CN111328806A - Double-linear alkyl quaternary ammonium salt complex iodine bactericide - Google Patents
Double-linear alkyl quaternary ammonium salt complex iodine bactericide Download PDFInfo
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- CN111328806A CN111328806A CN202010154034.1A CN202010154034A CN111328806A CN 111328806 A CN111328806 A CN 111328806A CN 202010154034 A CN202010154034 A CN 202010154034A CN 111328806 A CN111328806 A CN 111328806A
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- quaternary ammonium
- ammonium salt
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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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
- A01N33/12—Quaternary ammonium compounds
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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
- A01N59/12—Iodine, e.g. iodophors; Compounds thereof
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- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
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Abstract
The invention relates to the technical field of bactericide preparation, and discloses a double straight-chain alkyl quaternary ammonium salt complex iodine bactericide, which comprises the following steps: (1) dissolving the double-linear alkyl quaternary ammonium salt and an iodine simple substance in an ethanol solution, reacting at 40-60 ℃ for 3-7 h, and performing pressure distillation to obtain double-linear alkyl quaternary ammonium salt complex iodine; (2) mixing and stirring the double-linear alkyl quaternary ammonium salt complex iodine, the nonionic surfactant and the acid to obtain the double-linear alkyl quaternary ammonium salt complex iodine bactericide. The invention utilizes the iodine simple substance (I) which is rich in electrons and has larger volume2) The outer layer electron cloud and the nitrogen positive ion in the quaternary ammonium salt with a proper structure can form the electron transmission function of an electron donor-acceptor, and double straight chain quaternary ammonium salt complex iodine, gramThe defects that the traditional single iodine bactericide is difficult to dissolve in water, unstable to air and easy to sublimate and volatilize at a higher temperature are overcome; the compound technology is utilized to greatly improve the sterilization effect of the double straight chain quaternary ammonium salt complex iodine bactericide and reduce the dosage.
Description
Technical Field
The invention relates to the technical field of bactericide preparation, in particular to a double straight-chain alkyl quaternary ammonium salt complex iodine bactericide.
Background
With the development of animal husbandry and aquaculture, the demand for bactericides is increasing day by day. The common quaternary ammonium salt bactericide has no bactericidal effect on fungi, tubercle bacillus and the like, and belongs to low-efficiency bactericides. And the quaternary ammonium salt bactericide is easily influenced by external conditions such as temperature, concentration and the like. And the bacteria can easily generate drug resistance to the bacteria, so that the dosage is increased, and the pollution of water and the like is directly increased.
Iodine has a good sterilization effect and a high sterilization speed, but iodine simple substances are not easy to dissolve in water, simple iodine is easy to sublimate, is extremely unstable at room temperature, and has a strong yellow-dyeing property, so that the use of the iodine simple substances is limited, and the research of the composite bactericide becomes a current hotspot in order to overcome the characteristics of a single bactericide.
Chinese patent CN106259442A provides a preparation method of an iodine-containing compound bactericide, which is used in the field of veterinary sterilization. The main components of the disinfectant are 0.1 to 5 percent of iodine, 0 to 3 percent of potassium iodide, 0.1 to 40 percent of alkyl dimethyl ethyl benzyl ammonium chloride, 0 to 40 percent of quaternary ammonium salt bactericide, 0.1 to 25 percent of guanidine bactericide, 0.5 to 20 percent of acidity regulator and the balance of water, and the proportion of each component is 100 percent. The disadvantages are: a large amount of KI is added to promote the dissolution of iodine simple substances, but the KI has antagonistic action on the quaternary ammonium salt bactericide.
Chinese patent CN104604934A provides a novel compound iodine bactericide, a preparation method and application thereof, which are used for livestock sterilization and aquatic product field sterilization. The main components of the iodine-free iodine-. It has the following disadvantages: the reaction temperature is 80 ℃ at most, and the iodine simple substance is easy to sublimate.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a double straight-chain alkyl quaternary ammonium salt complex iodine bactericide, which solves the problems in the background art.
(II) technical scheme
The invention provides the following technical scheme: a double straight-chain alkyl quaternary ammonium salt complex iodine bactericide is characterized by being prepared by the following steps:
(1) dissolving a double straight-chain alkyl quaternary ammonium salt and an iodine simple substance in a certain mass ratio in an ethanol solution with a certain volume;
(2) heating the mixed solution in the step 1, and reacting for 3-7 h at 40-60 ℃;
(3) after the reaction is finished, carrying out reduced pressure distillation to obtain viscous liquid;
(4) mixing and stirring the double-linear alkyl quaternary ammonium salt complex iodine, the nonionic surfactant and the acid to obtain the double-linear alkyl quaternary ammonium salt complex iodine bactericide.
Preferably, the quaternary ammonium salt of di-linear alkyl is selected from one or a mixture of more than two of the following compounds: didecyl dimethyl ammonium chloride, dioctyl alkyl dimethyl ammonium chloride and didodecyl dimethyl ammonium chloride.
