CN112374464A - Method and equipment for preparing hypochlorous acid by combining ion exchange method with electrolysis method - Google Patents

Method and equipment for preparing hypochlorous acid by combining ion exchange method with electrolysis method Download PDF

Info

Publication number
CN112374464A
CN112374464A CN202010795866.1A CN202010795866A CN112374464A CN 112374464 A CN112374464 A CN 112374464A CN 202010795866 A CN202010795866 A CN 202010795866A CN 112374464 A CN112374464 A CN 112374464A
Authority
CN
China
Prior art keywords
solution
hypochlorous acid
hypochlorite
filter
electrolysis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010795866.1A
Other languages
Chinese (zh)
Inventor
东方晓
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhongshan Yuanyu Enterprise Investment Co ltd
Original Assignee
Zhongshan Yuanyu Enterprise Investment Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhongshan Yuanyu Enterprise Investment Co ltd filed Critical Zhongshan Yuanyu Enterprise Investment Co ltd
Priority to CN202010795866.1A priority Critical patent/CN112374464A/en
Publication of CN112374464A publication Critical patent/CN112374464A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B11/00Oxides or oxyacids of halogens; Salts thereof
    • C01B11/04Hypochlorous acid
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • C25B1/24Halogens or compounds thereof
    • C25B1/26Chlorine; Compounds thereof
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00Operating or servicing cells
    • C25B15/08Supplying or removing reactants or electrolytes; Regeneration of electrolytes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

The invention discloses a method and equipment for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, wherein the preparation method comprises the following steps: s1, treating tap water by adopting a pre-filter to obtain purified water; s2, adding hypochlorite solution and purified water into the hypochlorite solution diluter to obtain hypochlorite diluted solution; s3, adding the hypochlorite solution and the acid solution into a mixer for mixing reaction; or carbon dioxide gas is conveyed into the mixer through a pipeline to carry out mixing reaction; s4, carrying out ion exchange on the hypochlorous acid mixed solution through an ion exchanger; and S5, introducing the hypochlorous acid mixed solution into an electrolysis device for electrolysis to convert chloride ions in the solution into hypochlorous acid molecules, so as to reduce the content of the chloride ions in the solution and remove heavy metal ions. The method has simple process, can effectively remove heavy metal ions in the hypochlorous acid, effectively reduce the content of chloride ions in the solution, and improve the concentration of the hypochlorous acid, thereby effectively improving the concentration and stability of the hypochlorous acid.

