CN112674111A - Heteropoly acid air bactericide and preparation method and application thereof - Google Patents
Heteropoly acid air bactericide and preparation method and application thereof Download PDFInfo
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- CN112674111A CN112674111A CN202011524635.3A CN202011524635A CN112674111A CN 112674111 A CN112674111 A CN 112674111A CN 202011524635 A CN202011524635 A CN 202011524635A CN 112674111 A CN112674111 A CN 112674111A
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Abstract
The invention relates to the technical field of disinfectants, in particular to a heteropoly acid air bactericide and a preparation method and application thereof. The heteropoly acid air bactericide provided by the invention comprises the following raw materials in parts by weight: 1-5 parts of N, N-dimethylformamide, 1.5-5 parts of propionic acid, 2.5-3 parts of heteropolyacid, 3-10 parts of coupling agent, 10-30 parts of chlorine dioxide and 30-45 parts of water. The invention has the following beneficial effects: (1) the catalytic performance is controllable, which is beneficial to the design of the catalyst; (2) is easy to dissolve in water and organic solvent, can be loaded on substances such as silica gel or activated carbon and the like, shows high catalytic capability and selectivity, and can be used for homogeneous and heterogeneous catalytic reaction systems; (3) the product has good stability and can continuously and efficiently sterilize; (4) safe and green, and the effective components of the sterilization have no harm to human body.
Description
Technical Field
The invention relates to the technical field of disinfectants, in particular to a heteropoly acid air bactericide, and a preparation method and application thereof.
Background
Air is an important transmission path of microorganisms such as bacteria and viruses, and in our workplaces and living places, the air is always subjected to harm from bacteria and viruses in the air, and new corona viruses which are abused worldwide in recent years are examples of the air-borne viruses. Therefore, in order to effectively prevent the spread of the related diseases, it is necessary to effectively kill microorganisms such as bacteria and viruses in the air.
The existing air sterilization technology has certain defects when in use: for example, [ chinese invention ] CN201810776498.9 discloses an air sterilization device for a severe ward, which performs air sterilization by negative ions, but the negative ions have an insignificant air sterilization effect, the negative ions have a short retention time in the air, the place with much dust stays for only a few seconds, and the negative ions are generated by high voltage discharge, which often generates a large amount of ozone at the same time of the high voltage discharge, causing damage to the respiratory system of the human body; the invention of China CN202010382776.X discloses a photocatalyst air sterilization disinfectant and application thereof, wherein the photocatalyst air sterilization mainly utilizes ultraviolet light to irradiate a photocatalyst to generate action, and the ultraviolet light has harm to human body; chinese invention CN201910329921.5 discloses an air sterilization purifier, which utilizes the principle of activated carbon adsorption to perform the sterilization process, but activated carbon can only temporarily adsorb, and the adsorbed pollutants can be dissociated as the temperature and wind speed increase, so the filter material should be changed frequently to avoid the adsorption saturation.
The heteropoly acid is a kind of oxygen-containing polyacid which is formed by the coordination and bridging of hetero atom (such as P, Si, Fe, Co, etc.) and polyatomic atom (such as Mo, W, V, Nb, Ta, etc.) according to a certain structure through oxygen atom, has high catalytic activity and redox property, is a multifunctional novel catalyst, has good stability, can be used for homogeneous and heterogeneous reactions, even can be used as a phase transfer catalyst, has no pollution to the environment, is a green catalyst with great prospect, and can be used for alkylation and dealkylation reactions of aromatic hydrocarbon, esterification reactions, dehydration/combination reactions, redox reactions, ring opening, condensation, addition and etherification reactions, etc. Because of the unique acidity, quasi-liquid phase behavior, and multiple functions (acid, oxidation, photoelectrocatalysis) of heteropoly acid, they are widely regarded by researchers in the field of catalytic research.
