CN114873564A - Method for efficiently and continuously producing potassium hydrogen peroxymonosulfate composite salt - Google Patents
Method for efficiently and continuously producing potassium hydrogen peroxymonosulfate composite salt Download PDFInfo
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- 150000003839 salts Chemical class 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- OKBMCNHOEMXPTM-UHFFFAOYSA-M potassium peroxymonosulfate Chemical compound [K+].OOS([O-])(=O)=O OKBMCNHOEMXPTM-UHFFFAOYSA-M 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 56
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 33
- 238000002425 crystallisation Methods 0.000 claims abstract description 28
- 230000008025 crystallization Effects 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 239000012425 OXONE® Substances 0.000 claims abstract description 27
- 230000001590 oxidative effect Effects 0.000 claims abstract description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 7
- -1 alkali metal salt Chemical class 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 7
- 239000011591 potassium Substances 0.000 claims abstract description 7
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical group [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000003085 diluting agent Substances 0.000 claims description 13
- 239000012452 mother liquor Substances 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 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 description 11
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 239000002912 waste gas Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000003507 refrigerant Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000010327 methods by industry Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000010413 mother solution Substances 0.000 abstract 1
- 239000000725 suspension Substances 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000012267 brine Substances 0.000 description 6
- 239000012295 chemical reaction liquid Substances 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- FHHJDRFHHWUPDG-UHFFFAOYSA-N peroxysulfuric acid Chemical compound OOS(O)(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
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-
- C—CHEMISTRY; METALLURGY
- 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
-
- 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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
-
- 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
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for efficiently and continuously producing potassium hydrogen peroxymonosulfate composite salt, which comprises the following steps: 1. taking an oxidizing solution prepared by reacting sulfuric acid with hydrogen peroxide as a raw material A; 2. taking the diluted solution as a raw material B; 3. alkali metal salt of potassium as raw material C; 4. the raw material A and the raw material B flow through a mixer at the same time according to a set proportion through an automatic control system for continuous mixing, and the mixed solution is injected into a neutralization kettle; 5. continuously adding the raw material C into the neutralization kettle to prepare a neutralization solution; 6. until the neutralizing liquid reaches the inner volume of the neutralizing kettle
When the crystallization kettle is used, the neutralization solution in the kettle is continuously put into the crystallization kettle for crystallization; 7. continuously putting the suspension in the crystallization kettle into a continuous centrifuge for centrifugation to obtain a potassium hydrogen peroxymonosulfate composite salt wet product and a mother solution; 8. feeding the wet product to vibrationDrying the mixture in a fluidized bed to obtain the finished potassium peroxymonosulfate composite salt.
Description
Technical Field
The invention relates to the technical field of preparation of potassium monopersulfate composite salt, in particular to a real continuous production system and a real continuous production process of potassium monopersulfate composite salt.
Background
The potassium peroxymonosulfate composite salt is a white crystalline particulate matter, has a high oxidation potential, is an excellent strong acidic oxidant, and is a composite salt consisting of potassium peroxymonosulfate, potassium bisulfate and potassium sulfate. The potassium hydrogen peroxymonosulfate has wide application range, and relates to the fields of circuit board etching agents, swimming pool disinfectants, disinfectants in the animal protection industry, false tooth and oral cleaning agents, paper pulp bleaches, wool fabric shrink-proof treatment, precious metal extraction, free radical initiators of a plurality of polymerization reactions and the like.
The production process of potassium hydrogen peroxymonosulfate composite salt at the present stage mostly adopts a kettle type intermittent reaction or a pseudo-continuous production process of continuous reaction in partial process, and the probability of fluctuation of product quality is greatly increased as long as the intermittent reaction exists. In addition, the accurate addition of raw materials is difficult to control in the intermittent reaction process, the loss rate of hydrogen peroxide is high, the cooling efficiency is low, the potential safety hazard is large, the occupied space of equipment is large, the utilization rate is not high, and the equipment has the practical conditions of serious corrosion and difficult maintenance.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a method for efficiently and continuously producing potassium peroxymonosulfate composite salt. And the used equipment is convenient to maintain, small in occupied space and light in weight.