Description

Method and equipment for preparing hypochlorous acid by combining ion exchange method with electrolysis method
Technical Field
The invention relates to a method for preparing hypochlorous acid by combining an ion exchange method with an electrolytic method, and also relates to equipment for the preparation method.
Background
The disinfectant is used for killing pathogenic microorganisms on the transmission medium, so that the transmission medium meets the harmless requirement, and meanwhile, the disinfectant can cut off the transmission path of infectious diseases, so that the purpose of controlling the infectious diseases is achieved. At present, the disinfectants used on the surfaces of objects mainly comprise ozone disinfectants, alcohol disinfectants and chlorine disinfectants, wherein the chlorine disinfectants have wide application range and can be used for disinfecting human skin mucosa, drinking water, tableware, fruits and vegetables, environment and the like.
Chlorine disinfectant among the prior art is mainly sodium hypochlorite or calcium hypochlorite, and sodium hypochlorite or calcium hypochlorite can not directly be regarded as the disinfectant and use, need dilute sodium hypochlorite or calcium hypochlorite with water, utilize the hypochlorous acid that exists in sodium hypochlorite solution or the calcium hypochlorite solution to disinfect, and the hypochlorous acid molecule can permeate to the bacterium surface of taking the burden electricity to penetrate the cell wall and get into inside the cell, and the strong oxidizing property of hypochlorous acid can destroy the enzyme system of bacterium and make the bacterium die. For example, Chinese patent application No. 201010192336.4 discloses a method for preparing a long-acting sodium hypochlorite aqueous solution, which comprises the steps of taking 221g of sodium hypochlorite solid with 2 molecules of crystal water, adding water to prepare 1000mL of a solution with the molar concentration of 2mol/L, then adding 2.21g of a stabilizing agent into the solution, stirring for 15 minutes, standing and clarifying the stirred solution for 30 minutes, removing precipitates in the standing solution, and collecting the clarified solution to obtain 1151g of the long-acting sodium hypochlorite aqueous solution with the mass concentration of 7.72%.
Hypochlorous acid has been demonstrated internationally as one of the highly effective disinfecting and sterilizing products. The slightly acidic hypochlorous acid water is colorless and odorless electrolytic water with pH value of 4.0-6.8 and high bactericidal effect, and is also called slightly acidic electrolyzed water, SAEW for short and slightly acidic electrolyzed oxidizing water. Weakly acidic hypochlorous acid water is a weakly acidic water containing hypochlorous acid as a main component, and neutrophils, which are responsible for human immune functions, generate hypochlorous acid, which dominates biological immunity and is an indispensable active molecule even for human beings.
The existing methods for producing hypochlorous acid mainly comprise an electrolysis method and a two-liquid method. However, the supply of slightly acidic hypochlorous acid water is limited due to the electrolysis efficiency, and the electrolysis requires an electrolytic cell apparatus, which results in a very high maintenance cost. In addition, electrodes are required, the cost is too high, and only low-concentration hypochlorous acid can be produced by an electrolytic method. The two-solution method is to combine a sodium hypochlorite solution with a strong acid solution such as hydrochloric acid to prepare hypochlorous acid with an acidic pH value. This method is a process of adjusting the pH value with the acidity of hydrochloric acid or the like and mixing sodium hypochlorite with an acid, and thus a potential safety hazard occurs. In particular, chlorine gas is generated after sodium hypochlorite and acid are fused.
Therefore, the existing preparation method of hypochlorous acid is to be further improved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for preparing the hypochlorous acid by combining the ion exchange method with the electrolysis method, which has simple process, can effectively remove heavy metal ions in the hypochlorous acid, effectively reduce the content of chloride ions in the solution and improve the concentration of the hypochlorous acid so as to effectively improve the concentration and stability of the hypochlorous acid.
Another object of the invention is to provide a production apparatus for carrying out the above method.
In the method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, the invention adopts the following scheme in order to achieve the aim:
a method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method is characterized by comprising the following steps:
s1, treating tap water by adopting a pre-filter to obtain purified water;
s2, adding hypochlorite solution and purified water in the step S1 into a hypochlorite solution diluter to obtain hypochlorite diluted solution;
s3, adding the hypochlorite solution and the acid solution in the step S2 into a mixer for mixing reaction to obtain a hypochlorous acid mixed solution; or adding the hypochlorite solution obtained in the step S2 into a mixer, and conveying carbon dioxide gas into the mixer through a pipeline for mixing reaction to obtain a hypochlorous acid mixed solution with the pH value of 4.0-8.0;
s4, carrying out ion exchange on the hypochlorous acid mixed solution in the step S3 through an ion exchanger to remove heavy metal ions, and obtaining hypochlorous acid with the heavy metal ions removed;
s5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device, and electrolyzing at a current of 0.05-1.0A to convert chloride ions in the solution into hypochlorous acid molecules, so that the content of the chloride ions in the solution is reduced, and heavy metal ions are removed at the same time, and a hypochlorous acid product is obtained.
