CN114890387A - Preparation device and method for producing potassium hydrogen peroxymonosulfate composite salt by tower-type continuous flow - Google Patents
Preparation device and method for producing potassium hydrogen peroxymonosulfate composite salt by tower-type continuous flow Download PDFInfo
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- 150000003839 salts Chemical class 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- OKBMCNHOEMXPTM-UHFFFAOYSA-M potassium peroxymonosulfate Chemical compound [K+].OOS([O-])(=O)=O OKBMCNHOEMXPTM-UHFFFAOYSA-M 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 93
- 239000007788 liquid Substances 0.000 claims abstract description 79
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 72
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 49
- 239000012425 OXONE® Substances 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 239000012452 mother liquor Substances 0.000 claims abstract description 35
- 238000002425 crystallisation Methods 0.000 claims abstract description 31
- 230000008025 crystallization Effects 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 23
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 19
- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 claims abstract description 18
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000003112 potassium compounds Chemical class 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 230000003647 oxidation Effects 0.000 claims description 43
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 41
- 238000001816 cooling Methods 0.000 claims description 39
- 239000012295 chemical reaction liquid Substances 0.000 claims description 29
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 22
- 239000002826 coolant Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 12
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 11
- 230000001590 oxidative effect Effects 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000000110 cooling liquid Substances 0.000 claims description 3
- 239000012267 brine Substances 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims 3
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 claims 2
- 238000007710 freezing Methods 0.000 claims 1
- 230000008014 freezing Effects 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 abstract description 14
- 239000001301 oxygen Substances 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 13
- 238000010924 continuous production Methods 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 44
- 230000001276 controlling effect Effects 0.000 description 17
- 239000002253 acid Substances 0.000 description 4
- 238000004880 explosion Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 description 3
- 235000011151 potassium sulphates Nutrition 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 238000005502 peroxidation Methods 0.000 description 2
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 description 2
- FHHJDRFHHWUPDG-UHFFFAOYSA-N peroxysulfuric acid Chemical compound OOS(O)(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-N 0.000 description 2
- -1 potassium peroxymonosulfate compound salt Chemical class 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- SENRGCCOVBYBGK-UHFFFAOYSA-N [K].OOS(O)(=O)=O Chemical compound [K].OOS(O)(=O)=O SENRGCCOVBYBGK-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012809 cooling fluid Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
- C01B15/06—Peroxyhydrates; Peroxyacids or salts thereof containing sulfur
- C01B15/08—Peroxysulfates
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/04—Carbon disulfide; Carbon monoxide; Carbon dioxide
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- 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
- 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
- C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention provides a continuous production system of potassium monopersulfate composite salt, which comprises a raw material metering device, a tower type oxidation reaction device, a tower type neutralization reaction device, a continuous crystallization device, a separation device, a drying device and a mother liquor circulating device which are sequentially connected according to the flowing direction of a feed liquid; also provides a method for continuously producing the potassium hydrogen peroxymonosulfate composite salt by adopting the continuous production system. Hydrogen peroxide, fuming sulfuric acid (liquid sulfur trioxide) and an alkaline potassium compound are used as raw materials for preparation, and a tower reactor is used for replacing a traditional kettle reactor, so that heat released by reaction can be rapidly removed; the online quantity of materials in the equipment is greatly reduced, the safety is high, the controllability is high, the structural form is simple, and the equipment investment is low; compared with a tubular reactor and a microreactor, the tower reactor has the advantages that a material running channel is smooth, resistance is small, crystals generated in a neutralization reaction section are not blocked, the reaction material quantity is greatly improved, and a large amount of oxygen decomposed in the reaction can be discharged in time; the invention is easy to realize continuous automatic, large-scale and safe production.
Description
Technical Field
The invention relates to the technical field of peroxide synthesis processes, in particular to a preparation method for continuously producing potassium peroxymonosulfate composite salt.
Background
The potassium peroxymonosulfate compound salt is a compound composed of potassium peroxymonosulfate, potassium bisulfate and potassium sulfate, is an oxidation type disinfectant, has effect in killing various microorganisms, and has a molecular formula of 2KHSO 5 ·K 2 SO 4 ·KHSO 4 . The potassium monopersulfate composite salt product is safe and stable in solid state, is not easy to generate chemical reaction, continuously generates excited state oxygen free radicals through a series of chain reactions after being dissolved in water, has excellent sterilization effect, does not generate harmful substances because the potassium monopersulfate composite salt is decomposed in water to release oxygen and potassium sulfate, is safe and environment-friendly, and belongs to a green medicament.
