CN113754165B - Initiator waste acid recycling device system and method - Google Patents
Initiator waste acid recycling device system and method Download PDFInfo
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- CN113754165B CN113754165B CN202111048791.1A CN202111048791A CN113754165B CN 113754165 B CN113754165 B CN 113754165B CN 202111048791 A CN202111048791 A CN 202111048791A CN 113754165 B CN113754165 B CN 113754165B
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- 239000002699 waste material Substances 0.000 title claims abstract description 89
- 239000002253 acid Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000004064 recycling Methods 0.000 title claims abstract description 14
- 239000003999 initiator Substances 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000007788 liquid Substances 0.000 claims abstract description 88
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 33
- 239000000047 product Substances 0.000 claims abstract description 30
- 238000003860 storage Methods 0.000 claims abstract description 30
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003513 alkali Substances 0.000 claims abstract description 27
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 21
- 238000010306 acid treatment Methods 0.000 claims abstract description 20
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 20
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 20
- 238000010025 steaming Methods 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 19
- 150000002148 esters Chemical class 0.000 claims abstract description 17
- WYACBZDAHNBPPB-UHFFFAOYSA-N diethyl oxalate Chemical compound CCOC(=O)C(=O)OCC WYACBZDAHNBPPB-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000012546 transfer Methods 0.000 claims abstract description 14
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 230000008030 elimination Effects 0.000 claims abstract description 9
- 238000003379 elimination reaction Methods 0.000 claims abstract description 9
- 239000006227 byproduct Substances 0.000 claims abstract description 8
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 9
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 238000012544 monitoring process Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 230000001502 supplementing effect Effects 0.000 claims description 6
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000007689 inspection Methods 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000004880 explosion Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000013589 supplement Substances 0.000 claims description 3
- 238000013022 venting Methods 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- 239000002440 industrial waste Substances 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 3
- 239000012433 hydrogen halide Substances 0.000 description 2
- 229910000039 hydrogen halide Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/043—Details
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/046—Treatment of water, waste water, or sewage by heating by distillation or evaporation under vacuum produced by a barometric column
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature 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 a system and a method for recycling initiator waste acid, comprising a waste acid treatment system, a sodium sulfate recovery system and an accident elimination system, wherein the waste acid treatment system consists of an intermediate 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 alkali metering tank, a neutralization kettle, a transfer tank, MVR concentration equipment and a condenser, the intermediate kettle and the concentration tank are both 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 consists of an emergency tank, an accident tank and a rupture disk. The invention can recycle the heat source in the treatment process, can produce byproduct sodium sulfate after concentrating and neutralizing condensate, simultaneously reduces the dangerous coefficient of production, and is more beneficial to safe production.
Description
Technical Field
The invention relates to the technical field of chemical waste acid treatment, in particular to a device system and a method for recycling initiator waste acid.
Background
A large amount of dilute sulfuric acid is generated by separation in the reaction layering process of the di-tert-butyl peroxide production device and the tert-butyl hydrogen peroxide production device, which belongs to dangerous waste, enterprises need to input a large amount of funds to treat waste acid, and the resource recycling rate in the treatment process is lower, valuable substances in the waste acid can not be utilized, so that the economic benefit of the enterprises is reduced.
Through mass search, the prior art is found that the publication number is: CN108033433B discloses an industrial waste acid treatment system. The industrial waste acid treatment system comprises a waste acid concentration system, wherein 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 separates and concentrates the sulfuric acid waste liquid containing high-concentration nitric acid to obtain a nitric acid product; the first sulfuric acid concentration device is used for treating sulfuric acid waste liquid containing a small amount of nitric acid, separating and concentrating to obtain a nitric acid product and sulfuric acid A; and (3) treating the sulfuric acid waste liquid containing hydrogen halide by 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 treat various industrial waste acids with different components in a targeted and simultaneous manner, improves the treatment efficiency of the industrial waste acid, and ensures that 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 national first-class products.