As another improvement of the method for preparing hypochlorous acid by combining the ion exchange method and the electrolysis method, the volume concentration of the carbon dioxide gas in the step S3 is 1-99%, and a hypochlorous acid mixed solution with the concentration of 10ppm-5000ppm and the PPMPH of 4.0-8.0 is finally obtained.
As another improvement of the method for preparing hypochlorous acid by combining the ion exchange method with the electrolysis method, the water flow in the step S1 is adjusted to be 5-100L/min, and the water pressure is 0.01-0.5 MPa.
As another improvement of the method for preparing hypochlorous acid by combining the ion exchange method with the electrolysis method, the pre-filter in the step S1 is a three-stage filter device, the three-stage filter device comprises a 1 micron microporous PP cotton filter, a second-stage activated carbon filter and an acidic cation exchange resin filter which are sequentially connected, and large-particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter; heavy metal impurities and cations in tap water are filtered out by an acidic cation exchange resin filter.
As another improvement of the method for preparing hypochlorous acid by combining the ion exchange method and the electrolysis method, the hypochlorite solution in the step S2 is one or a mixture of more than two of sodium hypochlorite, calcium hypochlorite and potassium hypochlorite.
As another improvement of the method for preparing hypochlorous acid by combining the ion exchange method with the electrolysis method, the concentration of the hypochlorite solution in the step S2 is 4-15%, and the concentration of the hypochlorite diluted solution is 10-5000 ppm.
As another improvement of the method for preparing hypochlorous acid by combining the ion exchange method with the electrolysis method, the concentration of the acid solution in the step S3 is 1-37%.
As another modification of the method for preparing hypochlorous acid by combining the ion exchange method with the electrolysis method according to the present invention, the acidic solution in step S3 is one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, chloric acid, a disodium hydrogen phosphate buffer solution, or a sodium dihydrogen phosphate buffer solution.
As another improvement of the method for preparing hypochlorous acid by combining the ion exchange method with the electrolysis method, an acidic cation exchange resin is contained in the ion exchanger in the step S4.
As another improvement of the method for preparing hypochlorous acid by combining the ion exchange method with the electrolysis method, in step S4, the ion exchanger contains acidic cation exchange resin which is resin sulfonic acid group resin or/and carboxylic acid group resin.
In order to achieve the above object, the present invention adopts the following scheme with respect to a manufacturing apparatus:
the hypochlorous acid production apparatus for carrying out the method is characterized in that: the hypochlorite solution diluter is provided with a hypochlorite solution inlet pipe and an acid solution inlet pipe respectively, a carbon dioxide aeration pipe is arranged in the mixer, the air inlet end of the carbon dioxide aeration pipe extends out of the mixer.
In summary, compared with the prior art, the invention has the beneficial effects that:
the tap water is filtered through three stages, the first stage is filtered through a 1 micron microporous PP cotton filter to remove large-particle impurities, the second stage is used for adsorbing impurities such as organic matters and microorganisms through an activated carbon filter, and the third stage is used for filtering heavy metal impurities and cations through an acidic cation exchange resin filter to effectively reduce the impurities such as the impurities and the heavy metals in the treated tap water, so that the subsequent proper hypochlorous acid is effectively guaranteed, and the stability of the synthesized hypochlorous acid is effectively improved.
Secondly, in the preparation method, the hypochlorite solution is diluted to a proper concentration and then mixed with the acid solution or the carbon dioxide gas, so that the residual amount of hypochlorite in the hypochlorous acid water is effectively controlled, the prepared hypochlorous acid water is safer and more reliable, and the safety threat to people and livestock is avoided.
Thirdly, after the hypochlorous acid is synthesized, the impurity removal treatment is further carried out through cation exchange resin, heavy metal ions in the hypochlorous acid water are effectively removed, and therefore a purer slightly-acidic hypochlorous acid product with the pH value of 4.0-6.8 is obtained.
Fourthly, the weakly acidic hypochlorous acid solution passes through the electrolysis device, the electrode can achieve the purpose by using a common inert electrode, the chlorine ions in the solution can be converted into hypochlorous acid molecules in the electrolysis process under the current of 0.05A-1.0A, the content of the chlorine ions in the solution can be greatly reduced, the hypochlorous acid concentration is improved, and meanwhile, impurity gold such as copper ions and iron ions is precipitated as a metal simple substance by a cathode to achieve the impurity removal effect.
Drawings
FIG. 1 is a schematic view of a manufacturing apparatus of the present invention.
FIG. 2 is a schematic view of another embodiment of the manufacturing apparatus of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the specification of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The invention relates to a method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, which comprises the following steps:
s1, treating tap water by using a pre-filter 1 to obtain purified water; wherein the water flow is regulated to 5L/min, and the water pressure is 0.5 MPa. The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
S2, adding hypochlorite solution and purified water in the step S1 into the hypochlorite solution diluter 2 to obtain hypochlorite diluted solution; wherein the hypochlorite solution is sodium hypochlorite with the mass concentration of 4%, and the concentration of the hypochlorite dilution solution is 10 ppm.
