CN113754165A - Initiator waste acid recycling device system and method - Google Patents

Initiator waste acid recycling device system and method Download PDF

Info

Publication number
CN113754165A
CN113754165A CN202111048791.1A CN202111048791A CN113754165A CN 113754165 A CN113754165 A CN 113754165A CN 202111048791 A CN202111048791 A CN 202111048791A CN 113754165 A CN113754165 A CN 113754165A
Authority
CN
China
Prior art keywords
tank
concentration
kettle
waste acid
accident
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202111048791.1A
Other languages
Chinese (zh)
Other versions
CN113754165B (en
Inventor
王长海
王梦琦
王亚玲
曹爱凤
王翠芝
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Renate Chemical Co ltd
Original Assignee
Shandong Renate Chemical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shandong Renate Chemical Co ltd filed Critical Shandong Renate Chemical Co ltd
Priority to CN202111048791.1A priority Critical patent/CN113754165B/en
Publication of CN113754165A publication Critical patent/CN113754165A/en
Application granted granted Critical
Publication of CN113754165B publication Critical patent/CN113754165B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00Sulfates or sulfites of sodium, potassium or alkali metals in general
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/043Details
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/046Treatment of water, waste water, or sewage by heating by distillation or evaporation under vacuum produced by a barometric column
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/048Purification of waste water by evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/722Oxidation by peroxides
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/101Sulfur compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds

Abstract

The invention discloses an initiator waste acid recycling device system and method, which comprises a waste acid treatment system, a sodium sulfate recovery system and an accident removal system, wherein the waste acid treatment system consists of a middle kettle, a circulating pump, a finished product tank, a hydrogen peroxide metering tank and a concentration tank, the sodium sulfate recovery system consists of a heat exchanger, a diethyl oxalate cleaning water tank, a hot water tank, an ester steaming kettle, a condensed water storage tank, a liquid caustic soda metering tank, a neutralization kettle, a transfer tank, MVR concentration equipment and a condenser, the middle kettle and the concentration tank are connected with the condenser, the condenser is connected with the condensed water storage tank, and the neutralization kettle is sequentially connected with the transfer tank and the MVR concentration equipment; the accident elimination system is composed of an emergency tank, an accident tank and a rupture disk. The invention can recycle the heat source in the treatment process, can produce the byproduct sodium sulfate after the concentrated condensate is neutralized, simultaneously reduces the danger coefficient of production, and is more beneficial to safe production.

