connecting pipe 3, the purification tank being connected to the filter via a connecting pipe, the filter being connected to the intermediate storage tank via a connecting pipe 4, a discharge pipe being provided on the filter, and valves being provided on the connecting pipes 2, 3, 4 and the discharge pipe; and a heating structure and a cleaning structure for heating the distillation tank and the purification tank are also provided. The discharge port of the adsorption tank is connected to the reflux port of the intermediate storage tank through a circulation pipe, and a valve is provided on the circulation pipe; The heating structure includes a heater and an oil pump, the heater is connected to the oil pump, the outlet of the oil pump is connected to the heating interlayer of the distillation tank through a connecting pipe, and the heating interlayer of the distillation tank is connected to the heater through a connecting pipe to form a circulating heating loop; the outlet of the oil pump is connected to the radiator through a connecting pipe, and the radiator is connected to the heater through a connecting pipe to form a circulating heating loop, the air inlet of the radiator is provided with a fan, and the air outlet of the radiator is connected to the connecting pipe through a connecting pipe; valves are provided on the connecting pipes; The recovery method of a chloromethane waste liquid recovery device containing nitrogen peroxide comprises the following steps: S1, turn on the heater, the heater imports the thermal oil into the distillation tank by the oil pump and heats the distillation tank; the waste liquid is added to the distillation tank through the feed pipe, heated and evaporated in the distillation tank, the steam in the distillation tank enters the condenser through the distillation tank top by connecting pipe one and condenses, realizes the condensation of methyl chloride, the nitrogen peroxide in the condenser is discharged from the top of the condenser in a gaseous state, the methyl chloride liquid condensed by the condenser flows into the distillation tank by connecting pipe, carries out repeated condensation of methyl chloride and fully discharge of nitrogen peroxide; S2, after circulation, the methyl chloride condensed in the condenser enters the intermediate storage tank through the connecting pipe for storage. The intermediate storage tank pumps the methyl chloride liquid into the adsorption tank through the connecting pipe 2 and the circulation pump for adsorption, and then flows into the intermediate storage tank through the circulation pipe for circulation; S3, the methyl chloride after cyclic adsorption enters the purification tank through the connecting pipe three, then enters the filter through the connecting pipe for filtration, flows into the intermediate storage tank through the connecting pipe four, and is circulated for purification and filtration. The cycle treatment time is 1-3 hours; finally, the methyl chloride liquid is discharged through the discharge pipe; S4, the heater introduces the heat transfer oil into the radiator through the oil pump, the cold air in the radiator is heated, and the heated hot air is sent to the purification tank to desorb the purification tank, thereby realizing the recycling of the purification agent in the purification tank; S5. Turn on the cleaning pump and introduce the clean water in the cleaning pool into the distillation tank and the intermediate storage tank through the cleaning pipe, branch pipe 1, and branch pipe 2 for cleaning, and then flow into the cleaning pool through the connecting pipe; the clean water in the cleaning pool is introduced into the purification structure through the cleaning pipe and branch pipe 3 to clean the adsorption tank, purification tank and filter of the purification structure.
2. The device for recovering methyl chloride waste liquid containing nitrogen peroxide according to claim 1, wherein: The discharge port of the intermediate storage tank is connected to the reflux port of the distillation tank through a second connecting pipe and a reflux pipe.
3. The device for recovering methyl chloride waste liquid containing nitrogen peroxide according to claim 1, wherein: The cleaning structure includes a cleaning pool, a cleaning pump is provided on the cleaning pipe of the cleaning pool, the cleaning pipe is connected to the cleaning port of the distillation tank through branch pipe 1, the cleaning pipe is connected to the inlet of the intermediate storage tank through branch pipe 2, and the cleaning pipe is connected to the filter through branch pipe 3, and a valve is provided on branch pipe 3; the liquid outlets of the distillation tank and the intermediate storage tank are connected to the cleaning pool through connecting pipes, and a valve is provided on the connecting pipes.
4. The device for recovering methyl chloride waste liquid containing nitrogen peroxide according to claim 1, wherein: The volume of the distillation tank is greater than that of the intermediate storage tank.
5. The device for recovering methyl chloride waste liquid containing nitrogen peroxide according to claim 1, wherein: The heating temperature of the distillation tank is 100-200°C, and the condensing temperature of the condenser is 20-50°C.
6. The device for recovering methyl chloride waste liquid containing nitrogen peroxide according to claim 1, wherein: The adsorbent in the adsorption tank is fine-porous silica gel, and the mass ratio of the fine-porous silica gel to liquid methyl chloride is 1:(5-10).
7. The device for recovering methyl chloride waste liquid containing nitrogen peroxide according to claim 1, wherein: The purifying agent in the purification tank is activated carbon, and the mass ratio of the activated carbon to the liquid methyl chloride is 1:(5-10); the pore size of the filter is 100-500 meshes.
Citation Information
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