The potassium monopersulfate composite salt is an inorganic peroxide which is developed by DuPont in the sixties and seventies and has very wide application, belongs to an oxidation type disinfectant and has excellent sterilization effect; the oxidation potential energy is high and exceeds chloride, potassium permanganate, hydrogen peroxide and the like, so that chlorine ions in the aqueous solution can be oxidized into chlorine, and organic matters such as alcohols, aldehydes and the like can be oxidized into organic acid. And the potassium hydrogen peroxymonosulfate composite salt is decomposed in water to release oxygen and potassium sulfate, and no harmful substances are generated, so the potassium hydrogen peroxymonosulfate composite salt is known as peroxide with perfect combination of oxidizability and safety, and the latest fifth generation active oxygen water quality improver in the world is a 21 st century green environment-friendly product with the most application prospect, and has a wide application prospect.
At present, potassium peroxymonosulfate composite salt produced at home and abroad is mainly produced by a fuming sulfuric acid method, fuming sulfuric acid, hydrogen peroxide and potassium hydroxide solution or potassium carbonate are taken as raw materials, a kettle type batch process is adopted for production, firstly, hydrogen peroxide is added into an oxidation kettle for cooling, fuming sulfuric acid is added dropwise under the condition of low temperature, and peroxymonosulfate is synthesized; secondly, introducing the first-step synthesized peroxysulfuric acid into a neutralization kettle, and neutralizing with potassium hydroxide solution or potassium carbonate to generate potassium peroxymonosulfate; and thirdly, the potassium peroxymonosulfate generated in the second step is subjected to processes of cooling crystallization, centrifugal separation, drying and the like to produce potassium peroxymonosulfate composite salt products. The first step of peroxidation and the second step of neutralization are both massive exothermic reactions, particularly the exothermic quantity of the reaction of high-concentration hydrogen peroxide and fuming sulfuric acid is huge, once the temperature is out of control, the hydrogen peroxide can be instantaneously decomposed to release a large amount of oxygen, and the reaction liquid in the kettle can be rapidly heated and exploded. Potassium monopersulfate production enterprises need to eliminate explosion hidden dangers urgently, change kettle type intermittent operation into continuous automatic operation, and can realize continuous and automatic safe production.
Patent No. CN108640089B discloses a continuous preparation device and a preparation method of potassium peroxymonosulfate composite salt, and the invention adopts a kettle type overflow method to realize continuous reaction. The preparation method comprises the steps of firstly adding hydrogen peroxide containing a stabilizer and sulfuric acid into an oxidation kettle to prepare an oxidation solution, allowing the oxidation solution to flow into a mixing kettle containing a mother solution through an overflow pipe for mixing, allowing the mixed solution to flow into a neutralization kettle through the overflow pipe, adding a potassium hydroxide solution for neutralization, allowing the neutralization solution to flow into a crystallization kettle through the overflow pipe for cooling and crystallization, allowing a material containing crystals to flow into a centrifuge through the overflow pipe for centrifugation, and drying an obtained wet product through a fluidized bed to finally obtain the product. The continuous preparation method realizes the continuous preparation of the potassium monopersulfate composite salt, the products in each stage are continuously output to the next stage, the risk can be avoided, the potential safety hazard is reduced, the automatic production is realized, the products are continuously output, the yield is high, and the production operation cost and the labor intensity are greatly reduced. However, the method still adopts the conventional kettle type reaction in the process of preparing the oxidizing solution, and in order to maintain the normal operation of a production system, a large amount of oxidizing solution needs to be accumulated in a kettle, so that the risk of decomposition and explosion exists.
Patent No. CN112645290A discloses a continuous production system and a production method of potassium monopersulfate composite salt. The invention selects a tubular reactor to realize continuous reaction. The preparation process includes the contact reaction of hydrogen peroxide and fuming acid, the circular reaction in the oxidation reactor and the flow into the dilution device with mother liquid, the flow into the neutralizing reactor and the neutralization with potassium carbonate, the cooling of the neutralized liquid in the cooler and the flow into the crystallizer, the separation of the crystallized neutralized liquid in the separator, the further treatment of solid and the continuous output of the product, and the circular utilization of the mother liquid in the dilution device to dilute the oxidation liquid. The oxidation reactor, the neutralization reactor, the diluting device and the neutralization reactor are all tubular reactors, and compared with a kettle reactor, the tubular reactor can rapidly remove heat released by reaction, greatly reduce the on-line quantity of materials in equipment, and has the advantages of high intrinsic safety, high controllability, simple structural form, low equipment investment and easy realization of continuous, automatic and large-scale industrial production. However, the hydrogen peroxide and the fuming sulfuric acid can release a large amount of heat instantly when contacting with each other in a pipeline, the temperature is rapidly increased, a large amount of hydrogen peroxide is rapidly decomposed to generate a large amount of oxygen, the reaction system has overpressure, the feeding speed must be reduced for ensuring the stable reaction, and the large-scale production is not easy to realize, so that the problems are also faced when a microreactor is selected. The tubular reactor device is adopted in the neutralization section, the solid product separated out in the neutralization section is easy to block the tube wall, the long-term stable operation of the production system is difficult to ensure, the crystal grain size is difficult to control, and the fluctuation of the product quality can be caused.