Description

Initiator waste acid recycling device system and method
Technical Field
The invention relates to the technical field of chemical waste acid treatment, in particular to a system and a method for recycling initiator waste acid.
Background
A large amount of dilute sulfuric acid is generated in a layered reaction process of a di-tert-butyl peroxide production device and a tert-butyl hydroperoxide production device, the dilute sulfuric acid belongs to hazardous waste, enterprises need to invest a large amount of capital to treat waste acid, the resource recycling rate in the treatment process is low, valuable substances in the waste acid cannot be utilized, and therefore the economic benefit of the enterprises is reduced.
Through massive search, the prior art is found, and the publication number is as follows: CN108033433B discloses an industrial waste acid treatment system. The industrial waste acid treatment system comprises a waste acid concentration system, and the waste acid concentration system comprises a nitric acid concentration device, a first sulfuric acid concentration device and a second sulfuric acid concentration device; the nitric acid concentration device is used for separating and concentrating sulfuric acid waste liquid containing high-concentration nitric acid to obtain a nitric acid product; a first sulfuric acid concentration device is used for treating sulfuric acid waste liquid containing a small amount of nitric acid, and separating and concentrating the sulfuric acid waste liquid to obtain a nitric acid product and sulfuric acid A; and treating the sulfuric acid waste liquid containing the hydrogen halide by using a second sulfuric acid concentration device, and separating and removing the hydrogen halide to obtain sulfuric acid A. The industrial waste acid treatment system can be used for treating various industrial waste acids with different components in a targeted manner and at the same time, the treatment efficiency of the industrial waste acids is improved, and the sulfuric acid product and the nitric acid product obtained after treatment and recovery have high purity and good quality and reach the quality standard of the first-class national standard.
In conclusion, in the waste acid treatment process, the utilization rate of a heat source is low, meanwhile, a worker needs to perform patrol inspection on the site, the working environment is severe, certain potential safety hazards exist, waste liquid resources cannot be effectively recycled, and the economic benefits of enterprises can be reduced.
Disclosure of Invention
The invention aims to provide an initiator waste acid recycling device system and method to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: an initiator waste acid recycling device system and method comprises a waste acid treatment system, a sodium sulfate recovery system and an accident removal system, wherein the waste acid treatment system comprises an intermediate kettle, a circulating pump, a finished product tank, a hydrogen peroxide metering tank and a concentration tank, the intermediate kettle and the concentration tank are both connected with a waste acid conveying pipe, the intermediate kettle and the concentration tank are communicated, the concentration tank is connected with the hydrogen peroxide metering tank, and the concentration tank is connected with the finished product tank;
the sodium sulfate recovery system consists of a heat exchanger, a diethyl oxalate cleaning water tank, a hot water tank, an ester steaming kettle, a condensed water storage tank, a liquid caustic soda metering tank, a neutralization kettle, a transit tank, MVR concentration equipment and a condenser, wherein the intermediate kettle and the concentration tank are both connected with the condenser, the condenser is connected with the condensed water storage tank, the neutralization kettle is respectively connected with the condensed water storage tank and the liquid caustic soda metering tank, the neutralization kettle is sequentially connected with the transit tank and the MVR concentration equipment,
the heat exchanger is communicated with the hot water tank, the heat exchanger and the hot water tank are both communicated with a diethyl oxalate cleaning water tank, the diethyl oxalate cleaning water tank is connected with an ester steaming kettle, and the ester steaming kettle is communicated with MVR concentration equipment;
the accident removing system is composed of an emergency tank, an accident tank and a rupture disc, the accident tank is connected with the concentration tank, the rupture disc is arranged between the accident tank and the concentration tank, the accident tank is connected with the emergency tank, and the emergency tank is communicated with the finished product tank.
Preferably, based on the waste acid treatment system:
automatic valves are arranged at the joints of the intermediate kettle, the concentration tank and the waste acid conveying pipe, the intermediate kettle is connected with a steam pipe, the automatic valve is arranged at the joint of the steam pipe and the intermediate kettle, a flow meter is arranged at the joint of the concentration tank and the waste liquid conveying pipe and used for remotely controlling waste liquid conveying, and the flow meter is used for detecting the flow of waste acid input into the concentration tank;
magnetic turning plate liquid level meters are arranged in the middle kettle and the concentration tank respectively and used for monitoring the waste acid liquid levels in the middle kettle and the concentration tank, and the magnetic turning plate liquid level meters in the concentration tank are connected with automatic valves at the connection parts of the hydrogen peroxide metering tank and the concentration tank;
and a delivery pump is arranged between the concentration tank and the finished product tank and is used for pumping out the finished product liquid in the concentration tank and entering the finished product tank for storage.
Preferably, based on the sodium sulfate recovery system:
the intermediate kettle, the circulating pump and the heat exchanger form a circulating system, the hot water pool and the heat exchanger form a hot water and steam circulating system, and the concentration tank is connected with the hot water pool;