Preferably, the nonionic surfactant is selected from at least one or a mixture of two or more of the following compounds: AEO-7, AEO-9, polyethylene glycol 600/800/1000, lauryl polyoxyethylene ether and TX-10.
Preferably, the acid is selected from at least one of the following compounds: hydrochloric acid, sulfuric acid, phosphoric acid.
(III) advantageous effects
Compared with the prior art, the invention provides the double straight-chain alkyl quaternary ammonium salt complex iodine bactericide which has the following beneficial effects:
1. the prepared di-linear alkyl quaternary ammonium salt complex iodine bactericide has low requirement on reaction conditions, effectively eliminates antagonism, has easily-reached reaction temperature, can effectively avoid elemental iodine sublimation, is easy to control reaction time and pressurized distillation time, has mutual synergy and synergism of iodine and di-linear alkyl quaternary ammonium salt, can realize quick and efficient sterilization, can achieve better sterilization effect at low dosage, and can reduce use frequency.
2. The invention can be used in the field of aquaculture sterilization and has broad-spectrum sterilization.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments 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.
The first embodiment is as follows:
dissolving the double straight chain quaternary ammonium salt and iodine in a mass ratio of 10:0.3 in 100mL of ethanol solution, reacting for 5 hours in a water bath at 50 ℃, and distilling under reduced pressure after the reaction is finished to obtain a reddish brown viscous liquid. Taking 10 parts of product, 10 parts of nonionic surfactant, 0.5 part of acid and the balance of deionized water according to 100 parts by mass, and fully and uniformly stirring to obtain a reddish brown liquid.
Example two:
dissolving the double straight-chain alkyl quaternary ammonium salt and iodine in a mass ratio of 10:0.6 into 100mL of ethanol solution, reacting for 5 hours in a water bath at 50 ℃, and distilling under reduced pressure after the reaction is finished to obtain a reddish brown viscous liquid. Taking 10 parts of product, 10 parts of nonionic surfactant, 0.5 part of acid and the balance of deionized water according to 100 parts by mass, and fully and uniformly stirring to obtain a reddish brown liquid.
Example three:
dissolving the double straight-chain alkyl quaternary ammonium salt and iodine in a mass ratio of 10:0.9 into 100mL of ethanol solution, reacting for 5 hours in a water bath at 50 ℃, and distilling under reduced pressure after the reaction is finished to obtain a reddish brown viscous liquid. Taking 10 parts of product, 10 parts of nonionic surfactant, 0.5 part of acid and the balance of deionized water according to 100 parts by mass, and fully and uniformly stirring to obtain a reddish brown liquid.
Example four:
dissolving the double straight-chain alkyl quaternary ammonium salt and iodine in a mass ratio of 10:1.2 in 100mL of ethanol solution, reacting for 5 hours in a water bath at 50 ℃, and distilling under reduced pressure after the reaction is finished to obtain a reddish brown viscous liquid. Taking 10 parts of product, 10 parts of nonionic surfactant, 0.5 part of acid and the balance of deionized water according to 100 parts by mass, and fully and uniformly stirring to obtain a reddish brown liquid.
Example five:
dissolving the double straight-chain alkyl quaternary ammonium salt and iodine in a mass ratio of 10:1.5 in 100mL of ethanol solution, reacting for 5 hours in a water bath at 50 ℃, and distilling under reduced pressure after the reaction is finished to obtain a reddish brown viscous liquid. Taking 10 parts of product, 10 parts of nonionic surfactant, 0.5 part of acid and the balance of deionized water according to 100 parts by mass, and fully and uniformly stirring to obtain a reddish brown liquid.
The mass ratio of the di-linear alkyl quaternary ammonium salt to the iodine is preferably 10: 1.2.
The best selection obtained in the example is subjected to a sterilization experiment, so that the sterilization test result proves that the best selection has broad-spectrum sterilization, and the sterilization result is shown in tables 1 and 2.
1) Strains used in the experiments: escherichia coli and Staphylococcus aureus.
2) The inspection basis and method are as follows: sterilization specification (2002 edition) 2.1.8.4 minimum inhibitory concentration determination experiment (nutrient broth dilution method).
3) Test results
The product is diluted according to the ratio of 1:1000 to carry out sterilization experiments on escherichia coli and staphylococcus aureus.
TABLE 1 Sterilization Effect of Escherichia coli
TABLE 2 Bactericidal Effect of Staphylococcus aureus
The invention has the beneficial effects that: the prepared di-linear alkyl quaternary ammonium salt complex iodine bactericide has low requirement on reaction conditions, effectively eliminates antagonism, has easily-reached reaction temperature, can effectively avoid elemental iodine sublimation, is easy to control reaction time and pressurized distillation time, has mutual synergy and synergism of iodine and di-linear alkyl quaternary ammonium salt, can realize quick and efficient sterilization, and can achieve better sterilization effect under low dosage, thereby reducing use frequency, being used in the field of aquaculture sterilization, and having broad-spectrum sterilization.
