Dispersing agent, preparation method and pesticide dispersible oil suspending agent
By using dispersants prepared by dibasic acid, ricinoleic acid and alkyl alcohol polyoxyethylene polyoxypropylene ether, the problem of the decrease in stability of pesticide dispersible oil suspension agent when reducing viscosity is solved, the stability and fluidity are improved, and the preparation cost and environmental pollution are reduced.
Patent Information
- Application Number
- CN202411970090.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-30
- Publication Date
- 2025-04-15
AI Technical Summary
Existing pesticide dispersible oil suspensions often affect their stability while reducing their viscosity, and the use of a large number of surfactants and additives increases the production cost and environmental pollution risks.
A method of preparing a dispersant, including dibasic acid, ricinoleic acid and alkyl alcohol polyoxyethylene polyoxypropylene ether as raw materials, through esterification and polymerization, the final product with reduced acid value is prepared as a dispersant for use in pesticide dispersible oil suspension agent.
This dispersant can ensure the stability of pesticide dispersible oil suspension agent, while reducing its viscosity, reducing the amount of surfactant and additives, reducing the preparation cost and environmental pollution risks, and improving the dispersion effect and storage stability.
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Figure BDA0005219311440000102
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of pesticides, and in particular to a dispersant, a preparation method and a pesticide dispersible oil suspension. Background Art
[0002] Pesticide dispersible oil suspension is an important form of pesticide preparation. Its main feature is that the active ingredients of the pesticide are evenly dispersed in the oil medium in the form of tiny particles to form a stable suspension system. This preparation has good physical and chemical stability, and can effectively prevent the decomposition and loss of the active ingredients of the pesticide, thereby improving the use effect and safety of the pesticide. However, in the preparation process of pesticide dispersible oil suspension, it is often necessary to add a large amount of surfactants and other additives to emulsify the entire system so that it can enter the water in a good state and enhance the effect of the application. The use of these additives often reduces the stability of the pesticide suspension, and the viscosity cannot be improved, affecting its preparation and use performance.
[0003] In order to solve this problem, the existing solutions in the prior art are mainly to enhance the stability and viscosity by changing the type and amount of surfactants and adjusting the formula of other additives. For example, non-ionic surfactants such as alkylphenol polyoxyethylene ether can be used to reduce the viscosity of pesticide dispersible oil suspensions. In addition, the stability of pesticide dispersible oil suspensions can also be improved by adding additives such as thickeners and stabilizers.
[0004] However, the existing technology often affects the stability of pesticide dispersible oil suspensions while reducing their viscosity. This is because the use of surfactants and additives may change the physical and chemical properties of the active ingredients of the pesticide, resulting in reduced stability during storage and use. In addition, existing solutions often require the use of a large amount of surfactants and additives, which not only increases the preparation cost of pesticide dispersible oil suspensions, but may also cause environmental pollution. Therefore, how to reduce the viscosity of pesticide dispersible oil suspensions while ensuring their stability is a problem that needs to be solved urgently in this field. Summary of the invention
[0005] In order to solve the above technical problems, the present invention provides a dispersant, a preparation method and a pesticide dispersible oil suspension. The dispersant of the present invention is applied to the pesticide dispersible oil suspension, and can reduce the viscosity of the pesticide dispersible oil suspension while ensuring the stability of the pesticide dispersible oil suspension.