the concentrating tank and hot water tank connecting pipeline is provided with a bypass and automatic control valves, and a magnetic turning plate liquid level meter is arranged in the hot water tank.
Preferably, based on the accident elimination system:
the concentrated jar top is provided with temperature measurement meter and pressure gauge, accident jar upper end is provided with the spark arrester, and the internal diameter of spark arrester is 1.5 times of accident jar and concentrated jar connecting tube diameter.
Preferably, the use method of the waste acid treatment system is as follows:
s1: waste acid enters a concentration tank through an automatic control valve and a mass flow meter of a waste acid conveying pipe, reaches a specified liquid level through a magnetic turning plate liquid level meter, and the automatic control valve is closed;
s2: closing the automatic control valve, simultaneously opening the automatic control valve of the steam, then opening the automatic control valve, starting heating, and allowing condensed steam condensate water to enter a hot water pool through a drain valve;
s3: closing the automatic control valve, pumping waste acid into the intermediate kettle through the visual neutralization manual valve, reaching a specified liquid level through the magnetic turning plate liquid level meter, and closing the automatic discharge control valve of the waste acid storage tank;
s4: starting a circulating pump of the intermediate kettle, and circulating the waste acid through a heat exchanger; starting a hot water pool and a circulating pump, enabling collected hot water to enter a heat exchanger, and preheating waste acid in the intermediate kettle; the preheating process is condensed by a condenser to form a negative pressure distillation process, so that the concentration speed is increased;
s5: the concentrating tank is heated by steam and distilled under negative pressure, the evaporated gas is condensed by a condenser, the condensate is collected in a condensate storage tank, the condensate in the condensate storage tank can enter a neutralization kettle through vacuum, and the neutralization kettle is provided with a magnetic turning plate liquid level meter to turn off an automatic control valve to stop rotating materials;
s6: the sulfuric acid is fed in by starting an automatic control valve after being reduced to a specified liquid level through a magnetic turning plate liquid level meter; when the supplement amount of the intermediate kettle reaches a specified liquid level through a magnetic turning plate liquid level meter, an automatic control valve is opened, a discharge valve of a waste acid storage tank is interlocked, and new waste acid is supplemented from a tank area;
s7: calculating the total amount of waste acid added into the concentration tank through a mass flow meter, and stopping waste acid supplement through a control chamber when the required amount of the process is reached;
s8: in the concentration process of the concentration tank, an automatic control valve is informed, hydrogen peroxide is added in an automatic flow manner in the whole process, an on-line acid-base meter is used for monitoring acidity, the requirement on closing a steam inlet pipe, a steam condensate outlet pipe, a cooling circulating water outlet pipe and an inlet pipe control valve is met, the temperature is reduced, a double thermometer is arranged, the double thermometer is opened when the temperature is reduced to 35 ℃, and a tank bottom discharge valve and a material transfer pump are opened to transfer the material to a finished product tank; and stopping transferring the materials through a pressure transmitter of the material transferring pump, closing a discharge valve at the bottom of the tank and starting a new round of concentration.
Preferably, the accident elimination system is used as follows:
SS 1: the concentration tank is provided with two thermometers, one thermometer is displayed on site, one thermometer is remotely controlled, the temperature is corrected and remotely controlled, the concentration tank is provided with a positive and negative pressure vacuum pressure gauge, and the positive pressure gauge is interlocked with the automatic control valve of the cooling water at the positive pressure of 0.03MPa to carry out emergency cooling, so that safety accidents are prevented;
SS 2: the concentration tank is provided with a rupture disk of 0.3MPa and a manual explosion relief valve, when the patrol personnel finds overpressure, the pressure can be manually relieved, and when each monitoring means fails, the explosion disk is used for relief;
SS 3: the discharged liquid enters an accident tank, the accident tank is provided with a vent-pipe with a fire arrester, and the aperture is 1.5 times of that of the inlet; an emergency relief valve is arranged below the accident tank, and the accident liquid can enter the emergency tank through the emergency relief valve and can be transferred into a finished product tank or a neutralization kettle according to the quality of the entering materials.
Preferably, the sodium sulfate recovery system has the following use method:
a. neutralizing the collected liquid in a neutralization kettle by a liquid alkali metering tank, wherein the liquid alkali metering tank is provided with a magnetic turning plate liquid level meter, a control tank area is driven into the liquid alkali metering tank, an automatic control valve is arranged below the liquid alkali metering tank to add liquid alkali into the neutralization kettle, the neutralization kettle is provided with an online PH detector, and the dropwise addition of the liquid alkali is stopped when the PH reaches 6.8-7.2;
b. after neutralization, transferring the collected liquid into MVR concentration equipment for evaporation, crystallization and concentration to produce a byproduct sodium sulfate;
c. a liquid level meter is arranged in the hot water tank, when the liquid level of the hot water reaches an upper limit and a lower limit, an automatic valve is controlled to be opened, the residual heat water is pumped into a diethyl oxalate cleaning water tank for process cleaning water of the ester steaming kettle, and residual salts in the ester steaming kettle enter MVR concentration equipment to produce a byproduct sodium sulfate;
