CN115553300A - Broad-spectrum biocidal stripping agent and preparation method and application thereof - Google Patents
Broad-spectrum biocidal stripping agent and preparation method and application thereof Download PDFInfo
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- CN115553300A CN115553300A CN202111457874.6A CN202111457874A CN115553300A CN 115553300 A CN115553300 A CN 115553300A CN 202111457874 A CN202111457874 A CN 202111457874A CN 115553300 A CN115553300 A CN 115553300A
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- stripping agent
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- biocidal
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/02—Sulfur; Selenium; Tellurium; Compounds thereof
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Agronomy & Crop Science (AREA)
- General Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of water treatment agents, in particular to a broad-spectrum biocidal stripping agent and a preparation method thereof, wherein the broad-spectrum biocidal stripping agent comprises the following raw materials: sulfamic acid, inorganic compounds, bromine, chlorine and pure water. The invention can obtain a high-efficiency broad-spectrum bromine biocidal stripping agent by controlling the components and the proportion, is nontoxic to human bodies, is used for sterilizing and killing algae in a water system, can kill microorganisms, can decompose residual cells in a scaling manner, and kills fungal spores and viruses; by controlling the process steps and conditions, particularly the dropping temperature, the dropping time and the heat preservation time of the bromine and the chlorine, the stability of the biocidal stripping agent is effectively improved, the shelf life of the biocidal stripping agent can be prolonged to 1 year to one and a half years, and the standard requirements of chemical products are met.
Description
Technical Field
The invention relates to the technical field of water treatment agents, in particular to an IPC classification number A01N59/00, and more particularly relates to a broad-spectrum biocidal stripping agent and a preparation method and application thereof.
Background
The circulating cooling water is one of the main means for protecting environment and saving water resources, the oxidizing bactericide used for domestic circulating water treatment is mainly a chlorine product at present, and the product is easy to dissociate in alkaline or high-PH water to generate hypochlorous acid ions with extremely poor inactive biocidal power. And the products have the defects of high danger (such as chlorine), poor stability (floating water), large dust (TCCA) and the like. From the characteristics of the current bactericide market, the development of the bactericide for cooling water, which has the advantages of broad spectrum, high efficiency, high cost performance and environmental friendliness, is a necessary trend for future development, and bromine replaces chlorine to be a bactericide development direction, and the development of the bactericide is far away from chlorine and is transferred to a safer substitute.
Patent CN201210000710.5 discloses a preparation method of organic bromine biocide, which comprises the following steps: (1) Adding inorganic salts containing bromine and long-chain fatty alcohol carboxylic acid amide into a four-necked bottle, adding 20-50g of deionized water into the bottle, and cooling in water bath; (2) Dropwise adding sodium hypochlorite, controlling the temperature at 0-50 ℃, and then preserving the heat at the room temperature of 30-40 ℃ for 2-4 hours; and (3) obtaining a light yellow transparent liquid, namely the product. The product has the characteristics of small dosage, good biocidal effect and moderate price, so the product is very applied to the treatment of papermaking white water and oilfield reinjection water, and has large market capacity, but the biocide still has the problems of instability and short storage time.
Disclosure of Invention
In view of the above-mentioned technical problems, a first aspect of the present invention provides a broad spectrum biocidal stripping agent comprising the following raw materials: sulfamic acid, inorganic compounds, bromine, chlorine and pure water.
In some embodiments, the biocidal stripping agent comprises, in weight percent, the following raw materials: 10-20% of sulfamic acid, 20-35% of inorganic compound, 3-10% of bromine, 3-10% of chlorine and the balance of pure water.
Preferably, the biocidal stripping agent comprises the following raw materials in percentage by weight: 10-15% of sulfamic acid, 30-35% of inorganic compound, 8-10% of bromine, 4-6% of chlorine and the balance of pure water.
More preferably, the biocidal stripping agent comprises the following raw materials in percentage by weight: 12% of sulfamic acid, 32% of inorganic compound, 9% of bromine, 5% of chlorine and the balance of pure water.
In some embodiments, the inorganic compound comprises a base.
In some embodiments, the base is 50% sodium hydroxide.
Wherein 50% sodium hydroxide refers to 50% sodium hydroxide aqueous solution by mass.
