CN111387179A - Avermectin B2a solvation solid and preparation method thereof - Google Patents
Avermectin B2a solvation solid and preparation method thereof Download PDFInfo
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
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Abstract
The invention relates to the technical field of pesticides, and particularly discloses an abamectin B2a solvated solid and a preparation method thereof. The abamectin B2a solvation solid contains a small molecular organic solvent combined with abamectin B2a molecules through intermolecular weak interaction in a crystal structure, the mass content of the small molecular organic solvent is 10-25%, the small molecular organic solvent is at least one of an organic solvent A or an organic solvent B, and the organic solvent A is an ester compound or a furan compound; the organic solvent B is an ether compound or C5‑C15Of (a) an alkane. The abamectin B2a solvation solid provided by the invention has good stability, the decomposition rate is less than 5% after sealed storage for 12 months at 40 ℃, the decomposition rate is less than or equal to 0.7% after storage at 4 ℃, and the requirements of storage and transportation conditions of abamectin B2a are greatly reduced.
Description
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to an abamectin B2a solvated solid and a preparation method thereof.
Background
The abamectin B2 comprises two main components B2a and B2B, wherein the abamectin B2a has special effect on underground nematodes and pests on the body surfaces of animals. The extraction and purification technology of the abamectin B2a in the industrial production has gained a qualitative leap, and the abamectin B2a technical product with the content of more than 90 percent can be prepared. However, the abamectin B2a has poor stability, high decomposition speed in storage at room temperature and decomposition rate of more than 50% in sealed storage at room temperature for 12 months, so the abamectin B2a must be stored at low temperature, which brings inconvenience to the use, storage and transportation of the abamectin B2 a.
At present, the abamectin B2a technical product still needs to be stored below 20 ℃ below zero, so that the abamectin B2a solid stable at room temperature needs to be developed urgently, the decomposition speed of the abamectin B2a is reduced, and the abamectin B2a technical product is convenient to use, store and transport.
Disclosure of Invention
Aiming at the problems of poor stability and high room-temperature decomposition speed of the existing abamectin B2a, the invention provides an abamectin B2a solvation solid and a preparation method thereof.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
an abamectin B2a solvation solid, the crystal structure of which contains a small molecular organic solvent combined with abamectin B2a molecules by weak intermolecular interaction, the mass content of the small molecular organic solvent is 10-25%,
the micromolecular organic solvent is at least one of an organic solvent A or an organic solvent B,
the organic solvent A is an ester compound or a furan compound; the organic solvent B is an ether compound or C5-C15Of (a) an alkane.
Compared with the prior art, the abamectin B2a solvated solid provided by the invention has the advantages that the abamectin B2a is dissolved in the organic solvent for recrystallization, the small molecular organic solvent is introduced into the crystal structure of the abamectin B2a to obtain the abamectin B2a solvated solid, the stability of the abamectin B2a is obviously improved, the abamectin B2a is hermetically stored at 40 ℃ for 12 months, the decomposition rate is less than 5%, almost no decomposition is generated during storage at 4 ℃, and the requirements of the abamectin B2a on storage and transportation conditions are greatly reduced.
Further, the ester compound is one of propyl acetate, isopropyl acetate, butyl acetate, sec-butyl acetate or tert-butyl acetate, and is doped into the crystal structure of the avermectin B2a, so that the stability of the avermectin B2a is improved.
Further, the furan compound is tetrahydrofuran or methyltetrahydrofuran, and forms a solvation solid with the abamectin B2a in the crystallization and drying processes, so that the stability of the abamectin B2a is improved.
Further, the ether compound is one of propyl ether, isopropyl ether, n-butyl ether, isobutyl ether or methyl tert-butyl ether, and is singly doped into the crystal structure of the avermectin B2a together with the ester compound and the furan compound to form the avermectin B2a to form a solvated solid, so that the stability of the avermectin B2a is improved.