Therefore, the technical personnel in the field need to solve the problem of how to provide an air bactericide which has good stability, safety, green color and capability of continuously and efficiently sterilizing by utilizing the chemical characteristics of heteropoly acid.
Disclosure of Invention
In view of the above, the invention provides a heteropoly acid air bactericide, and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the heteropoly acid air bactericide comprises the following raw materials in parts by weight: 1-5 parts of N, N-dimethylformamide, 1.5-5 parts of propionic acid, 2.5-3 parts of heteropolyacid, 3-10 parts of coupling agent, 10-30 parts of chlorine dioxide and 30-45 parts of water.
Preferably, the coupling agent is a silane coupling agent.
Preferably, the heteropoly acid is one or the combination of two or more of phosphotungstic acid, phosphomolybdic acid, silicotungstic acid and silicomolybdic acid in equal proportion.
The invention also provides a preparation method of the heteropoly acid air bactericide, which comprises the following steps:
(A) mixing N, N-dimethylformamide and propionic acid in proportion, adding water in proportion, and stirring to completely dissolve the mixture to obtain a mixed solution;
(B) under the protection of inert gas, adding heteropoly acid and a coupling agent into the mixed solution obtained in the step (A) according to a certain proportion, then pouring the mixture into a reaction tank for reaction, and stirring;
(C) and (C) taking out the reaction liquid obtained in the step (B), adding chlorine dioxide in proportion, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
Preferably, the reaction time in the step (B) is 0.5-1h, and the reaction temperature is 100-.
Preferably, during the reaction in the step (B), a pH value regulator is used to control the pH value of the solution system to be between 5 and 7.
Preferably, the pH value regulator is one of citric acid, potassium citrate, lactic acid and tartaric acid.
Preferably, the stirring time in the step (A) is 30-60min, the stirring speed is 800-2000 rpm, and the temperature is 45-65 ℃.
It should be noted that, the ratio of the compressed air charged in the step (C) is adjusted according to the volume of the container or the specific product requirement, etc., according to the actual situation.
The invention further provides application of the heteropoly acid air bactericide in sterilization of various closed occasions.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) because the heteropoly acid has the main structural characteristics of a common complex and a metal oxide, different elements can show the difference between the acidity and the oxidation-reduction property, so that the catalytic performance of the heteropoly acid is controllable, and the design of a catalyst is facilitated;
(2) is easy to dissolve in water and organic solvent, can be loaded on substances such as silica gel or activated carbon and the like, shows high catalytic capability and selectivity, and can be used for homogeneous and heterogeneous catalytic reaction systems;
(3) the bactericide has better thermal stability, so that the stability of sterilization and the stability of storage of the bactericide can be effectively ensured by using the heteropoly acid as the catalyst, and the bactericide can be continuously and efficiently sterilized;
(4) the sterilization agent is safe and green, has no harm to human bodies due to the sterilization active ingredients, and can be used in crowded places for a long time.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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 heteropoly acid air bactericide comprises the following raw materials in parts by weight: 1 part of N, N-dimethylformamide, 1.5 parts of propionic acid, 2.5 parts of phosphotungstic acid, 3 parts of a silane coupling agent, 10 parts of chlorine dioxide and 30 parts of water.
A preparation method of heteropoly acid air bactericide comprises the following steps:
(A) mixing N, N-dimethylformamide and propionic acid in proportion, adding water in proportion, and stirring to completely dissolve the mixture to obtain a mixed solution; the stirring time is 30min, the stirring speed is 800rpm, and the temperature is 45-65 ℃.
(B) Under the protection of inert gas, adding phosphotungstic acid and a silane coupling agent into the mixed solution obtained in the step (A) in proportion, then pouring the mixture into a reaction tank for reaction, and stirring; the reaction time is 0.5h, the reaction temperature is 100 ℃, and a pH value regulator is required to be used for controlling the pH value of a solution system to be between 5 and 7 in the reaction process; the pH regulator is citric acid.
