CN114009448A - Long-acting bactericide based on disodium hydrogen phosphite - Google Patents
Long-acting bactericide based on disodium hydrogen phosphite Download PDFInfo
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Abstract
The application belongs to the technical field of bactericides, and particularly relates to a long-acting bactericide based on disodium hydrogen phosphite, which adopts the following method: (1) dissolving chitosan in an acid solution to obtain a chitosan solution, dissolving disodium hydrogen phosphite in water to obtain a disodium hydrogen phosphite solution, and dissolving a water-soluble carrier in water to obtain a carrier solution; (2) adding disodium hydrogen phosphite solution into chitosan solution, stirring for 20-40 min, adjusting pH to neutral, stirring for 10-30 min, standing for aging, filtering, washing with water, and filtering to obtain bactericidal body; (3) adding the sterilizing body into the carrier solution, stirring, homogenizing, and spray drying to obtain the long-acting bactericide. According to the preparation method, the chitosan and the disodium hydrogen phosphite are mixed in a solution state, so that the disodium hydrogen phosphite is better dispersed in the chitosan, the sustained release of the disodium hydrogen phosphite is facilitated, and the sodium ions in the disodium hydrogen phosphite can improve the antibacterial effect of the chitosan; the water-soluble carrier is used for dispersing the sterilizing body, so that the solubility of the sterilizing body can be improved, and the sterilizing effect can be better exerted.
Description
Technical Field
The application belongs to the technical field of bactericides, and particularly relates to a long-acting bactericide based on disodium hydrogen phosphite.
Background
Phosphite was originally derived from fosetyl-aluminum developed by bayer corporation in germany, and then many foreign companies began to produce a biological bactericide containing phosphite as a main component with the expiration of the patent term for effective components of fosetyl-aluminum. Disodium hydrogen phosphite is used as a main product in phosphite, has a certain bactericidal effect, can stimulate plants to improve the resistance to diseases and enhance disease attack resistance, can be used as a systemic bactericide, and has relatively limited bactericidal effect.
The chitosan is a product obtained by converting chitosan deacetylation, and has multiple physiological functions of biodegradability, biocompatibility, nontoxicity, bacteriostasis, cancer resistance, lipid reduction, immunity enhancement and the like. Chitosan has the above properties and is widely used in various fields such as agriculture, environmental protection, food industry, medicine, and light textile industry. In agriculture, chitosan can improve crop yield and crop quality, and has good bactericidal effect, on one hand, the chitosan can induce plants to generate a mechanism of spectral resistance, and on the other hand, the chitosan has strong direct inhibition effect on the growth of a plurality of plant pathogenic bacteria. However, chitosan can only be dissolved in an acidic solution with a pH of less than 6.5, which limits the antibacterial application of chitosan.
In view of the advantages of disodium hydrogen phosphite and chitosan in the sterilization and antibiosis aspects, the disodium hydrogen phosphite and chitosan need to be combined to develop a bactericide with better antibacterial effect and wider application range, and simultaneously can play a long-term sterilization role, and particularly can expand the application of the disodium hydrogen phosphite and chitosan in the field of crop sterilization.
Disclosure of Invention
In order to solve the problems, the application discloses a long-acting bactericide based on disodium hydrogen phosphite, which is prepared by mixing chitosan and disodium hydrogen phosphite in a solution state, so that disodium hydrogen phosphite is better dispersed in chitosan to form a certain coating effect of chitosan on disodium hydrogen phosphite, thereby being beneficial to the slow release of disodium hydrogen phosphite and prolonging the sterilization time limit on one hand, and being beneficial to improving the antibacterial effect of chitosan by sodium ions in disodium hydrogen phosphite on the other hand; later can help obtaining more even tiny sterilizing body granule through coprecipitation to be favorable to the even dispersion of sterilizing body granule in carrier solution, disperse sterilizing body through water-soluble carrier, can effectively improve sterilizing body's solubility, be favorable to exerting bactericidal effect better.