The invention also provides a preparation method of the abamectin B2a solvation solid, which comprises the following steps:
dissolving the abamectin B2a solid into a small molecular organic solvent, cooling, crystallizing, filtering, and drying or not drying to obtain the abamectin B2a solvated solid.
Further, dissolving the abamectin B2a solid into an organic solvent A, cooling, crystallizing, filtering, and drying or not drying to obtain an abamectin B2a solvation solid containing the organic solvent A, wherein the using amount of the organic solvent A is 2-5 times of the mass of the abamectin B2a solid; if drying, the drying temperature is 40-60 deg.C, and the time is 1-3 h.
Further, dissolving the abamectin B2a solid into an organic solvent A, adding an organic solvent B until crystals are separated out, cooling, crystallizing, filtering, and drying or not, so as to obtain an abamectin B2a solvation solid containing the organic solvent B or the organic solvents A and B, wherein the using amount of the organic solvent A is 2-5 times of the mass of the abamectin B2a solid; the dosage of the organic solvent B is 1-6 times of the solid mass of the abamectin B2 a; if drying, the drying temperature is 40-80 deg.C, and the time is 3-5 h.
Further, dissolving the abamectin B2a solid into a mixture of an organic solvent A and an organic solvent B, cooling, crystallizing, filtering, drying or not drying to obtain an abamectin B2a solvation solid containing the organic solvent B or the organic solvent A and the organic solvent B, wherein the using amount of the organic solvent A is 2-5 times of the mass of the abamectin B2a solid; the dosage of the organic solvent B is 1-6 times of the solid mass of the abamectin B2 a; if drying, the drying temperature is 60-80 deg.C, and the time is 3-5 h.
Further, the dissolving temperature is 40-60 ℃; the temperature is reduced and the crystallization temperature is 0-20 ℃, and the time is 5-10 h.
Further, an antioxidant, such as 2, 6-di-tert-butyl-4-methylphenol (BHT), is added in the process of cooling crystallization to ensure the stability of the abamectin B2 a.
Further, nitrogen or argon inert gas is introduced for protection in the cooling crystallization process.
Compared with the prior art, the preparation method of the abamectin B2a solvated solid provided by the invention is simple in process and convenient to operate, the small-molecule organic solvent is doped into the crystal structure of abamectin B2a through recrystallization and drying treatment, the abamectin B2a solvated solid with good stability and low decomposition rate is obtained, and the defects of high requirement on storage conditions and inconvenience in use, storage and transportation are overcome.
Drawings
FIG. 1 is a first visualization model diagram of single crystal diffraction of the solvated solid of avermectin B2a in example 1;
FIG. 2 is a second visualization model diagram of single crystal diffraction of the solvated solid of avermectin B2a in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides an abamectin B2a solvation solid, the crystal structure of which contains a small molecular organic solvent combined with abamectin B2a molecules through weak intermolecular interaction, the mass content of the small molecular organic solvent is 10-25%,
the micromolecular organic solvent is at least one of an organic solvent A or an organic solvent B,
the organic solvent A is an ester compound or a furan compound; the organic solvent B is an ether compound or C5-C15Of (a) an alkane.
Specifically, a small-molecule organic solvent is doped and introduced into the crystal structure of the abamectin B2a, and a solvation solid of the abamectin B2a is formed through weak intermolecular interaction (van der Waals force), namely the small-molecule organic solvent is filled in the space gap of the abamectin B2a, and the doping of the small-molecule organic solvent changes the accumulation mode of molecules in the abamectin B2a crystal, so that the stability of the abamectin B2a crystal is improved.
To better illustrate the solvated solid of avermectin B2a provided in the examples of the present invention, further examples are provided below.
