CN112210092A - Preparation method of sodium chlorite hydrogel - Google Patents

Preparation method of sodium chlorite hydrogel Download PDF

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Publication number
CN112210092A
CN112210092A CN202011193572.8A CN202011193572A CN112210092A CN 112210092 A CN112210092 A CN 112210092A CN 202011193572 A CN202011193572 A CN 202011193572A CN 112210092 A CN112210092 A CN 112210092A
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hydrogel
sodium chlorite
solution
preparing
steps
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袁宏明
李志峰
李志才
李超
李小文
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Jilin Baihao Technology Co ltd
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Jilin Baihao Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/16Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
    • A61L2/20Gaseous substances, e.g. vapours
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/56Acrylamide; Methacrylamide
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2202/00Aspects relating to methods or apparatus for disinfecting or sterilising materials or objects
    • A61L2202/10Apparatus features
    • A61L2202/11Apparatus for generating biocidal substances, e.g. vaporisers, UV lamps
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/24Homopolymers or copolymers of amides or imides
    • C08J2333/26Homopolymers or copolymers of acrylamide or methacrylamide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/324Alkali metal phosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
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  • Veterinary Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Disinfection, Sterilisation Or Deodorisation Of Air (AREA)

Abstract

The invention discloses a preparation method of a sodium chlorite hydrogel, which comprises the following steps: s1, preparation of hydrogel solution: preparing an acrylamide aqueous solution with the concentration of 3-5 mol/L; s2, graft copolymerization: adding potassium persulfate and N, N-methylene-bisacrylamide to the obtained acrylamide aqueous solution at the temperature of 10-30 ℃ while stirring for mixed reaction, and stirring for 30-40min, wherein the mass ratio of acrylamide to potassium persulfate to N, N-methylene-bisacrylamide is (300-) -400): 1: (1.7-2); s3, formation of sodium chlorite hydrogel: and heating the reacted solution at 50-70 ℃ for 0.5-1.5 hours to obtain hydrogel, drying the hydrogel, putting the dried hydrogel into a sodium chlorite solution, and waiting for the gel to absorb and swell in a light-tight environment to form the sodium chlorite hydrogel. The preparation method provided by the invention is convenient to operate and simple to produce, and the prepared sodium chlorite hydrogel is highly transparent, strong in adsorption capacity and oxidation resistance and has a good absorption effect on ultraviolet light.

