CN112574424A - Organic silicon surfactant for killing tetranychus by contact and preparation method thereof - Google Patents
Organic silicon surfactant for killing tetranychus by contact and preparation method thereof Download PDFInfo
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Abstract
The technical scheme of the invention discloses an organic silicon surfactant for killing tetranychus by contact and a preparation method thereof, wherein the organic silicon surfactant comprises low-molecular hydrogen-containing silicone oil, special allyl polyether and a catalyst C; the low-molecular hydrogen-containing silicone oil comprises octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and a catalyst A; specific allyl polyethers include allyl alcohol, ethylene oxide, propylene oxide, butylene oxide and catalyst B; the mass ratio of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide is 100: (50-80): (0-10): (20-40); the catalyst B is one or two of sodium-based catalyst or potassium-based catalyst, and the catalyst B is 0.01-0.1% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide. The organic silicon surfactant capable of killing tetranychus mites in a contact way is prepared by reacting low-molecular hydrogen-containing silicone oil with special allyl polyether, has a good contact killing effect, and is environment-friendly.
Description
Technical Field
The invention relates to the technical field of preparation of agricultural chemical preparations, in particular to an organic silicon surfactant for killing tetranychus by contact and a preparation method thereof.
Background
The organosilicon surfactant is a special surfactant prepared by addition reaction. Compared with the traditional carbon-based surfactant, the organic silicon surfactant has lower surface tension, particularly the surface tension of an aqueous solution of the organic silicon surfactant can reach below 20 dyne in a low molecular state, and the organic silicon surfactant is an excellent dispersing, leveling, wetting and penetrating aid.
Tetranychus, also known as red spider mite and spider mite, gnaws stems and leaves and fruits of plants, adult mites entangle a layer of sparse wire mesh on the plants, and when the plants are seriously damaged, leaves become thin and white to enable the leaves to fall off completely. Currently, pyrethroid insecticides such as permethrin, fenpropathrin, and the like are commonly used for the control of spider mites. As a big agricultural country, China has always high pesticide consumption, and reducing the pesticide consumption is an important aspect beneficial to the environment and organisms. However, in recent years, agricultural pests and diseases frequently burst, and it is important to reduce the amount of agricultural chemicals without reducing the effect. The surfactant is one of important auxiliary agents in modern pesticides, and is an auxiliary agent for enhancing the spreading and attaching effects of the liquid medicine on the surfaces of plants. But at present, the application of singly adopting a surfactant for killing insects is not available.
In the prior art, ethylene oxide, propylene oxide and the like are mostly adopted in the preparation of the organic silicon surfactant, and patent CN108409971A discloses a method for preparing organic silicon modified polyether polyol, wherein allyl alcohol, ethylene oxide and propylene oxide are adopted in the preparation of allyl polyether, butylene oxide is not used, the surface activity of the obtained organic silicon surfactant is not ideal, the surface tension of an aqueous solution is not low enough, and the dispersion, leveling, wetting and permeation effects cannot be achieved. Patent CN 107011507B discloses allyl alcohol compounds and epoxy compounds polymerized to produce allyl polyether polyol, the epoxy compound component is one or more of propylene oxide, ethylene oxide and butylene oxide, but does not disclose the ratio of butylene oxide to ethylene oxide and propylene oxide, and is used for preparing polyurethane memory sponge, and is not used in the agricultural insecticidal field. Therefore, the development of a low-molecular organosilicon surfactant with low surface tension of an aqueous solution and good tetranychus miticide contact effect is needed.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides the organic silicon surfactant for killing the tetranychus by contact and the preparation method thereof.