and d, evaporating and crystallizing the condensed water by using MVR concentration equipment, and feeding the condensed water into a condensed water storage tank for acid, alkali and cleaning water preparation of a di-tert-butyl peroxide production device and a tert-butyl hydroperoxide production device.
Compared with the prior art, the invention has the following beneficial effects:
1. the heat source can be recycled in the treatment process, and the recycled orderly condensed water can be used as the cleaning water for the process of the diethyl oxalate kettle;
2. after the concentrated condensate is neutralized, the MVR concentration equipment is adopted to produce a byproduct sodium sulfate salt, so that extra economic benefits of enterprises can be increased, water generated by the MVR concentration equipment can be recycled, the sewage discharge amount and the use amount of fresh water are reduced, and the cost of waste acid treatment of the enterprises is reduced;
3. the emergency accident handling part is additionally arranged, so that the risk factors are reduced, the working environment of workers is improved, and the safety of practical application is improved.
Drawings
FIG. 1 is a schematic view of the process flow structure of the present invention.
In the figure: 1. an intermediate kettle; 2. a circulation pump; 3. a heat exchanger; 4. cleaning a water tank by using diethyl oxalate; 5. a hot water tank; 6. ester steaming kettle; 7. a condensed water storage tank; 8. a liquid caustic metering tank; 9. a neutralization kettle; 10. a transfer tank; 11. an MVR concentration device; 12. a finished product tank; 13. an emergency tank; 14. an accident can; 15. a rupture disk; 16. a condenser; 17. a hydrogen peroxide metering tank; 18. and (7) concentrating the mixture.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1, three embodiments of the present invention are provided: an initiator waste acid recycling device system and a method thereof comprise a waste acid treatment system, a sodium sulfate recycling system and an accident elimination system,
the first embodiment is as follows:
the waste acid treatment system is composed of a middle kettle 1, a circulating pump 2, a finished product tank 12, a hydrogen peroxide metering tank 17 and a concentration tank 18, wherein the middle kettle 1 and the concentration tank 18 are both connected with a waste acid conveying pipe, the middle kettle 1 is communicated with the concentration tank 18, the concentration tank 18 is connected with the hydrogen peroxide metering tank 17, and the concentration tank 18 is connected with the finished product tank 12;
based on among the waste acid processing system:
automatic valves are arranged at the joints of the intermediate kettle 1 and the concentration tank 18 with the waste acid conveying pipe, the intermediate kettle 1 is connected with a steam pipe, the joint of the steam pipe and the intermediate kettle 1 is provided with the automatic valve, the joint of the concentration tank 18 with the waste liquid conveying pipe is provided with a flow meter for remotely controlling waste liquid conveying, and the flow meter is used for detecting the flow of waste acid input into the concentration tank 18;
magnetic turning plate liquid level meters are arranged in the intermediate kettle 1 and the concentration tank 18 and used for monitoring the waste acid liquid levels in the intermediate kettle 1 and the concentration tank 18, and the magnetic turning plate liquid level meters in the concentration tank 18 are connected with automatic valves at the connection positions of the hydrogen peroxide metering tank 17 and the concentration tank 18;
a transfer pump is arranged between the concentration tank 18 and the finished product tank 12 and is used for pumping out the finished product liquid in the concentration tank 18 into the finished product tank 12 for storage.
The application method of the waste acid treatment system comprises the following steps:
s1: waste acid enters a concentration tank 18 through an automatic control valve and a mass flow meter of a waste acid conveying pipe, reaches a specified liquid level through a magnetic turning plate liquid level meter, and the automatic control valve is closed;
s2: closing the automatic control valve, simultaneously opening the automatic control valve of the steam, then opening the automatic control valve, starting heating, and enabling condensed steam condensate water to enter the hot water pool 5 through the drain valve;
s3: closing the automatic control valve, simultaneously pumping waste acid into the intermediate kettle 1 through the visual neutralization manual valve, reaching a specified liquid level through the magnetic turning plate liquid level meter, and closing the automatic discharge control valve of the waste acid storage tank;
s4: starting a circulating pump 2 of the intermediate kettle 1, and circulating waste acid through a heat exchanger 3; starting a hot water tank 5 and a circulating pump 2, enabling collected hot water to enter a heat exchanger 3, and preheating waste acid in the intermediate kettle 1; the preheating process is condensed by a condenser 16 to form a negative pressure distillation process, so that the concentration speed is increased;
s5: the concentrating tank 18 is heated by steam and distilled at negative pressure, the evaporated gas is condensed by the condenser 16, the condensate is collected in the condensate storage tank 7, the condensate in the condensate storage tank 7 can enter the neutralizing kettle 9 through vacuum, and the neutralizing kettle 9 is provided with a magnetic turning plate liquid level meter on-off automatic control valve to stop rotating materials;
s6: the sulfuric acid is fed in by starting an automatic control valve after being reduced to a specified liquid level through a magnetic turning plate liquid level meter; when the supplement amount of the intermediate kettle 1 reaches a specified liquid level through a magnetic turning plate liquid level meter, an automatic control valve is opened, a discharge valve of a waste acid storage tank is interlocked, and new waste acid is supplemented from a tank area;
s7: calculating the total amount of the waste acid added into the concentration tank 18 through a mass flow meter, and stopping waste acid supplement through a control chamber when the required amount of the process is reached;