S3, adding the hypochlorite solution and the hydrochloric acid solution in the step S2 into a mixer 3 for mixing reaction to obtain a hypochlorous acid mixed solution; wherein the concentration of the hydrochloric acid solution is 1 percent, and a hypochlorous acid mixed solution with the concentration of 10ppm and the pH value of 4.0 is obtained;
s4, removing heavy metal ions by carrying out ion exchange on the hypochlorous acid mixed solution in the step S3 through an ion exchanger 4 to obtain hypochlorous acid with pH of 4.0 and without heavy metal ions; the ion exchanger 4 contains a sulfonic acid resin.
And S5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device 4, and electrolyzing at the current of 0.05A, wherein a general inert electrode is used as the electrode, the electrolysis time is 30S, the chlorine ions in the solution are converted into hypochlorous acid molecules, the content of the chlorine ions in the solution is reduced, and meanwhile, heavy metal ions are removed, so that the heavy metal ion-removed hypochlorous acid with the pH value of 4.5 is obtained.
Example 2
The invention relates to a method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, which comprises the following steps:
s1, treating tap water by using a pre-filter 1 to obtain purified water; wherein the water flow is regulated to be 100L/min, and the water pressure is 0.1 MPa. The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
S2, adding hypochlorite solution and purified water in the step S1 into the hypochlorite solution diluter 2 to obtain hypochlorite diluted solution; wherein the hypochlorite solution is calcium hypochlorite with the mass concentration of 15%, and the concentration of the hypochlorite diluted solution is 5000 ppm.
S3, adding the hypochlorite solution and the disodium hydrogen phosphate buffer solution in the step S2 into a mixer 3 for mixing reaction to obtain a hypochlorous acid mixed solution; wherein the concentration of the disodium phosphate buffer is 37%; obtain a hypochlorous acid mixed solution with 5000ppmPH of 8.0;
s4, carrying out ion exchange on the hypochlorous acid mixed solution in the step S3 by an ion exchanger 4 to remove heavy metal ions, and obtaining hypochlorous acid with pH of 6.8 and without heavy metal ions; wherein the ion exchanger 4 contains a sulfonic resin.
And S5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device 4, electrolyzing at the current of 1.0A for 5min by using a general inert electrode, converting chloride ions in the solution into hypochlorous acid molecules, reducing the content of the chloride ions in the solution, and removing heavy metal ions to obtain a hypochlorous acid product.
Example 3
The invention relates to a method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, which comprises the following steps:
s1, treating tap water by using a pre-filter 1 to obtain purified water; wherein the water flow is regulated to 50L/min, and the water pressure is 0.3 MPa. The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
S2, adding hypochlorite solution and purified water in the step S1 into the hypochlorite solution diluter 2 to obtain hypochlorite diluted solution; wherein the hypochlorite solution is a potassium hypochlorite solution. The concentration of the potassium hypochlorite solution is 10 percent, and the concentration of the hypochlorite diluted solution is 2000 ppm.
S3, adding the hypochlorite solution and the phosphoric acid solution in the step S2 into a mixer 3 for mixing reaction to obtain a hypochlorous acid mixed solution; wherein the concentration of the phosphoric acid solution is 15%.
S4, the hypochlorous acid mixed solution in the step S3 is ion-exchanged by the ion exchanger 4 to remove heavy metal ions, and hypochlorous acid with pH of 6.0 is obtained as heavy metal ions. The ion exchanger 4 contains a carboxylic acid-based resin.
And S5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device 4, electrolyzing at the current of 0.2A for 2min by using a general inert electrode, converting chloride ions in the solution into hypochlorous acid molecules, reducing the content of the chloride ions in the solution, and removing heavy metal ions to obtain a hypochlorous acid product.
Example 4
The invention relates to a method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, which comprises the following steps:
s1, treating tap water by using a pre-filter 1 to obtain purified water; wherein the water flow is adjusted to 80L/min, and the water pressure is 0.2 MPa. The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
S2, adding hypochlorite solution and purified water in the step S1 into the hypochlorite solution diluter 2 to obtain hypochlorite diluted solution; wherein the hypochlorite solution is one or a mixture of more than two of sodium hypochlorite, calcium hypochlorite and potassium hypochlorite. The concentration of the hypochlorite solution is 8%, and the concentration of the hypochlorite diluted solution is 1000 ppm.
S3, adding the hypochlorite solution and the sodium dihydrogen phosphate buffer solution in the step S2 into a mixer 3 for mixing reaction to obtain a hypochlorous acid mixed solution; wherein the concentration of the sodium dihydrogen phosphate buffer solution is 20%.
S4, the hypochlorous acid mixed solution in the step S3 is ion exchanged by the ion exchanger 4 to remove heavy metal ions, so as to obtain the heavy metal ion-removed solution. The ion exchanger 4 contains an acidic cation exchange resin. The acidic cation exchange resin is sulfonic resin or/and carboxylic resin.
And S5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device 4, and electrolyzing at the current of 0.8A for 4min by using a general inert electrode to convert chloride ions in the solution into hypochlorous acid molecules, so that the content of the chloride ions in the solution is reduced, and heavy metal ions are removed at the same time, thereby obtaining a hypochlorous acid product.
Example 5