The second aspect of the invention provides a preparation method of a broad-spectrum biocidal stripping agent, which at least comprises the following steps:
(1) Dividing inorganic compounds into inorganic compounds a, inorganic compounds b and inorganic compounds c, adding pure water and sulfamic acid into a reaction kettle, dropwise adding the inorganic compounds a, and stirring to obtain a bottom material;
(2) Adding an inorganic compound b into the base material, beginning to dropwise add bromine after 1-3min, and preserving heat after dropwise adding to obtain a mixture A;
(3) And (3) dropwise adding the inorganic compound c into the mixture A, introducing chlorine gas after 1-3min, and discharging after heat preservation to obtain the catalyst.
In some embodiments, the inorganic compound a is 50 to 54wt% of the total amount of inorganic compounds, the inorganic compound b is 20 to 22wt% of the total amount of inorganic compounds, and the balance is inorganic compound c.
Preferably, the inorganic compound a is 52wt% of the total amount of the inorganic compounds, the inorganic compound b is 21.6wt% of the total amount of the inorganic compounds, and the balance is the inorganic compound c.
Preferably, the preparation method of the broad-spectrum biocidal stripping agent at least comprises the following steps:
(1) Adding pure water and sulfamic acid into a reaction kettle, slowly dripping the inorganic compound a, and uniformly stirring to obtain a bottom material;
(2) Adding the inorganic compound b into the base material, beginning to dropwise add bromine after 2min, and preserving heat after dropwise addition to obtain a mixture A;
(3) And (3) dropwise adding the inorganic compound c into the mixture A, introducing chlorine gas after 2min, and discharging after heat preservation to obtain the catalyst.
In some embodiments, the dropping temperature in step (1) is less than 70 ℃.
In some embodiments, the dropping temperature in the step (2) is 25 to 35 ℃ and the dropping time is 0.5 to 1.5 hours.
Preferably, the dropping temperature in the step (2) is 30 ℃, and the dropping time is 1h.
In some embodiments, the incubation temperature in step (2) is 25-35 ℃.
Preferably, the incubation temperature in step (2) is 30 ℃.
In some embodiments, the incubation time in step (2) is 0.5 to 1.5h.
Preferably, the holding time in the step (2) is 1h.
In some embodiments, the temperature of the incubation in step (3) is 20-25 ℃ and the incubation time is 0.5-1.5h.
In some embodiments, the inorganic compound is added prior to the addition of bromine in step (2), and the inorganic compound is added prior to the addition of chlorine in step (3).
In some embodiments, the pH after the end of the bromine addition in step (2) is greater than 13, and the pH after the chlorine addition in step (3) is greater than 13.
The applicant finds in the research process that by controlling the components and the proportion, the bromine biocidal stripping agent with high efficiency and broad spectrum can be obtained, is non-toxic to human bodies, can be used for killing bacteria and algae in a water system, can kill microorganisms, can decompose residual cells in a scaling manner, and can kill fungal spores, viruses and the like, and the sterilization effect is not influenced by the change of pH when the agent is used. However, the applicant finds that although the sterilization rate of the prepared biocidal stripping agent is high, the stability of the product is poor and can only be kept for about 6 months, the applicant finds that the stability of the biocidal stripping agent is effectively improved by controlling the process steps and conditions, particularly the dropping temperature, the dropping time and the heat preservation time of bromine and chlorine, so that the shelf life of the biocidal stripping agent can be prolonged to 1 year to one year and a half, and the biocidal stripping agent meets the standard requirements of chemical products.
In a third aspect the invention provides the use of a broad spectrum biocidal stripping agent for the disinfection of circulating cooling water.
Has the advantages that:
(1) The invention can obtain a high-efficiency broad-spectrum bromine biocidal stripping agent by controlling the components and the proportion, is nontoxic to human bodies, is used for sterilizing and killing algae in a water system, can kill microorganisms, can decompose residual cells in a scaling manner, and kills fungal spores and viruses;
(2) The biocidal stripping agent disclosed by the invention has no influence on the sterilization effect due to the change of PH when in use, and is suitable for the treatment of alkaline water;
(3) According to the invention, by controlling the process steps and conditions, especially the dropping temperature, the dropping time and the heat preservation time of bromine and chlorine, the stability of the biocidal stripping agent is effectively improved, so that the quality guarantee period of the biocidal stripping agent can be prolonged to 1 year to one and a half years, and the standard requirements of chemical products are met;
(4) According to the invention, the pH value after bromine and chlorine are added is controlled to be more than 13, so that the escape of bromine and chlorine is avoided, the content of effective components in the product is ensured, the sterilization effect is further ensured, and the environmental pollution is also avoided.