Patent No. CN113860264A discloses a method for continuously producing potassium peroxymonosulfate composite salt, comprising the first step of carrying out peroxidation reaction on hydrogen peroxide and fuming sulfuric acid to prepare peroxymonosulfate oxidizing solution, and adopting a tubular reactor; and secondly, carrying out neutralization reaction on the peroxymonosulfuric acid and an alkaline potassium compound to prepare potassium peroxymonosulfuric acid, and adopting a kettle type reactor. The tubular reactor is adopted in the first step, so that the liquid storage amount of the system is small, the risk of easy decomposition and explosion caused by the large storage of the oxidation liquid is reduced, the intrinsic safety problem of the reaction is solved, and the continuous and automatic production is convenient to realize; and in the second step, a kettle type reactor is adopted, so that the control of the crystallization granularity is facilitated. But the whole process is not easy to realize continuous and automatic production.
Therefore, according to the preparation characteristics of potassium monopersulfate composite salt products, the defects of the traditional production method are avoided, and the development of a continuous, automatic, safe, efficient and stable potassium monopersulfate composite salt production method is a technical problem which needs to be solved urgently by technical personnel in the field.
Disclosure of Invention
The invention aims to provide a method for continuously producing potassium monopersulfate composite salt, which realizes continuous, automatic, safe, efficient and stable production.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
in a first aspect, an embodiment of the present invention provides a continuous production system for potassium monopersulfate complex salt, including a raw material metering device, a tower oxidation reaction device, a tower neutralization reaction device, a continuous crystallization device, a separation device, a drying device, and a mother liquor circulating device, which are connected in sequence according to a flow direction of a feed liquid.
The raw material metering device comprises a raw material storage tank, a pump (preferably a metering pump), a reactor or a hydrogen peroxide cooler or a mixer which are connected in sequence.
The tower type oxidation reaction device comprises a hydrogen peroxide cooler, a tower type oxidation reactor 1 and a reaction liquid circulating pump 1 which are sequentially connected, wherein the tower type oxidation reactor 1 is provided with a fuming sulfuric acid feeding port, a dispersing device, a circulating oxidation liquid outlet, a circulating oxidation liquid inlet, an overflow outlet of oxidation liquid, and a built-in cooling coil pipe for cooling reaction materials.
The tower type neutralization reaction device comprises a mixer of oxidizing liquid and mother liquor, a tower type neutralization reactor 2 and a reaction liquid circulating pump 2 which are sequentially connected, wherein the tower type neutralization reactor 2 is provided with a potassium hydroxide solution feed inlet and a dispersing device, the mixer is provided with a powdery potassium carbonate feed inlet, a circulating neutralization liquid outlet, a circulating neutralization liquid inlet and a neutralization liquid outlet, and a cooling coil is arranged in the tower type neutralization reaction device and used for cooling reaction materials.
The continuous crystallization device comprises a crystallization tank and a built-in cooling coil pipe, is used for cooling reaction materials, and is provided with a neutralization liquid inlet and a crystallization liquid outlet.
The separation device is a centrifugal machine, the centrifugal machine is provided with a feed liquid inlet, and a mother liquid outlet is connected with the mother liquid pool.
The drying device is a fluidized bed dryer and is provided with a material liquid inlet and a material outlet.
The mother liquor circulating device comprises a mother liquor pool and a mother liquor circulating pump 1, the mother liquor pool is provided with a mother liquor inlet and a circulating outlet which are communicated with the centrifugal machine, and the mother liquor circulating outlet is connected with the inlet of the mixer through the mother liquor circulating pump.
In a second aspect, the embodiment of the present invention further provides a method for continuously producing potassium hydrogen peroxymonosulfate composite salt by using the continuous production system. The catalyst is prepared by taking hydrogen peroxide, fuming sulfuric acid (liquid sulfur trioxide) and an alkaline potassium compound as raw materials.