The invention relates to a method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, which comprises the following steps:
s1, treating tap water by using a pre-filter 1 to obtain purified water; wherein the water flow is adjusted to 80L/min, and the water pressure is 0.2 MPa. The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
S2, adding hypochlorite solution and purified water in the step S1 into the hypochlorite solution diluter 2 to obtain hypochlorite diluted solution; wherein the hypochlorite solution is one or a mixture of more than two of sodium hypochlorite, calcium hypochlorite and potassium hypochlorite. The concentration of the hypochlorite solution is 8%, and the concentration of the hypochlorite diluted solution is 1000 ppm.
S3, adding the hypochlorite solution obtained in the step S2 into a mixer 3, and conveying carbon dioxide gas with the volume concentration of 1% into the mixer 3 through a pipeline for mixing reaction to obtain a hypochlorous acid mixed solution with the pH value of 4.0;
s4, the hypochlorous acid mixed solution in the step S3 is ion exchanged by the ion exchanger 4 to remove heavy metal ions, so as to obtain the heavy metal ion-removed solution. The ion exchanger 4 contains an acidic cation exchange resin. The acidic cation exchange resin is sulfonic resin or/and carboxylic resin.
And S5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device 4, electrolyzing at the current of 0.1A for 1min by using a general inert electrode, converting chloride ions in the solution into hypochlorous acid molecules, reducing the content of the chloride ions in the solution, and removing heavy metal ions to obtain a hypochlorous acid product.
Example 6
The invention relates to a method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, which comprises the following steps:
s1, treating tap water by using a pre-filter 1 to obtain purified water; wherein the water flow is adjusted to 80L/min, and the water pressure is 0.2 MPa. The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
S2, adding hypochlorite solution and purified water in the step S1 into the hypochlorite solution diluter 2 to obtain hypochlorite diluted solution; wherein the hypochlorite solution is one or a mixture of more than two of sodium hypochlorite, calcium hypochlorite and potassium hypochlorite. The concentration of the hypochlorite solution is 8%, and the concentration of the hypochlorite diluted solution is 1000 ppm.
S3, adding the hypochlorite solution obtained in the step S2 into a mixer 3, and conveying carbon dioxide gas with the volume concentration of 99% into the mixer 3 through a pipeline for mixing reaction to obtain a hypochlorous acid mixed solution with the pH value of 7.0;
s4, the hypochlorous acid mixed solution in the step S3 is ion exchanged by the ion exchanger 4 to remove heavy metal ions, so as to obtain the heavy metal ion-removed solution. The ion exchanger 4 contains an acidic cation exchange resin. The acidic cation exchange resin is sulfonic resin or/and carboxylic resin.
And S5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device 4, electrolyzing at the current of 0.6A for 3min by using a general inert electrode, converting chloride ions in the solution into hypochlorous acid molecules, reducing the content of the chloride ions in the solution, and removing heavy metal ions to obtain a hypochlorous acid product.
Example 7
The invention relates to a method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method, which comprises the following steps:
s1, treating tap water by using a pre-filter 1 to obtain purified water; wherein the water flow is adjusted to 80L/min, and the water pressure is 0.2 MPa. The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
S2, adding hypochlorite solution and purified water in the step S1 into the hypochlorite solution diluter 2 to obtain hypochlorite diluted solution; wherein the hypochlorite solution is one or a mixture of more than two of sodium hypochlorite, calcium hypochlorite and potassium hypochlorite. The concentration of the hypochlorite solution is 8%, and the concentration of the hypochlorite diluted solution is 1000 ppm.
S3, adding the hypochlorite solution obtained in the step S2 into a mixer 3, and conveying carbon dioxide gas with the volume concentration of 1-99% into the mixer 3 through a pipeline for mixing reaction to obtain a hypochlorous acid mixed solution with the pH value of 4.0-8.0;
s4, the hypochlorous acid mixed solution in the step S3 is ion exchanged by the ion exchanger 4 to remove heavy metal ions, so as to obtain the heavy metal ion-removed solution. The ion exchanger 4 contains an acidic cation exchange resin. The acidic cation exchange resin is sulfonic resin or/and carboxylic resin.
And S5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device 4, and electrolyzing at the current of 0.8A for 3min by using a general inert electrode to convert chloride ions in the solution into hypochlorous acid molecules, so that the content of the chloride ions in the solution is reduced, and heavy metal ions are removed at the same time, thereby obtaining a hypochlorous acid product.
The method for preparing hypochlorous acid by combining the ion exchange method with the electrolysis method in examples 1 to 4 of the present invention can be carried out by the manufacturing apparatus of example 8 or 9.
Example 8
The invention provides hypochlorite manufacturing equipment, which comprises a mixer 3, wherein the liquid inlet end of the mixer 3 is connected with a hypochlorite solution diluter 2, the liquid outlet end of the mixer 3 is connected with the liquid inlet end of an ion exchanger 4, a first pH value detection device 7 and a second pH value detection device 9 are arranged on a liquid outlet pipe 8 of the ion exchanger 4 at intervals, an electrolytic tank is arranged on the liquid outlet pipe 8 between the first pH value detection device 7 and the second pH value detection device 9, the first pH value detection device 7 and the second pH value detection device 9 are connected with a controller 10 in different parts, a purified water conveying pipe 5 is arranged on one side of the hypochlorite solution diluter 2, the water inlet end of the purified water conveying pipe 5 is connected with the water outlet end of a pre-filter 1, the water inlet end of the pre-filter 1 is connected with a tap water pipe 14, and a hypochlorite solution pipe 30 and an acidic solution liquid inlet pipe 40 are respectively arranged on the hypochlorite solution diluter 2 And a carbon dioxide aeration pipe 50 is arranged in the mixer 3, and the air inlet end of the carbon dioxide aeration pipe 50 extends out of the mixer 3.