In summary, in the waste acid treatment process, the utilization rate of the heat source is low, meanwhile, workers are required to carry out inspection on 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, which are used for solving the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the waste acid treatment system consists of an intermediate kettle, a circulating pump, a finished product tank, a hydrogen peroxide metering tank and a concentrating tank, wherein the intermediate kettle and the concentrating tank are connected with a waste acid conveying pipe, the intermediate kettle is communicated with the concentrating tank, the concentrating tank is connected with the hydrogen peroxide metering tank, and the concentrating 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 alkali metering tank, a neutralization kettle, a transfer tank, MVR concentration equipment and a condenser, wherein the middle kettle and the concentration tank are 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 alkali metering tank, and the neutralization kettle is sequentially connected with the transfer 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 the 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 elimination system comprises an emergency tank, an accident tank and a rupture disk, wherein the accident tank is connected with a concentration tank, the rupture disk 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 a finished product tank.
Preferably, the waste acid treatment system comprises:
the automatic valves are arranged at the joints of the middle kettles, the concentration tank and the waste acid conveying pipe, the middle kettles are connected with steam pipes, the automatic valves are arranged at the joints of the steam pipes and the middle kettles, a flowmeter 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 flowmeter is used for detecting the flow of waste acid input into the concentration tank;
the inside of the middle kettle and the inside of the concentration tank are respectively provided with a magnetic flap liquid level meter for monitoring the waste acid liquid level in the middle kettle and the inside of the concentration tank, and the magnetic flap liquid level meters in the inside of the concentration tank are connected with an automatic valve at the joint of the hydrogen peroxide metering tank and the concentration tank;
and a conveying pump is arranged between the concentrating tank and the finished product tank and is used for pumping out the finished product liquid in the concentrating tank to enter the finished product tank for storage.
Preferably, in the sodium sulfate based recovery system:
the middle kettle, the circulating pump and the heat exchanger form a circulating system, the hot water tank and the heat exchanger form a hot water and steam circulating system, and the concentration tank is connected with the hot water tank;
the concentrating tank and the hot water tank connecting pipeline are provided with bypasses, and are all provided with automatic control valves, and a magnetic flap level gauge is arranged inside the hot water tank.
Preferably, in the accident-based abatement system:
the top end of the concentration tank is provided with a temperature meter and a pressure meter, the upper end of the accident tank 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 and the concentration tank.
Preferably, the waste acid treatment system is used as follows:
s1: the waste acid enters the concentration tank through an automatic control valve and a mass flowmeter of the waste acid conveying pipe, reaches a specified liquid level through a magnetic flap liquid level meter, and closes the automatic control valve;
s2: closing the automatic control valve, opening the automatic control valve for steam, opening the automatic control valve after that, starting to heat up, and enabling condensed steam condensate water to enter the hot water tank through the drain valve;
s3: closing the automatic control valve, simultaneously pumping waste acid into the intermediate kettle through the vision middle and manual valves, reaching a specified liquid level through the magnetic flap liquid level meter, and closing the waste acid storage tank discharging automatic control valve;
s4: starting a circulating pump of the intermediate kettle, and circulating the waste acid through a heat exchanger; starting a hot water tank and a circulating pump to enable the 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 improved;
s5: the condensing tank is subjected to steam heating and negative pressure distillation, evaporated gas is condensed by a condenser, condensate is collected into a condensate storage tank, condensate in the condensate storage tank can enter a neutralization kettle through vacuum, and the neutralization kettle is provided with a magnetic flap level meter to stop material turning by an automatic control valve;
s6: the automatic control valve is opened to supplement preheated sulfuric acid by descending to a specified liquid level through the magnetic flap liquid level meter; when the supplementing amount of the intermediate kettle reaches a specified liquid level through a magnetic flap 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 by a tank area;
s7: calculating the total amount of waste acid added into a concentration tank through a mass flowmeter, and stopping waste acid supplementing through a control room when the total amount of the waste acid reaches the process requirement amount;
s8: in the concentrating process of the concentrating tank, an automatic control valve is notified, hydrogen peroxide is fed in automatically in the whole process, acidity is monitored through an on-line acid-base meter, the steam inlet pipe is required to be closed, a steam condensate water outlet pipe is required to be opened, a cooling circulating water outlet pipe and a pipe inlet control valve are opened, cooling is carried out, a double-branch thermometer is arranged, when the temperature is reduced to 35 ℃, a tank bottom discharge valve and a transfer pump are opened, and materials are transferred into a finished product tank; and stopping material rotation through a pressure transmitter of the material rotation pump, closing a tank bottom discharge valve, and starting a new round of concentration.