Description

Preparation method of sodium chlorite hydrogel
Technical Field
The invention belongs to the technical field of space disinfection, and particularly relates to a preparation method of a sodium chlorite hydrogel.
Background
The chlorine dioxide has strong oxidizing power, and compared with the traditional liquid chlorine, the chlorine dioxide has strong sterilizing power, can not generate chlorophenol with strange odor with phenols in water, and can not react with humus to form carcinogenic substances. In the late 80 s of the last century, chlorine dioxide has received acceptance by the United States Department of Agriculture (USDA) and the united states Environmental Protection Agency (EPA) as a food disinfectant and a disinfectant for drinking water. The World Health Organization (WHO) confirms that the substance has no carcinogenicity and teratogenicity, has multiple functions of disinfection, sterilization, corrosion prevention, deodorization, fresh keeping, bleaching and the like, is a broad-spectrum, safe and efficient disinfectant, and is advocated as a fourth-generation disinfectant and also widely applied to the fields of paper pulp bleaching, food processing, medicine and health and the like.
However, chlorine dioxide gas is unstable, inconvenient to transport and store, and must be prepared on-site. A typical chemical method is to produce chlorine dioxide gas by reacting chloride with acid, but the chemical reaction occurs rapidly and the generation of chlorine dioxide gas at high concentration in a short time causes harm to human or animals. Although patent documents report that gel or adsorption type solid preparations are used for achieving long-acting slow release of chlorine dioxide in space, experiments prove that the concentration of chlorine dioxide gas specified by national standards is difficult to achieve, the release speed of the chlorine dioxide gas cannot be controlled so as to solve the problem of quantitative release of the chlorine dioxide gas, the operation process is complex, the wide application of the chlorine dioxide is hindered, and inconvenience is brought to users.
As chlorite is known to decompose under ultraviolet light to produce chlorine dioxide gas, prior studies have shown that chlorine dioxide gas can also be produced by irradiating sodium chlorite particles or sodium chlorite gel with ultraviolet light. However, the sodium chlorite hydrogel obtained by the traditional method has low transparency, and the application of the sodium chlorite hydrogel is limited.
Disclosure of Invention
Aiming at the problems, the invention researches and designs a preparation method of sodium chlorite hydrogel to solve the defect of low transparency of the sodium chlorite hydrogel obtained by the traditional method. The technical means adopted by the invention are as follows:
a preparation method of a sodium chlorite hydrogel comprises the following preparation steps:
s1, preparation of hydrogel solution: preparing an acrylamide aqueous solution with the concentration of 3-5 mol/L;
s2, graft copolymerization: adding potassium persulfate and N, N-methylene-bisacrylamide into the obtained acrylamide aqueous solution at room temperature while stirring for mixed reaction, and stirring for 30-40min, wherein the mass ratio of acrylamide to potassium persulfate to N, N-methylene-bisacrylamide is (300-) -400): 1: (1.7-2);
s3, formation of highly transparent sodium chlorite hydrogel: heating the uniformly reacted solution at 50-70 ℃ for 0.5-1.5 hours to obtain hydrogel, drying the hydrogel, putting the dried hydrogel into a sodium chlorite solution, and waiting for the gel to absorb and swell in a dark place (namely under the environment without ultraviolet irradiation) to form the sodium chlorite hydrogel.
Preferably, in step S2, the stirring speed is 300-500 r/min.
Preferably, in step S3, the drying temperature is 100-120 ℃.
Preferably, in step S3, the sodium chlorite solution has a mass concentration of 10 to 30%.
Preferably, in step S3, the sodium chlorite solution contains an activator.
Preferably, the activator is one or more of sodium dihydrogen phosphate, oxalic acid, citric acid, tartaric acid and hydrogen chlorite.
Preferably, the activating agent is sodium dihydrogen phosphate, and the mass ratio of the sodium chlorite to the sodium dihydrogen phosphate is (145-) -436): 1.
compared with the prior art, the preparation method of the sodium chlorite hydrogel has the following beneficial effects: the sodium chlorite hydrogel prepared by the method has the advantages of high transparency, strong adsorption capacity, strong oxidation resistance, safe and convenient use and the like, has a good absorption effect on ultraviolet light with the wavelength of less than 350nm, can be efficiently decomposed to prepare chlorine dioxide gas under the irradiation of the ultraviolet light, has oxidation resistance stability and light stability, and cannot cause the problem of aging cracking under the irradiation of the ultraviolet light. By controlling the light source irradiating the sodium chlorite hydrogel, the control of the release speed of the chlorine dioxide gas can be realized, the gel can be used for a long time, and the problems of acidification, uncontrollable release, storage and transportation, inconvenient use and the like of the chlorine dioxide products in the current market can be solved.
Drawings
FIG. 1 shows the transmittance of the sodium chlorite hydrogel obtained in example 1 of the present invention measured by UV-Vis spectrophotometry at a wavelength range of 300-800 nm.