The application provides a long-acting bactericide based on disodium hydrogen phosphite, which adopts the following technical scheme:
a long-acting bactericide based on disodium hydrogen phosphite is prepared by the following method:
(1) dissolving chitosan in an acid solution to obtain a chitosan solution, dissolving disodium hydrogen phosphite in water to obtain a disodium hydrogen phosphite solution, and dissolving a water-soluble carrier in water to obtain a carrier solution;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 20-40 min, adjusting the pH value to be neutral, then continuously stirring for 10-30 min, standing for aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Preferably, in the step (1): the acid solution is acetic acid solution with mass concentration of 1-3%, the pH value of the chitosan solution is 5-6, and the mass concentration of the water-soluble carrier in the carrier solution is 20-30%.
Preferably, in the step (1): the molecular weight of chitosan is 5 × 103 - 5×105The mass ratio of the chitosan to the disodium hydrogen phosphite is 70-120:1, and the mass ratio of the chitosan to the water-soluble carrier is 1: 0.5-1.5.
Preferably, the chitosan has a molecular weight of 1X 104 - 1×105The mass ratio of the chitosan to the disodium hydrogen phosphite is 80-100:1, and the mass ratio of the chitosan to the water-soluble carrier is 1: 1-1.5.
Preferably, the water-soluble carrier in step (1) is one or more of polyethylene glycol, poloxamer, polyvinyl alcohol, povidone, methyl cellulose, ethyl cellulose, hydroxypropyl cellulose and carboxymethyl cellulose.
Preferably, the water-soluble carrier in the step (1) is polyethylene glycol.
Preferably, the water-soluble carrier in the step (1) is polyethylene glycol 8000.
Preferably, the long-acting bactericide based on the disodium hydrogen phosphite can be sprayed alone, or mixed with foliar fertilizer for spraying, or irrigated to roots.
The application has the following beneficial effects:
(1) according to the long-acting bactericide based on the disodium hydrogen phosphite, the chitosan and the disodium hydrogen phosphite are mixed in a solution state, so that the disodium hydrogen phosphite is better dispersed in the chitosan, and a certain coating effect of the chitosan on the disodium hydrogen phosphite is formed, so that the sustained release of the disodium hydrogen phosphite is facilitated, the sterilization time limit is prolonged, and the sodium ions in the disodium hydrogen phosphite are beneficial to improving the antibacterial effect of the chitosan; later can help obtaining more even tiny bactericidal body granule through the coprecipitation to be favorable to the even dispersion of bactericidal body granule in carrier solution, disperse the bactericidal body through water-soluble carrier, can effectively improve the solubility of bactericidal body, be favorable to exerting bactericidal effect better, in addition, chitosan can also improve crop output, improves crop quality.
(2) The chitosan with relatively small molecular weight is adopted, so that a better antibacterial effect is obtained; the mass ratio of the chitosan to the disodium hydrogen phosphite is controlled to be 80-120:1, which is beneficial to improving the sterilization/antibacterial performance through the synergistic effect of sodium ions in the disodium hydrogen phosphite and the chitosan; the mass ratio of the chitosan to the water-soluble carrier is controlled to be 1:0.5-1.5, so that the solubility of the bactericide can be effectively improved, and the bactericidal effect of the bactericide can be improved.
(3) The water-soluble carrier is preferably polyethylene glycol 8000, and tests show that the polyethylene glycol 8000 is favorable for obtaining better sterilization effect and longer sterilization time limit compared with other water-soluble carriers.
Drawings
The present application is further described below with reference to the drawings and examples.
FIG. 1 is a flow chart of the preparation of the long acting biocide of the present application.
Detailed Description
The present application will now be described in further detail with reference to examples.
