CN112574422A - Organosilicon surfactant for contact killing spider mite eggs and preparation method thereof - Google Patents
Organosilicon surfactant for contact killing spider mite eggs and preparation method thereof Download PDFInfo
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Abstract
The technical scheme of the invention discloses an organic silicon surfactant for killing spider mite eggs by contact and a preparation method thereof, wherein the organic silicon surfactant comprises low-molecular hydrogen-containing silicone oil, special allyl polyether X, special allyl polyether Y and a catalyst C; the low-molecular hydrogen-containing silicone oil comprises octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, tetramethyldisiloxane and a catalyst A; the special allyl polyether X comprises allyl alcohol, ethylene oxide, butylene oxide and a catalyst B; the special allyl polyether Y comprises allyl alcohol, ethylene oxide, propylene oxide, butylene oxide and a catalyst B. The organic silicon surfactant capable of killing spider mite eggs by contact is prepared by reacting low-molecular hydrogen-containing silicone oil, special allyl polyether X and special allyl polyether Y, and is good in contact killing effect and 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 spider mite eggs 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.
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.
Tetranychus is a common pest and disease damage of most crops, if the adult Tetranychus is poisoned, female insects pierce eggs into plant leaves through an ovipositor, photosynthesis of the pierced leaves is reduced, young plants can die, and the eggs can be hatched out of adults again in the near future to continuously damage crops, so that killing of the eggs of the Tetranychus is particularly important. The insecticides on the market today are not effective against spider mites of all developmental stages, for example pyrethroid insecticides like permethrin, fenpropathrin are very effective against adults but not much against larvae. Thus, killing adults and eggs of spider mites may require different substances.
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 or worm eggs 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 CN 108409971A discloses a method for preparing organic silicon modified polyether polyol, wherein allyl alcohol, ethylene oxide, propylene oxide and butylene 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 dispersing, leveling, wetting and penetrating 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 an organosilicon surfactant which has low molecular weight, low surface tension of an aqueous solution and good effect of killing spider mite eggs by contact is needed.
Disclosure of Invention
In order to solve the technical problem in the prior art, the invention provides the organic silicon surfactant for killing the spider mite eggs by contact and the preparation method thereof.
An organosilicon surfactant for killing spider mite eggs by contact comprises low-molecular hydrogen-containing silicone oil, special allyl polyether X, special allyl polyether Y and a catalyst C; the low-molecular hydrogen-containing silicone oil comprises octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, tetramethyldisiloxane and a catalyst A; the special allyl polyether X comprises allyl alcohol, ethylene oxide, butylene oxide and a catalyst B; the special allyl polyether Y comprises allyl alcohol, ethylene oxide, propylene oxide, butylene oxide and a catalyst B;
the mass ratio of the octamethylcyclotetrasiloxane, the tetramethylcyclotetrasiloxane and the tetramethyldisiloxane is (0-1.63): (0-0.44): 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 0.5-1.5% of the total mass of octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and tetramethyldisiloxane;
in the special allyl polyether X, the mass ratio of allyl alcohol, ethylene oxide and butylene oxide is 8: (3-5): (1-3); 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 and butylene oxide;
in the special allyl polyether Y, the mass ratio of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide is 9: (5-7): (0-1): (2-4); 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 0.05-0.1% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide;
the mass ratio of the special allyl polyether X to the special allyl polyether Y is (1-2): (3-5);
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 0.05-0.5%, and the mass of the catalyst C is 0.1-1% of the total mass of the low-molecular hydrogen-containing silicone oil, the special allyl polyether X and the special allyl polyether Y.
