CN115072667B - Preparation method of reactive chlorine dioxide solid preparation using sodium chlorate as raw material - Google Patents
Preparation method of reactive chlorine dioxide solid preparation using sodium chlorate as raw material Download PDFInfo
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- CN115072667B CN115072667B CN202210672707.1A CN202210672707A CN115072667B CN 115072667 B CN115072667 B CN 115072667B CN 202210672707 A CN202210672707 A CN 202210672707A CN 115072667 B CN115072667 B CN 115072667B
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- chlorine dioxide
- sodium
- solid preparation
- preparation
- reaction
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- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000004155 Chlorine dioxide Substances 0.000 title claims abstract description 34
- 235000019398 chlorine dioxide Nutrition 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000007787 solid Substances 0.000 title claims abstract description 28
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000002994 raw material Substances 0.000 title claims abstract description 10
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 32
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229940045872 sodium percarbonate Drugs 0.000 claims abstract description 18
- 229940063656 aluminum chloride Drugs 0.000 claims abstract description 16
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 15
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 15
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 15
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 15
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims abstract description 14
- 229910000342 sodium bisulfate Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 229940100996 sodium bisulfate Drugs 0.000 claims abstract description 4
- 229940080281 sodium chlorate Drugs 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 6
- 238000009472 formulation Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 8
- 239000001569 carbon dioxide Substances 0.000 abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000460 chlorine Substances 0.000 abstract description 2
- 229910052801 chlorine Inorganic materials 0.000 abstract description 2
- -1 Aluminum ions Chemical class 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- 239000012190 activator Substances 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 229910001437 manganese ion Inorganic materials 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 15
- 239000000843 powder Substances 0.000 description 15
- 239000000243 solution Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 description 4
- 229960002218 sodium chlorite Drugs 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 241000700605 Viruses Species 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- VGVRPFIJEJYOFN-UHFFFAOYSA-N 2,3,4,6-tetrachlorophenol Chemical class OC1=C(Cl)C=C(Cl)C(Cl)=C1Cl VGVRPFIJEJYOFN-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/02—Oxides of chlorine
- C01B11/022—Chlorine dioxide (ClO2)
- C01B11/023—Preparation from chlorites or chlorates
- C01B11/026—Preparation from chlorites or chlorates from chlorate ions in the presence of a peroxidic compound, e.g. hydrogen peroxide, ozone, peroxysulfates
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Zoology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Wood Science & Technology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Detergent Compositions (AREA)
Abstract
The invention relates to a preparation method of a reactive chlorine dioxide solid preparation taking sodium chlorate as a raw material. The technical scheme of the invention comprises the following components: sodium chlorate, sodium bisulfate, sodium percarbonate, aluminum chloride and manganese sulfate. The mass ratio of each component is 3-5: 55-65: 1.5 to 2.5:0.05 to 0.1:0.05 to 0.1. The sodium percarbonate of the invention can be dissolved in acid solution to generate carbon dioxide, and can be used as protective gas of chlorine dioxide, so that the absorption of the chlorine dioxide is carried out stably; sodium percarbonate can be used as a disintegrating agent, and generated carbon dioxide gas can enable the solid preparation to be rapidly dissolved, so that the reaction rate is quickened. Aluminum ions and manganese ions formed by dissolving aluminum chloride and manganese sulfate in water can be used as catalysts, so that the time required by the reaction is reduced, and the synergistic effect is achieved; the chloride ion of aluminum chloride is used as an activator of the reaction, and can promote the speed of starting the reaction. The chlorine dioxide prepared by the reaction is high-purity gas, and the chlorine content is very small.
Description
Technical Field
The invention belongs to the field of disinfectant preparation. In particular to a preparation method of a reactive chlorine dioxide solid preparation taking sodium chlorate as a raw material.
Background
Chlorine dioxide has extremely strong oxidizing property, and researches show that the oxidizing capability is 2.7 times that of chlorine. Chlorine dioxide can react with many organic matters and inorganic matters rapidly, for example, harmful iron, manganese, nickel and other heavy metal ions can be converted into harmless states, phenols in sewage can be converted into chlorophenols by generating phenol free radicals to purify the sewage, and the chlorine dioxide can react with toxic naphthalene, aniline, formaldehyde and the like to be converted into harmless matters, and can kill bacteria, viruses, putrescence organisms and other internal enzymes through cell walls to further kill the bacteria, viruses, putrescence organisms and the like, thereby having a disinfection effect. The world health organization therefore authenticates chlorine dioxide as a class A1 disinfectant.