Preferably, the accident elimination system is used as follows:
SS1: the concentration tank is provided with two thermometers, one thermometer is displayed on site, one thermometer is remotely controlled, the temperature is corrected, the other thermometer is remotely controlled, the concentration tank is provided with a positive and negative pressure vacuum pressure gauge, and the thermometer is interlocked with an automatic cooling water control valve when the positive pressure is 0.03Mpa, so that emergency cooling is performed, and safety accidents are prevented;
SS2: the concentration tank is provided with a rupture disk 0.3MPa and a manual explosion venting valve, when an inspection personnel finds that the pressure is excessive, the pressure can be manually relieved, and when each monitoring means fails, the pressure is relieved through the rupture disk;
SS3: the discharged liquid enters an accident tank, the accident tank is provided with an evacuation device with a flame arrester, and the aperture is 1.5 times of that of the inlet; an emergency release valve is arranged below the accident tank, and accident liquid can enter the emergency tank through the emergency release valve and can be transferred into a finished product tank or a neutralization kettle according to the mass of the entering materials.
Preferably, the sodium sulfate recovery system is used as follows:
a. neutralizing the collecting liquid in the neutralization kettle by a liquid alkali metering tank, arranging a magnetic flap liquid level meter on the liquid alkali metering tank, controlling the tank area to be driven into the liquid alkali metering tank, arranging an automatic control valve below the liquid alkali metering tank to add liquid alkali into the neutralization kettle, arranging a PH on-line detector on the neutralization kettle, and stopping dripping liquid alkali when PH reaches 6.8-7.2;
b. after the neutralization is finished, transferring the collected liquid into MVR concentration equipment for evaporation, crystallization and concentration to produce sodium sulfate as a byproduct;
c. a liquid level meter is arranged in the hot water tank, when the liquid level of the hot water reaches the upper limit and the lower limit, an automatic valve is controlled to be opened, redundant hot water is pumped into a diethyl oxalate cleaning water tank for cleaning water of an ester steaming kettle process, residual salts in the ester steaming kettle enter MVR concentration equipment, and sodium sulfate as a byproduct is produced;
and d, evaporating and crystallizing condensed water by using MVR concentration equipment, and feeding the evaporated and crystallized condensed water into a condensed water storage tank for acid and alkali matching and washing water 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 steam condensate water can be used for the process cleaning water of the diethyl oxalate steaming kettle;
2. after the condensate liquid is concentrated and neutralized, MVR concentration equipment is adopted to produce byproduct sodium sulfate salt, so that extra economic benefits of enterprises can be increased, water produced by the MVR concentration equipment can be reused, the sewage discharge amount and the fresh water use amount are reduced, and the cost of waste acid treatment of 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 diagram 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. diethyl oxalate cleaning water tank; 5. a hot water tank; 6. steaming the ester kettle; 7. a condensed water storage tank; 8. a liquid alkali metering tank; 9. a neutralization kettle; 10. a transfer tank; 11. MVR concentration equipment; 12. a finished product tank; 13. an emergency tank; 14. an accident can; 15. rupture disk; 16. a condenser; 17. a hydrogen peroxide metering tank; 18. a concentrating tank.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific direction, be configured and operated in the specific direction, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, 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 should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "provided," "connected," and the like are to be construed broadly, and may be fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Referring to fig. 1, three embodiments of the present invention are provided: an initiator waste acid recycling device system and method comprises a waste acid treatment system, a sodium sulfate recycling system and an accident elimination system.
Embodiment one:
the waste acid treatment system consists of an intermediate kettle 1, a circulating pump 2, a finished product tank 12, a hydrogen peroxide metering tank 17 and a concentration tank 18, wherein the intermediate kettle 1 and the concentration tank 18 are connected with a waste acid conveying pipe, the intermediate 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 the waste acid treatment system:
the connection parts of the middle kettle 1 and the concentration tank 18 as well as the waste acid conveying pipe are provided with automatic valves, the middle kettle 1 is connected with a steam pipe, the connection part of the steam pipe and the middle kettle 1 is provided with an automatic valve, the connection part of the concentration tank 18 and the waste liquid conveying pipe is provided with a flowmeter for remotely controlling the waste liquid conveying, and the flowmeter is used for detecting the flow of the waste acid input into the concentration tank 18;
the inner parts of the intermediate kettle 1 and the concentration tank 18 are respectively provided with a magnetic flap level meter for monitoring the waste acid level in the intermediate kettle 1 and the concentration tank 18, and the magnetic flap level meters in the concentration tank 18 are connected with an automatic valve at the joint of the hydrogen peroxide metering tank 17 and the concentration tank 18;
a transfer pump is provided between the concentrate tank 18 and the product tank 12 for pumping the product liquid from the concentrate tank 18 into the product tank 12 for storage.