A preparation method of an organosilicon surfactant for contact killing spider mite eggs comprises the following steps:
s1, preparing low-molecular hydrogen-containing silicone oil, placing octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, tetramethyldisiloxane 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 X, adding allyl alcohol and a catalyst B into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing moisture at normal temperature and negative pressure, heating, adding a mixture of ethylene oxide and butylene oxide, reacting until the pressure is not reduced any more, and treating the catalyst B to obtain the special allyl polyether X;
s3, preparing special allyl polyether Y, adding allyl alcohol and a catalyst B into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing moisture 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 Y;
further, when moisture is removed at the normal temperature and the negative pressure in S2, the pressure is not more than-0.05 to-0.08 Mpa, when moisture is removed at the normal temperature and the negative pressure in S3, the pressure is not more than-0.08 to-0.1 Mpa, and the temperature is 110 to 130 ℃ after temperature rise;
further, when the catalyst B is treated in the S2 and S3, 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 adsorption time is 40-50 min, the mass of the activated clay in S2 is 0.3-2% of the total mass of allyl alcohol, ethylene oxide and butylene oxide, the mass of the activated clay in S3 is 0.3-2% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide, the mass of the diatomite in S2 is 0.1-0.5% of the total mass of allyl alcohol, ethylene oxide and butylene oxide, and the mass of the diatomite in S3 is 0.1-0.5% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide;
s4, preparing an organic silicon surfactant, namely adding the special allyl polyether X and the special allyl polyether Y into a reaction kettle, adding the 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 S4, the pressure is less than or equal to-0.1 MPa;
s5, 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 tetramethyldisiloxane 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 X is prepared by polymerizing allyl alcohol, ethylene oxide and butylene oxide under the condition of an alkaline catalyst B, and treating the catalyst B to obtain the special allyl polyether X. The special allyl polyether Y 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 Y. In the process of preparing the organic silicon surfactant, low-molecular hydrogen-containing silicone oil, special propyl alcohol polyether X and special propyl alcohol polyether Y react at high temperature to be transparent in the presence of a platinum catalyst, so that the low-molecular organic silicon surfactant capable of killing spider mite eggs by contact is obtained.
The main difference between the organic silicon surfactant and the preparation method of the organic silicon surfactant for killing spider mites by contact in the company is that the organic silicon surfactant needs to be prepared in a targeted manner according to the characteristics of surface cells of spider mite eggs because special propyl alcohol polyether X and special propyl alcohol polyether Y are properly proportioned, cells on the surfaces of adults and eggs of spider mites are different, the sensitivity of the cells to the organic silicon surfactant is different. According to the invention, in the preparation process of the organic silicon surfactant, the butylene oxide plays an important role, and the prepared organic silicon surfactant can destroy the phospholipid layer of cells of spider mite eggs and dissolve cell membranes so as to dehydrate and die the spider mite eggs through the specific mass ratio of the butylene oxide to the ethylene oxide and the propylene oxide and the mass ratio of the special propyl alcohol polyether X to the special propyl alcohol polyether Y. After the epoxybutane is removed or the mass ratio of the epoxybutane to the ethylene oxide to the propylene oxide is changed and the mass ratio of the special-base propyl alcohol polyether X to the special-base propyl alcohol polyether Y is changed, the generated organic silicon surfactant can only play a role in enhancing the spreading and adhesion of liquid medicine on the surface of the plant, and has poor contact killing effect on spider mite eggs. 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, so that eggs of spider mites die and fall off within 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.
By adopting the technical scheme, the invention has the following beneficial effects:
(1) the organic silicon surfactant for contact killing of the spider mite eggs, which is prepared by the invention, is diluted by tap water in a high multiple and then sprayed on pest places of crops, so that the spider mite eggs can die and fall off within 12-24h, the use of pesticides is reduced, obvious toxicity is avoided, and the organic silicon surfactant is beneficial to environmental protection.
(2) In the preparation process, a small amount of byproduct water is generated only in the step of removing moisture at normal temperature and negative pressure in the process of preparing the special allyl polyether X and the special allyl polyether Y, three wastes are not generated, the environment pollution caused by chemical substances is prevented, the waste of the chemical substances is prevented, resources are saved, and the danger in the chemical operation process is reduced.
(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 contact killing spider mite eggs according to the invention;
FIG. 2 is a picture of spider mite eggs of crops that were not sprayed with silicone surfactant;
FIG. 3 is a picture of eggs broken by spider mite eggs sprayed on crops for 24 hours in example 3.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
An organosilicon surfactant for killing spider mite eggs by contact comprises low-molecular hydrogen-containing silicone oil, special allyl polyether X, special allyl polyether Y and a catalyst C; the low-molecular hydrogen-containing silicone oil comprises 44g of tetramethylcyclotetrasiloxane, 100g of tetramethyldisiloxane and 0.72g of concentrated sulfuric acid; the special allyl polyether X comprises 20g of allyl alcohol, 7.5g of ethylene oxide, 2.5g of butylene oxide and 3mg of sodium hydroxide; the special allyl polyether Y comprises 45g of allyl alcohol, 35g of ethylene oxide, 10g of butylene oxide and 45mg of sodium hydroxide;
the catalyst C is chloroplatinic acid, the mass fraction of pure chloroplatinic acid contained in the catalyst C is 0.05%, and the mass of the catalyst C is 0.264 g.