An organosilicon surfactant for killing tetranychus mites by contact comprises low-molecular hydrogen-containing silicone oil, special allyl polyether and a catalyst C; the low-molecular hydrogen-containing silicone oil comprises octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and a catalyst A; the special allyl polyether comprises allyl alcohol, ethylene oxide, propylene oxide, butylene oxide and a catalyst B;
the mass ratio of the octamethylcyclotetrasiloxane, the hexamethyldisiloxane to the tetramethylcyclotetrasiloxane is (0-1.35): (0.1-0.37): 1; the catalyst A is one or more of concentrated sulfuric acid, acid clay and trifluoromethanesulfonic acid, and the mass of the catalyst A is 0.01-0.5% of the total mass of octamethylcyclotetrasiloxane, hexamethyldisiloxane and tetramethylcyclotetrasiloxane;
the mass ratio of the allyl alcohol to the ethylene oxide to the propylene oxide to the butylene oxide is 100: (50-80): (0-10): (20-40); the catalyst B is one or two of a sodium-based catalyst or a potassium-based catalyst, and the mass of the catalyst B is 0.01-0.1% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide;
the catalyst C is one or more of chloroplatinic acid solution of chloroplatinic acid and isopropanol and complex solution of tetramethyl divinyl disiloxane-chloroplatinic acid, the mass fraction of pure chloroplatinic acid contained in the catalyst C is 0.1-0.5%, and the mass of the catalyst C is 0.06-1% of the total mass of the low-molecular hydrogen-containing silicone oil and the special allyl polyether.
A preparation method of an organosilicon surfactant for killing tetranychus by contact comprises the following steps:
s1, preparing low-molecular hydrogen-containing silicone oil, placing octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and catalyst A in a closed stirring kettle protected by nitrogen, stirring uniformly, reacting for 6-12h at the temperature of 60-80 ℃, and filtering to obtain the low-molecular hydrogen-containing silicone oil;
further, when the catalyst A is concentrated sulfuric acid, adding sodium bicarbonate for neutralization after the heat preservation reaction is finished, and then filtering, wherein the mass ratio of the sodium bicarbonate to the concentrated sulfuric acid is (1.7-2): 1;
s2, preparing special allyl polyether, adding allyl alcohol and a catalyst B into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing water at normal temperature and negative pressure, heating, adding a mixture of ethylene oxide, propylene oxide and butylene oxide, reacting until the pressure is not reduced any more, and treating the catalyst B to obtain the special allyl polyether;
further, when water is removed at the normal temperature and under the negative pressure in the S2, the pressure is less than or equal to-0.1 Mpa, and the temperature is 110-130 ℃ after the temperature is increased;
further, when the catalyst B is treated in the step S2, acetic acid is added to neutralize the catalyst B, then an adsorbent is added, and the filtration is carried out;
further, the adsorbent is one of activated clay or diatomite, the mass of the activated clay is 0.3-2% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide, the mass of the diatomite is 0.1-0.5% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide, and the adsorption time is 40-50 min;
s3, preparing an organic silicon surfactant, adding special allyl polyether into a reaction kettle, adding a catalyst C, stirring at normal temperature for 10-15 min, adding low-molecular hydrogen-containing silicone oil while stirring, maintaining stirring, heating to 60-100 ℃ under the protection of nitrogen, reacting to be transparent, and removing low-volatile substances under negative pressure to obtain the organic silicon surfactant;
further, when low-volatility substances are removed under negative pressure in the S3, the pressure is less than or equal to-0.1 MPa;
s4, diluting the organic silicon surface active agent by 1000-2000 times by using tap water, and then spraying for use.