FIG. 2 is a graph showing the transmittance of the sodium chlorite hydrogel obtained in example 2 of the present invention measured by UV-Vis spectrophotometry at a wavelength range of 300-800 nm.
FIG. 3 shows the transmittance of the sodium chlorite hydrogel obtained in example 3 of the present invention measured by UV-Vis spectrophotometry at a wavelength range of 300-800 nm.
Detailed Description
Example 1:
s1, preparation of hydrogel solution:
a certain amount of acrylamide was poured into a beaker, and 120 ml of distilled water was added to prepare an aqueous acrylamide solution having a concentration of 3 to 5 mol/L.
S2, graft copolymerization:
stirring at room temperature at the rotating speed of 300r/min by using a stirrer, adding potassium persulfate and N, N-methylene-bisacrylamide while stirring for mixing reaction, and stirring for 30 min; wherein the mass ratio of the acrylamide to the potassium persulfate to the N, N-methylene-bisacrylamide is 400:1: 2.
S3, formation of highly transparent sodium chlorite hydrogel:
pouring the solution with uniform reaction into a mould, and heating in a water bath kettle at 50 ℃ for 1 hour to obtain the high-transparency hydrogel. Then the gel is put into a 110 ℃ oven for drying, and then the gel is put into a sodium chlorite solution containing an activating agent sodium dihydrogen phosphate, wherein the mass concentration of the sodium chlorite solution is 30 percent, and the mass ratio of the sodium chlorite to the sodium dihydrogen phosphate is (145-: 1, waiting for the gel to absorb and swell in a dark place to form the highly transparent sodium chlorite hydrogel.
Example 2:
s1, preparation of hydrogel solution:
a certain amount of acrylamide was poured into a beaker, and 150 ml of distilled water was added to prepare an aqueous acrylamide solution having a concentration of 3 to 5 mol/L.
S2, graft copolymerization:
stirring at room temperature at the rotating speed of 300r/min by using a stirrer, adding potassium persulfate and N, N-methylene-bisacrylamide while stirring for mixing reaction, and stirring for 40 min; wherein the mass ratio of the acrylamide to the potassium persulfate to the N, N-methylene-bisacrylamide is 330:1: 1.8.
S3, formation of highly transparent sodium chlorite hydrogel:
pouring the solution with uniform reaction into a mould, and heating in a water bath kettle at 60 ℃ for 1.5 hours to obtain the high-transparency hydrogel. And then putting the gel into a 110 ℃ oven for drying, then putting the gel into a sodium chlorite solution, wherein the mass concentration of the sodium chlorite solution is 20%, and waiting for the gel to absorb and swell in a dark place to form the high-transparency sodium chlorite hydrogel.
Example 3:
s1, preparation of hydrogel solution:
a certain amount of acrylamide was poured into a beaker, and 150 ml of distilled water was added to prepare an aqueous acrylamide solution having a concentration of 3 to 5 mol/L.
S2, graft copolymerization:
stirring at room temperature at the rotating speed of 300r/min by using a stirrer, adding potassium persulfate and N, N-methylene-bisacrylamide while stirring for mixing reaction, and stirring for 40 min; wherein the mass ratio of the acrylamide to the potassium persulfate to the N, N-methylene-bisacrylamide is 300:1: 1.7.
S3, formation of highly transparent sodium chlorite hydrogel:
pouring the solution with uniform reaction into a mould, and heating in a water bath kettle at 70 ℃ for 0.5-1 hour to obtain the high-transparency hydrogel. And then putting the gel into a 110 ℃ oven for drying, putting the gel into a sodium chlorite solution with the mass concentration of 10%, and waiting for the gel to absorb and swell in a dark place to form the high-transparency sodium chlorite hydrogel.
FIGS. 1-3 show the results of UV-Vis spectrophotometry of the sodium chlorite hydrogels prepared in examples 1-3, and the light transmittance of the substances was measured in the wavelength range of 300-800 nm. When light passes through a substance to be measured, the degree of absorption of light by the substance varies depending on the wavelength of the light. Therefore, the absorption spectrum of the measured substance is obtained by measuring the light transmittance of the substance at different wavelengths and drawing a relation graph of the light transmittance and the wavelengths.
When the incident light intensity I0At a certain time, the medium absorbs the intensity of light IaThe greater the intensity of transmitted light ItThe smaller. By means of It/I0Representing the ability of light to pass through the medium, called light transmittance, denoted by T, i.e. T ═ It/I0. The light transmittance is a percentage and ranges from 0 to 100 percent. If the light is totally absorbed by the medium ItT is 0. And if the light is totally transmitted, then It=I0For example, a light transmittance of 90% means that 90% of light can be transmitted by the substance. As can be seen from the figure, the obtained sodium chlorite hydrogel is in the visible light range of 400-760nmThe sodium chlorite hydrogel has good transparency, has poor transparency to ultraviolet light with the wavelength of less than 400nm, and particularly has nearly zero transmittance to ultraviolet light with the wavelength of less than 350nm, which shows that the absorption effect to the ultraviolet light is very good at the moment, and the obtained sodium chlorite hydrogel can be used for generating chlorine dioxide gas under the irradiation of the ultraviolet light with the wavelength of less than 350 nm.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.