In order to achieve the aim, the invention provides a method for efficiently and continuously producing potassium hydrogen peroxymonosulfate composite salt, which comprises the following steps:
(1) pumping an oxidizing solution formed by reacting sulfuric acid and hydrogen peroxide, namely a peroxymonosulfuric acid solution, into a raw material tank 1, and cooling the oxidizing solution to a set temperature to obtain a raw material A;
(2) the diluent is injected into the raw material tank 2 and cooled to a set temperature to be used as a raw material B;
(3) conveying the raw material A and the raw material B in the steps 1) and 2) to a mixer through automatic control equipment according to a specific flow ratio for mixing to obtain a mixed solution, wherein the heat exchange area of the mixer is selected to be proper, and the temperature of the mixed solution in a heat exchanger is controlled to be proper;
(4) continuously pumping the mixed liquid obtained in the step 3) into a neutralization kettle, and keeping the neutralization kettle at a certain temperature.
(5) Adding alkali metal salt of potassium into a storage bin, continuously adding into a neutralization kettle through a flood dragon, keeping a certain temperature in the neutralization kettle, and discharging waste gas into a waste gas treatment device through micro negative pressure.
(6) Until the neutralizing liquid reaches the inner volume of the neutralizing kettle
When in use, the neutralization solution in the crystallization kettle is continuously put into the crystallization kettle for crystallization, and the temperature of the solution system in the crystallization kettle is properly controlled;
(7) and continuously putting the turbid liquid in the crystallization kettle into a continuous centrifuge for centrifugation to obtain a potassium peroxymonosulfate composite salt wet product and mother liquor, and then conveying the wet product into a vibrating fluidized bed through a lifter for drying to obtain a finished product of potassium peroxymonosulfate composite salt.
(8) The method for efficiently and continuously producing the potassium hydrogen peroxymonosulfate composite salt is characterized in that the raw material A in the step 1) is sulfuric acid solution with the concentration of 30-65% fuming sulfuric acid; the concentration of the selected hydrogen peroxide is 10-70%.
(9) The method for efficiently and continuously producing the potassium hydrogen peroxymonosulfate composite salt is characterized in that the temperature of the raw material A in the step 1) is controlled to be-20-50 ℃.
(10) The method for efficiently and continuously producing the potassium peroxymonosulfate composite salt is characterized in that the diluent of the raw material B in the step 2) is one or more of mother liquor obtained by centrifuging the potassium peroxymonosulfate composite salt, tap water and deionized water.
(11) The method for efficiently and continuously producing the potassium hydrogen peroxymonosulfate composite salt is characterized in that the temperature of the raw material B in the step 2) is controlled to be-20-50 ℃.
(12) The method for efficiently and continuously producing the potassium monopersulfate composite salt is characterized in that in the step 3), the flow and the weight of the diluent and the oxidizing solution are controlled by adopting a mass flow meter and an automatic regulating valve, a DCS control system is adopted, the diluent and the oxidizing solution are simultaneously conveyed into a mixer through a pump and are continuously mixed, and the flow ratio of the diluent water to the oxidizing solution is 1: 0.5-3.0.
(13) The method for efficiently and continuously producing the potassium monopersulfate composite salt is characterized in that in the step 3), the mixer can be a micro-channel mixer, a spiral plate mixer, a tubular mixer or a static mixer, and the heat exchange area of the mixer is 0.5m 2 ～50m 2 。
(14) The method for efficiently and continuously producing the potassium hydrogen peroxymonosulfate composite salt is characterized in that in the step 3), the temperature of the mixed liquid in the mixer is controlled to be-20-100 ℃.
(15) The method for efficiently and continuously producing the potassium hydrogen peroxymonosulfate composite salt is characterized in that in the step 4) and the step 5), the transfer kettle is cooled by a refrigerant jacket, and the temperature of the mixed solution is controlled to be-2-100 ℃.
(16) The method for efficiently and continuously producing the potassium monopersulfate composite salt is characterized in that in the step 5), the alkali metal salt of potassium can be potassium carbonate and potassium hydroxide.
(17) The method for efficiently and continuously producing the potassium monopersulfate composite salt is characterized in that in the step 6), the temperature of a solution system in a crystallization kettle is controlled to be-20-0 ℃, the growth speed of potassium monopersulfate composite salt crystals and the size of crystal grains can be controlled by controlling the stirring speed, and the equipment is also a key step designed in the whole process engineering.
(18) The method for efficiently and continuously producing the potassium monopersulfate composite salt is characterized in that in the step 7), the continuous centrifuge is efficient equipment capable of continuously centrifuging and discharging materials.