When the low-molecular hydrogen-containing silicone oil is prepared, octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and hexamethyldisiloxane are subjected to ring opening polymerization under an acidic condition, and after polymerization, the catalyst A is treated to obtain the low-molecular hydrogen-containing silicone oil. The special allyl polyether is prepared by polymerizing allyl alcohol, ethylene oxide, propylene oxide and butylene oxide under the condition of an alkaline catalyst B, and treating the catalyst B to obtain the special allyl polyether. In the process of preparing the organic silicon surfactant, low-molecular hydrogen-containing silicone oil and special propyl alcohol polyether are reacted at high temperature to be transparent in the presence of a platinum catalyst, so that the low-molecular organic silicon surfactant capable of killing tetranychus urticae by contact is obtained. In the preparation process of the organic silicon surfactant, the butylene oxide plays an important role, and the organic silicon surfactant generated by the reaction of the prepared special allyl polyether and the low-molecular hydrogen-containing silicone oil can destroy the phospholipid layer of cells of the spider mites and dissolve cell membranes by the specific mass ratio of the butylene oxide, the ethylene oxide and the propylene oxide, so that the spider mites die. The generated organic silicon surfactant can only play a role in enhancing the spreading and adhesion of liquid medicine on the surface of a plant by removing butylene oxide or changing the mass ratio of butylene oxide to ethylene oxide and propylene oxide, has no obvious effect on phospholipid layers of cells of spider mites, cannot dissolve cell membranes of the spider mites, and cannot be used alone for killing the spider mites. The organic silicon surfactant prepared by the invention can be diluted by 1000-2000 times by using tap water and then sprayed on pest parts of crops to completely cover the pest parts, spider mites die and fall off in 12-24 hours, and the organic silicon surfactant can be diluted by using the tap water, has high dilution ratio, does not need water with higher requirements such as pure water and the like, reduces the cost, is easy to operate, and has obvious effect. The dilution is 1000-2000 times, which not only can ensure good insecticidal effect, but also can prevent the plant from being damaged due to the spraying of the surfactant. In addition, the organic silicon surfactant provided by the invention also has a certain effect on other insect pests such as aphids and cotton spider mites.
By adopting the technical scheme, the invention has the following beneficial effects:
(1) the organic silicon surfactant for killing tetranychus urticae by contact prepared by the invention is free from obvious toxicity and harm, is environment-friendly, is an excellent surfactant, can be diluted by running water at a high multiple and then sprayed to pest and pest places of crops, can kill and drop tetranychus urticae within 12-24 hours, has a certain contact killing effect on other insect pests such as aphids and cotton tetranychus urticae, and reduces the use of pesticides.
(2) In the preparation process, a small amount of byproduct water is generated only in the step of removing water at normal temperature and negative pressure in the process of preparing the special allyl polyether, no three wastes are generated, the waste of resources is reduced, and the environmental pollution caused by chemical substances is prevented.
(3) The preparation method is simple, time-saving and labor-saving, and has the advantages of easily available raw materials and low cost.
Drawings
FIG. 1 is a flow chart of a method for preparing an organosilicon surfactant for touch-killing tetranychus urticae.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
An organosilicon surfactant for killing tetranychus mites by contact comprises low-molecular hydrogen-containing silicone oil, special allyl polyether and a catalyst C; the low-molecular hydrogen-containing silicone oil comprises 37g of hexamethyldisiloxane, 100g of tetramethylcyclotetrasiloxane and 13.7mg of concentrated sulfuric acid; the special allyl polyether comprises 100g of allyl alcohol, 50g of ethylene oxide, 20g of butylene oxide and 17mg of sodium hydroxide;
the catalyst C is chloroplatinic acid, the mass fraction of pure chloroplatinic acid contained in the catalyst C is 0.5%, and the mass of the catalyst C is 184.2 mg.