S1: continuously adding hydrogen peroxide into a hydrogen peroxide cooler through a hydrogen peroxide metering pump, cooling the hydrogen peroxide to 10 ℃, enabling the cooled hydrogen peroxide to enter an inlet of a self circulating pump of a tower type oxidation reactor, starting a self circulating system and a cooling system when the liquid level of the tower type oxidation reactor reaches 90%, continuously adding fuming sulfuric acid into the tower type oxidation reactor, controlling the molar ratio of the fuming sulfuric acid (the content of sulfur trioxide is 65%) to the hydrogen peroxide (calculated by 100%) to be 1.0-2.0: 1, and controlling the reaction temperature to be 0-30 ℃ to obtain an oxidation liquid.
S2: and overflowing the oxidizing liquid into a mixer through a pipeline, adding a mother liquid into the mixer at the same time, wherein the mass ratio of the oxidizing liquid to the mother liquid is 1: 1.0-3.0, flowing into the tower type neutralization reactor through a mixer device, starting a self-circulation system and a cooling system, continuously adding a potassium hydroxide solution into the neutralization reactor, controlling the mass ratio of the potassium hydroxide (100%) to the oxidizing liquid to be 0.3-0.5: 1, and controlling the neutralization reaction temperature to be 5-20 ℃.
S3: and overflowing the neutralization reaction liquid to a continuous crystallization tank, and introducing a cooling liquid into the crystallization tank to cool the material to 0 to-10 ℃ for crystallization.
S4: and (3) separating the crystallized material in a centrifuge, allowing the separated mother liquor 1 to flow into the mother liquor pool, and further drying the separated solid 1.
S5: and (3) carrying out air flow drying on the wet potassium peroxymonosulfate composite salt obtained by centrifugation, adding an anti-caking agent, and mixing to obtain a finished potassium peroxymonosulfate composite salt product.
S6: and starting the mother liquor metering pump to quantitatively feed the mother liquor 1 in the mother liquor pool into the mixer.
Further, the concentration of the raw material of oleum is 105-122.5%, and when the oleum has the highest concentration, the oleum can be replaced by liquid SO 3; further, the alkaline potassium compound used as a neutralization raw material is mainly a potassium hydroxide solution, the mass fraction of the solution is 20-60%, and the potassium hydroxide solution feeding part is arranged on a mixer device; further, the alkaline potassium compound used as the neutralization raw material can also be potassium carbonate, the mass fraction of the solution is 70-99%, and the potassium carbonate feeding part is arranged on a mixer device.
Furthermore, the oxidation section device is a thin and high tower type continuous flow reactor, and is provided with a reaction liquid internal circulation device and a cooling coil pipe, so that the reaction temperature is convenient to control.
Furthermore, the neutralization section device is a thin and high tower type continuous flow reactor, and is provided with a reaction liquid internal circulation device and a cooling pipe, so that the reaction temperature is convenient to control.
Further, the crystallization device is a horizontal continuous crystallizer or a kettle type crystallizer.
Further, the drying is ebullated bed drying.
Further, the cooling medium refers to conventional chilled brine, glycol refrigerating fluid, and freon series cooling fluid.
The invention has the beneficial effects that.
1. The tower reactor replaces the traditional kettle type reactor, and can quickly remove the heat released by the reaction.
2. The online quantity of materials in the equipment is greatly reduced, the safety is high, the controllability is high, the structural form is simple, and the equipment investment is low.
3. Compared with a tubular reactor and a microreactor, the tower reactor has the advantages of smooth material running channel, small resistance and no blockage of crystals generated in a neutralization reaction section.
4. Compared with a tubular reactor and a micro-reactor, the tower reactor has the advantages that the reaction material amount is greatly improved, and a large amount of oxygen decomposed in the reaction can be discharged in time.
5. The invention is easy to realize continuous automatic, large-scale and safe production.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
In fig. 1:1 metering pump, 2 hydrogen peroxide cooler, 3 circulating pump 1, 4 tower oxidation reactor 1, 5 mixer, 6 circulating pump 2, 7 tower neutralization reactor 2, 8 crystallizer, 9 centrifuge, 10 mother liquor pool, 11 mother liquor metering pump, 12 boiling bed dryer.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
Referring to fig. 1, a continuous manufacturing device of potassium monopersulfate complex salt comprises a raw material metering device, a hydrogen peroxide solution cooling device, a tower oxidation reactor 1, a circulating pump 1, a mixer, a tower neutralization reactor 2, a circulating pump 2, a crystallizer, a centrifuge, a mother liquor pool, a mother liquor pump and a fluidized bed drying device. According to the invention, the raw material metering device, the tower type oxidation device, the tower type neutralization device, the crystallization device, the separation device and the airflow drying device are used for continuously preparing the potassium monopersulfate composite salt, so that the products in each stage are continuously output to the next stage, the explosion caused by violent heat release is avoided, the potential safety hazard is reduced, the automatic production is realized, the products are continuously output, the yield is high, and the production operation cost and the labor intensity are greatly reduced. The hydrogen peroxide cooler, the tower type oxidation reactor, the tower type neutralization reactor and the crystallizer are respectively provided with a cooling medium inlet and outlet pipe, and valves are arranged on the cooling medium inlet and outlet pipes to adjust the reaction temperature.