The invention has the beneficial effects that: the invention adopts a mixer to continuously mix the oxidizing solution and the diluent, adopts a screw feeder to continuously add the alkali metal salt of potassium, and adopts a crystallization kettle and a continuous centrifuge to continuously discharge, thereby ensuring the complete continuity of the whole process. The equipment occupies a small space, the whole set of process can realize automatic and accurate control, the produced product has stable quality, the raw materials have small online amount, the safety is high, the energy efficiency utilization rate is high, the equipment maintenance is convenient, and the product can be continuously produced, so that the equipment is particularly suitable for large-scale industrial production.
Drawings
FIG. 1 is a schematic diagram of the inventive process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to fig. 1 and the embodiments.
Example 1
(1) Raw materials: weighing 150kg of oxidizing solution by a mass flowmeter, pumping the oxidizing solution into a raw material tank 1, starting frozen brine, reducing the temperature of the oxidizing solution to-10 ℃, and taking the oxidizing solution as a raw material A for later use; weighing 250kg of mother liquor by a mass flow meter, pumping into a raw material tank 2, starting frozen brine, reducing the temperature of the mother liquor to-10 ℃ and taking the mother liquor as a raw material B for later use; 90kg of potassium carbonate is weighed and put into a storage bin for standby.
The reactor equipment: the mixer is a spiral plate mixer with a heat exchange area of 5m 2 。
A neutralization kettle: the transfer kettle is a 300L stainless steel reaction kettle.
(2) Conveying the raw material A and the raw material B by using a pump, and pumping the raw materials into a mixer through a flowmeter, wherein the flow rate of the raw material A is controlled to be 75kg/h, and the flow rate of the raw material B is controlled to be 125 kg/h; the inlet frozen saline is-20 ℃, and the outlet frozen saline is 5 ℃; the temperature of the reaction liquid in the mixer is lower than 0 ℃, the reaction liquid flows into a neutralization kettle after 2min, simultaneously potassium carbonate solid is added into the neutralization kettle through a flood dragon, the adding speed is 45kg/h, and the temperature of the neutralization liquid in the neutralization kettle is kept at 35 ℃.
(3) Until the neutralizing liquid reaches the inner volume of the neutralizing kettle
When the temperature is high, the neutralization solution in the crystallization kettle is continuously put into the crystallization kettle, and the temperature in the crystallization kettle is controlled to be-5 ℃.
(4) And continuously putting the turbid liquid in the crystallization kettle into a continuous centrifuge for centrifugation to obtain a potassium peroxymonosulfate composite salt wet product and mother liquor, and then conveying the wet product into a vibrating fluidized bed through a lifter for drying to obtain a finished product of potassium peroxymonosulfate composite salt.
The results of the oxidation liquid obtained by the reaction are shown in table 1:
example 2
The difference from example 1 is that the alkali metal salt of potassium is chosen to be KOH.
(1) Raw materials: weighing 150kg of oxidizing solution by a mass flow meter, pumping into a raw material tank 1, starting frozen brine, reducing the temperature of peroxide to-10 ℃ and taking the peroxide as a raw material A for later use; weighing 250kg of mother liquor by a mass flow meter, pumping into a raw material tank 2, starting frozen brine, reducing the temperature of the mother liquor to-10 ℃ and taking the mother liquor as a raw material B for later use; 74kg of potassium hydroxide is weighed into a storage bin for standby.
The reactor equipment: the mixer is a spiral plate mixer with a heat exchange area of 5m 2 。
A neutralization kettle: the transfer kettle is a 300L stainless steel reaction kettle.
(2) Conveying the raw material A and the raw material B by using a pump, and pumping the raw materials into a mixer through a flowmeter, wherein the flow rate of the raw material A is controlled to be 75kg/h, and the flow rate of the raw material B is controlled to be 125 kg/h; the inlet frozen saline is-20 ℃, and the outlet frozen saline is 5 ℃; the temperature of the reaction liquid in the mixer is lower than 0 ℃, the reaction liquid flows into a neutralization kettle after 2min, simultaneously potassium carbonate solid is added into the neutralization kettle through a flood dragon, the adding speed is 37kg/h, and the temperature of the neutralization liquid in the neutralization kettle is kept at 35 ℃.
(3) Until the neutralizing liquid reaches the inner volume of the neutralizing kettle
When the temperature is high, the neutralization solution in the crystallization kettle is continuously put into the crystallization kettle, and the temperature in the crystallization kettle is controlled to be at-5 ℃.