s8: in the concentration process of the concentration tank 18, an automatic control valve is informed, hydrogen peroxide is added in an automatic flow mode in the whole process, an on-line acid-base meter is used for monitoring acidity, the requirement for closing a steam inlet pipe, a steam condensate outlet pipe, a cooling circulating water outlet pipe and a pipe inlet control valve is met, the temperature is reduced, a double thermometer is arranged, the double thermometer is opened when the temperature is reduced to 35 ℃, and a tank bottom discharge valve and a material transfer pump are opened to transfer the material to the finished product tank 12; stopping transferring the material by a pressure transmitter of a transferring pump, closing a tank bottom discharge valve and starting a new round of concentration
Example two:
the sodium sulfate recovery system comprises a heat exchanger 3, a diethyl oxalate cleaning water tank 4, a hot water tank 5, an ester steaming kettle 6, a condensed water storage tank 7, a liquid caustic soda metering tank 8, a neutralization kettle 9, a transfer tank 10, an MVR concentration device 11 and a condenser 16, wherein the intermediate kettle 1 and the concentration tank 18 are connected with the condenser 16, the condenser 16 is connected with the condensed water storage tank 7, the neutralization kettle 9 is respectively connected with the condensed water storage tank 7 and the liquid caustic soda metering tank 8, and the neutralization kettle 9 is sequentially connected with the transfer tank 10 and the MVR concentration device 11;
heat exchanger 3 and hot-water tank 5 communicate each other, and heat exchanger 3 and hot-water tank 5 all are linked together with diethyl oxalate washing water tank 4, and diethyl oxalate washing water tank 4 is connected with evaporates ester cauldron 6, evaporates ester cauldron 6 and MVR concentrator 11 and is linked together.
Sodium sulfate based recovery system:
the intermediate kettle 1, the circulating pump 2 and the heat exchanger 3 form a circulating system, the hot water pool 5 and the heat exchanger 3 form a hot water and steam circulating system, and the concentration tank 18 is connected with the hot water pool 5;
the pipeline connecting the concentration tank 18 and the hot water tank 5 is provided with a bypass and is provided with an automatic control valve, and a magnetic turning plate liquid level meter is arranged in the hot water tank 5.
The use method of the sodium sulfate recovery system comprises the following steps:
a. neutralizing the collected liquid in a neutralization kettle 9 through a liquid alkali metering tank 8, wherein the liquid alkali metering tank 8 is provided with a magnetic turning plate liquid level meter, a control tank area is pumped into the liquid alkali metering tank 8, an automatic control valve is arranged below the liquid alkali metering tank 8 to add liquid alkali into the neutralization kettle 9, the neutralization kettle 9 is provided with a PH online detector, and the dropwise addition of the liquid alkali is stopped when the PH reaches 6.8-7.2;
b. after the neutralization, the collected liquid is transferred to MVR concentration equipment 11 for evaporation, crystallization and concentration to produce a byproduct sodium sulfate;
c. the hot water tank 5 is provided with a liquid level meter, when the liquid level of the hot water reaches an upper limit and a lower limit, an automatic valve is controlled to be opened, the residual heat water is pumped into a diethyl oxalate cleaning water tank 4 for cleaning the process of the ester steaming kettle 6, and the residual salts in the ester steaming kettle 6 enter an MVR concentration device 11 to produce a byproduct sodium sulfate;
d, evaporating and crystallizing condensed water by using MVR concentration equipment 11, feeding the condensed water into a condensed water storage tank 7, and using the condensed water for acid and alkali preparation and cleaning water of a di-tert-butyl peroxide production device and a tert-butyl hydroperoxide production device
Example three:
the accident removing system is composed of an emergency tank 13, an accident tank 14 and a rupture disk 15, wherein the accident tank 14 is connected with a concentration tank 18, the rupture disk 15 is arranged between the accident tank 14 and the concentration tank 18, the accident tank 14 is connected with the emergency tank 13, and the emergency tank 13 is communicated with a finished product tank 12.
In an accident-based rejection system:
the top end of the concentration tank 18 is provided with a temperature measuring meter and a pressure meter, the upper end of the accident tank 14 is provided with a flame arrester, and the inner diameter of the flame arrester is 1.5 times of the diameter of a connecting pipeline of the accident tank 14 and the concentration tank 18.
The accident elimination system has the following use method:
SS 1: the concentration tank 18 is provided with two thermometers, one thermometer is displayed on site, one thermometer is remotely controlled, the temperature is corrected and remotely controlled, the concentration tank 18 is provided with a positive and negative pressure vacuum pressure gauge, and the positive pressure gauge is interlocked with the automatic control valve of the cooling water when the positive pressure is 0.03MPa to carry out emergency cooling, so that safety accidents are prevented;
SS 2: the concentration tank 18 is provided with a rupture disk of 150.3MPa and a manual explosion relief valve, when the patrol personnel finds overpressure, the pressure can be manually relieved, and when each monitoring means fails, the pressure is relieved through the rupture disk 15;
SS 3: the discharged liquid enters the accident tank 14, the accident tank 14 is provided with a vent-out device with a fire damper, and the aperture is 1.5 times of that of the inlet; an emergency relief valve is arranged below the accident tank 14, and accident liquid can enter the emergency tank 13 through the emergency relief valve and can be transferred into the finished product tank 12 or the neutralization kettle 9 according to the quality of entering materials.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (7)