A preparation method of an organosilicon surfactant for contact killing spider mite eggs comprises the following steps:
s1, preparing low-molecular hydrogen-containing silicone oil, placing octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, tetramethyldisiloxane and concentrated sulfuric acid in a closed stirring kettle protected by nitrogen, uniformly stirring, reacting for 12 hours at the temperature of 60 ℃, adding 1.44g of sodium bicarbonate for neutralization, and filtering to obtain the low-molecular hydrogen-containing silicone oil;
s2, preparing special allyl polyether X, 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 activated clay 0.09g, adsorbing for 40min, and filtering to obtain the special allyl polyether X;
s3, preparing special allyl polyether Y, 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, increasing the pressure to-0.1 Mpa, heating to 110 ℃, adding a mixture of ethylene oxide, propylene oxide and butylene oxide, reacting until the pressure is not reduced, adding acetic acid to neutralize the sodium hydroxide, adding 0.27g of activated clay, absorbing for 40min, and filtering to obtain the special allyl polyether Y;
s4, preparing an organic silicon surfactant, namely adding special allyl polyether X and special allyl polyether Y into a reaction kettle, adding chloroplatinic acid, stirring for 10min at normal temperature, adding low-molecular hydrogen-containing silicone oil while stirring, keeping stirring, heating to 60 ℃ 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-0.1 Mpa;
s5, diluting the organic silicon surfactant by 1000 times with tap water, spraying the diluted organic silicon surfactant on the tetranychus urticae koch eggs of crops to enable the tetranychus urticae koch eggs to be completely covered by the organic silicon surfactant.
Example 2
An organosilicon surfactant for killing spider mite eggs by contact comprises low-molecular hydrogen-containing silicone oil, special allyl polyether X, special allyl polyether Y and a catalyst C; the low-molecular hydrogen-containing silicone oil comprises 81.5g of octamethylcyclotetrasiloxane, 22g of tetramethylcyclotetrasiloxane, 50g of tetramethyldisiloxane and 2.3g of acid clay; the special allyl polyether X comprises 20g of allyl alcohol, 12.5g of ethylene oxide, 7.5g of butylene oxide and 0.04g of potassium hydroxide; the special allyl polyether Y comprises 45g of allyl alcohol, 30g of ethylene oxide, 5g of propylene oxide, 20g of butylene oxide and 0.1g 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 2.935 g.
A preparation method of an organosilicon surfactant for contact killing spider mite eggs comprises the following steps:
s1, preparing low-molecular hydrogen-containing silicone oil, placing octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, tetramethyldisiloxane 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 X, 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, heating to 130 ℃, adding a mixture of ethylene oxide and butylene oxide, reacting until the pressure is not reduced, adding acetic acid to neutralize the potassium hydroxide, then adding 0.2g of diatomite, adsorbing for 50min, filtering, and processing a catalyst B to obtain the special allyl polyether X;
s3, preparing special allyl polyether Y, adding allyl alcohol and a catalyst B into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing moisture 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 potassium hydroxide, then adding 0.5g of diatomite, and absorbing for 50min, filtering, and treating the catalyst B to obtain the special allyl polyether Y;
s4, preparing an organic silicon surfactant, namely adding special allyl polyether X and special allyl polyether Y into a reaction kettle, adding a catalyst C, stirring for 15min at normal temperature, adding low-molecular hydrogen-containing silicone oil while stirring, keeping 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 at the pressure of-0.07 Mpa;
s5, diluting the organic silicon surfactant by 1000 times with tap water, spraying the diluted organic silicon surfactant on the tetranychus urticae koch eggs of crops to enable the tetranychus urticae koch eggs to be completely covered by the organic silicon surfactant.
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 the spider mite eggs of the crops to completely cover the eggs.
Blank control group
No reagent is sprayed on the eggs of the tetranychus urticae.
Comparative example 1
The difference from the solution of example 2 is the deletion of the special allyl polyether X.
Comparative example 2
The difference from the solution of example 2 is the deletion of the special allyl polyether Y.