(4) And continuously putting the turbid liquid in the crystallization kettle into a continuous centrifuge for centrifugation to obtain a potassium peroxymonosulfate composite salt wet product and mother liquor, and then conveying the wet product into a vibrating fluidized bed through a lifter for drying to obtain a finished product of potassium peroxymonosulfate composite salt.
The results of the oxidation liquid obtained by the reaction are shown in table 1:
example 3
The difference from example 1 and the difference in the heat exchange area of the mixer used.
Weighing 150kg of oxidation liquid through a mass flow meter, pumping the oxidation liquid into a raw material tank 1, starting frozen brine, reducing the temperature of the oxidation liquid to-10 ℃ to be used as a raw material A for later use, weighing 250kg of mother liquid through the mass flow meter, pumping the mother liquid into a raw material tank 2, starting the frozen brine, reducing the temperature of the mother liquid to-10 ℃ to be used as a raw material B for later use, weighing 90kg of potassium carbonate, and putting the potassium carbonate into a storage bin for later use.
The reactor equipment: the mixer is a spiral plate mixer with a heat exchange area of 10m 2 。
A neutralization kettle: the transfer kettle is a 300L stainless steel reaction kettle.
(2) Conveying the raw material A and the raw material B by using a pump, and pumping the raw materials into a mixer through a flowmeter, wherein the flow rate of the raw material A is controlled to be 75kg/h, and the flow rate of the raw material B is controlled to be 125 kg/h; the inlet frozen saline is-20 ℃, and the outlet frozen saline is 5 ℃; the temperature of the reaction liquid in the mixer is lower than 30 ℃, the reaction liquid flows into a neutralization kettle after 2min, simultaneously potassium carbonate solid is added into the neutralization kettle through a flood dragon, the adding speed is 45kg/h, and the temperature of the neutralization liquid in the neutralization kettle is kept at 30 ℃.
(3) Until the neutralizing liquid reaches the inner volume of the neutralizing kettle
When the temperature is high, the neutralization solution in the kettle is continuously put into a crystallization kettle, and the temperature in the crystallizer is controlled to be-5 ℃.
(4) And continuously putting the turbid liquid in the crystallization kettle into a continuous centrifuge for centrifugation to obtain a potassium peroxymonosulfate composite salt wet product and mother liquor, and then conveying the wet product into a vibrating fluidized bed through a lifter for drying to obtain a finished product of potassium peroxymonosulfate composite salt.
The results of the oxidation liquid obtained by the reaction are shown in table 1:
comparative example 1:
comparative example 1 comparative data of the oxidation liquid prepared by the kettle type batch reaction commonly used by enterprises at the present stage. The batch ratio of example 1 was used.
TABLE 1 test results of oxidizing solutions obtained in examples 1 to 3 and comparative example 1
As can be seen from table 1, in the method for efficiently and continuously producing potassium monopersulfate composite salt provided in embodiments 1 to 3, when the mixer, the crystallization kettle, the continuous centrifuge, and the vibrated fluidized bed are used for continuously producing potassium monopersulfate composite salt, the product quality is stable and high-quality, the yield is high, the occupied space of the equipment is small, the production process is safe and efficient, the labor intensity is low, the intelligent degree is high, the production process is obviously superior to the batch reaction process, and the method is particularly suitable for industrial mass production.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for efficiently and continuously producing potassium hydrogen peroxymonosulfate composite salt comprises the following steps:
(1) pumping an oxidizing solution formed by reacting sulfuric acid and hydrogen peroxide, namely a peroxosulfuric acid solution, into a raw material tank 1, and cooling the oxidizing solution to a set temperature to obtain a raw material A;
(2) the diluent is injected into the raw material tank 2 and cooled to a set temperature to be used as a raw material B;
(3) conveying the raw material A and the raw material B in the steps 1) and 2) to a mixer through automatic control equipment according to a specific flow ratio for mixing to obtain a mixed solution, wherein the heat exchange area of the mixer is properly selected, and the temperature of the mixed solution in the mixer is properly controlled;
(4) continuously pumping the mixed liquid obtained in the step 3) into a neutralization kettle, and keeping the neutralization kettle at a certain temperature.
(5) Adding alkali metal salt of potassium into a storage bin, continuously adding into a neutralization kettle through a flood dragon, keeping a certain temperature in the neutralization kettle, and discharging waste gas into a waste gas treatment device through micro negative pressure.