The tower type oxidation reactor, the tower type neutralization reactor, the circulating pump and the pipeline are arranged to form a self circulating system for controlling the reaction temperature.
According to the figure 1, the continuous preparation method of the potassium peroxymonosulfate composite salt is prepared by taking fuming sulfuric acid, hydrogen peroxide and an alkaline potassium compound as raw materials, and the preparation method comprises the following steps.
Example 1
(1) Hydrogen peroxide with the mass fraction of 50% is pumped into a hydrogen peroxide cooler by a metering pump at the flow rate of 10kg/h, the hydrogen peroxide is precooled to 10 ℃ and then enters a tower type oxidation reactor 1, when the liquid level in the reactor 1 reaches 90%, a cooling medium circulating pump 1 of the reactor 1 is started, the reaction liquid is cooled, and the flow rate of the circulating pump 1 is controlled to be 200 kg/h; oleum with mass fraction of 115% was added to the top of the reactor 1 at a rate of 20kg/h using a metering pump, and the reaction temperature was controlled below 20 ℃.
(2) The reaction liquid overflowing from the reactor 1 flows into a mixer, is mixed with 20kg/h of mother liquid in the mixer, and then overflows into a tower type neutralization reactor 2; and starting a cooling medium circulating pump 2 of the reactor 2, cooling the reaction liquid, and controlling the flow of the circulating pump 2 to be 100 kg/h. Injecting potassium hydroxide with the mass fraction of 48% into the top of the reactor 2 at the flow rate of 24kg/h by using a metering pump, and carrying out acid-base neutralization reaction in the reactor 2; controlling the reaction temperature to be below 20 ℃ by adjusting the flow of a circulating pump, the feeding speed of potassium hydroxide and the flow of a cooling medium to obtain a neutralization solution of a target product potassium monopersulfate composite salt; and simultaneously, the neutralization solution flows into the crystallizer from an overflow port at the bottom of the reactor.
(3) Cooling the crystallizer by a jacket or a cooling coil, controlling the crystallization temperature to be below-3 ℃, separating the crystallization liquid from the crystallizer by a centrifugal machine to obtain a wet potassium peroxymonosulfate composite salt product, drying the wet product by a fluidized bed, adding an anti-caking agent after drying, and mixing to obtain a potassium peroxymonosulfate composite salt product; the continuous production is carried out for 48 hours, 980kg of potassium hydrogen peroxymonosulfate composite salt product is obtained in total, and the active oxygen content of the product is 5.1 percent.
Example 2
(1) Hydrogen peroxide with the mass fraction of 70% is pumped into a hydrogen peroxide cooler by a metering pump at the flow rate of 100kg/h, precooled to 10 ℃, then enters a tower type oxidation reactor 1, when the liquid level in the reactor 1 reaches 80%, a cooling medium circulating pump 1 of the reactor 1 is started, reaction liquid is cooled, and the flow rate of the circulating pump is controlled to be 2000 kg/h. Oleum with a mass fraction of 115% is added to the top of the reactor 1 by a metering pump at a flow rate of 280kg/h, and the reaction temperature is controlled below 20 ℃.
(2) The reaction liquid overflowing from the reactor 1 flows into a mixer, is mixed with 220kg/h mother liquor in the mixer, and then overflows into a tower type neutralization reactor 2; starting a cooling medium circulating pump of the reactor 2, cooling the reaction liquid, and controlling the flow of the circulating pump to be 1000 kg/h; and (3) injecting potassium hydroxide with the mass fraction of 48% into the top of the reactor 2 at the flow rate of 340kg/h by using a metering pump, and carrying out acid-base neutralization reaction in the reactor 2. The reaction temperature is controlled below 20 ℃ by adjusting the flow rate of a circulating pump, the feeding speed of potassium hydroxide and the flow rate of a cooling medium. Controlling the acid value of the neutralization reaction liquid to be 120mg/g, obtaining the neutralization liquid of the target product potassium peroxymonosulfate, and simultaneously overflowing the neutralization liquid into the crystallizer from the overflow port at the bottom.