The chlorine dioxide has strong oxidizing property and the equal killing rate to various viruses can reach 100 percent. Chlorine dioxide and chlorine dioxide can maintain a constant sterilizing effect in a wider pH range, and the duration is long, so that the method is very suitable for household use.
Chlorine dioxide is active in nature and difficult to preserve, and is usually prepared into a stable solution or preserved in a solid preparation mode. For daily life, solid preparations which can be sterilized for a long time are obviously more convenient to use. Chlorine dioxide solid formulations are generally classified as adsorptive and reactive, and the reactive solid formulation material is typically sodium chlorate or sodium chlorite. Sodium chlorite is used as a reaction raw material in the market at present, but the price of sodium chlorite is more expensive than that of sodium chlorate, and the use cost is higher. In addition, sodium chlorite is difficult to preserve in a moist environment, which limits the environment in which such solid formulations can be used.
Disclosure of Invention
The invention aims to solve the problems of providing a preparation method of a novel chlorine dioxide solid preparation, which has low preparation cost and convenient raw material preservation, and the produced chlorine dioxide is high-purity gas.
The invention solves the problems by the following technical proposal:
a reactive chlorine dioxide solid preparation using sodium chlorate as raw material comprises sodium chlorate, sodium bisulfate, sodium percarbonate, aluminum chloride and manganese sulfate.
The mass ratio of the sodium chlorate to the sodium bisulfate to the sodium percarbonate to the aluminum chloride to the manganese sulfate is 3-5: 55-65: 1.5 to 2.5:0.05 to 0.1:0.05 to 0.1.
The mass ratio of the aluminum chloride to the manganese sulfate is preferably 1:2.
the preparation method of the reactive chlorine dioxide solid preparation taking sodium chlorate as a raw material comprises the following operation steps: mixing sodium chlorate, sodium bisulfate, sodium percarbonate, aluminum chloride and manganese sulfate according to the mass ratio to obtain a solid preparation, then adding water for dilution, and standing to release chlorine dioxide.
The raw materials are all powder after drying treatment.
The mass volume ratio of the solid preparation to water is 60-70 g: 400-600 mL, preferably 60-70 g:500mL.
The method of the invention has the following advantages:
the method for preparing chlorine dioxide by adopting sodium chlorate has the advantages of low cost, more stable property of sodium chlorate and easy preservation. Sodium percarbonate is used as a reducing agent, almost no byproducts are generated, the prepared chlorine dioxide is high-purity, and the sodium percarbonate is dissolved in sodium bisulfate solution to generate carbon dioxide as a shielding gas; the carbon dioxide generated by the sodium percarbonate has a disintegrating effect, can help the solid preparation to be dissolved rapidly, and reduces the waiting time of the reaction for generating the chlorine dioxide.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
Preparing a solid preparation: 4g of sodium chlorate, 65g of sodium bisulfate, 1.8g of sodium percarbonate, 0.05g of aluminum chloride and 0.1g of manganese sulfate are taken, ground into powder, uniformly mixed and placed into a constant temperature drying oven for drying at 60 ℃ for 6 hours.
Adding 500mL distilled water at 25deg.C into the above powder, dissolving completely, and standing for 1 hr.
The final detection solution of the scheme contains 175.3mg/L of chlorine dioxide.
Example 2
Preparing a solid preparation: 5g of sodium chlorate, 70g of sodium bisulfate, 2.5g of sodium percarbonate, 0.1g of aluminum chloride and 0.1g of manganese sulfate are taken, ground into powder, uniformly mixed and placed into a constant temperature drying oven for drying at 60 ℃ for 6 hours.
Adding 500mL distilled water at 25deg.C into the above powder, dissolving completely, and standing for 1 hr.
The final detection solution of the scheme has 253.1mg/L of chlorine dioxide content.
Example 3
Preparing a solid preparation: 3g of sodium chlorate, 60g of sodium bisulfate, 1.7g of sodium percarbonate, 0.1g of aluminum chloride and 0.05g of manganese sulfate are taken, ground into powder, uniformly mixed and placed into a constant temperature drying oven for drying at 60 ℃ for 6 hours.
Adding 500mL distilled water at 25deg.C into the above powder, dissolving completely, and standing for 1 hr.