(6) Until the neutralizing liquid reaches the inner volume of the neutralizing kettle
When in use, the neutralization solution in the crystallization kettle is continuously put into the crystallization kettle for crystallization, and the temperature of the crystallization kettle is properly controlled;
(7) and continuously putting the turbid liquid in the crystallization kettle into a continuous centrifuge for centrifugation to obtain a potassium peroxymonosulfate composite salt wet product and mother liquor, and conveying the wet product into a vibrating fluidized bed through a lifter for drying to obtain a finished potassium peroxymonosulfate composite salt.
2. The raw material A of the step 1) according to claim 1, characterized in that the selected sulfuric acid concentration is 30% sulfuric acid to 65% oleum; the concentration of the selected hydrogen peroxide is 10-70%, and the cooling temperature of the raw material A is controlled to be-20-50 ℃.
3. The raw material B in the step 2) according to claim 1, wherein the selected diluent is one or more of mother liquor obtained by centrifuging potassium hydrogen peroxymonosulfate composite salt, tap water and deionized water, and the cooling temperature of the diluent is controlled to be-20-50 ℃.
4. The step 3) of claim 1, wherein the diluent and the oxidizing solution are simultaneously pumped into a mixer for continuous mixing, the flow rate and the weight of the diluent and the oxidizing solution are controlled by a mass flow meter and an automatic regulating valve, the diluent and the oxidizing solution are precisely controlled by a DCS control system, the flow rate ratio of the diluent to the oxidizing solution is 2: 0.5-3.0, the mixer is cooled by a refrigerant, the mixer can be a microchannel mixer, a spiral plate mixer, a tubular mixer or a static mixer, and the heat exchange area of the mixer is 0.5m 2 ～50m 2 。
5. The step 3) according to claim 1, wherein the temperature of the mixed liquid in the mixer is controlled to be-20 to 100 ℃.
6. The steps 4) and 5) according to claim 1, wherein the neutralization kettle is used for cooling the mixed solution by a refrigerant jacket, and the temperature of the mixed solution is controlled to be-2-100 ℃.
7. The process 5) according to claim 1, wherein the alkali metal salt of potassium is selected from potassium carbonate and potassium hydroxide.
8. The step 6) as recited in claim 1, wherein the temperature in the crystallization kettle is controlled to be-20 to 0 ℃, and the growth rate and the grain size of the potassium monopersulfate complex salt crystal can be controlled by controlling the stirring speed, and the equipment is also a key step of the design of the invention in the whole process engineering.
9. Step 7) according to claim 1, wherein the continuous centrifuge is a high-efficiency apparatus capable of continuous uninterrupted centrifugation and discharge.
10. The reaction equation involved in the invention is as follows:
H 2 O 2 +H 2 SO 4 →H 2 SO 5 +H 2 O
4H 2 SO 5 +4H 2 SO 4 +10K + →2(2KHSO 5 ·KHSO 4 ·K 2 SO 4 )+5H 2 O。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210074602.6A CN114873564A (en) | 2022-01-21 | 2022-01-21 | Method for efficiently and continuously producing potassium hydrogen peroxymonosulfate composite salt |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5139763A (en) * | 1991-03-06 | 1992-08-18 | E. I. Du Pont De Nemours And Company | Class of stable potassium monopersulfate compositions |
| CN102311100A (en) * | 2011-05-11 | 2012-01-11 | 宋海鹏 | Method for preparing potassium hydrogen peroxymonosulfate composite salt |
| CN108640089A (en) * | 2018-07-12 | 2018-10-12 | 绍兴上虞洁华化工有限公司 | Potassium hydrogen persulfate composite salts serialization making apparatus and preparation method |
| CN112645290A (en) * | 2020-12-24 | 2021-04-13 | 河北纳泰化工有限公司 | Continuous production system and production method of potassium monopersulfate composite salt |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5139763A (en) * | 1991-03-06 | 1992-08-18 | E. I. Du Pont De Nemours And Company | Class of stable potassium monopersulfate compositions |
| CN102311100A (en) * | 2011-05-11 | 2012-01-11 | 宋海鹏 | Method for preparing potassium hydrogen peroxymonosulfate composite salt |
| CN108640089A (en) * | 2018-07-12 | 2018-10-12 | 绍兴上虞洁华化工有限公司 | Potassium hydrogen persulfate composite salts serialization making apparatus and preparation method |
| CN112645290A (en) * | 2020-12-24 | 2021-04-13 | 河北纳泰化工有限公司 | Continuous production system and production method of potassium monopersulfate composite salt |
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