(3) Cooling the crystallizer by a jacket or a cooling coil, controlling the crystallization temperature to be below-3 ℃, separating the crystallization liquid from the crystallizer by a centrifugal machine to obtain a wet potassium peroxymonosulfate composite salt product, drying the wet product by a fluidized bed, adding an anti-caking agent after drying, and mixing to obtain the potassium peroxymonosulfate composite salt product. The continuous production is carried out for 48 hours, 14050kg of potassium hydrogen peroxymonosulfate composite salt product is obtained in total, and the active oxygen content of the product is 5.2 percent.
Example 3
(1) Hydrogen peroxide with the mass fraction of 50 percent is pumped into a hydrogen peroxide cooler by a metering pump at the flow rate of 200kg/h, the hydrogen peroxide is precooled to 10 ℃ and then enters a tower type oxidation reactor 1, when the liquid level in the reactor 1 reaches 80 percent, a cooling medium circulating pump of the reactor 1 is started, the reaction liquid is cooled, and the flow rate of the circulating pump is controlled to be 4000 kg/h; oleum (namely liquid sulfur trioxide) with the mass fraction of 122.5 percent is added into the top of the tower type oxidation reactor 1 by a metering pump at the flow rate of 370kg/h, and the reaction temperature is controlled below 20 ℃.
(2) The reaction liquid overflowing from the reactor 1 flows into a mixer, is mixed with 400kg/h of mother liquor and then overflows into a tower type neutralization reactor 2, a cooling medium circulating pump 2 of the reactor 2 is started, the reaction liquid is cooled, and the flow of the circulating pump is controlled to be 3000 kg/h; injecting potassium hydroxide with the mass fraction of 48% into the upper part of the reactor 2 at the flow rate of 480kg/h by using a metering pump, and carrying out acid-base neutralization reaction in the reactor 2; controlling the reaction temperature below 20 ℃ by adjusting the flow of the circulating pump 2, the feeding speed of potassium hydroxide and the flow of a cooling medium; controlling the acid value of the neutralization reaction liquid to be 98mg/g, obtaining the neutralization liquid of the target product potassium peroxymonosulfate, and simultaneously overflowing the neutralization liquid into the crystallizer from the overflow port at the bottom.
(3) Cooling the crystallizer by a jacket or a cooling coil, controlling the crystallization temperature to be below-3 ℃, separating the crystallization liquid from the crystallizer by a centrifugal machine to obtain a wet potassium peroxymonosulfate composite salt product, drying the wet product by a fluidized bed, adding an anti-caking agent after drying, and mixing to obtain the potassium peroxymonosulfate composite salt product. The continuous production is carried out for 48 hours, 21120 kg of potassium peroxymonosulfate composite salt products are obtained in total, and the active oxygen content of the products is 4.9 percent.
Example 4
(1) Hydrogen peroxide with the mass fraction of 50 percent is pumped into a hydrogen peroxide cooler by a metering pump at the flow rate of 100kg/h, the hydrogen peroxide is precooled to 10 ℃ and then enters a tower type oxidation reactor 1, when the liquid level in the reactor 1 reaches 90 percent, a cooling medium circulating pump 1 of the reactor is started, reaction liquid is cooled, and the flow rate of the circulating pump 1 is controlled to be 2500 kg/h; oleum with a mass fraction of 115% was added to the top of the reactor 1 at a rate of 210kg/h using a metering pump, and the reaction temperature was controlled below 20 ℃.
(2) The reaction liquid overflowing from the reactor 1 is mixed with 270kg/h mother liquid in a mixer, and then overflows into a tower type neutralization reactor 2, a cooling medium circulating pump 2 of the reactor 2 is started, the reaction liquid is cooled, and the flow of the circulating pump 2 is controlled to be 1600 kg/h; adding powdery potassium carbonate into a mixer at a rate of 142kg/h, overflowing the neutralized liquid into a reactor 2, continuing to perform acid-base neutralization reaction in the reactor 2, controlling the reaction temperature below 20 ℃ by adjusting the pump flow, the potassium carbonate feeding speed and the cooling medium flow, obtaining the neutralized liquid of the target product potassium hydrogen peroxymonosulfate composite salt, and simultaneously overflowing the neutralized liquid into a crystallizer from a bottom overflow port.
(3) Cooling the crystallizer by a jacket or a cooling coil, controlling the crystallization temperature to be below-3 ℃, separating the crystallization liquid from the crystallizer by a centrifugal machine to obtain a wet potassium peroxymonosulfate composite salt product, drying the wet product by a fluidized bed, adding an anti-caking agent after drying, and mixing to obtain the potassium peroxymonosulfate composite salt product. The continuous production is carried out for 48 hours, and 9800kg of potassium peroxymonosulfate composite salt products are obtained in total, and the active oxygen content of the products is 4.9 percent.