Example 1
The solvated solid of avermectin B2a consists of avermectin B2a crystals and isopropyl acetate in avermectin B2a crystal structures, wherein the mass content of the isopropyl acetate in the solvated solid is 25 percent, and the specific preparation method comprises the following steps:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of isopropyl acetate is added, the mixture is heated to 60 ℃, stirred and dissolved until the mixture is clear, the temperature is slowly reduced to 0-10 ℃, and crystallization is carried out for 5 hours, and filtration is carried out to obtain 110g of avermectin B2a solvated solid containing isopropyl acetate, wherein the content of isopropyl acetate is 25% (detected by adopting gas chromatography).
Example 2
The solvated solid of avermectin B2a consists of avermectin B2a crystals and isopropyl acetate in avermectin B2a crystal structures, wherein the mass content of the isopropyl acetate in the solvated solid is 10 percent, and the specific preparation method comprises the following steps:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of isopropyl acetate is added, the mixture is heated to 60 ℃ to be dissolved until the mixture is clear, the temperature is slowly reduced to 0-10 ℃ to be crystallized for 6h, the mixture is filtered, and the mixture is dried in vacuum for 3h at the temperature of 40 ℃ to obtain 93.5g of avermectin B2a solvation solid containing the isopropyl acetate, wherein the content of the isopropyl acetate is 10% (detected by adopting a gas chromatography).
Example 3
The solvated solid of avermectin B2a consists of avermectin B2a crystals and sec-butyl acetate in the avermectin B2a crystal structure, wherein the mass content of the sec-butyl acetate in the solvated solid is 12 percent, and the specific preparation method comprises the following steps:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 240g of sec-butyl acetate is added, the mixture is heated to 40 ℃, stirred for 4 hours until the mixture is dissolved and clarified, slowly cooled to 0-10 ℃, filtered and dried in vacuum for 1 hour at 40 ℃, and 70g of avermectin B2a solvation solid containing sec-butyl acetate is obtained, wherein the content of sec-butyl acetate is 12% (detected by adopting a gas chromatography).
Example 4
An avermectin B2a solvation solid consists of an avermectin B2a crystal and isopropyl acetate and n-butyl ether in an avermectin B2a crystal structure, the mass contents of the isopropyl acetate and the n-butyl ether in the solvation solid are respectively 3% and 18%, and the specific preparation method is as follows:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 600g of isopropyl acetate is added, the mixture is heated to 40 ℃, stirred and dissolved until the solution is clear, 600g of n-butyl ether is added, the mixture is continuously stirred until the mixture is uniform, after crystallization occurs, the mixture is slowly cooled to 10-20 ℃, crystallized for 10 hours, filtered and dried in vacuum at 60 ℃ for 3 hours, and 111g of avermectin B2a solvation solid is obtained, wherein the content of isopropyl acetate is 3%, and the content of n-butyl ether is 18% (detected by adopting gas chromatography).
Example 5
An avermectin B2a solvation solid consists of an avermectin B2a crystal and isopropyl acetate and n-butyl ether in an avermectin B2a crystal structure, the mass contents of the isopropyl acetate and the n-butyl ether in the solvation solid are 0.2 percent and 15 percent respectively, and the specific preparation method is as follows:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 600g of isopropyl acetate is added, the mixture is heated to 40 ℃, stirred and dissolved until the solution is clear, 600g of n-butyl ether is added, the mixture is uniformly stirred, after crystallization occurs, the temperature is slowly reduced to 10-20 ℃, the crystallization is carried out for 8 hours, the mixture is filtered, and vacuum drying is carried out for 3 hours at the temperature of 80 ℃, so that 104g of avermectin B2a solvated solid is obtained, wherein the content of the isopropyl acetate is 0.2%, and the content of the n-butyl ether is 15% (detected.