Example 1
(1) 80 g of molecular weight is 1X 104Dissolving chitosan in 2% acetic acid solution, filtering to remove insoluble substances, adjusting pH to 5 with 1M NaOH solution to obtain chitosan solution, dissolving 1 g of disodium hydrogen phosphite in water to obtain disodium hydrogen phosphite solution, and dissolving 40 g of poloxamer in water to obtain 20% carrier solution;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 20 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 10 min, standing and aging, filtering, washing with water and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 2
(1) 100 g of molecular weight is 3X 104Dissolving chitosan in 2% acetic acid solution, filtering to remove insoluble substances, adjusting pH to 6 with 1M NaOH solution to obtain chitosan solution, dissolving 1 g of disodium hydrogen phosphite in water to obtain disodium hydrogen phosphite solution, and dissolving 80 g of polyvidone in water to obtain carrier solution with mass concentration of 30%;
(2) adding disodium hydrogen phosphite solution into chitosan solution, stirring for 30 min, adjusting pH to neutral to completely precipitate, continuing stirring for 20 min, standing for aging, filtering, washing with water, and filtering to obtain bactericidal body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 3
(1) 110 g of molecular weight 8X 104The chitosan is dissolved in acetic acid solution with mass concentration of 2%, insoluble substances are filtered out, the pH value is adjusted to 5.5 by using 1M NaOH solution to obtain chitosan solution, 1 g of disodium hydrogen phosphite is dissolved in water to obtain disodium hydrogen phosphite solution, and 110 g of hydroxypropyl cellulose is dissolved in water to obtain carrier solution with mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 40 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 30 min, standing and aging, filtering, washing with water and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 4
(1) 120 g of molecular weight is 1X 105Dissolving chitosan in 2% acetic acid solution, filtering to remove insoluble substances, adjusting pH to 5.4 with 1M NaOH solution to obtain chitosan solution, dissolving 1 g of disodium hydrogen phosphite in water to obtain disodium hydrogen phosphite solution, and dissolving 180 g of polyvinyl alcohol in water to obtain carrier solution with mass concentration of 30%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 5
(1) 90 g of molecular weight 5X 104The chitosan is dissolved in acetic acid solution with the mass concentration of 2%, insoluble substances are filtered out, the pH value is adjusted to 5.4 by using 1M NaOH solution to obtain chitosan solution, 1 g of disodium hydrogen phosphite is dissolved in water to obtain disodium hydrogen phosphite solution, 108 g of polyethylene glycol 8000 is dissolved in water to obtain carrier solution with the mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 6
(1) 90 g of molecular weight 5X 104Dissolving the chitosan in an acetic acid solution with the mass concentration of 2%, filtering out insoluble substances, adjusting the pH to 5.4 by using a 1M NaOH solution to obtain a chitosan solution, dissolving 1 g of disodium hydrogen phosphite in water to obtain a disodium hydrogen phosphite solution, and dissolving 108 g of polyethylene glycol 6000 in water to obtain a carrier solution with the mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 7
(1) 90 g of molecular weight 5X 104The chitosan is dissolved in acetic acid solution with mass concentration of 2%, insoluble substances are filtered out, the pH value is adjusted to 5.4 by using 1M NaOH solution to obtain chitosan solution, 1 g of disodium hydrogen phosphite is dissolved in water to obtain disodium hydrogen phosphite solution, 108 g of polyethylene glycol 10000 is dissolved in water to obtain carrier solution with mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 8
(1) 90 g of molecular weight 5X 104The chitosan is dissolved in acetic acid solution with mass concentration of 2%, insoluble substances are filtered out, the pH value is adjusted to 5.4 by using 1M NaOH solution to obtain chitosan solution, 1 g of disodium hydrogen phosphite is dissolved in water to obtain disodium hydrogen phosphite solution, and 108 g of poloxamer is dissolved in water to obtain carrier solution with mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 9
(1) 90 g of molecular weight 5X 104The chitosan is dissolved in acetic acid solution with mass concentration of 2%, insoluble substances are filtered out, the pH value is adjusted to 5.4 by using 1M NaOH solution to obtain chitosan solution, 1 g of disodium hydrogen phosphite is dissolved in water to obtain disodium hydrogen phosphite solution, and 108 g of polyvinyl alcohol is dissolved in water to obtain carrier solution with mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 10
(1) 90 g of molecular weight 5X 104The chitosan is dissolved in acetic acid solution with mass concentration of 2%, insoluble substances are filtered out, the pH value is adjusted to 5.4 by using 1M NaOH solution to obtain chitosan solution, 1 g of disodium hydrogen phosphite is dissolved in water to obtain disodium hydrogen phosphite solution, and 108 g of povidone is dissolved in water to obtain carrier solution with mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 11