Comparative example 3
The difference from the technical scheme of the embodiment 2 is as follows: the special allyl polyether X comprises 20g of allyl alcohol, 7g of ethylene oxide, 13g of butylene oxide and 0.04g of potassium hydroxide; the special allyl polyether Y comprises 45g of allyl alcohol, 35g of ethylene oxide, 15g of propylene oxide, 5g of butylene oxide and 0.1g of potassium hydroxide;
the above examples 1 to 3, blank control group and comparative examples 1 to 3 were cultured under the same conditions for 24 hours, and the egg breaking rate of the spider mite eggs was observed and calculated under a microscope, and the picture of the egg breaking rate of the spider mite eggs of the crops not sprayed with the silicone surfactant is shown in fig. 2, and the picture of the egg breaking rate of the spider mite eggs of the crops 24 hours after the example 3 was sprayed on the eggs of the spider mites of the crops is shown in fig. 3. The egg breaking rate of the spider mite eggs is detected at 4h, 12h and 24h respectively, and the leaf protecting rate of the crops is detected at 24h, and specific results are shown in table 1.
TABLE 1 egg-breaking rate of Tetranychus urticae eggs and leaf-protecting rate of crops
| Group of | Egg breaking rate of tetranychus urticae eggs | Egg breaking rate of spider mite eggs of 12h | Egg breaking rate of spider mite eggs of 24h | Leaf retention rate |
| Blank control group | 0 | 0 | 0 | 100％ |
| Example 1 | 20％ | 48％ | 77％ | 94％ |
| Example 2 | 25％ | 50％ | 80％ | 96％ |
| Example 3 | 20％ | 40％ | 64％ | 96％ |
| Comparative example 1 | 13％ | 25％ | 36％ | 96％ |
| Comparative example 2 | 10％ | 18％ | 28％ | 94％ |
| Comparative example 3 | 13％ | 28％ | 42％ | 94％ |
As can be seen from the results in Table 1, the eggs of the spider mites in examples 1-3 died obviously in 12-24h, and the results in examples 2 and 3 show that the effect of killing the eggs of the spider mites after 2000-fold dilution is slightly worse than that of killing the eggs of the spider mites after 1000-fold dilution, but the egg breaking rate of the eggs of the spider mites after 24h is still higher than 60% after 2000-fold dilution, and the effect is better. The egg breaking rate of the spider mite eggs of the comparative examples 1 to 2 is low, which shows that the effect of the organic silicon surfactant prepared by only using the special allyl polyether X or the special allyl polyether Y on contact killing of the spider mite eggs is poor, and the result of the comparative example 3 shows that the egg breaking rate of the spider mite eggs of the organic silicon surfactant can be obviously reduced by changing the mass ratio of ethylene oxide, propylene oxide and butylene oxide in the special allyl polyether X or the special allyl polyether Y, and that the organic silicon surfactant has good contact killing effect of the spider mite eggs only through the mass ratio. In addition, the examples 1 to 3 have good leaf retention rate, which shows that the organic silicon surfactant disclosed by the invention has very little damage to crops after being diluted by 1000 times or 2000 times, and the crops are effectively prevented from being damaged due to the spraying of the organic silicon surfactant.
Claims (7)
1. An organosilicon surfactant for killing spider mite eggs by contact, which is characterized in that: comprises low molecular hydrogen-containing silicone oil, special allyl polyether X, special allyl polyether Y and catalyst C; the low-molecular hydrogen-containing silicone oil comprises octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, tetramethyldisiloxane and a catalyst A; the special allyl polyether X comprises allyl alcohol, ethylene oxide, butylene oxide and a catalyst B; the special allyl polyether Y comprises allyl alcohol, ethylene oxide, propylene oxide, butylene oxide and a catalyst B;
the mass ratio of the octamethylcyclotetrasiloxane, the tetramethylcyclotetrasiloxane and the tetramethyldisiloxane is (0-1.63): (0-0.44): 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 0.5-1.5% of the total mass of octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane and tetramethyldisiloxane;
in the special allyl polyether X, the mass ratio of allyl alcohol, ethylene oxide and butylene oxide is 8: (3-5): (1-3); 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 and butylene oxide;
in the special allyl polyether Y, the mass ratio of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide is 9: (5-7): (0-1): (2-4); 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 0.05-0.1% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide;
the mass ratio of the special allyl polyether X to the special allyl polyether Y is (1-2): (3-5);
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 0.05-0.5%, and the mass of the catalyst C is 0.1-1% of the total mass of the low-molecular hydrogen-containing silicone oil, the special allyl polyether X and the special allyl polyether Y.