The invention also aims to provide a high-efficiency and stable bactericide, which utilizes the iodine simple substance (I) which is rich in electrons and large in volume2) The outer layer electron cloud and the nitrogen positive ion in the quaternary ammonium salt with a proper structure can form the electron transmission function of an electron donor-acceptor, and double straight chain quaternary ammonium salt complex iodine is selected and synthesized, wherein the double straight chain quaternary ammonium salt complex iodine is used for iodine simple substance (I)2) The complex load overcomes the defects that the traditional single iodine bactericide is difficult to dissolve in water, unstable to air and easy to sublimate and volatilize at a higher temperature, also overcomes the defect of insufficient sterilizing capability of the single quaternary ammonium salt bactericide, and also solves the problem of easy biodegradability of organisms in water after the bactericide is used by introducing the proper double straight-chain alkyl quaternary ammonium salt.
The invention utilizes the compounding technology, and modulates the surface tension of the double straight-chain alkyl quaternary ammonium salt complex iodine aqueous solution by adding proper non-ionic surfactant and the like to improve the contact stability of the double straight-chain alkyl quaternary ammonium salt complex iodine with water and air.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. The double straight-chain alkyl quaternary ammonium salt complex iodine bactericide is characterized by comprising the following steps:
1) dissolving a double straight-chain alkyl quaternary ammonium salt and an iodine simple substance in a certain mass ratio in an ethanol solution with a certain volume;
2) heating the mixed solution in the step 1, and reacting for 3-7 h at 40-60 ℃;
3) after the reaction is finished, carrying out reduced pressure distillation to obtain viscous liquid;
4) mixing and stirring the double-linear alkyl quaternary ammonium salt complex iodine, the nonionic surfactant and the acid to obtain the double-linear alkyl quaternary ammonium salt complex iodine bactericide.
2. The complex iodine bactericide of di-linear alkyl quaternary ammonium salt according to claim 1, wherein said di-linear alkyl quaternary ammonium salt is selected from one or a mixture of two or more of the following compounds: dioctylalkyl dimethyl ammonium chloride, didecyl alkyl dimethyl ammonium chloride, didodecyl dimethyl ammonium chloride.
3. The complex iodine bactericide of linear alkyl quaternary ammonium salt of claim 1, wherein said nonionic surfactant is selected from at least one of the following compounds: AEO-7, AEO-9, polyethylene glycol 600/800/1000, lauryl polyoxyethylene ether and TX-10.
4. The bi-linear alkyl quaternary ammonium salt complex iodine bactericide as claimed in any one of claims 1 to 3, wherein said acid is selected from at least one of the following compounds: hydrochloric acid, sulfuric acid, phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010154034.1A CN111328806A (en) | 2020-03-07 | 2020-03-07 | Double-linear alkyl quaternary ammonium salt complex iodine bactericide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010154034.1A CN111328806A (en) | 2020-03-07 | 2020-03-07 | Double-linear alkyl quaternary ammonium salt complex iodine bactericide |
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| CN111328806A true CN111328806A (en) | 2020-06-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202010154034.1A Pending CN111328806A (en) | 2020-03-07 | 2020-03-07 | Double-linear alkyl quaternary ammonium salt complex iodine bactericide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114532358A (en) * | 2021-12-01 | 2022-05-27 | 山东志存科技有限公司 | Synthesis process of mixed double-chain quaternary ammonium salt complex iodine for aquaculture |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101711527A (en) * | 2009-12-31 | 2010-05-26 | 蚌埠丰原医药科技发展有限公司 | Bactericidal composition and preparation method thereof |
| CN102550602A (en) * | 2010-11-30 | 2012-07-11 | 中国科学院成都有机化学有限公司 | High-iodine controlled-release type sanitizer |
| CN103766399A (en) * | 2012-10-22 | 2014-05-07 | 洛阳惠中兽药有限公司 | Iodine-containing disinfectant and preparation method thereof |
| CN104604934A (en) * | 2015-01-21 | 2015-05-13 | 成都科宏达科技有限公司 | Novel composite iodine disinfectant as well as preparation method and application thereof |
-
2020
- 2020-03-07 CN CN202010154034.1A patent/CN111328806A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101711527A (en) * | 2009-12-31 | 2010-05-26 | 蚌埠丰原医药科技发展有限公司 | Bactericidal composition and preparation method thereof |
| CN102550602A (en) * | 2010-11-30 | 2012-07-11 | 中国科学院成都有机化学有限公司 | High-iodine controlled-release type sanitizer |
| CN103766399A (en) * | 2012-10-22 | 2014-05-07 | 洛阳惠中兽药有限公司 | Iodine-containing disinfectant and preparation method thereof |
| CN104604934A (en) * | 2015-01-21 | 2015-05-13 | 成都科宏达科技有限公司 | Novel composite iodine disinfectant as well as preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114532358A (en) * | 2021-12-01 | 2022-05-27 | 山东志存科技有限公司 | Synthesis process of mixed double-chain quaternary ammonium salt complex iodine for aquaculture |
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Application publication date: 20200626 |