(1) 90 g of molecular weight 5X 104Dissolving chitosan in 2% acetic acid solution, and filteringAdjusting the pH value to 5.4 by using a 1M NaOH solution to obtain a chitosan solution, dissolving 1 g of disodium hydrogen phosphite in water to obtain a disodium hydrogen phosphite solution, and dissolving 108 g of hydroxypropyl cellulose in water to obtain a carrier solution with the mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 12
(1) 110 g of molecular weight 8X 104The chitosan is dissolved in acetic acid solution with mass concentration of 2%, insoluble substances are filtered out, the pH value is adjusted to 5.5 by using 1M NaOH solution to obtain chitosan solution, 1 g of disodium hydrogen phosphite is dissolved in water to obtain disodium hydrogen phosphite solution, 88 g of hydroxypropyl cellulose is dissolved in water to obtain carrier solution with mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 40 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 30 min, standing and aging, filtering, washing with water and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 13
(1) 110 g of molecular weight is 3X 104Dissolving chitosan in 2% acetic acid solution, filtering to remove insoluble substances, adjusting pH to 6 with 1M NaOH solution to obtain chitosan solution, dissolving 1 g of disodium hydrogen phosphite in water to obtain disodium hydrogen phosphite solution, and dissolving 88 g of polyvidone in water to obtain carrier solution with mass concentration of 30%;
(2) adding disodium hydrogen phosphite solution into chitosan solution, stirring for 30 min, adjusting pH to neutral to completely precipitate, continuing stirring for 20 min, standing for aging, filtering, washing with water, and filtering to obtain bactericidal body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 14
(1) 70 g of molecular weight 1X 104Dissolving chitosan in 2% acetic acid solution, filtering to remove insoluble substances, adjusting pH to 5 with 1M NaOH solution to obtain chitosan solution, dissolving 1 g of disodium hydrogen phosphite in water to obtain disodium hydrogen phosphite solution, and dissolving 35 g of poloxamer in water to obtain 20% carrier solution;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 20 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 10 min, standing and aging, filtering, washing with water and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 15
(1) 90 g of molecular weight 5X 103The chitosan is dissolved in acetic acid solution with the mass concentration of 2%, insoluble substances are filtered out, the pH value is adjusted to 5.4 by using 1M NaOH solution to obtain chitosan solution, 1 g of disodium hydrogen phosphite is dissolved in water to obtain disodium hydrogen phosphite solution, 108 g of polyethylene glycol 8000 is dissolved in water to obtain carrier solution with the mass concentration of 25%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Example 16
(1) 90 g of molecular weight 5X 105Dissolving the chitosan in 2% acetic acid solution, filtering to remove insoluble substances, adjusting pH to 5.4 with 1M NaOH solution to obtain chitosan solution, and dissolving 1 g disodium hydrogen phosphite in water to obtain disodium hydrogen phosphiteDissolving 108 g of polyethylene glycol 8000 in water to obtain a carrier solution with the mass concentration of 25 percent;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Comparative example 1
(1) 120 g of molecular weight is 1X 105Dissolving chitosan in an acetic acid solution with the mass concentration of 2%, filtering out insoluble substances, adjusting the pH to 5.4 by using a 1M NaOH solution to obtain a chitosan solution, dissolving 1 g of disodium hydrogen phosphite in water to obtain a disodium hydrogen phosphite solution, and dissolving 204 g of polyvinyl alcohol in water to obtain a carrier solution with the mass concentration of 30%;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Comparative example 2
(1) 90 g of molecular weight 5X 104Dissolving the chitosan in an acetic acid solution with the mass concentration of 2%, filtering out insoluble substances, adjusting the pH to 5.4 by using a 1M NaOH solution to obtain a chitosan solution, and dissolving 1 g of disodium hydrogen phosphite in water to obtain a disodium hydrogen phosphite solution;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 30 min, adjusting the pH value to be neutral to completely separate out the precipitate, then continuing stirring for 20 min, standing and aging, filtering, washing with water, and filtering to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
Comparative example 3
(1) Dissolving 108 g of polyethylene glycol 8000 in water to obtain a carrier solution with the mass concentration of 25%;
(3) 90 g of molecular weight 5X 104Adding the chitosan and 1 g of disodium hydrogen phosphite into a carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
The sterilization tests show that the sterilization rates of the long-acting disodium hydrogen phosphite-based fungicides prepared in examples 1 to 16 and comparative examples 1 to 3 are shown in table 1.