1. The utility model provides an initiator spent acid recycle device system which characterized in that: the waste acid treatment system comprises a waste acid treatment system, a sodium sulfate recovery system and an accident removal system, wherein the waste acid treatment system is composed of a middle kettle (1), a circulating pump (2), a finished product tank (12), a hydrogen peroxide metering tank (17) and a concentration tank (18), the middle kettle (1) and the concentration tank (18) are both connected with a waste acid conveying pipe, the middle kettle (1) and the concentration tank (18) are communicated, the concentration tank (18) is connected with the hydrogen peroxide metering tank (17), and the concentration tank (18) is connected with the finished product tank (12);
the sodium sulfate recovery system comprises a heat exchanger (3), a diethyl oxalate cleaning water tank (4), a hot water tank (5), an ester steaming kettle (6), a condensed water storage tank (7), a liquid caustic soda metering tank (8), a neutralization kettle (9), a transfer tank (10), MVR concentration equipment (11) and a condenser (16), wherein the intermediate kettle (1) and the concentration tank (18) are both connected with the condenser (16), the condenser (16) is connected with the condensed water storage tank (7), the neutralization kettle (9) is respectively connected with the condensed water storage tank (7) and the liquid caustic soda metering tank (8), the neutralization kettle (9) is sequentially connected with the transfer tank (10) and the MVR concentration equipment (11),
the heat exchanger (3) is communicated with the hot water tank (5), the heat exchanger (3) and the hot water tank (5) are both communicated with a diethyl oxalate cleaning water tank (4), the diethyl oxalate cleaning water tank (4) is connected with an ester steaming kettle (6), and the ester steaming kettle (6) is communicated with an MVR concentration device (11);
the accident removing system is composed of an emergency tank (13), an accident tank (14) and a rupture disc (15), the accident tank (14) is connected with a concentration tank (18), the rupture disc (15) is arranged between the accident tank (14) and the concentration tank (18), the accident tank (14) is connected with the emergency tank (13), and the emergency tank (13) is communicated with a finished product tank (12).
2. The initiator waste acid recycling device system of claim 1, wherein: based on among the waste acid processing system:
automatic valves are arranged at the joints of the intermediate kettle (1) and the concentration tank (18) with the waste acid conveying pipe, the intermediate kettle (1) is connected with a steam pipe, the joint of the steam pipe and the intermediate kettle (1) is provided with the automatic valve, a flow meter is arranged at the joint of the concentration tank (18) with the waste liquid conveying pipe and used for remotely controlling waste liquid conveying, and the flow meter is used for detecting the flow of waste acid input into the concentration tank (18);
magnetic turning plate liquid level meters are arranged in the intermediate kettle (1) and the concentration tank (18) and used for monitoring waste acid liquid levels in the intermediate kettle (1) and the concentration tank (18), and the magnetic turning plate liquid level meters in the concentration tank (18) are connected with automatic valves at the connection positions of the hydrogen peroxide metering tank (17) and the concentration tank (18);
a delivery pump is arranged between the concentration tank (18) and the finished product tank (12) and is used for pumping out the finished product liquid in the concentration tank (18) to enter the finished product tank (12) for storage.
3. The initiator waste acid recycling device system of claim 1, wherein: sodium sulfate based recovery system:
the intermediate kettle (1), the circulating pump (2) and the heat exchanger (3) form a circulating system, the hot water pool (5) and the heat exchanger (3) form a hot water and steam circulating system, and the concentration tank (18) is connected with the hot water pool (5);
the connecting pipeline of the concentration tank (18) and the hot water tank (5) is provided with a bypass and automatic control valves, and a magnetic turning plate liquid level meter is arranged in the hot water tank (5).
4. The initiator waste acid recycling device system of claim 1, wherein: in an accident-based rejection system:
the top end of the concentration tank (18) is provided with a temperature measuring meter and a pressure meter, the upper end of the accident tank (14) is provided with a flame arrester, and the inner diameter of the flame arrester is 1.5 times of the diameter of a connecting pipeline between the accident tank (14) and the concentration tank (18).
5. The method for recycling the initiator waste acid as claimed in claims 1 and 2, wherein the method comprises the following steps: the application method of the waste acid treatment system comprises the following steps:
s1: waste acid enters a concentration tank (18) through an automatic control valve and a mass flow meter of a waste acid conveying pipe, reaches a specified liquid level through a magnetic turning plate liquid level meter, and the automatic control valve is closed;
s2: closing the automatic control valve, simultaneously opening the automatic control valve of the steam, then opening the automatic control valve, starting heating, and enabling condensed steam condensate water to enter a hot water pool (5) through a drain valve;
s3: when the automatic control valve is closed, the waste acid is pumped into the intermediate kettle (1) through the visual neutralization manual valve, a specified liquid level is reached through the magnetic turning plate liquid level meter, and the automatic discharge control valve of the waste acid storage tank is closed;
s4: starting a circulating pump (2) of the intermediate kettle (1), and enabling waste acid to form circulation through a heat exchanger (3); starting a hot water tank (5) and a circulating pump (2), enabling collected hot water to enter a heat exchanger (3), and preheating waste acid in the intermediate kettle (1); the preheating process is condensed by a condenser (16) to form a negative pressure distillation process, so that the concentration speed is increased;
s5: the concentrating tank (18) is heated by steam and distilled under negative pressure, the evaporated gas is condensed by a condenser (16), condensate is collected in a condensate storage tank (7), the condensate in the condensate storage tank (7) can enter a neutralization kettle (9) through vacuum, and the neutralization kettle (9) is provided with a magnetic turning plate liquid level meter to automatically control the closing of the valve to stop rotating materials;
s6: the sulfuric acid is fed in by starting an automatic control valve after being reduced to a specified liquid level through a magnetic turning plate liquid level meter; when the supplement amount reaches the specified liquid level through a magnetic turning plate liquid level meter, the intermediate kettle (1) opens an automatic control valve, interlocks a discharge valve of a waste acid storage tank, and supplements new waste acid from a tank area;
s7: the total amount of the waste acid added into the concentration tank (18) is calculated by a mass flow meter, and when the required amount of the process is reached, the waste acid is stopped to be supplemented by a control chamber;
s8: in the concentration process of the concentration tank (18), an automatic control valve is informed, hydrogen peroxide is added in the whole process in an automatic flow mode, the acidity is monitored through an online acid-base meter, the requirement for closing a steam inlet pipe, a steam condensate outlet pipe, a cooling circulating water outlet pipe and a pipe inlet control valve is met, the temperature is reduced, a double thermometer is arranged, the double thermometer is opened when the temperature is reduced to 35 degrees, and a tank bottom discharge valve and a material transfer pump are opened to transfer the materials to a finished product tank (12); and stopping transferring the materials through a pressure transmitter of the material transferring pump, closing a discharge valve at the bottom of the tank and starting a new round of concentration.
6. The method for recycling the initiator waste acid as claimed in claims 1 and 4, wherein the method comprises the following steps: the accident elimination system has the following using method:
SS 1: the concentration tank (18) is provided with two thermometers, one thermometer is displayed on site, one thermometer is controlled by remote transmission, the temperature is corrected and controlled by remote transmission, the concentration tank (18) is provided with a positive and negative pressure vacuum pressure gauge, and the positive pressure gauge is interlocked with the automatic control valve of the cooling water when the positive pressure is 0.03Mpa so as to carry out emergency cooling and prevent safety accidents;
SS 2: the concentration tank (18) is provided with a rupture disk (15) with the pressure of 0.3MPa and a manual explosion relief valve, when the patrol personnel finds overpressure, the pressure can be manually relieved, and when each monitoring means fails, the explosion disk (15) is used for releasing;
SS 3: the discharged liquid enters an accident tank (14), the accident tank (14) is provided with a vent with a fire arrester, and the aperture is 1.5 times of that of the inlet; an emergency relief valve is arranged below the accident tank (14), and accident liquid can enter the emergency tank (13) through the emergency relief valve and can be transferred into the finished product tank (12) or the neutralization kettle (9) according to the quality of the entering materials.
7. The method for recycling the initiator waste acid as claimed in claims 1 and 3, wherein the method comprises the following steps: the use method of the sodium sulfate recovery system comprises the following steps:
a. neutralizing the collected liquid in a neutralization kettle (9) through a liquid caustic soda metering tank (8), wherein the liquid caustic soda metering tank (8) is provided with a magnetic turning plate liquid level meter, a control tank area is driven into the liquid caustic soda metering tank (8), an automatic control valve is arranged below the liquid caustic soda metering tank (8) to add liquid caustic soda into the neutralization kettle (9), the neutralization kettle (9) is provided with a PH online detector, and the dropwise addition of the liquid caustic soda is stopped when the PH reaches 6.8-7.2;
b. after neutralization, the collected liquid is transferred into MVR concentration equipment (11) for evaporation, crystallization and concentration to produce a byproduct sodium sulfate;
c. the hot water tank (5) is provided with a liquid level meter, when the liquid level of the hot water reaches an upper limit and a lower limit, an automatic valve is controlled to be opened, the excess heat water is pumped into a diethyl oxalate cleaning water tank (4) for process cleaning water of the ester steaming kettle (6), and residual salts in the ester steaming kettle (6) enter MVR concentration equipment (11) to produce a byproduct sodium sulfate;
and d, evaporating and crystallizing condensed water by using the MVR concentration equipment (11), and feeding the condensed water into a condensed water storage tank (7) for acid, alkali and cleaning water of the di-tert-butyl peroxide production device and the tert-butyl hydroperoxide production device.
CN202111048791.1A 2021-09-08 2021-09-08 Initiator waste acid recycling device system and method Active CN113754165B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111048791.1A CN113754165B (en) 2021-09-08 2021-09-08 Initiator waste acid recycling device system and method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111048791.1A CN113754165B (en) 2021-09-08 2021-09-08 Initiator waste acid recycling device system and method