The chlorine dioxide content in the final detection solution of the scheme is 115.6mg/L.
Comparative example 1
Preparing a solid preparation: taking 4g of sodium chlorate, 65g of sodium bisulfate, 1.8g of sodium percarbonate, 0g of aluminum chloride and 0g of manganese sulfate, grinding into powder, uniformly mixing, and drying in a constant-temperature drying oven at 60 ℃ for 6h.
Adding 500mL distilled water at 25deg.C into the above powder, dissolving completely, and standing for 1 hr.
The final detection solution of the scheme has the chlorine dioxide content of 84.4mg/L.
Comparative example 2
Preparing a solid preparation: 4g of sodium chlorate, 65g of sodium bisulfate, 1.8g of sodium percarbonate, 0.1g of aluminum chloride and 0g of manganese sulfate are taken, ground into powder, uniformly mixed and placed into a constant temperature drying oven for drying at 60 ℃ for 6 hours.
Adding 500mL distilled water at 25deg.C into the above powder, dissolving completely, and standing for 1 hr.
The final detection solution of the scheme has the chlorine dioxide content of 159.2mg/L.
Comparative example 3
Preparing a solid preparation: 3g of sodium chlorate, 60g of sodium bisulfate, 1.7g of sodium percarbonate, 0g of aluminum chloride and 0g of manganese sulfate are taken, ground into powder, uniformly mixed and placed into a constant-temperature drying oven for drying at 60 ℃ for 6 hours.
Adding 500mL distilled water at 25deg.C into the above powder, dissolving completely, and standing for 1 hr.
The final detection solution of the scheme has the chlorine dioxide content of 53.9mg/L.
Comparative example 4
Preparing a solid preparation: 3g of sodium chlorate, 60g of sodium bisulfate, 1.7g of sodium percarbonate, 0g of aluminum chloride and 0.1g of manganese sulfate are taken, ground into powder, uniformly mixed and placed into a constant temperature drying oven for drying at 60 ℃ for 6 hours.
Adding 500mL distilled water at 25deg.C into the above powder, dissolving completely, and standing for 1 hr.
The final detection solution of the scheme has the chlorine dioxide content of 98.4mg/L.
Claims (4)
1. A reactive chlorine dioxide solid preparation is characterized in that the reaction raw materials comprise 5g of sodium chlorate, 70g of sodium bisulfate, 0.1g of aluminum chloride, 0.1g of manganese sulfate and 2.5g of sodium percarbonate.
2. A method of using the chlorine dioxide solid formulation of claim 1, comprising the steps of: mixing sodium chlorate, sodium bisulfate, sodium percarbonate, aluminum chloride and manganese sulfate according to mass to obtain a solid preparation, then adding water for dilution, and standing to release chlorine dioxide.
3. The method of use according to claim 2, wherein: the mass volume ratio of the solid preparation to water is 60-70 g: 400-600 mL.
4. The use method according to claim 2, characterized in that the mass-to-volume ratio of the solid preparation to water is 60-70 g:500mL.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210672707.1A CN115072667B (en) | 2022-06-14 | 2022-06-14 | Preparation method of reactive chlorine dioxide solid preparation using sodium chlorate as raw material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210672707.1A CN115072667B (en) | 2022-06-14 | 2022-06-14 | Preparation method of reactive chlorine dioxide solid preparation using sodium chlorate as raw material |
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| Publication Number | Publication Date |
|---|---|
| CN115072667A CN115072667A (en) | 2022-09-20 |
| CN115072667B true CN115072667B (en) | 2024-01-16 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105692559A (en) * | 2016-01-26 | 2016-06-22 | 张旭 | Preparation method of chlorine dioxide |
| CN110558318A (en) * | 2019-09-19 | 2019-12-13 | 河南省化工研究所有限责任公司 | Stable chlorine dioxide effervescent agent and preparation method thereof |
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2022
- 2022-06-14 CN CN202210672707.1A patent/CN115072667B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105692559A (en) * | 2016-01-26 | 2016-06-22 | 张旭 | Preparation method of chlorine dioxide |
| CN110558318A (en) * | 2019-09-19 | 2019-12-13 | 河南省化工研究所有限责任公司 | Stable chlorine dioxide effervescent agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 天津市化工研究院技术情报室."关于二氧化氯生产路线的几点看法".天津化工.1977,(第1期),第41-50页. * |
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| CN115072667A (en) | 2022-09-20 |
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