(C) And (C) taking out the reaction liquid obtained in the step (B), adding chlorine dioxide in proportion, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
Example 2
The heteropoly acid air bactericide comprises the following raw materials in parts by weight: 5 parts of N, N-dimethylformamide, 5 parts of propionic acid, 3 parts of phosphomolybdic acid, 10 parts of a silane coupling agent, 30 parts of chlorine dioxide and 45 parts of water.
A preparation method of heteropoly acid air bactericide comprises the following steps:
(A) mixing N, N-dimethylformamide and propionic acid in proportion, adding water in proportion, and stirring to completely dissolve the mixture to obtain a mixed solution; the stirring time is 60min, the stirring speed is 2000rpm, and the temperature is 45-65 ℃.
(B) Under the protection of inert gas, adding phosphomolybdic acid and a silane coupling agent into the mixed solution obtained in the step (A) in proportion, then pouring the mixture into a reaction tank for reaction, and stirring the mixture; the reaction time is 1h, the reaction temperature is 255 ℃, and a pH value regulator is required to be used for controlling the pH value of a solution system to be 5-7 in the reaction process; the pH value regulator is potassium citrate.
(C) And (C) taking out the reaction liquid obtained in the step (B), adding chlorine dioxide in proportion, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
Example 3
The heteropoly acid air bactericide comprises the following raw materials in parts by weight: 3 parts of N, N-dimethylformamide, 3.25 parts of propionic acid, 2.75 parts of silicotungstic acid, silicon molybdenate (the adding ratio of the tungstic acid to the silicomolybdic acid is 1: 1), 6.5 parts of a silane coupling agent, 20 parts of chlorine dioxide and 37.5 parts of water.
A preparation method of heteropoly acid air bactericide comprises the following steps:
(A) mixing N, N-dimethylformamide and propionic acid in proportion, adding water in proportion, and stirring to completely dissolve the mixture to obtain a mixed solution; the stirring time was 45min, the stirring rate was 1400rpm, and the temperature was 45-65 ℃.
(B) Under the protection of inert gas, adding silicotungstic acid, silicomolybdic acid and a silane coupling agent into the mixed solution obtained in the step (A) in proportion, then pouring the mixture into a reaction tank for reaction, and stirring the mixture; the reaction time is 0.75h, the reaction temperature is 177.5 ℃, and a pH value regulator is required to be used for controlling the pH value of a solution system to be between 5 and 7 in the reaction process; the pH regulator is tartaric acid.
(C) And (C) taking out the reaction liquid obtained in the step (B), adding chlorine dioxide in proportion, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
Example 4
A preparation method of heteropoly acid air bactericide comprises the following steps:
(A) mixing 2 parts by weight of N, N-dimethylformamide and 4 parts by weight of propionic acid, adding 35 parts by weight of water, and fully stirring to completely dissolve the N, N-dimethylformamide and the propionic acid to obtain a mixed solution; the stirring time was 60min, the stirring rate was 2000rpm, and the stirring temperature was 45-65 ℃.
(B) Adding 2.8 parts by weight of phosphotungstic acid and 4 parts by weight of silane coupling agent into the mixed solution obtained in the step (A) under the protection of inert gas, pouring the mixed solution into a reaction tank, mixing and stirring for 1 hour at the reaction temperature of 100 ℃, and controlling the pH value of a solution system to be between 5 and 7 by using tartaric acid in the reaction process;
(C) and (3) taking out the liquid reacted in the step (2), adding 10 parts of chlorine dioxide, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
Example 5
A preparation method of heteropoly acid air bactericide comprises the following steps:
(A) mixing 2 parts by weight of N, N-dimethylformamide and 4 parts by weight of propionic acid, adding the mixture into 35 parts by weight of water, and fully stirring to completely dissolve the mixture to obtain a mixed solution; the stirring time was 60min, the stirring rate was 2000rpm, and the stirring temperature was 45-65 ℃.