The using method of the waste acid treatment system is as follows:
s1: the waste acid enters the concentration tank 18 through an automatic control valve and a mass flowmeter of the waste acid conveying pipe, reaches a specified liquid level through a magnetic flap liquid level meter, and closes the automatic control valve;
s2: closing the automatic control valve, opening the automatic control valve for steam, opening the automatic control valve after that, starting to heat up, and enabling condensed steam condensate water to enter the hot water tank 5 through the drain valve;
s3: closing an automatic control valve, simultaneously pumping waste acid into the intermediate kettle 1 through a vision middle and manual valve, reaching a specified liquid level through a magnetic flap liquid level meter, and closing a waste acid storage tank discharging automatic control valve;
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 improved;
s5: the condensing tank 18 is used for heating and distilling by steam under negative pressure, the evaporated gas is condensed by the condenser 16, the condensed liquid is collected into the condensed water storage tank 7, the condensed liquid in the condensed water storage tank 7 can enter the neutralization kettle 9 through vacuum, and the neutralization kettle 9 is provided with a magnetic flap level meter and an automatic control valve for stopping material turning;
s6: the automatic control valve is opened to supplement preheated sulfuric acid by descending to a specified liquid level through the magnetic flap liquid level meter; when the supplementing amount of the intermediate kettle 1 reaches a specified liquid level through a magnetic flap 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 by a tank area;
s7: calculating the total amount of the waste acid added into the concentration tank 18 through a mass flowmeter, and stopping the waste acid supplementing through a control room when the total amount of the waste acid reaches the process requirement amount;
s8: the concentration tank 18 notifies an automatic control valve during the concentration process, hydrogen peroxide is automatically fed in the whole process, acidity is monitored through an online acid-base meter, the steam inlet pipe is required to be closed, a steam condensate outlet pipe is required to be opened, a cooling circulating water outlet pipe and a pipe inlet control valve are opened for cooling, a double-branch thermometer is arranged, the temperature is opened when the temperature is reduced to 35 ℃, and a tank bottom discharge valve and a transfer pump are opened to transfer materials into the finished product tank 12; and stopping material rotation through a pressure transmitter of the material rotation pump, closing a tank bottom discharge valve, and starting a new round of concentration.
Embodiment two:
the sodium sulfate recovery system consists of 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 alkali metering tank 8, a neutralization kettle 9, a transfer tank 10, MVR concentration equipment 11 and a condenser 16, wherein the middle 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 alkali metering tank 8, and 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 communicated with the diethyl oxalate cleaning water tank 4, the diethyl oxalate cleaning water tank 4 is connected with the ester steaming kettle 6, and the ester steaming kettle 6 is communicated with the MVR concentration equipment 11.
Based on sodium sulfate recovery system:
the middle kettle 1, the circulating pump 2 and the heat exchanger 3 form a circulating system, the hot water tank 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 tank 5;
the connecting pipeline of the concentration tank 18 and the hot water tank 5 is provided with a bypass, and is provided with automatic control valves, and a magnetic flap level gauge is arranged inside the hot water tank 5.
The sodium sulfate recovery system comprises the following using method:
a. neutralizing the collected liquid in the neutralization kettle 9 by a liquid alkali metering tank 8, arranging a magnetic flap liquid level meter on the liquid alkali metering tank 8, controlling the tank area to be driven into the liquid alkali metering tank 8, arranging an automatic control valve below the liquid alkali metering tank 8 to neutralize the collected liquid in the neutralization kettle 9, arranging a PH on-line detector on the neutralization kettle 9, and stopping dripping the liquid alkali when the PH reaches 6.8-7.2;
b. after neutralization, transferring the collected liquid into MVR concentration equipment 11 for evaporation, crystallization and concentration to produce sodium sulfate as a byproduct;
c. a liquid level meter is arranged on the hot water tank 5, when the liquid level of the hot water reaches the upper limit and the lower limit, an automatic valve is controlled to be opened, redundant hot water is pumped into the diethyl oxalate cleaning water tank 4 and is used for steaming the 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 sodium sulfate as a byproduct;
and d, evaporating and crystallizing condensed water by using MVR concentration equipment 11, and feeding the evaporated and crystallized condensed water into a condensed water storage tank 7 for acid and alkali matching and washing water of a di-tert-butyl peroxide production device and a tert-butyl hydroperoxide production device.