Claims (7)

1. A method for preparing a sodium chlorite hydrogel is characterized by comprising the following steps: the method comprises the following steps:
s1, preparation of hydrogel solution: preparing an acrylamide aqueous solution with the concentration of 3-5 mol/L;
s2, graft copolymerization: adding potassium persulfate and N, N-methylene-bisacrylamide to the obtained acrylamide aqueous solution at the temperature of 10-30 ℃ while stirring for mixed reaction, and stirring for 30-40min, wherein the mass ratio of acrylamide to potassium persulfate to N, N-methylene-bisacrylamide is (300-) -400): 1: (1.7-2);
s3, formation of sodium chlorite hydrogel: and heating the reacted solution at 50-70 ℃ for 0.5-1.5 hours to obtain hydrogel, drying the hydrogel, putting the dried hydrogel into a sodium chlorite solution, and waiting for the gel to absorb and swell in a light-tight environment to form the sodium chlorite hydrogel.
2. The method for preparing a sodium chlorite hydrogel according to claim 1, wherein the method comprises the following steps: in step S2, the stirring speed is 300-500 r/min.
3. The method for preparing a sodium chlorite hydrogel according to claim 1, wherein the method comprises the following steps: in step S3, the drying temperature is 100-120 ℃.
4. The method for preparing a sodium chlorite hydrogel according to claim 1, wherein the method comprises the following steps: in step S3, the mass concentration of the sodium chlorite solution is 10-30%.
5. The method for preparing a sodium chlorite hydrogel according to claim 1, wherein the method comprises the following steps: in step S3, the sodium chlorite solution contains an activator.
6. The method for preparing a sodium chlorite hydrogel according to claim 5, wherein: the activator is one or more of sodium dihydrogen phosphate, oxalic acid, citric acid, tartaric acid and hydrogen chlorite.
7. The method for preparing a sodium chlorite hydrogel according to claim 6, wherein the method comprises the following steps: the activating agent is sodium dihydrogen phosphate, and the mass ratio of the sodium chlorite to the sodium dihydrogen phosphate is (145-: 1.
CN202011193572.8A 2020-10-30 2020-10-30 Preparation method of sodium chlorite hydrogel Pending CN112210092A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116217795A (en) * 2023-02-21 2023-06-06 台州市黄岩鸿瀚工贸有限公司 Gel for sterilizing and disinfecting air, removing aldehyde and removing peculiar smell and preparation method thereof

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Publication number Priority date Publication date Assignee Title
US20100086493A1 (en) * 2007-03-15 2010-04-08 Taiko Pharmaceutical Co., Ltd. Pure chlorine dioxide solution, and gel-like composition and foaming composition each comprising the same
CN103931652A (en) * 2014-05-06 2014-07-23 涂远曦 Controllable and visual chlorine dioxide slow-release gel and preparation method thereof
CN107236079A (en) * 2017-07-13 2017-10-10 山东大学 A kind of preparation method of chelating type acrylamide gel
CN111387204A (en) * 2020-04-15 2020-07-10 广东爱锝医药技术研究院有限公司 Color-changeable bactericidal gel

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100086493A1 (en) * 2007-03-15 2010-04-08 Taiko Pharmaceutical Co., Ltd. Pure chlorine dioxide solution, and gel-like composition and foaming composition each comprising the same
CN103583566A (en) * 2007-03-15 2014-02-19 大幸药品株式会社 Pure chlorine dioxide solution, and gel-like composition and foaming composition each comprising the same
CN103931652A (en) * 2014-05-06 2014-07-23 涂远曦 Controllable and visual chlorine dioxide slow-release gel and preparation method thereof
CN107236079A (en) * 2017-07-13 2017-10-10 山东大学 A kind of preparation method of chelating type acrylamide gel
CN111387204A (en) * 2020-04-15 2020-07-10 广东爱锝医药技术研究院有限公司 Color-changeable bactericidal gel

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116217795A (en) * 2023-02-21 2023-06-06 台州市黄岩鸿瀚工贸有限公司 Gel for sterilizing and disinfecting air, removing aldehyde and removing peculiar smell and preparation method thereof

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