Example 6
The solvated solid of abamectin B2a consists of abamectin B2a crystals and n-butyl ether in an abamectin B2a crystal structure, wherein the mass content of the n-butyl ether in the solvated solid is 13 percent, and the specific preparation method comprises the following steps:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 600g of isopropyl acetate is added, 0.12g of antioxidant BHT is added, nitrogen is introduced for protection, the mixture is heated to 40 ℃, stirred and dissolved until the solution is clear, 600g of n-butyl ether is added, the mixture is continuously stirred and uniformly stirred, after crystallization occurs, the temperature is slowly reduced to 10-20 ℃ for crystallization for 6 hours, the mixture is filtered, and vacuum drying is carried out for 5 hours at 80 ℃, so that 112g of avermectin B2a solvated solid is obtained, wherein the content of isopropyl acetate is 0% and the content of n-butyl ether is 13% (detected by.
Example 7
An avermectin B2a solvation solid consists of sec-butyl acetate and n-butyl ether in avermectin B2a crystal and avermectin B2a crystal structures, the mass contents of the sec-butyl acetate and the n-butyl ether in the solvation solid are respectively 7% and 18%, and the specific preparation method comprises the following steps:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of sec-butyl acetate is added, the mixture is heated to 40 ℃, stirred and dissolved until the solution is clear, 360g of n-butyl ether is added, the mixture is stirred uniformly, after crystallization occurs, the temperature is slowly reduced to 10-20 ℃, the crystallization is carried out for 5 hours, the mixture is filtered, and vacuum drying is carried out for 4 hours at 70 ℃, so that 125g of avermectin B2a solvation solid is obtained, wherein the content of sec-butyl acetate is 7%, and the content of n-butyl ether is 18% (detected by adopting.
Example 8
An avermectin B2a solvation solid consists of sec-butyl acetate and n-butyl ether in avermectin B2a crystal and avermectin B2a crystal structures, the mass contents of the sec-butyl acetate and the n-butyl ether in the solvation solid are respectively 1% and 16%, and the specific preparation method comprises the following steps:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of sec-butyl acetate and 360g of n-butyl ether are added, the mixture is heated to 40 ℃ and stirred for 10h, slowly and naturally cooled to 10-20 ℃ for crystallization for 7h, filtered and dried in vacuum for 5h at 80 ℃ to obtain 123g of avermectin B2a solvated solid, wherein the content of sec-butyl acetate is 1% and the content of n-butyl ether is 16% (detected by adopting a gas chromatography).
Example 9
The solvated solid of abamectin B2a consists of tert-butyl acetate and heptane in the crystal structures of abamectin B2a and abamectin B2a, wherein the mass contents of the tert-butyl acetate and the heptane in the solvated solid are respectively 0.1 percent and 15 percent, and the specific preparation method comprises the following steps:
120g of crude abamectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, a mixed solvent of 240g of tert-butyl acetate and 240g of heptane is added, the temperature is reduced to 20 ℃ after dissolution, stirring and crystallization are carried out for 10h, filtration is carried out, vacuum drying is carried out for 3h at the temperature of 60 ℃, and 108g of abamectin B2a solvation solid is obtained, wherein the content of the tert-butyl acetate is 0.1%, and the content of the heptane is 15% (detected by adopting gas chromatography).
Example 10
An abamectin B2a solvation solid consists of tetrahydrofuran and n-butyl ether in an abamectin B2a crystal and an abamectin B2a crystal structure, wherein the mass contents of the tetrahydrofuran and the n-butyl ether in the solvation solid are respectively 4% and 19%, and the specific preparation method comprises the following steps:
60g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 240g of tetrahydrofuran is added, the mixture is heated to 40 ℃ to be dissolved until the mixture is clear, 360g of n-butyl ether is added and stirred uniformly, after crystallization occurs, the mixture is slowly and naturally cooled to 10-20 ℃ to be crystallized for 6 hours, and filtration is carried out to obtain 52.8g of avermectin B2a solvated solid, wherein the tetrahydrofuran content is 4% and the n-butyl ether content is 19% (detected by adopting gas chromatography).