TABLE 1
| Sterilizing rate after 24h | Sterilization rate after 15 days | Sterilization rate after 30d | |
| Example 1 | 86.8% | 83.3% | 78.4% |
| Example 2 | 91.0% | 88.7% | 84.3% |
| Example 3 | 98.9% | 98.9% | 98.8% |
| Example 4 | 98.6% | 98.6% | 98.6% |
| Example 5 | 100% | 100% | 100% |
| Example 6 | 99.3% | 99.3% | 99.1% |
| Example 7 | 98.2% | 98.4% | 98.7% |
| Example 8 | 98.6% | 98.9% | 99.1% |
| Example 9 | 98.1% | 98.1% | 98.3% |
| Example 10 | 98.2% | 98.2% | 98.2% |
| Example 11 | 98.7% | 98.6% | 98.7% |
| Example 12 | 90.8% | 88.3% | 85.0% |
| Example 13 | 89.4% | 89.5% | 89.5% |
| Example 14 | 97.6% | 90.4% | 72.6% |
| Example 15 | 100% | 96.7% | 90.8% |
| Example 16 | 96.3% | 96.3% | 96.2% |
| Comparative example 1 | 98.7% | 98.7% | 98.6% |
| Comparative example 2 | 76.3% | 71.2% | 63.5% |
| Comparative example 3 | 100% | 85.7% | 60.5% |
From examples 1 to 16, it can be seen that the long-acting bactericide based on disodium hydrogen phosphite prepared by the present application has a bactericidal rate of more than 86.8% in 24 hours, and a bactericidal rate of more than 72.6% after 30 days, and has a better continuous bactericidal effect. The bactericides prepared in examples 1 and 2 may have poor solubility of the bactericidal body due to the small amount of the water-soluble carrier added, poor bactericidal effect, and a slight decrease in bactericidal effect with the lapse of time. In examples 3-4, the sterilization rate was slightly lower in 24 hours, but the sustained-release property was good, and the relatively long-lasting sterilization effect could be maintained, probably because the chitosan content was relatively high and the disodium hydrogen phosphite content was relatively low. As can be seen from examples 5-7, the use of polyethylene glycol 8000 as the water-soluble carrier is most effective, and a higher degree of polymerization is advantageous for increasing hydrophilicity, but as the degree of polymerization increases, it may result in an increase in viscosity and affect the release of the bactericidal substance. In examples 8 to 11, poloxamer, polyethylene glycol, povidone, and hydroxypropylcellulose were used as water-soluble carriers, respectively, and the bactericidal effect was relatively poor but the long-term stable bactericidal effect was maintained as compared with example 5. Example 12 compared with example 3, the amount of the water-soluble carrier used was reduced, the hydrophilicity of the bactericidal substance was lowered, the bactericidal rate was largely lowered in 24 hours, and the bactericidal effect was slightly lowered with the lapse of time. Compared with the example 2, the relative content of chitosan in the bactericidal body is increased, the relative content of disodium hydrogen phosphite is reduced, the ratio of the water-soluble carrier and the chitosan is not changed, the 24-hour sterilization rate of the example 13 is slightly reduced, but the slow release effect is good, and the long-term sterilization effect is maintained. Example 14 compared with example 1, the content of chitosan in the bactericidal body was reduced, the content of disodium hydrogen phosphite was increased, the ratio of the water-soluble carrier to chitosan was unchanged, and 24 hours were spentThe sterilization rate is obviously higher than that of example 1, but the continuous sterilization effect is poor, and the slow release effect is possibly poor due to the reduction of the chitosan content. When the molecular weight is 5X 10 in example 153The chitosan of (3) can achieve a 24-hour sterilization rate consistent with that of example 5, but the molecular weight of chitosan is too small, which may affect the sustained release effect of disodium hydrogenphosphite, and thus deteriorate the sustained sterilization effect. When the molecular weight is 5X 10 in example 165The larger molecular weight of the chitosan of (3) results in a decrease in antibacterial performance for 24 hours, but the maintenance of the continuous bactericidal effect is relatively good.