A preparation method of an organosilicon surfactant for killing tetranychus urticae by contact comprises the following steps as shown in figure 1:
s1, preparing low-molecular hydrogen-containing silicone oil, placing hexamethyldisiloxane, tetramethylcyclotetrasiloxane and concentrated sulfuric acid in a closed stirring kettle protected by nitrogen to be uniformly stirred, keeping the temperature at 60 ℃ to react for 12 hours, adding sodium bicarbonate to neutralize, wherein the mass of the sodium bicarbonate is 26.03mg, and filtering to obtain the low-molecular hydrogen-containing silicone oil;
s2, preparing special allyl polyether, adding allyl alcohol and sodium hydroxide into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing water at normal temperature and negative pressure, heating to 110 ℃, adding a mixture of ethylene oxide and butylene oxide, reacting until the pressure is not reduced, adding acetic acid to neutralize the sodium hydroxide, adding 0.51g of activated clay, adsorbing for 40min, and filtering to obtain the special allyl polyether;
s3, preparing an organic silicon surfactant, namely adding special allyl polyether into a reaction kettle, adding chloroplatinic acid, stirring for 10min at normal temperature, adding low-molecular hydrogen-containing silicone oil while stirring, maintaining stirring, heating to 60 ℃ under the protection of nitrogen, reacting to be transparent, removing low-volatile substances under negative pressure, wherein the pressure is-0.1 Mpa, and thus obtaining the organic silicon surfactant;
and S4, diluting the organic silicon surfactant by 1000 times with tap water, and spraying the diluted organic silicon surfactant to pest places of crops to completely cover the pest places.
Example 2
An organosilicon surfactant for killing tetranychus mites by contact comprises low-molecular hydrogen-containing silicone oil, special allyl polyether and a catalyst C; the low-molecular hydrogen-containing silicone oil comprises 135g of octamethylcyclotetrasiloxane, 10g of hexamethyldisiloxane, 100g of tetramethylcyclotetrasiloxane and 1.225g of acid clay; the special allyl polyether comprises 100g of allyl alcohol, 80g of ethylene oxide, 10g of propylene oxide, 40g of butylene oxide and 0.23g of potassium hydroxide;
the catalyst C is a chloroplatinic acid solution of isopropanol, the mass fraction of pure chloroplatinic acid contained in the catalyst C is 0.5%, and the mass of the catalyst C is 4.75 g.
A preparation method of an organosilicon surfactant for killing tetranychus by contact comprises the following steps:
s1, preparing low-molecular hydrogen-containing silicone oil, placing octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and acid clay in a closed stirring kettle protected by nitrogen to be uniformly stirred, carrying out heat preservation reaction at 80 ℃ for 6 hours, and filtering to obtain low-molecular hydrogen-containing silicone oil;
s2, preparing special allyl polyether, adding allyl alcohol and potassium hydroxide into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing water at normal temperature and negative pressure, increasing the pressure to-0.08 Mpa, heating to 130 ℃, adding a mixture of ethylene oxide, propylene oxide and butylene oxide, reacting until the pressure is not reduced, adding acetic acid to neutralize the potassium hydroxide, then adding 1.15g of diatomite, wherein the adsorption time is 50min, and filtering to obtain the special allyl polyether;
s3, preparing an organic silicon surfactant, namely adding special allyl polyether into a reaction kettle, adding a chloroplatinic acid solution of isopropanol, stirring for 15min at normal temperature, adding low-molecular hydrogen-containing silicone oil while stirring, maintaining stirring, heating to-100 ℃ under the protection of nitrogen, reacting to be transparent, removing low-volatile substances under negative pressure, and obtaining the organic silicon surfactant, wherein the pressure is-0.05 Mpa;
and S4, diluting the organic silicon surfactant by 1000 times with tap water, and spraying the diluted organic silicon surfactant to pest places of crops to completely cover the pest places.
Example 3
The difference from the technical scheme of the embodiment 2 is that the organic silicon surfactant is diluted by 2000 times by using tap water and then sprayed on pest parts of crops to completely cover the pest parts.
Blank control group
The pest damage of the crops is not sprayed with any reagent.
Comparative example 1
The difference from the technical solution of example 2 is that the mass of butylene oxide is 0 g.
Comparative example 2
The difference from the technical scheme of the embodiment 2 is that the special allyl polyether comprises 100g of allyl alcohol, 50g of ethylene oxide, 75g of propylene oxide, 5g of butylene oxide and 0.23g of potassium hydroxide.