Example 11
An abamectin B2a solvation solid consists of tetrahydrofuran and n-butyl ether in an abamectin B2a crystal and an abamectin B2a crystal structure, wherein the mass contents of the tetrahydrofuran and the n-butyl ether in the solvation solid are 0.1 percent and 18 percent respectively, and the specific preparation method comprises the following steps:
60g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 240g of tetrahydrofuran is added, the mixture is heated to 40 ℃ to be dissolved until the mixture is clear, 360g of n-butyl ether is added and stirred uniformly, after crystallization occurs, the mixture is slowly and naturally cooled to 10-20 ℃ to be crystallized for 5 hours, and filtered and dried in vacuum at 40 ℃ for 3 hours to obtain 52.8g of avermectin B2a solvated solid, wherein the content of tetrahydrofuran is 0.1%, and the content of n-butyl ether is 18% (detected by adopting a gas chromatography).
Example 12
The solvated solid of abamectin B2a consists of tert-butyl acetate and isobutyl ether in abamectin B2a crystal and abamectin B2a crystal structures, the mass contents of the tert-butyl acetate and the isobutyl ether in the solvated solid are respectively 0.1 percent and 16 percent, and the specific preparation method comprises the following steps:
120g of crude abamectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of tert-butyl acetate and 600g of isobutyl ether are added, the mixture is heated to 40 ℃ and stirred for 10h, slowly and naturally cooled to 10-20 ℃ for crystallization for 6h, filtered and dried in vacuum for 5h at 80 ℃ to obtain 119g of abamectin B2a solvated solid, wherein the content of the tert-butyl acetate is 0.1%, and the content of the isobutyl ether is 16% (detected by adopting a gas chromatography).
Example 13
The solvated solid of abamectin B2a consists of butyl acetate and propyl ether in abamectin B2a crystal and abamectin B2a crystal structures, the mass contents of the butyl acetate and the propyl ether in the solvated solid are respectively 10% and 15%, and the specific preparation method comprises the following steps:
120g of crude abamectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of butyl acetate is added, the mixture is heated to 40 ℃, stirred, dissolved and cleared, 600g of propyl ether is added, the temperature is slowly and naturally reduced to 10-20 ℃, crystallization is carried out for 7 hours, and filtration is carried out, thus obtaining 126g of abamectin B2a solvated solid, wherein the content of the butyl acetate is 10%, and the content of the propyl ether is 15% (detected by adopting a gas chromatography).
Example 14
The solvated solid of abamectin B2a consists of butyl acetate and propyl ether in abamectin B2a crystal and abamectin B2a crystal structures, the mass contents of the butyl acetate and the propyl ether in the solvated solid are respectively 10% and 15%, and the specific preparation method comprises the following steps:
120g of crude abamectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of butyl acetate is added, the mixture is heated to 40 ℃, stirred, dissolved and cleared, 600g of propyl ether is added, the temperature is slowly and naturally reduced to 10-20 ℃, crystallization is carried out for 7 hours, and filtration is carried out, thus obtaining 126g of abamectin B2a solvated solid, wherein the content of the butyl acetate is 10%, and the content of the propyl ether is 15% (detected by adopting a gas chromatography).
The content of the small molecular organic solvent in the abamectin B2a solvation solid obtained in the embodiment of the invention is detected by adopting a gas chromatography. Toluene or isopropyl acetate or n-heptane is used as an internal standard, acetonitrile is used as a solvent, and the specific gas chromatography conditions are as follows: the model of the chromatographic column is DM-624, the gasification temperature is 250 ℃, the detection temperature is 250 ℃, the temperature is programmed to rise, the temperature is kept at 50 ℃ for 5 minutes, the temperature rises to 125 ℃ at 15 ℃/minute, the temperature rises to 235 ℃ at 60 ℃/minute, and the temperature is kept for 3 minutes.
In order to better illustrate the technical solution of the present invention, further comparison is made below by means of a comparative example and an example of the present invention.