[0006] In order to achieve the technical effects of the present invention, the following technical solutions are adopted:
[0007] A method for preparing a dispersant, wherein the raw materials include dibasic acid, ricinoleic acid and alkyl alcohol polyoxyethylene polyoxypropylene ether; the preparation method comprises the following steps:
[0008] Step 1: conducting an esterification reaction between a dibasic acid and ricinoleic acid in the presence of a catalyst 1 until the acid value decreases from more than 280 mg / g to less than 180 mg / g to obtain an esterified product;
[0009] Step 2: adding alkyl alcohol polyoxyethylene polyoxypropylene ether and catalyst 2 to the esterification product, reacting at a temperature of 200-220° C. to prepare a final product having an acid value reduced to below 50 mg / g;
[0010] The molecular structure formula of the alkyl alcohol polyoxyethylene polyoxypropylene ether includes:
[0011] R-0-(CH2CH2O)m-(CH2(CH3)CH2O)nH; R is a normal alkyl group containing 12-14 carbon atoms; wherein m is an integer of 5-12, and n is 2.5-5.0; and the dibasic acid is a dibasic acid containing 19-22 carbon atoms.
[0012] As a further improvement, the raw materials for preparation include 30% dibasic acid, 15% ricinoleic acid and 55% alkyl alcohol polyoxyethylene polyoxypropylene ether; the amount of catalyst 1 and catalyst 2 is 0.5‰ of the amount of the raw materials for preparation; the catalyst 1 and catalyst 2 are both organic tin; the dibasic acid containing 19-22 carbon atoms is a dibasic acid containing 21 carbon atoms, and its molecular structure formula is:
[0013] X+Y=12, X, Y are integers and X≥0, Y≥0;
[0014] One of R1 and R2 is a carboxyl group and the other is a hydrogen atom.
[0015] As a further improvement, the preparation method of step 1 comprises: adding a dibasic acid, ricinoleic acid and a catalyst 1 into a reaction device, heating to 200-220° C. under nitrogen protection and stirring conditions, carrying out an esterification reaction at 200-220° C., and stopping heating when the acid value decreases from more than 280 mg / g to less than 180 mg / g; and stopping stirring when the temperature decreases to less than 60° C. to obtain an esterification product; and the dispersant is a pesticide dispersible oil suspension dispersant.
[0016] As a further improvement, the reactions of step 1 and step 2 are both carried out under nitrogen protection; the alkyl alcohol polyoxyethylene polyoxypropylene ether is a product sold by Jiangsu Secco Chemical Co., Ltd. under the trade names of SECOL-EP-5035, SECOL-EP-7025, SECOL-EP-9050, and SECOL-EP-12030; the molecular structural formula of the alkyl alcohol polyoxyethylene polyoxypropylene ether comprises the following structural formula:
[0017] Wherein, m is an integer of 5-12, n is 2.5-5.0, and when m is 7, n is not 4.5.
[0018] The present invention also provides a dispersant, which is prepared by the above-mentioned dispersant preparation method.
[0019] The present invention also provides a pesticide dispersible oil suspension, which comprises the above-mentioned dispersant, and the mass percentage of the dispersant in the pesticide dispersible oil suspension is 2-4%.
[0020] As a further improvement, the pesticide dispersible oil suspension comprises the following components by mass percentage: 30-40% of the original drug, 2-4% of the dispersant according to claim 6, 15% of the emulsifier, 3-7% of the stabilizer, and the balance is vegetable oil.
[0021] As a further improvement, the pesticide dispersible oil suspension is an insecticide, which contains the following components by mass percentage: 15% of dinotefuran, 15% of spirotetramat, 2-4% of the dispersant according to claim 6, OD-24%, 0D-711%, 1% of organic soil, 2% of white carbon black, and the balance is vegetable oil.
[0022] As a further improvement, the pesticide dispersible oil suspension is a herbicide, which contains the following components by mass percentage: 4% nicosulfuron, 12% mesotrione, 24% atrazine, 2-4% of the dispersant according to claim 4, 11% OD-7; 4% OD-2; 1% BHT; 1% organic soil, 1% white carbon, and the balance is vegetable oil.
[0023] The present invention has the following beneficial effects:
[0024] 1) The dispersant prepared by the present invention has good emulsification and dispersibility, and can effectively reduce the viscosity of the pesticide dispersible oil suspension, especially the viscosity after hot storage.