Publications (2)

Publication Number Publication Date
CN113754165A true CN113754165A (en) 2021-12-07
CN113754165B CN113754165B (en) 2023-04-25

Family

ID=78793763

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111048791.1A Active CN113754165B (en) 2021-09-08 2021-09-08 Initiator waste acid recycling device system and method

Country Status (1)

Country Link
CN (1) CN113754165B (en)

Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4239748C1 (en) * 1992-11-26 1994-02-10 Guetling Gmbh Retardation system with compressed air diaphragm pump and stroke counter
JPH0957002A (en) * 1995-08-25 1997-03-04 Konica Corp Heat pump type evaporating concentrator and treatment using same
JP2004195400A (en) * 2002-12-19 2004-07-15 Jfe Engineering Kk Method for producing mixed salt from waste in gasification modification process
UA78936C2 (en) * 2005-12-19 2007-04-25 Open Joint Stock Company Conce Method for obtaining of nitrite-nitrate salts
SE0600154L (en) * 2006-01-24 2007-07-25 Bengt H Nilsson Med Ultirec Fa Procedure for incremental energy conversion
CN201010528Y (en) * 2007-03-06 2008-01-23 天津市聚鑫源水处理技术开发有限公司 Processing system for recycling ferrous chloride crystal and hydrochloric acid from hydrochloric acid waste liquid
JP2008291052A (en) * 2007-05-22 2008-12-04 Teijin Chem Ltd Method for recovering alkali metal hydroxide aqueous solution of purified aromatic dihydroxy compound
CN101570316A (en) * 2009-05-27 2009-11-04 无锡市星亿涂装环保设备有限公司 Method and device for refining and recycling hydrochloric acid from hydrochloric acid pickling waste liquid
EP2407230A1 (en) * 2010-07-16 2012-01-18 Immoplan Technische Gebäudeausstattung Method for sorption drying using potassium salts, device for performing the method and processing of the products from the method
CN106219850A (en) * 2016-08-17 2016-12-14 江苏泫槿环境科技有限公司 The recycling and processing device of a kind of hydrazine hydrate waste liquid and recovery and treatment method
CN106467341A (en) * 2016-08-24 2017-03-01 内蒙古兰太实业股份有限公司 Sym-closene production wastewater treatment system and method
CN106966451A (en) * 2017-04-12 2017-07-21 赵琪 A kind of method for solving cyclohexanone saponification waste lye secondary pollution
CN106967864A (en) * 2016-01-14 2017-07-21 武汉科技大学 A kind of production method of novel liquid steel dephosphorization slag former
CN107188354A (en) * 2017-05-16 2017-09-22 北京清大天工能源技术研究所有限公司 A kind of vegetable protein beans stripping water recovery method based on film Yu heat pump complex technique
CN108159719A (en) * 2018-01-08 2018-06-15 南京工业大学 A kind of energy-efficient MVR evaporation concentration systems
CN109626684A (en) * 2017-10-09 2019-04-16 中国石油化工股份有限公司 The processing unit and its technique of high nitrate wastewater
CN111747467A (en) * 2020-07-03 2020-10-09 兰州节能环保工程有限责任公司 Sewage treatment method and device
CN114893792A (en) * 2022-05-24 2022-08-12 苏州金宏气体股份有限公司 Remote ignition system and method for hydrogen bromide synthesis furnace