Comparative example 1
The solvated solid of abamectin B2a consists of abamectin B2a crystals and toluene in the abamectin B2a crystal structure, wherein the mass content of the toluene in the solvated solid is 10 percent, and the specific preparation method comprises the following steps:
60g of crude avermectin B2a (with the content of 85%) is taken and added into a 500m L four-mouth bottle, 480g of toluene is added, the mixture is stirred and dissolved at the temperature of 60 ℃ until the solution is clear, the temperature is slowly reduced to 10 ℃ for crystallization for 5 hours, a large amount of crystals appear, the solution is filtered, and vacuum drying is carried out at the temperature of 40 ℃ for 1 hour to remove part of the toluene solvent, so that 35g of avermectin B2a solvation solid is obtained, and the toluene content is 10% (detected by adopting a gas.
Comparative example 2
The solvated solid of abamectin B2a consists of abamectin B2a crystals and toluene in the abamectin B2a crystal structure, wherein the mass content of the toluene in the solvated solid is 10 percent, and the specific preparation method comprises the following steps:
60g of crude abamectin B2a (with the content of 85%) is taken and added into a 500m L four-mouth bottle, 480g of toluene is added, the mixture is stirred and dissolved at the temperature of 60 ℃ until the solution is clear, the temperature is slowly reduced to 10 ℃ for crystallization for 5 hours, a large amount of crystals appear, and filtration is carried out to obtain 42g of abamectin B2a solvated solid, and the content of toluene is 25% (detected by adopting a gas chromatography).
Comparative example 3
An avermectin B2a solvation solid consists of avermectin B2a crystals and n-butyl ether in an avermectin B2a crystal structure, the mass content of the n-butyl ether in the solvation solid is respectively 1% (compared with example 8, the mass content of the n-butyl ether is low without sec-butyl acetate), and the specific preparation method comprises the following steps:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of sec-butyl acetate and 360g of n-butyl ether are added, the mixture is heated to 40 ℃ and stirred for 10h, slowly and naturally cooled to 10-20 ℃ for crystallization for 7h, filtered and dried in vacuum for 5h at 110 ℃ to obtain 101g of avermectin B2a solvated solid, wherein the content of sec-butyl acetate is 0% and the content of n-butyl ether is 1% (detected by adopting a gas chromatography).
Comparative example 4
An avermectin B2a solvation solid is composed of avermectin B2a crystals and isopropyl acetate in an avermectin B2a crystal structure, wherein the mass content of the isopropyl acetate in the solvation solid is 0.1% (compared with example 1, the content of the isopropyl acetate is low and almost non-existent), and the specific preparation method is as follows:
120g of crude avermectin B2a (with the content of 85%) is taken and added into a four-mouth bottle of 1L, 360g of isopropyl acetate is added, the mixture is heated to 60 ℃, stirred and dissolved until the mixture is clear, the temperature is slowly reduced to 0-10 ℃, crystallization is carried out for 5 hours, filtration is carried out, and drying is carried out for 2 hours at 80 ℃, so that 110g of avermectin B2a solvation solid containing isopropyl acetate is obtained, wherein the content of isopropyl acetate is 0.1% (detected by adopting a gas chromatography).
In order to better illustrate the characteristics of the abamectin B2a solvated solid provided by the embodiment of the invention, the abamectin B2a solvated solid obtained in the embodiment 1 is subjected to an X-ray single crystal diffraction test, and three-dimensional crystal structure data are obtained and a visual model is established, as shown in FIGS. 1 and 2. As shown in fig. 1 and 2, the isopropyl acetate is filled in the molecular space of the avermectin B2a, the abamectin B2a solvation solid is formed through weak intermolecular interaction (van der waals force), and the doping of the small molecular organic solvent isopropyl acetate changes the accumulation mode of molecules in the avermectin B2a crystal, thereby improving the stability of the avermectin B2a crystal.
Meanwhile, the abamectin B2a solvated solids prepared in examples 1 to 14 and comparative examples 1 to 5 were stored for 12 months to examine the decomposition rate of abamectin B2a, and the results are shown in table 1.