Example 5
(1) Hydrogen peroxide with the mass fraction of 50% is pumped into a hydrogen peroxide cooler at the flow rate of 10000kg/h by a metering pump, the hydrogen peroxide is precooled to 10 ℃ and then enters a tower-type oxidation reactor 1, when the liquid level of the reactor 1 reaches 85%, a cooling medium circulating pump 1 of the reactor 1 is started to cool reaction liquid, the flow rate of the circulating pump 1 is controlled to be 280000kg/h, fuming sulfuric acid with the mass fraction of 115% is added into the top of the reactor 2 at the flow rate of 20000kg/h by the metering pump, and the reaction temperature is controlled to be below 20 ℃.
(2) The reaction liquid overflowing from the reactor 1 flows into a mixer, is mixed with 20000kg/h mother liquid and then overflows into a tower type neutralization reactor 2, a cooling medium circulating pump 2 of the reactor is started to cool the reaction liquid, the flow of the circulating pump 2 is controlled to be 200000kg/h, potassium hydroxide with the mass fraction of 48% is pumped into the upper part of the reactor 2 at the flow of 34000kg/h by a metering pump, acid-base neutralization reaction is carried out in the reactor 2, the reaction temperature is controlled to be below 20 ℃ by regulating the flow of the circulating pump, the feeding speed of the potassium hydroxide and the flow of the cooling medium, the acid value of the neutralization reaction liquid is controlled to be 98mg/g, the neutralization liquid of the target product potassium monopersulfate composite salt is obtained, and simultaneously the neutralization liquid overflows into a crystallizer from a bottom overflow port.
(3) Cooling the crystallizer by a jacket or a cooling coil, controlling the crystallization temperature to be below-3 ℃, separating the crystallization liquid from the crystallizer by a centrifugal machine to obtain a wet potassium peroxymonosulfate composite salt product, drying the wet product by a fluidized bed, and adding an anti-caking agent to obtain the potassium peroxymonosulfate composite salt product. The continuous production is carried out for 48 hours, 970000kg of potassium hydrogen peroxymonosulfate composite salt product is obtained in total, and the active oxygen content of the product is 5.2 percent.
In summary, the results obtained in the examples show that the potassium hydrogen peroxymonosulfate composite salt can realize continuous, automatic and large-scale safe production, and the active oxygen content of the product is qualified, so that the method has good economic benefit and is suitable for industrial production.
The above description is only a preferred embodiment of the present invention, and does not limit the scope of the present invention, and all the modifications made by the equivalent structures in the content of the description and the drawings of the present invention, which can be directly or indirectly applied to other related technical fields, are within the scope of the present invention.
Claims (9)
1. A tower continuous flow preparation device for producing potassium peroxymonosulfate composite salt is characterized by comprising a raw material metering device, a tower oxidation reaction device, a tower neutralization reaction device, a continuous crystallization device, a separation device, a drying device and a mother liquor circulating device which are sequentially connected according to the flowing direction of a material liquid; the raw material metering device comprises a raw material storage tank, a pump (preferably a metering pump), a reactor or a hydrogen peroxide cooler or a mixer which are connected in sequence; the tower type oxidation reaction device comprises a hydrogen peroxide cooler, a tower type oxidation reactor 1 and a reaction liquid circulating pump 1 which are sequentially connected, wherein the tower type oxidation reactor 1 is provided with a fuming sulfuric acid feeding port, a dispersing device, a circulating oxidation liquid outlet, a circulating oxidation liquid inlet and an oxidation liquid overflow outlet, and a cooling coil is arranged in the tower type oxidation reaction device and used for cooling reaction materials; the tower type neutralization reaction device comprises a mixer of oxidation liquid and mother liquor, a tower type neutralization reactor 2 and a reaction liquid circulating pump 2 which are sequentially connected, wherein the tower type neutralization reactor 2 is provided with a potassium hydroxide solution feed inlet and a dispersing device, the mixer is provided with a powdery potassium carbonate feed inlet, a circulating neutralization liquid outlet, a circulating neutralization liquid inlet and a neutralization liquid outlet, and a cooling coil is arranged in the tower type neutralization reaction device and used for cooling reaction materials; the continuous crystallization device comprises a crystallization tank and a built-in cooling coil pipe, is used for cooling reaction materials, and is provided with a neutralization liquid inlet and a crystallization liquid outlet; the separation device is a centrifugal machine, the centrifugal machine is provided with a feed liquid inlet, and a mother liquid outlet is connected with the mother liquid pool; the drying device is a fluidized bed dryer and is provided with a material liquid inlet and a material outlet; the mother liquor circulating device comprises a mother liquor pool and a mother liquor circulating pump 1, the mother liquor pool is provided with a mother liquor inlet and a circulating outlet which are communicated with the centrifugal machine, and the mother liquor circulating outlet is connected with the inlet of the mixer through the mother liquor circulating pump; the preparation method for producing the potassium hydrogen peroxymonosulfate composite salt takes hydrogen peroxide, fuming sulfuric acid (liquid sulfur trioxide) and an alkaline potassium compound as raw materials for preparation, and specifically comprises the following steps:
s1: continuously adding hydrogen peroxide into a hydrogen peroxide cooler through a hydrogen peroxide metering pump, cooling the hydrogen peroxide to 10 ℃, enabling the cooled hydrogen peroxide to enter an inlet of a self circulating pump of a tower type oxidation reactor, starting a self circulating system and a cooling system when the liquid level of the tower type oxidation reactor reaches 90%, continuously adding fuming sulfuric acid into the tower type oxidation reactor, controlling the molar ratio of the fuming sulfuric acid (the content of sulfur trioxide is 65%) to the hydrogen peroxide (calculated by 100%) to be 1.0-2.0: 1, and controlling the reaction temperature to be 0-30 ℃ to obtain an oxidation liquid;
s2: overflowing the oxidizing liquid into a mixer through a pipeline, simultaneously adding a mother liquid into the mixer, enabling the oxidizing liquid and the mother liquid to flow into the tower-type neutralization reactor through a mixer device, starting a self-circulation system and a cooling system, continuously adding a potassium hydroxide solution into the neutralization reactor, controlling the mass ratio of the potassium hydroxide (100%) to the oxidizing liquid to be 0.3-0.5: 1, and enabling the neutralization reaction temperature to be 5-20 ℃;
s3: overflowing the neutralization reaction liquid to a continuous crystallization tank, and introducing cooling liquid into the crystallization tank to cool the material to 0 to-10 ℃ for crystallization;
s4: separating the crystallized material in a centrifuge, allowing the separated mother liquor 1 to flow into the mother liquor pool, and further drying the separated solid 1;
s5: drying the wet potassium peroxymonosulfate composite salt obtained by centrifugation by airflow, adding an anti-caking agent, and mixing to obtain a finished potassium peroxymonosulfate composite salt product;
s6: and starting the mother liquor metering pump to quantitatively feed the mother liquor 1 in the mother liquor pool into the mixer.
2. The tower-type continuous flow potassium hydrogen monosulfate preparation device of claim 1, wherein the oxidation section device is a thin and high tower-type continuous flow reactor, and is provided with a reaction liquid internal circulation device and a cooling coil pipe, so as to control the reaction temperature.
3. The tower-type continuous flow potassium hydrogen monosulfate preparation device of claim 1, wherein the neutralization section device is a thin and high tower-type continuous flow reactor, and is provided with a reaction liquid internal circulation device and a cooling pipe, so as to control the reaction temperature.
4. The tower-type continuous flow potassium monopersulfate salt preparing apparatus as set forth in claim 1, wherein the crystallizing apparatus is a horizontal continuous crystallizer or a kettle-type crystallizer.
5. The tower-type continuous flow potassium monopersulfate complex salt production apparatus of claim 1, wherein the drying is ebullated bed drying.
6. The tower-type continuous flow potassium monopersulfate salt preparing apparatus as set forth in claim 1, wherein the cooling medium is normal frozen brine, glycol freezing liquid, freon series cooling liquid.
7. The tower-type continuous flow preparation method of potassium monopersulfate complex salt according to claim 1, wherein the concentration of fuming sulfuric acid is 105-122.5%, and when fuming sulfuric acid is selected to have the highest concentration, fuming sulfuric acid can be replaced by liquid SO 3.
8. The tower-type continuous flow potassium monopersulfate salt preparation method as claimed in claim 1, wherein the alkaline potassium compound as the neutralization raw material is mainly potassium hydroxide solution, the mass fraction of the solution is 20-60%, and the potassium hydroxide solution feeding part is arranged on a mixer device.
9. The preparation method of the potassium monopersulfate composite salt according to claim 1, wherein the alkaline potassium compound used as a raw material for neutralization is potassium carbonate, the mass fraction of the solution is 70-99%, and the feeding part of the potassium carbonate is arranged on a mixer device.
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| CN115448257B (en) * | 2022-09-15 | 2023-07-14 | 浙江金科日化新材料股份有限公司 | Potassium hydrogen peroxymonosulfate compound salt spherulites and preparation method thereof |
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