2. The method of claim 1, comprising the steps of:
s1, preparing low-molecular hydrogen-containing silicone oil, placing octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, tetramethyldisiloxane 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 X, adding allyl alcohol and a catalyst B into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing moisture at normal temperature and negative pressure, heating, adding a mixture of ethylene oxide and butylene oxide, reacting until the pressure is not reduced any more, and treating the catalyst B to obtain the special allyl polyether X;
s3, preparing special allyl polyether Y, adding allyl alcohol and a catalyst B into a reaction kettle, replacing air in the reaction kettle with nitrogen, removing moisture 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 Y;
s4, preparing an organic silicon surfactant, namely adding the special allyl polyether X and the special allyl polyether Y into a reaction kettle, adding the 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;
s5, 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 organosilicon surfactant for killing the eggs of the spider mites according to claim 2, wherein the organosilicon surfactant comprises the following components in percentage by weight: when the catalyst A is concentrated sulfuric acid, sodium bicarbonate is added for neutralization after the heat preservation reaction is finished, and then filtration is carried out, wherein the mass ratio of the sodium bicarbonate to the concentrated sulfuric acid is (1.7-2): 1.
4. The method for preparing the organosilicon surfactant for killing the eggs of the spider mites according to claim 2, wherein the organosilicon surfactant comprises the following components in percentage by weight: when the moisture is removed under the normal-temperature negative pressure in S2, the pressure is not more than-0.05 to-0.08 MPa, when the moisture is removed under the normal-temperature negative pressure in S3, the pressure is not more than-0.08 to-0.1 MPa, and the temperature is 110 to 130 ℃ after the temperature is raised.
5. The method for preparing the organosilicon surfactant for killing the eggs of the spider mites according to claim 2, wherein the organosilicon surfactant comprises the following components in percentage by weight: when the catalyst B was treated in the above S2 and S3, acetic acid was added to neutralize the catalyst B, followed by addition of an adsorbent and filtration.
6. The method for preparing the organosilicon surfactant for killing spider mite eggs by contact according to claim 5, wherein the organosilicon surfactant comprises the following components: the adsorbent is one of activated clay or diatomite, the adsorption time is 40-50 min, the mass of the activated clay in S2 is 0.3-2% of the total mass of allyl alcohol, ethylene oxide and butylene oxide, the mass of the activated clay in S3 is 0.3-2% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide, the mass of the diatomite in S2 is 0.1-0.5% of the total mass of allyl alcohol, ethylene oxide and butylene oxide, and the mass of the diatomite in S3 is 0.1-0.5% of the total mass of allyl alcohol, ethylene oxide, propylene oxide and butylene oxide.
7. The method for preparing the organosilicon surfactant for killing the eggs of the spider mites according to claim 2, wherein the organosilicon surfactant comprises the following components in percentage by weight: when the low volatile substances are removed under the negative pressure in the S4, the pressure is less than or equal to-0.1 Mpa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB716339A (en) * | 1951-04-02 | 1954-10-06 | California Research Corp | Improvements in or relating to copoly-ethers for use as synthetic lubricants |
| CN101690878A (en) * | 2009-10-13 | 2010-04-07 | 广州天赐有机硅科技有限公司 | Method for manufacturing organosilicon surfactant with T-shaped structure for pesticide |
| WO2013097167A1 (en) * | 2011-12-27 | 2013-07-04 | 广东标美硅氟新材料有限公司 | Silicone surfactant, and preparation method and use thereof |
| CN108409971A (en) * | 2018-02-07 | 2018-08-17 | 江西三越新材料有限公司 | A kind of preparation method of organosilicon modified polyether polyalcohol |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB716339A (en) * | 1951-04-02 | 1954-10-06 | California Research Corp | Improvements in or relating to copoly-ethers for use as synthetic lubricants |
| CN101690878A (en) * | 2009-10-13 | 2010-04-07 | 广州天赐有机硅科技有限公司 | Method for manufacturing organosilicon surfactant with T-shaped structure for pesticide |
| WO2013097167A1 (en) * | 2011-12-27 | 2013-07-04 | 广东标美硅氟新材料有限公司 | Silicone surfactant, and preparation method and use thereof |
| CN108409971A (en) * | 2018-02-07 | 2018-08-17 | 江西三越新材料有限公司 | A kind of preparation method of organosilicon modified polyether polyalcohol |
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