As can be seen from comparative example 1, comparative example 1 increased the content of the water-soluble carrier as compared to example 4, but the antibacterial effect was not significantly improved, indicating that an excessive amount of the water-soluble carrier failed to further increase the antibacterial effect. As can be seen from comparative example 2, when a water-soluble carrier is not used, the solubility of the bactericidal body becomes poor, resulting in a significant decrease in the bactericidal effect. It can be seen from comparative example 3 that, when chitosan and disodium hydrogen phosphite were not previously treated as sterilizing bodies but were directly added to the carrier solution for spray drying, the sterilizing rate of the prepared sterilizing agent reached 100% in 24 hours, but the sterilizing rate decreased significantly with the passage of time, since the chitosan did not slowly release the coating of disodium hydrogen phosphite.
The long-acting bactericide based on disodium hydrogen phosphite prepared in examples 1-16 and comparative examples 1-3 was used for testing in a Chinese cabbage plantation site, the test area of each test group was 1 mu, 1 mu was used as a blank control group, and the test groups were sprayed with 800-fold liquid and watered with 200-fold liquid except the blank control group, wherein the 800-fold and 200-fold dilutions were performed on the basis of the bactericide (i.e. the amount of water-soluble carrier removed) in the long-acting bactericide. The Chinese cabbage variety, sowing mode and management mode selected by the blank control group and the test group are the same. The growth rate of the outer diameter, the growth rate of the plant height, the growth rate of the root weight, the growth rate of the clean vegetable seeds and the growth rate of the yield per mu of each test group are calculated on the basis of the blank control group, and are shown in table 2.
TABLE 2
| Rate of increase of outer diameter | Plant height growth rate | Root weight growth rate | Growth rate of clean vegetable seeds | Growth rate of yield per mu | |
| Example 1 | 6.7% | 1.7% | 19.1% | 9.7% | 10.8% |
| Example 2 | 8.0% | 2.1% | 22.7% | 11.5% | 12.6% |
| Example 3 | 10.3% | 2.9% | 22.0% | 15.1% | 16.2% |
| Example 4 | 10.1% | 2.7% | 24.7% | 14.5% | 16.0% |
| Example 5 | 10.6 % | 3.1% | 21.4% | 15.6% | 16.8% |
| Example 6 | 10.4% | 3.0% | 21.5% | 15.3% | 16.4% |
| Example 7 | 9.7% | 2.4% | 22.6% | 14.3% | 15.6% |
| Example 8 | 10.0% | 2.5% | 21.7% | 14.8% | 16.2% |
| Example 9 | 9.5% | 2.4% | 22.3% | 14.2% | 15.2% |
| Example 10 | 9.7% | 2.3% | 21.8% | 14.3% | 15.3% |
| Example 11 | 10.0% | 2.6% | 22.4% | 14.5% | 15.9% |
| Example 12 | 8.3% | 2.4% | 21.8% | 13.8% | 14.5% |
| Example 13 | 8.9% | 2.2% | 23.0% | 12.3% | 13.2% |
| Example 14 | 7.2% | 1.9% | 17.4% | 10.4% | 11.5% |
| Example 15 | 9.6% | 2.3% | 21.8% | 13.2% | 14.2% |
| Example 16 | 9.8% | 2.3% | 21.2% | 13.5% | 14.6% |
| Comparative example 1 | 10.2% | 2.5% | 25.2% | 14.5% | 16.1% |
| Comparative example 2 | 5.1% | 1.4% | 21.0% | 7.9% | 8.7% |
| Comparative example 3 | 6.4% | 1.6% | 21.5% | 9.4% | 10.3% |
As can be seen from Table 2, the test groups to which the long-acting fungicides of examples 1 to 16 of the present application were applied showed significant improvements in growth characteristics such as outer diameter, plant height and net vegetable seed of the harvested chinese cabbage, and the increase rate per mu was up to 10.8% or more, as compared with the blank control group. The long-acting bactericide obtained by the application is beneficial to reducing bacterial harm, improving the growth condition of crops, improving the quality of the crops and increasing the yield of the crops.