Embodiment III:
the accident elimination 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 the accident-based abatement system:
the top end of the concentration tank 18 is provided with a temperature 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 eliminating system is used as follows:
SS1: the concentration tank 18 is provided with two thermometers, one thermometer is displayed on site, one thermometer is remotely controlled, the temperature is corrected, the other thermometer is remotely controlled, the concentration tank 18 is provided with a positive and negative pressure vacuum pressure gauge, and the thermometer is interlocked with an automatic cooling water control valve when the positive pressure is 0.03MPa, so that emergency cooling is performed, and safety accidents are prevented;
SS2: the concentration tank 18 is provided with a rupture disk 15 of 0.3MPa and a manual explosion venting valve, when an inspection personnel finds out overpressure, the pressure can be manually relieved, and when each monitoring means fails, the pressure is relieved through the rupture disk 15;
SS3: the discharged liquid enters an accident tank 14, the accident tank 14 is provided with an evacuation device with a flame arrester, and the aperture is 1.5 times of that of the inlet; an emergency release valve is arranged below the accident tank 14, and accident liquid can enter the emergency tank 13 through the emergency release valve and can be transferred into the finished tank 12 or the neutralization kettle 9 according to the mass of the 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 characteristics 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. An initiator waste acid recycle system which is characterized in that: the waste acid treatment system comprises a waste acid treatment system, a sodium sulfate recovery system and an accident elimination system, wherein the waste acid treatment system comprises an intermediate kettle (1), a circulating pump (2), a finished product tank (12), a hydrogen peroxide metering tank (17) and a concentration tank (18), the intermediate kettle (1) and the concentration tank (18) are connected with a waste acid conveying pipe, the intermediate 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);
the sodium sulfate recovery system consists of a heat exchanger (3), a diethyl oxalate cleaning water tank (4), a hot water tank (5) and an ester steaming kettle (6), a condensed water storage tank (7), a liquid alkali metering tank (8), a neutralization kettle (9), a middle transfer tank (10), MVR concentration equipment (11) and a condenser (16), wherein the middle kettle (1) is connected with the concentration tank (18) through 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 alkali metering tank (8), the neutralization kettle (9) is sequentially connected with the middle 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 the 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 MVR concentration equipment (11);
the accident elimination 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).
2. The system for recycling waste acid of initiator according to claim 1, wherein: based on the waste acid treatment system:
the waste acid concentration device is characterized in that automatic valves are arranged at the joints of the middle kettle (1) and the concentration tank (18) and the waste acid conveying pipe, the middle kettle (1) is connected with a steam pipe, the joints of the steam pipe and the middle kettle (1) are provided with automatic valves, and a flowmeter is arranged at the joint of the concentration tank (18) and the waste liquid conveying pipe and used for remotely controlling waste liquid conveying and used for detecting the flow of waste acid input into the concentration tank (18);
the internal parts of the intermediate kettle (1) and the concentration tank (18) are respectively provided with a magnetic flap level meter for monitoring the waste acid level in the internal parts of the intermediate kettle (1) and the concentration tank (18), and the magnetic flap level meters in the internal parts of the concentration tank (18) are connected with automatic valves at the joints 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 system for recycling waste acid of initiator according to claim 1, wherein: based on sodium sulfate recovery system:
the intermediate kettle (1), the circulating pump (2) and the heat exchanger (3) form a circulating system, the hot water tank (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 tank (5);
the concentrating tank (18) and the hot water tank (5) are connected through a pipeline, bypass is arranged, automatic control valves are arranged, and a magnetic flap liquid level meter is arranged in the hot water tank (5).
4. The system for recycling waste acid of initiator according to claim 1, wherein: in the accident-based abatement system:
the top end of the concentration tank (18) is provided with a temperature 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).