(B) Adding 1 part by weight of phosphotungstic acid and 4 parts by weight of silane coupling agent into the mixed solution obtained in the step (A) under the protection of inert gas, pouring the mixed solution into a reaction tank, mixing and stirring for 1 hour at the reaction temperature of 100 ℃, and controlling the pH value of a solution system to be between 5 and 7 by using tartaric acid in the reaction process;
(C) and (3) taking out the liquid reacted in the step (2), adding 10 parts of chlorine dioxide, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
Example 6
A preparation method of heteropoly acid air bactericide comprises the following steps:
(A) mixing 2 parts by weight of N, N-dimethylformamide and 4 parts by weight of propionic acid, adding the mixture into 35 parts by weight of water, and fully stirring to completely dissolve the mixture to obtain a mixed solution; the stirring time was 60min, the stirring rate was 2000rpm, and the stirring temperature was 45-65 ℃.
(B) Adding 5 parts by weight of phosphotungstic acid and 4 parts by weight of silane coupling agent into the mixed solution obtained in the step (A) under the protection of inert gas, pouring the mixed solution into a reaction tank, mixing and stirring for 1 hour at the reaction temperature of 100 ℃, and controlling the pH value of a solution system to be between 5 and 7 by using tartaric acid in the reaction process;
(C) and (3) taking out the liquid reacted in the step (2), adding 10 parts of chlorine dioxide, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
Example 7
A preparation method of heteropoly acid air bactericide comprises the following steps:
(A) mixing 2 parts by weight of N, N-dimethylformamide and 4 parts by weight of propionic acid, adding the mixture into 35 parts by weight of water, and fully stirring to completely dissolve the mixture to obtain a mixed solution; the stirring time was 60min, the stirring rate was 2000rpm, and the stirring temperature was 45-65 ℃.
(B) And (2) adding 4 parts of silane coupling agent into the mixed solution obtained in the step (A) under the protection of inert gas, wherein the weight part of heteropoly acid is 0 part.
Pouring the mixed solution into a reaction tank, mixing and stirring, wherein the reaction time is 1 hour, the reaction temperature is 100 ℃, and the pH value of a solution system is controlled to be 5-7 by using tartaric acid in the reaction process;
(C) and (3) taking out the liquid reacted in the step (2), adding 10 parts of chlorine dioxide, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
Example 8
Two groups of commercially available air disinfectants were used as comparative example 1.
The air sanitizers obtained in examples 4 to 7 were divided into two groups;
the first group is that the same amount of bacteria is sprayed in a plurality of rooms with the same size, meanwhile, the bacteria amount and the bacteria species in each room are manually controlled to keep a relatively stable state, 10 minutes passes after the bacteria amount and the bacteria species are sprayed, and then the sterilization rate of each room is detected;
the second group is that the same amount of bacteria is sprayed in a plurality of rooms with the same size, meanwhile, the bacteria amount and the bacteria species in each room are manually controlled to keep a relatively stable state, after the bacteria amount and the bacteria species are sprayed, the bacteria species are sprayed for three hours, and then the sterilization rate of each room is detected; the data collection described above is collated into the following table:
| first group sterilization Rate (%) | Second group sterilization Rate (%) | |
| Example 4 | 99.8％ | 95.1％ |
| Example 5 | 99.2％ | 90.1％ |
| Example 6 | 98.6％ | 81.8％ |
| Example 7 | 91.1％ | 78.1％ |
| Comparative example 1 | 98.2％ | 70.3％ |
And (4) analyzing results:
1. as can be seen from the data in the table, the sterilization rate of the examples 4-6 in the first group is higher than that of the comparative example 1, and the sterilization rate of the examples 4-6 in the second group is obviously higher than that of the comparative example 1, so that the heteropoly acid air bactericide has good sterilization effect, durable and stable sterilization effect and better effect than similar products in the market.