The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
Example 9
The invention provides hypochlorite manufacturing equipment, which comprises a mixer 3, wherein the liquid inlet end of the mixer 3 is connected with a hypochlorite solution diluter 2, the liquid outlet end of the mixer 3 is connected with the liquid inlet end of an ion exchanger 4, a first pH value detection device 7 and a second pH value detection device 9 are arranged on a liquid outlet pipe 8 of the ion exchanger 4 at intervals, an electrolytic tank is arranged on the liquid outlet pipe 8 between the first pH value detection device 7 and the second pH value detection device 9, the first pH value detection device 7 and the second pH value detection device 9 are connected with a controller 10 in different parts, a purified water conveying pipe 5 is arranged on one side of the hypochlorite solution diluter 2, the water inlet end of the purified water conveying pipe 5 is connected with the water outlet end of a pre-filter 1, the water inlet end of the pre-filter 1 is connected with a tap water pipe 14, and a hypochlorite solution pipe 30 and an acidic solution liquid inlet pipe 40 are respectively arranged on the hypochlorite solution diluter 2 And a carbon dioxide aeration pipe 50 is arranged in the mixer 3, and the air inlet end of the carbon dioxide aeration pipe 50 extends out of the mixer 3.
A first flow control valve 15 is arranged on the tap water pipe 14, a second flow control valve 16 is arranged on a pipeline connecting the hypochlorite solution diluter 2 and the mixer 3, a third flow control valve 17 is arranged on the purified water delivery pipe 5, a first electromagnetic control valve 18 is arranged on the liquid outlet pipe 8 of the ion exchanger 4, the second pH detection device 9 is arranged on the outlet pipe 8 between the ion exchanger 4 and the first electromagnetic control valve 18, a liquid return pipe 19 is arranged on the liquid outlet pipe 8 between the ion exchanger 4 and the first electromagnetic control valve 18, the liquid outlet end of the liquid return pipe 19 is connected with the liquid inlet pipe 6 of the ion exchanger 4, a second electromagnetic control valve 20 is arranged on the liquid return pipe 19, and the first flow control valve 15, the second flow control valve 16, the third flow control valve 17, the first electromagnetic control valve 18 and the second electromagnetic control valve 20 are respectively connected with the controller 10.
The pre-filter 1 is a three-stage filter device which comprises a 1 micron microporous PP cotton filter 11, a second-stage activated carbon filter 12 and an acidic cation exchange resin filter 13 which are sequentially connected, and large particle impurities in tap water are filtered by the 1 micron microporous PP cotton filter 11; adsorbing organic matters and microorganism impurities in the tap water through a second-stage activated carbon filter 12; heavy metal impurities and cations in the tap water are filtered off by an acidic cation exchange resin filter 13.
In the invention, a first flow control valve 15 is controlled to be opened, so that tap water enters a pre-filter 1, and the tap water is filtered from the pre-filter 1 through a 1 micron microporous PP cotton filter 11 to remove large-particle impurities in the tap water; then adsorbing organic matters and microorganism impurities in the tap water by a second-stage activated carbon filter 12; then passes through an acidic cation exchange resin filter 13 to filter out heavy metal impurities and cations in the tap water. And then into the hypochlorite solution diluter 2, the amount of which entering may be controlled by the first flow control valve 15. The diluted hypochlorite solution and the acid solution are added into the mixer 3 in proportion for mixing reaction, and the mixed solution is sent into the ion exchanger 4 for cation exchange after the reaction is finished, so that the heavy metal impurities and cations in the hypochlorous acid water are further removed, and the hypochlorous acid water is more stable and has a wider concentration range.
The mixer 3 of the invention can be provided with a stirring device and a heating device, so that the solution in the mixer 3 can be mixed more uniformly, and the mixed solution can be ensured to react at normal temperature or at a specific temperature.
In the invention, in order to improve the productivity, a water storage tank is arranged between the pre-filter 1 and the hypochlorite solution diluter 2, the water inlet end of the water storage tank is connected with the water outlet end of the pre-filter 1, the water outlet end of the water storage tank is connected with the water inlet end of the hypochlorite solution diluter 2, a water feeding pump and a flow meter are respectively arranged on a connecting pipeline between the water outlet end of the water storage tank and the water inlet end of the hypochlorite solution diluter 2, the water feeding pump and the flow meter are respectively connected with the controller 10, and the flow meter can accurately detect the amount of purified water input into the hypochlorite solution diluter 2, so that hypochlorite solution with preset concentration can be accurately prepared.