TABLE 1
The data show that the abamectin B2a solvated solid provided by the embodiment of the invention has good stability, the decomposition rate is less than 5% after being hermetically stored for 12 months at 40 ℃, almost no decomposition (the decomposition rate is less than or equal to 0.7%) is generated after being stored at 4 ℃, and the requirements on storage and transportation conditions of abamectin B2a are greatly reduced.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. An abamectin B2a solvation solid, which is characterized in that: the crystal structure of the abamectin benzoate-abamectin composite material contains a small molecular organic solvent which is combined with abamectin B2a molecules through weak intermolecular interaction, the mass content of the small molecular organic solvent is 10-25%,
the micromolecular organic solvent is at least one of an organic solvent A or an organic solvent B,
the organic solvent A is an ester compound or a furan compound; the organic solvent B is an ether compound or C5-C15Of (a) an alkane.
2. The solvated solid of abamectin B2a of claim 1, wherein: the ester compound is one of propyl acetate, isopropyl acetate, butyl acetate, sec-butyl acetate or tert-butyl acetate.
3. The solvated solid of abamectin B2a of claim 1, wherein: the furan compound is tetrahydrofuran or methyltetrahydrofuran.
4. The solvated solid of abamectin B2a of claim 1, wherein: the ether compound is one of propyl ether, isopropyl ether, n-butyl ether, isobutyl ether or methyl tert-butyl ether.
5. A process for preparing abamectin B2a solvated solid according to any one of claims 1 to 4, comprising the steps of:
dissolving the abamectin B2a solid into a small molecular organic solvent, cooling, crystallizing, filtering, and drying or not drying to obtain the abamectin B2a solvated solid.
6. A process for the preparation of abamectin B2a solvated solid according to claim 5, wherein: dissolving the abamectin B2a solid into an organic solvent A, cooling, crystallizing, filtering, and drying or not, so as to obtain an abamectin B2a solvated solid containing the organic solvent A, wherein the using amount of the organic solvent A is 2-5 times of the mass of the abamectin B2a solid; if drying, the drying temperature is 40-60 deg.C, and the time is 1-3 h.
7. A process for the preparation of abamectin B2a solvated solid according to claim 5, wherein: dissolving the abamectin B2a solid into an organic solvent A, adding an organic solvent B until crystals are separated out, cooling, crystallizing, filtering, drying or not, and obtaining an abamectin B2a solvation solid containing the organic solvent B or the organic solvents A and B, wherein the using amount of the organic solvent A is 2-5 times of the mass of the abamectin B2a solid, and the using amount of the organic solvent B is 1-6 times of the mass of the abamectin B2a solid; if drying, the drying temperature is 40-80 deg.C, and the time is 3-5 h.
8. A process for the preparation of abamectin B2a solvated solid according to claim 5, wherein: dissolving the abamectin B2a solid into a mixture of an organic solvent A and an organic solvent B, cooling, crystallizing, filtering, and drying or not, so as to obtain an abamectin B2a solvation solid containing the organic solvent B or the organic solvents A and B, wherein the using amount of the organic solvent A is 2-5 times of the mass of the abamectin B2a solid; the dosage of the organic solvent B is 1-6 times of the solid mass of the abamectin B2 a; if drying, the drying temperature is 60-80 deg.C, and the time is 3-5 h.
9. A process for the preparation of an avermectin B2a solvated solid according to any of claims 5 to 8, wherein: the dissolving temperature is 40-60 ℃; the temperature is reduced and the crystallization temperature is 0-20 ℃, and the time is 5-10 h.
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| WO2021218001A1 (en) * | 2020-04-29 | 2021-11-04 | 河北威远生物化工有限公司 | Avermectin b2a solvated solid and preparation method therefor |
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| CN114137121A (en) * | 2021-12-01 | 2022-03-04 | 河北威远生物化工有限公司 | Method for determining content of stable solvent in abamectin B2a technical material |
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