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4239748C1 (en) * 1992-11-26 1994-02-10 Guetling Gmbh Retardation system with compressed air diaphragm pump and stroke counter
JPH0957002A (en) * 1995-08-25 1997-03-04 Konica Corp Heat pump type evaporating concentrator and treatment using same
JP2004195400A (en) * 2002-12-19 2004-07-15 Jfe Engineering Kk Method for producing mixed salt from waste in gasification modification process
UA78936C2 (en) * 2005-12-19 2007-04-25 Open Joint Stock Company Conce Method for obtaining of nitrite-nitrate salts
SE0600154L (en) * 2006-01-24 2007-07-25 Bengt H Nilsson Med Ultirec Fa Procedure for incremental energy conversion
CN201010528Y (en) * 2007-03-06 2008-01-23 天津市聚鑫源水处理技术开发有限公司 Processing system for recycling ferrous chloride crystal and hydrochloric acid from hydrochloric acid waste liquid
JP2008291052A (en) * 2007-05-22 2008-12-04 Teijin Chem Ltd Method for recovering alkali metal hydroxide aqueous solution of purified aromatic dihydroxy compound
CN101570316A (en) * 2009-05-27 2009-11-04 无锡市星亿涂装环保设备有限公司 Method and device for refining and recycling hydrochloric acid from hydrochloric acid pickling waste liquid
EP2407230A1 (en) * 2010-07-16 2012-01-18 Immoplan Technische Gebäudeausstattung Method for sorption drying using potassium salts, device for performing the method and processing of the products from the method
CN106967864A (en) * 2016-01-14 2017-07-21 武汉科技大学 A kind of production method of novel liquid steel dephosphorization slag former
CN106219850A (en) * 2016-08-17 2016-12-14 江苏泫槿环境科技有限公司 The recycling and processing device of a kind of hydrazine hydrate waste liquid and recovery and treatment method
CN106467341A (en) * 2016-08-24 2017-03-01 内蒙古兰太实业股份有限公司 Sym-closene production wastewater treatment system and method
CN106966451A (en) * 2017-04-12 2017-07-21 赵琪 A kind of method for solving cyclohexanone saponification waste lye secondary pollution
CN107188354A (en) * 2017-05-16 2017-09-22 北京清大天工能源技术研究所有限公司 A kind of vegetable protein beans stripping water recovery method based on film Yu heat pump complex technique
CN109626684A (en) * 2017-10-09 2019-04-16 中国石油化工股份有限公司 The processing unit and its technique of high nitrate wastewater
CN108159719A (en) * 2018-01-08 2018-06-15 南京工业大学 A kind of energy-efficient MVR evaporation concentration systems
CN111747467A (en) * 2020-07-03 2020-10-09 兰州节能环保工程有限责任公司 Sewage treatment method and device
CN114893792A (en) * 2022-05-24 2022-08-12 苏州金宏气体股份有限公司 Remote ignition system and method for hydrogen bromide synthesis furnace

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
席浩君等: "机械式蒸汽再压缩技术应用于盐废水回收实验研究", 《甘肃科技》 *
杜红莲: "酸站结晶机二次蒸汽外排的技术改造", 《人造纤维》 *
黄晶: "浓缩蒸发冷凝水用于浓缩器清洗的研究", 《安徽农业科学》 *

Also Published As

Publication number Publication date
CN113754165B (en) 2023-04-25

Similar Documents

Publication Publication Date Title
CN107055569A (en) A kind of comprehensive utilization process of liquid containing ammonium sulfate industrial wastewater
CN204588694U (en) A kind of production system of used in electronic industry hydrofluoric acid
CN206587734U (en) A kind of chloroacetate reaction kettle system of accident disposal
CN113754165A (en) Initiator waste acid recycling device system and method
CN212425437U (en) Dilute hydrochloric acid recovery processing system
CN211971803U (en) Novel materialized wastewater triple-effect evaporation system
CN209019924U (en) A kind of uranyl nitrate solution enrichment facility
CN207079005U (en) A kind of wire rope factory abraum salt acid treatment device
CN207950720U (en) The system of condensing recovery dinitrogen tetroxide exhaust gas resource
CN216497530U (en) Bromine distillation circulation heating system
CN206424599U (en) Akali sulphide two-effect evaporation process system
CN106397289B (en) The process units and its production method of a kind of Sodium Dimethyldithiocarbamate
CN211496947U (en) Sulfur trioxide preparation facilities
CN204147564U (en) A kind of equipment utilizing solar energy concentrated vitriol zinc solution
CN202012732U (en) Novel anticorrosion vaporization device system used for liquid chlorine vaporization
CN220939129U (en) Waste acid concentration device
CN218380659U (en) Cleaning pretreatment device for horizontal spiral plate heat exchanger
CN208071611U (en) The separator of acetic acid sodium crystal in a kind of lye
CN208087250U (en) The device that high-salt wastewater low-temperature evaporation is concentrated using hot industry waste water
CN204380525U (en) Titanium white waste acid membrane distillation concentration device
CN214075856U (en) Liquid level detection device and exhaust treatment system comprising same
CN212832849U (en) Recovery processing system of chlor-alkali industry dilute sulfuric acid
CN105668533A (en) Reactor cleaning method for phosphorus trichloride production
CN209575781U (en) A kind of interactive heat exchange type vapo(u)rization system
CN212491615U (en) Vacuum distillation device for cysteamine hydrochloride

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CB03 Change of inventor or designer information
CB03 Change of inventor or designer information

Inventor after: Wang Changhai

Inventor after: Zhang Keqin

Inventor after: Zhang Kehan

Inventor after: Zhang Liangping

Inventor after: Wang Mengqi

Inventor after: Wang Yaling

Inventor after: Zhang Zongfu

Inventor before: Wang Changhai

Inventor before: Wang Mengqi

Inventor before: Wang Yaling

Inventor before: Cao Aifeng

Inventor before: Wang Cuizhi