In the above examples 1-3, the blank control group and the comparative examples 1-2 were cultured under the same conditions for 24h, and the mites were selected from the pests and tested, and the survival rates of the mites were observed and calculated under a microscope, and the survival rates of the mites were measured at 4h, 12h and 24h, respectively, and the leaf retention rate of the crops was measured at 24h, and the specific results are shown in table 1.
TABLE 1 survival rate of spider mites and leaf protection rate of crops
| Group of | Survival rate of 4h spider mites | Survival rate of spider mites of 12h | Survival rate of spider mites of 24h | Leaf retention rate |
| Blank control group | 100％ | 100％ | 100％ | 100％ |
| Example 1 | 75％ | 50％ | 5％ | 94％ |
| Example 2 | 73％ | 48％ | 1％ | 98％ |
| Example 3 | 75％ | 60％ | 19％ | 98％ |
| Comparative example 1 | 93％ | 90％ | 89％ | 94％ |
| Comparative example 2 | 93％ | 86％ | 84％ | 94％ |
As can be seen from the results in table 1, the spider mites died after 12h to 24h in examples 1 to 3 and had good effect of killing spider mites at 24h, and the results in examples 2 and 3 show that the effect of killing spider mites after 2000 times dilution is slightly worse than that after 1000 times dilution, but the survival rate of spider mites after 24h is less than 20%, and the effect is better. The comparative examples 1-2 have poor tetranychus-killing effect, which shows that the tetranychus-killing effect of the organic silicon surfactant can be obviously reduced by changing the mass ratio of ethylene oxide, propylene oxide and butylene oxide, and the tetranychus-killing effect can be obviously killed only by the mass ratio of the organic silicon surfactant. The leaf retention rate of the examples 1 to 3 is very high, which shows that the examples 1 to 3 have very little damage to crops, and effectively avoid the crops from being damaged by the examples 1 to 3.
In the above examples 1-2, the blank control group and the comparative examples 1-2 were cultured under the same conditions for 24h, aphids and spider mites were selected for insect pests and tested, the survival rates of the aphids and the spider mites were observed and calculated under a microscope, the survival rates of the aphids and the spider mites were detected at 24h, and the leaf protection rates of crops were detected, and the specific results are shown in table 2.
TABLE 2 survival rate and leaf retention rate of aphids and tetranychid mites
| Group of | Survival rate of aphids | Leaf retention rate of aphid group | Survival rate of cotton spider mite | Leaf retention rate of tetranychus urticae group |
| Blank control group | 100％ | 100％ | 100％ | 100％ |
| Example 1 | 4％ | 94％ | 3％ | 94％ |
| Example 2 | 3％ | 98％ | 3％ | 98％ |
| Example 3 | 20％ | 98％ | 19％ | 98％ |
| Comparative example 1 | 94％ | 94％ | 90％ | 94％ |
| Comparative example 2 | 94％ | 94％ | 88％ | 94％ |
As can be seen from the results in Table 2, the survival rates of the aphids and the cotton spider mites are lower than 20% after 24 hours in examples 1 to 3, and the insecticidal effect after the dilution by 2000 times is slightly worse than that after the dilution by 1000 times, which shows that the insecticidal effects of examples 1 to 3 are good, and the effect with low dilution times is better. The comparative examples 1-2 have poor aphid and tetranychus urticae-killing effects, which shows that the aphid and tetranychus urticae-killing effect of the organic silicon surfactant can be obviously reduced by changing the mass ratio of ethylene oxide, propylene oxide and butylene oxide, and the aphid and tetranychus urticae-killing effect can be well achieved only by the mass ratio of the invention. The leaf retention rate of the examples 1 to 3 is very high, which shows that the examples 1 to 3 have very little damage to crops and effectively avoid the crops from being damaged due to the use of the organosilicon surfactant.