In the invention, the first pH value detection device 7 and the second pH value detection device 9 can respectively monitor the pH values of the liquid inlet end and the liquid outlet end of the ion exchanger, and when the pH value of the liquid outlet end is lower than a preset value, the controller 10 controls the second electromagnetic control valve 20 to be opened and controls the first electromagnetic control valve 18 to be closed, so that the hypochlorous acid water is subjected to secondary cation exchange treatment.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A method for preparing hypochlorous acid by combining an ion exchange method with an electrolysis method is characterized by comprising the following steps:
s1, treating tap water by adopting a pre-filter (1) to obtain purified water;
s2, adding hypochlorite solution and purified water in the step S1 into a hypochlorite solution diluter (2) to obtain hypochlorite diluted solution;
s3, adding the hypochlorite solution and the acid solution in the step S2 into a mixer (3) for mixing reaction to obtain a hypochlorous acid mixed solution; or adding the hypochlorite solution obtained in the step S2 into a mixer (3), and conveying carbon dioxide gas into the mixer (3) through a pipeline for mixing reaction to obtain a hypochlorous acid mixed solution with the pH value of 4.0-8.0;
s4, carrying out ion exchange on the hypochlorous acid mixed solution in the step S3 through an ion exchanger (4) to remove heavy metal ions, and obtaining hypochlorous acid with the heavy metal ions removed;
s5, feeding the hypochlorous acid mixed solution in the step S4 into an electrolysis device (4), and electrolyzing at a current of 0.05-1.0A to convert chloride ions in the solution into hypochlorous acid molecules, so that the content of the chloride ions in the solution is reduced, and heavy metal ions are removed to obtain a hypochlorous acid product.
2. The ion exchange method combined with electrolysis for preparing hypochlorous acid as claimed in claim 1, wherein the volume concentration of carbon dioxide gas in step S3 is 1-99%.
3. The method for preparing hypochlorous acid by combining an ion exchange method and an electrolysis method according to claim 1, wherein the water flow rate in step S1 is adjusted to 5-100L/min, and the water pressure is 0.01-0.5 MPa.
4. The method for preparing hypochlorous acid by combining an ion exchange method and an electrolysis method according to claim 1 or 2, wherein the prefilter (1) in step S1 is a three-stage filter device comprising a 1-micron microporous PP cotton filter (11), a second-stage activated carbon filter (12) and an acidic cation exchange resin filter (13) which are connected in sequence, and the large-particle impurities in tap water are filtered by the 1-micron microporous PP cotton filter (11); organic matters and microorganism impurities in the tap water are adsorbed by a second-stage activated carbon filter (12); heavy metal impurities and cations in the tap water are filtered out by an acidic cation exchange resin filter (13).
5. The method for preparing hypochlorous acid by combining an ion exchange method and an electrolysis method according to claim 1, wherein the hypochlorite solution in step S2 is one or a mixture of more than two of sodium hypochlorite, calcium hypochlorite and potassium hypochlorite.
6. The method for preparing hypochlorous acid by combining an ion exchange process with an electrolysis process as claimed in claim 1 or 5, wherein the concentration of said hypochlorite solution in step S2 is 4-15%, and the concentration of said hypochlorite diluted solution is 10-5000 ppm.
7. The method for preparing hypochlorous acid by combining an ion exchange method and an electrolysis method according to claim 1, wherein the concentration of the acidic solution in step S3 is 1-37%.
8. The method for preparing hypochlorous acid by ion exchange combined electrolysis according to claim 1 or 7, wherein the acidic solution is one of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, chloric acid, disodium hydrogen phosphate buffer solution, and sodium dihydrogen phosphate buffer solution in step S3.
9. The method for preparing hypochlorous acid by combining an ion exchange method and an electrolysis method according to claim 1, wherein the ion exchanger (4) in step S4 contains acidic cation exchange resin, and the acidic cation exchange resin is resin sulfonate or/and carboxylic acid resin.
10. The hypochlorous acid production apparatus for performing the method according to claim 1, wherein: including blender (3), the inlet end of blender (3) is connected with hypochlorite solution diluter (2), the play liquid end of blender (3) is connected with the inlet end of ion exchanger (4) be provided with first pH value check out test set (7) and second pH value check out test set (9) on drain pipe (8) of ion exchanger (4) the interval be equipped with electrolysis trough (60) on drain pipe (8) between first pH value check out test set (7) and second pH value check out test set (9), first pH value check out test set (7), second pH value check out test set (9) subsection are connected with controller (10) be equipped with purification water conveyer pipe (5) on hypochlorite solution diluter (2) one side, the end of intaking of purification water conveyer pipe (5) is connected with the outlet end of leading filter (1), the water inlet end of the pre-filter (1) is connected with a tap water pipe (14), a hypochlorite solution inlet pipe (30) and an acid solution inlet pipe (40) are respectively arranged on the hypochlorite solution diluter (2), a carbon dioxide aeration pipe (50) is arranged in the mixer (3), and the air inlet end of the carbon dioxide aeration pipe (50) extends out of the mixer (3).
CN202010795866.1A 2020-08-10 2020-08-10 Method and equipment for preparing hypochlorous acid by combining ion exchange method with electrolysis method Pending CN112374464A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010795866.1A CN112374464A (en) 2020-08-10 2020-08-10 Method and equipment for preparing hypochlorous acid by combining ion exchange method with electrolysis method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010795866.1A CN112374464A (en) 2020-08-10 2020-08-10 Method and equipment for preparing hypochlorous acid by combining ion exchange method with electrolysis method