The present embodiment is merely illustrative and not restrictive, and various changes and modifications may be made by persons skilled in the art without departing from the scope of the present invention as defined in the appended claims. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (8)
1. A long-acting bactericide based on disodium hydrogen phosphite is characterized in that: the preparation method comprises the following steps:
(1) dissolving chitosan in an acid solution to obtain a chitosan solution, dissolving disodium hydrogen phosphite in water to obtain a disodium hydrogen phosphite solution, and dissolving a water-soluble carrier in water to obtain a carrier solution;
(2) adding the disodium hydrogen phosphite solution into the chitosan solution, stirring for 20-40 min, adjusting the pH value to be neutral, then continuously stirring for 10-30 min, standing for aging, filtering, washing with water, and filtering to obtain a sterilization body;
(3) and adding the sterilizing body into the carrier solution, stirring, homogenizing, and then spray drying to obtain the long-acting bactericide based on the disodium hydrogen phosphite.
2. The long-acting disodium hydrogenphosphite-based bactericide according to claim 1, wherein: in the step (1): the acid solution is acetic acid solution with mass concentration of 1-3%, the pH value of the chitosan solution is 5-6, and the mass concentration of the water-soluble carrier in the carrier solution is 20-30%.
3. The long-acting disodium hydrogenphosphite-based bactericide according to claim 1, wherein: in the step (1): the molecular weight of chitosan is 5 × 103 - 5×105The mass ratio of the chitosan to the disodium hydrogen phosphite is 70-120:1, and the mass ratio of the chitosan to the water-soluble carrier is 1: 0.5-1.5.
4. The long-acting disodium hydrogenphosphite-based bactericide according to claim 3, wherein: the chitosan has a molecular weight of 1 × 104 - 1×105The mass ratio of the chitosan to the disodium hydrogen phosphite is 80-100:1, and the mass ratio of the chitosan to the water-soluble carrier is 1: 1-1.5.
5. The long-acting disodium hydrogenphosphite-based bactericide according to claim 1, wherein: the water-soluble carrier in the step (1) is one or more of polyethylene glycol, poloxamer, polyvinyl alcohol, povidone, methylcellulose, ethyl cellulose, hydroxypropyl cellulose and carboxymethyl cellulose.
6. The long-acting disodium hydrogenphosphite-based bactericide according to claim 1, wherein: the water-soluble carrier in the step (1) is polyethylene glycol.
7. The long-acting disodium hydrogenphosphite-based bactericide according to claim 1, wherein: the water-soluble carrier in the step (1) is polyethylene glycol 8000.
8. The long-acting disodium hydrogenphosphite-based bactericide according to claim 1, wherein: the long-acting bactericide based on the disodium hydrogen phosphite can be sprayed alone, or mixed with a foliar fertilizer for spraying, or irrigated to roots.
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