Detailed Description
Example 1
One aspect of this embodiment provides a broad-spectrum biocidal stripping agent, which comprises the following raw materials in percentage by weight: 12% of sulfamic acid, 32% of alkaline substances, 9% of bromine, 5% of chlorine and the balance of pure water.
The alkali substance is sodium hydroxide with the mass concentration of 50%.
Another aspect of this embodiment provides a method for preparing a broad-spectrum biocidal stripping agent, comprising the following steps:
(1) Dividing inorganic compounds into inorganic compounds a, inorganic compounds b and inorganic compounds c, adding pure water and sulfamic acid into a reaction kettle, slowly dripping the inorganic compounds a at the temperature of 65 ℃, and uniformly stirring to obtain a bottom material;
(2) Adding the inorganic compound b into the base material, beginning to dropwise add bromine after 2min, and preserving heat after dropwise addition to obtain a mixture A;
(3) And (3) dropwise adding the inorganic compound c into the mixture A, introducing chlorine gas after 2min, and discharging after heat preservation to obtain the catalyst.
The inorganic compound a, the inorganic compound b and the inorganic compound c are all alkaline substances.
The inorganic compound a accounts for 52wt% of the total amount of the alkali substances, the inorganic compound b accounts for 21.6wt% of the total amount of the alkali substances, and the balance of the alkali substances is the inorganic compound c.
In the step (2), the dropping temperature of bromine is controlled to be 30 ℃, the dropping time is controlled to be 1h, the heat preservation temperature is controlled to be 30 ℃, and the heat preservation time is controlled to be 1h.
In the step (2), the alkali substances are dripped before the bromine, and in the step (3), the alkali substances are dripped before the chlorine.
The temperature for heat preservation in the step (3) is 23 ℃, and the time for heat preservation is 1h.
Example 2
One aspect of this example provides a broad-spectrum biocidal stripping agent and a method for preparing the same, and the specific embodiment is the same as example 1, except that the dropping temperature in step (2) is 40 ℃.
Example 3
One aspect of this embodiment provides a broad-spectrum biocidal stripping agent and a method for preparing the same, and the specific embodiment is the same as in example 1, except that the dropping time in step (2) is 2h.
Performance testing
1. Physical Properties
The physical properties of the biocidal stripping agent prepared in example 1 were measured for 5 batches of the production, and the results are shown in table 1.
TABLE 1
2. Energy efficiency evaluation
The energy efficiency evaluation of the biocidal stripping agent in example 1 is carried out according to the GB/T22595-2008 standard, the adding concentration is 20ppm, the biocidal stripping agent is respectively determined for 5 batches of products in production, and the test results are shown in Table 2.
TABLE 2
| Number of | Sterilizing rate/%) |
| Batch one | 99.7 |
| Batch two | 99.9 |
| Batch three | 99.5 |
| Batch four | 99.3 |
| Batch five | 99.5 |
3. Stability of
The biocidal stripping agents prepared in 1-3 were left in a water bath at 55 ℃ for 30 days to observe whether precipitation or turbidity occurred, and the results are reported in Table 3.
TABLE 3
| Number of | Stability of |
| Example 1 | No precipitation and turbidity |
| Example 2 | Has obvious precipitation and turbidity |
| Example 3 | Has slight precipitation and turbidity |
Claims (10)
1. A broad-spectrum biocidal stripping agent is characterized by comprising the following raw materials: sulfamic acid, inorganic compounds, bromine, chlorine and pure water.
2. The broad-spectrum biocidal stripping agent according to claim 1, comprising the following raw materials in percentage by weight: 10-20% of sulfamic acid, 20-35% of inorganic compound, 3-10% of bromine, 3-10% of chlorine and the balance of pure water.
3. The broad-spectrum biocidal stripping agent according to claim 1, wherein said inorganic compound comprises a base.
4. The broad spectrum biocidal stripping agent of claim 3, wherein said base is 50% sodium hydroxide.
5. A method for preparing the broad-spectrum biocidal stripping agent according to any one of claims 1 to 4, characterized by at least the following steps:
(1) Dividing inorganic compounds into inorganic compounds a, inorganic compounds b and inorganic compounds c, adding pure water and sulfamic acid into a reaction kettle, dropwise adding the inorganic compounds a, and stirring to obtain a bottom material;
(2) Adding an inorganic compound b into the base material, beginning to dropwise add bromine after 1-3min, and preserving heat after dropwise adding to obtain a mixture A;
(3) And (3) dropwise adding the inorganic compound c into the mixture A, introducing chlorine after 1-3min, preserving heat and discharging to obtain the catalyst.