5. The method for using the initiator waste acid recycling system according to any one of claims 1 to 2, characterized in that: the using method of the waste acid treatment system is as follows:
s1: the waste acid enters a concentration tank (18) through an automatic control valve and a mass flowmeter of a waste acid conveying pipe, reaches a specified liquid level through a magnetic flap liquid level meter, and closes the automatic control valve;
s2: closing an automatic control valve, opening the automatic control valve of steam, opening the automatic control valve, starting heating, and enabling condensed steam condensate water to enter a hot water tank (5) through a drain valve;
s3: closing an automatic control valve, simultaneously pumping waste acid into an intermediate kettle (1) through a vision-middle and manual valve, reaching a specified liquid level through a magnetic flap liquid level meter, and closing a waste acid storage tank discharging automatic control valve;
s4: starting a circulating pump (2) of the intermediate kettle (1), and circulating the 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 improved;
s5: the condensing tank (18) is used for heating and distilling by steam under negative pressure, evaporated gas is condensed by the condenser (16), condensate is collected into the condensate storage tank (7), condensate in the condensate storage tank (7) enters the neutralization kettle (9) through vacuum, and the neutralization kettle (9) is provided with a magnetic flap level meter to stop material turning by an automatic control valve;
s6: the magnetic flap level gauge is lowered to a specified liquid level, and an automatic control valve is opened to supplement preheated sulfuric acid; when the supplementing quantity of the intermediate kettle (1) reaches a specified liquid level through a magnetic flap 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 flowmeter, and stopping the waste acid supplementing through a control room when the total amount of the waste acid reaches the process requirement amount;
s8: the concentration tank (18) informs an automatic control valve in the concentration process, hydrogen peroxide is automatically fed in the whole process, acidity is monitored through an online acid-base meter, the steam inlet pipe is required to be closed, the steam condensate outlet pipe is opened, the cooling circulating water outlet pipe and the inlet pipe control valve are opened for cooling, a double-branch thermometer is arranged, the tank bottom discharge valve and the transfer pump are opened when the temperature is reduced to 35 ℃, and materials are transferred into the finished product tank (12); and stopping material rotation through a pressure transmitter of the material rotation pump, closing a tank bottom discharge valve, and starting a new round of concentration.
6. The method for using the initiator waste acid recycling system according to any one of claims 1 to 4, which is characterized in that: the accident elimination system comprises the following using method:
SS1: the concentration tank (18) is provided with a double thermometer, one thermometer is displayed on site, one thermometer is remotely controlled, the temperature is corrected, the thermometer is remotely controlled, the concentration tank (18) is provided with a positive and negative pressure vacuum manometer, and the thermometer is interlocked with an automatic cooling water control valve when the positive pressure is 0.03MPa, so that emergency cooling is performed, and safety accidents are prevented;
SS2: the concentration tank (18) is provided with a rupture disk (15) of 0.3MPa and a manual explosion venting valve, and when an inspection personnel finds overpressure and manual pressure relief, each monitoring means is ineffective, the pressure relief is carried out through the rupture disk (15);
SS3: the discharged liquid enters an accident tank (14), an emptying pipe with a flame arrester is arranged on the accident tank (14), and the aperture is 1.5 times of that of the inlet; an emergency release valve is arranged below the accident tank (14), and accident liquid enters the emergency tank (13) through the emergency release valve and is transferred into the finished product tank (12) or the neutralization kettle (9) according to the mass of the entering materials.
7. A method of using an initiator spent acid recycling system according to any one of claims 1-3, characterized by: the sodium sulfate recovery system comprises the following using method:
a. neutralizing the collected liquid in a neutralization kettle (9) through a liquid alkali metering tank (8), controlling the tank area to be driven into the liquid alkali metering tank (8), setting an automatic control valve below the liquid alkali metering tank (8) to add liquid alkali into the neutralization kettle (9), setting a PH on-line detector in the neutralization kettle (9), and stopping dripping liquid alkali when the PH reaches 6.8-7.2;
b. after neutralization, transferring the collected liquid into MVR concentration equipment (11) for evaporation, crystallization and concentration to produce sodium sulfate as a byproduct;
c. a liquid level meter is arranged in the hot water tank (5), when the liquid level of the hot water reaches the upper limit and the lower limit, an automatic valve is controlled to be opened, redundant hot water is pumped into the diethyl oxalate cleaning water tank (4) for steaming the 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 sodium sulfate as a byproduct;
and d, evaporating and crystallizing condensed water by MVR concentration equipment (11), and entering a condensed water storage tank (7) for preparing acid, alkali and cleaning water for the di-tert-butyl peroxide production device and the tert-butyl hydroperoxide production device.
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