Claims (7)
1. An organosilicon surfactant for killing tetranychus by contact, which is characterized in that: comprises low molecular hydrogen-containing silicone oil, special allyl polyether and catalyst C; the low-molecular hydrogen-containing silicone oil comprises octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and a catalyst A; the special allyl polyether comprises allyl alcohol, ethylene oxide, propylene oxide, butylene oxide and a catalyst B;
the mass ratio of the octamethylcyclotetrasiloxane, the hexamethyldisiloxane to the tetramethylcyclotetrasiloxane is (0-1.35): (0.1-0.37): 1; the catalyst A is one or more of concentrated sulfuric acid, acid clay and trifluoromethanesulfonic acid, and the mass of the catalyst A is 0.01-0.5% of the total mass of octamethylcyclotetrasiloxane, hexamethyldisiloxane and tetramethylcyclotetrasiloxane;
the mass ratio of the allyl alcohol to the ethylene oxide to the propylene oxide to the butylene oxide is 100: (50-80): (0-10): (20-40); the catalyst B is one or two of a sodium-based catalyst or a potassium-based catalyst, and the mass of the catalyst B is 0.01-0.1% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide;
the catalyst C is one or more of chloroplatinic acid solution of chloroplatinic acid and isopropanol and complex solution of tetramethyl divinyl disiloxane-chloroplatinic acid, the mass fraction of pure chloroplatinic acid contained in the catalyst C is 0.1-0.5%, and the mass of the catalyst C is 0.06-1% of the total mass of the low-molecular hydrogen-containing silicone oil and the special allyl polyether.
2. The method of claim 1, comprising the steps of:
s1, preparing low-molecular hydrogen-containing silicone oil, placing octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and catalyst A in a closed stirring kettle protected by nitrogen, stirring uniformly, reacting for 6-12h at the temperature of 60-80 ℃, and filtering to obtain the low-molecular hydrogen-containing silicone oil;
s2, preparing special allyl polyether, adding allyl alcohol and a catalyst B into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing water at normal temperature and negative pressure, heating, adding a mixture of ethylene oxide, propylene oxide and butylene oxide, reacting until the pressure is not reduced any more, and treating the catalyst B to obtain the special allyl polyether;
s3, preparing an organic silicon surfactant, adding special allyl polyether into a reaction kettle, adding a catalyst C, stirring at normal temperature for 10-15 min, adding low-molecular hydrogen-containing silicone oil while stirring, maintaining stirring, heating to 60-100 ℃ under the protection of nitrogen, reacting to be transparent, and removing low-volatile substances under negative pressure to obtain the organic silicon surfactant;
s4, diluting the organic silicon surface active agent by 1000-2000 times by using tap water, and then spraying for use.
3. The method for preparing the silicone surfactant for killing tetranychus urticae as claimed in claim 2, wherein: and when the catalyst A in the S1 is concentrated sulfuric acid, adding sodium bicarbonate for neutralization after the heat preservation reaction is finished, and filtering, wherein the mass ratio of the sodium bicarbonate to the concentrated sulfuric acid is (1.7-2): 1.
4. The method for preparing the silicone surfactant for killing tetranychus urticae as claimed in claim 2, wherein: when water is removed at the normal temperature under negative pressure in the S2, the pressure is less than or equal to-0.1 Mpa, and the temperature is 110-130 ℃ after the temperature is raised.
5. The method for preparing the silicone surfactant for killing tetranychus urticae as claimed in claim 2, wherein: when the catalyst B is treated in the step S2, acetic acid is added to neutralize the catalyst B, and then an adsorbent is added to filter the solution.
6. The method for preparing the silicone surfactant for killing tetranychus urticae as claimed in claim 5, wherein: the adsorbent is one of activated clay or diatomite, the mass of the activated clay is 0.3-2% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide, the mass of the diatomite is 0.1-0.5% of the total mass of the allyl alcohol, the ethylene oxide, the propylene oxide and the butylene oxide, and the adsorption time is 40-50 min.
7. The method for preparing the silicone surfactant for killing tetranychus urticae as claimed in claim 2, wherein: when the low volatile substances are removed under the negative pressure in the S3, the pressure is less than or equal to-0.1 Mpa.
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