Publications (1)

Publication Number Publication Date
CN112374464A true CN112374464A (en) 2021-02-19

Family

ID=74586487

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010795866.1A Pending CN112374464A (en) 2020-08-10 2020-08-10 Method and equipment for preparing hypochlorous acid by combining ion exchange method with electrolysis method

Country Status (1)

Country Link
CN (1) CN112374464A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113213593A (en) * 2021-05-28 2021-08-06 淄博瀚泓环保科技有限公司 Subacid electrolyzed water generating device with concentration automatic regulating function

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103501605A (en) * 2011-03-11 2014-01-08 仿生健康产业有限公司 A stable composition of HOCl, processes for its production and uses thereof
CN110385050A (en) * 2018-04-23 2019-10-29 陈云涛 A kind of dynamic booster-type subacidity multifunctional disinfectant generating means
WO2019225599A1 (en) * 2018-05-22 2019-11-28 株式会社トクヤマデンタル Method for producing weakly acidic hypochlorous acid aqueous solution
CN209835849U (en) * 2019-04-17 2019-12-24 张辰光 Desulfurization waste water utilization system
CN111346532A (en) * 2020-03-13 2020-06-30 唐山市新概念科技有限公司 Preparation method of carbonic acid-hypochlorous acid water

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103501605A (en) * 2011-03-11 2014-01-08 仿生健康产业有限公司 A stable composition of HOCl, processes for its production and uses thereof
CN110385050A (en) * 2018-04-23 2019-10-29 陈云涛 A kind of dynamic booster-type subacidity multifunctional disinfectant generating means
WO2019225599A1 (en) * 2018-05-22 2019-11-28 株式会社トクヤマデンタル Method for producing weakly acidic hypochlorous acid aqueous solution
CN209835849U (en) * 2019-04-17 2019-12-24 张辰光 Desulfurization waste water utilization system
CN111346532A (en) * 2020-03-13 2020-06-30 唐山市新概念科技有限公司 Preparation method of carbonic acid-hypochlorous acid water

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113213593A (en) * 2021-05-28 2021-08-06 淄博瀚泓环保科技有限公司 Subacid electrolyzed water generating device with concentration automatic regulating function

Similar Documents

Publication Publication Date Title
AU2008303538B2 (en) Electrochemical device for biocide treatment in agricultural applications
CN101774711B (en) Method for reducing chlorite as disinfection by-product of drinking water
CN102138568B (en) Method and equipment for preparing isosmotic disinfection cleaning solution
JP2009274950A (en) Method for preparing molecular hypochlorous acid solution
US20080003507A1 (en) Formulation Of Electrolyte Solutions For Electrochemical Chlorine Dioxide Generators
CN101001806A (en) Chlorine dioxide solution generator
JP2011068521A (en) Method for preparing molecular hypochlorous acid solution by ion exchange and molecular hypochlorous acid solution
CN101492193B (en) Method for treating wastewater containing methanal and methanoic acid
CN201587893U (en) Household water purifying equipment with double-absorption and double-filtration ozone sterilization and disinfection
CN112374464A (en) Method and equipment for preparing hypochlorous acid by combining ion exchange method with electrolysis method
CN214400748U (en) A large-traffic electrolysis water equipment for beasts and birds plant
EP3867422B1 (en) Electrochemical system for the synthesis of aqueous oxidising agent solutions
CN113215596A (en) System suitable for industrial production hypochlorous acid sterilized water
CN112501638A (en) Process and equipment for preparing hypochlorous acid by combining two-liquid method with electrolysis method
CN112499800A (en) Method and equipment for preparing hypochlorous acid by combining two-liquid synthesis and ion exchange method
CN112093930A (en) Method and equipment for preparing hypochlorous acid by combining gas-liquid synthesis with electrolysis method
CN112499591A (en) Method and equipment for preparing hypochlorous acid by combining two-liquid synthesis with microporous molecular sieve
CN112499799A (en) Method and equipment for preparing hypochlorous acid by combining gas-liquid synthesis with ion exchange method
CN216549989U (en) Medical pure water production equipment
CN203382604U (en) Device for processing and automatically conveying purified water used in perfume
JPH06206076A (en) Method and apparatus for producing sterilizing water
CN215667580U (en) Direct drinking water purification treatment device
CN212263120U (en) High concentration ozone water preparation system
KR100947847B1 (en) Device for producing complex sterilizing water
US20220073346A1 (en) Method for preparing hydronium ion-dissolveld water

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20210219