6. The preparation method of the broad-spectrum biocidal stripping agent according to claim 5, wherein the dripping temperature in step (1) is less than 70 ℃.
7. The preparation method of the broad-spectrum biocidal stripping agent according to claim 5, wherein the dripping temperature in the step (2) is 25-35 ℃, and the dripping time is 0.5-1.5h.
8. The method for preparing the broad-spectrum biocidal stripping agent according to claim 7, wherein the temperature of the incubation in step (2) is 25-35 ℃.
9. The preparation method of the broad-spectrum biocidal stripping agent according to claim 7, wherein the temperature for the heat preservation in step (3) is 20-25 ℃, and the time for the heat preservation is 0.5-1.5h.
10. Use of a broad spectrum biocidal stripping agent according to any one of claims 1 to 4 for sterilization of circulating cooling water.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1430894A (en) * | 2002-01-11 | 2003-07-23 | 中国石油天然气集团公司 | Biocide agent coutaining bromine named as powered bromine chlorin |
| CN101010007A (en) * | 2004-09-07 | 2007-08-01 | 雅宝公司 | Concentrated aqueous bromine solutions and their preparation |
| CN102550597A (en) * | 2012-01-04 | 2012-07-11 | 常州市科威精细化工有限公司 | Method for preparing organic brominated biocide |
| CN102771513A (en) * | 2012-07-21 | 2012-11-14 | 辽宁力普工业技术有限公司 | Preparation method of liquid stable bromine bactericide using elemental bromine as bromine source |
| JP2013136609A (en) * | 1999-09-24 | 2013-07-11 | Albemarle Corp | Bactericide application of concentrated aqueous bromine chloride solution |
| CN103734189A (en) * | 2013-11-04 | 2014-04-23 | 乌鲁木齐市科发展精细化工有限公司 | Active bromine liquid oxidizability germicidal algicide and preparation method thereof |
| CN105517959A (en) * | 2013-08-28 | 2016-04-20 | 奥加诺株式会社 | Method for producing stabilized hypobromous acid composition, stabilized hypobromous acid composition, and slime inhibition method for separation membrane |
| JP2016120487A (en) * | 2014-12-25 | 2016-07-07 | オルガノ株式会社 | Method for sterilizing water |
| CN111631228A (en) * | 2020-06-16 | 2020-09-08 | 常州市新未来化工有限公司 | Novel broad-spectrum efficient biocidal stripping agent and preparation method thereof |
-
2021
- 2021-12-02 CN CN202111457874.6A patent/CN115553300A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013136609A (en) * | 1999-09-24 | 2013-07-11 | Albemarle Corp | Bactericide application of concentrated aqueous bromine chloride solution |
| CN1430894A (en) * | 2002-01-11 | 2003-07-23 | 中国石油天然气集团公司 | Biocide agent coutaining bromine named as powered bromine chlorin |
| CN101010007A (en) * | 2004-09-07 | 2007-08-01 | 雅宝公司 | Concentrated aqueous bromine solutions and their preparation |
| CN102550597A (en) * | 2012-01-04 | 2012-07-11 | 常州市科威精细化工有限公司 | Method for preparing organic brominated biocide |
| CN102771513A (en) * | 2012-07-21 | 2012-11-14 | 辽宁力普工业技术有限公司 | Preparation method of liquid stable bromine bactericide using elemental bromine as bromine source |
| CN105517959A (en) * | 2013-08-28 | 2016-04-20 | 奥加诺株式会社 | Method for producing stabilized hypobromous acid composition, stabilized hypobromous acid composition, and slime inhibition method for separation membrane |
| CN103734189A (en) * | 2013-11-04 | 2014-04-23 | 乌鲁木齐市科发展精细化工有限公司 | Active bromine liquid oxidizability germicidal algicide and preparation method thereof |
| JP2016120487A (en) * | 2014-12-25 | 2016-07-07 | オルガノ株式会社 | Method for sterilizing water |
| CN111631228A (en) * | 2020-06-16 | 2020-09-08 | 常州市新未来化工有限公司 | Novel broad-spectrum efficient biocidal stripping agent and preparation method thereof |
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