2. From the comparison of the bactericidal effects of examples 4 to 6 and example 7, it is seen that the bactericidal effect of the air bactericide without the addition of the heteropolyacid is much lower than that of the air bactericide with the addition of the heteropolyacid in both short-term and long-term bactericidal effects, so that the stability of sterilization and storage stability of the bactericide can be effectively ensured by using the heteropolyacid as the catalyst, and the air bactericide can be continuously and efficiently sterilized.
3. From the comparison of the bactericidal effects of examples 4 and 5 and example 6, the more heteropoly acid is added, the better the bactericidal effect is, the less the heteropoly acid is added, and the difference of the bactericidal effect in a short period is not large, but the bactericidal rate of the second group of examples 5 and 6 is significantly lower than that of example 4, so that the proper proportion of heteropoly acid needs to be selected to achieve excellent and long-lasting bactericidal effect.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The heteropoly acid air bactericide is characterized by comprising the following raw materials in parts by weight: 1-5 parts of N, N-dimethylformamide, 1.5-5 parts of propionic acid, 2.5-3 parts of heteropolyacid, 3-10 parts of coupling agent, 10-30 parts of chlorine dioxide and 30-45 parts of water.
2. The heteropoly acid air disinfectant of claim 1, wherein the coupling agent is a silane coupling agent.
3. The heteropoly acid air bactericide of claim 1, wherein the heteropoly acid is one or any combination of two or more of phosphotungstic acid, phosphomolybdic acid, silicotungstic acid and silicomolybdic acid in equal proportion.
4. A process for the preparation of a heteropolyacid air-fungicide according to any one of claims 1 to 3, comprising the steps of:
(A) mixing N, N-dimethylformamide and propionic acid in proportion, adding water in proportion, and stirring to completely dissolve the mixture to obtain a mixed solution;
(B) under the protection of inert gas, adding heteropoly acid and a coupling agent into the mixed solution obtained in the step (A) according to a certain proportion, then pouring the mixture into a reaction tank for reaction, and stirring;
(C) and (C) taking out the reaction liquid obtained in the step (B), adding chlorine dioxide in proportion, mixing and stirring uniformly, filling into a spray bottle, and filling compressed air to obtain the heteropoly acid air bactericide.
5. The method as claimed in claim 4, wherein the reaction time in step (B) is 0.5-1h, and the reaction temperature is 100-255 ℃.
6. The method for preparing heteropoly acid air bactericide as claimed in claim 4, wherein pH regulator is used to control pH value of solution system between 5-7 during reaction in step (B).
7. The method for preparing heteropoly acid air bactericide as claimed in claim 6, wherein the pH value regulator is one of citric acid, potassium citrate, lactic acid, tartaric acid.
8. The preparation method of the heteropoly acid air bactericide as claimed in claim 4, wherein the stirring time in step (A) is 30-60min, and the stirring speed is 800-2000 rpm. The temperature is 45-65 ℃.
9. Use of a heteropolyacid air-biocide as claimed in any one of claims 1-3 in the sterilisation of various enclosed applications.
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| CN111493094A (en) * | 2020-04-24 | 2020-08-07 | 杨小垒 | Air disinfectant and spreading method thereof |
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2020
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| CN102950023A (en) * | 2011-08-31 | 2013-03-06 | 中国石油化工股份有限公司 | Load-type phosphotungstic acid catalyst and preparation method thereof as well as n-butyl acrylate preparation method |
| CN106342890A (en) * | 2016-08-25 | 2017-01-25 | 齐齐哈尔大学 | Heteropoly acid and amino acid compound antibacterial agent, and preparation method and application thereof |
| CN110250199A (en) * | 2019-05-20 | 2019-09-20 | 天津大学 | A kind of disinfection agent of chlorine dioxide containing load-type solid acid and preparation method and application |
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Application publication date: 20210420 |