[0025] 2) The dispersant of the present invention is used as a dispersant in a pesticide dispersible oil suspension, which can make the pesticide dispersible oil suspension form a stable dispersion system, thereby improving the stability and fluidity of the pesticide dispersible oil suspension, making the pesticide dispersible oil suspension more convenient and more effective during use.
[0026] 3) The dispersant of the present invention is used as a dispersant in pesticide dispersible oil suspensions, which can reduce the amount of surfactants and additives used, thereby reducing the preparation cost of the pesticide dispersible oil suspension and the pollution to the environment.
[0027] 4) The dispersant of the present invention is used as a dispersant in pesticide dispersible oil suspensions, and the amount used is small, which can greatly save production and use costs.
[0028] 5) In addition, for the dispersible oil suspensions whose original drugs are dinotefuran and spirotetramat or whose original drugs are nicosulfuron, mesotrione and atrazine, it is difficult to achieve a good dispersing effect by using the dispersants in the prior art, but by using the dispersants of the present invention, a good dispersing effect can be achieved by using only 2-4%, thereby making the original drugs play a good role. DETAILED DESCRIPTION
[0029] A method for preparing a dispersant, wherein the raw materials include dibasic acid, ricinoleic acid and alkyl alcohol polyoxyethylene polyoxypropylene ether; the preparation method comprises the following steps:
[0030] Step 1: conducting an esterification reaction between a dibasic acid and ricinoleic acid in the presence of a catalyst 1 until the acid value decreases from more than 280 mg / g to less than 180 mg / g to obtain an esterified product;
[0031] Step 2: adding alkyl alcohol polyoxyethylene polyoxypropylene ether and catalyst 2 to the esterification product, reacting at a temperature of 200-220° C. to prepare a final product having an acid value reduced to below 50 mg / g;
[0032] The molecular structure formula of the alkyl alcohol polyoxyethylene polyoxypropylene ether includes:
[0033] R-0-(CH2CH2O)m-(CH2(CH3)CH2O)nH; R is a normal alkyl group containing 12-14 carbon atoms; wherein m is an integer of 5-12, and n is 2.5-5.0; and the dibasic acid is a dibasic acid containing 19-22 carbon atoms.
[0034] Preferably, the raw materials for preparation include 30% dibasic acid, 15% ricinoleic acid and 55% alkyl alcohol polyoxyethylene polyoxypropylene ether; the amount of catalyst 1 and catalyst 2 is 0.5‰ of the amount of the raw materials for preparation; the catalyst 1 and catalyst 2 are both organic tin; the dibasic acid containing 19-22 carbon atoms is a dibasic acid containing 21 carbon atoms (C21 dibasic acid), and its molecular structure formula is: X+Y=12, X and Y are integers and X≥0, Y≥0; one of R1 and R2 is a carboxyl group and the other is hydrogen.
[0035] Preferably, the preparation method of step 1 comprises: adding a dibasic acid, ricinoleic acid and a catalyst 1 into a reaction device, heating to 200-220° C. under nitrogen protection and stirring conditions, carrying out an esterification reaction at 200-220° C., and stopping heating when the acid value decreases from more than 280 mg / g to less than 180 mg / g; and stopping stirring when the temperature decreases to less than 60° C. to obtain an esterification product; and the dispersant is a pesticide dispersible oil suspension dispersant.
[0036] Preferably, the reactions of step 1 and step 2 are carried out under nitrogen protection; the alkyl alcohol polyoxyethylene polyoxypropylene ether is a product sold by Jiangsu Secco Chemical Co., Ltd. under the trade names of SECOL-EP-5035, SECOL-EP-7025, SECOL-EP-9050, and SECOL-EP-12030; the molecular structural formula of the alkyl alcohol polyoxyethylene polyoxypropylene ether comprises the following structural formula:
[0037] Wherein, m is an integer of 5-12, n is 2.5-5.0, and when m is 7, n is not 4.5.
[0038] Example 1
[0039] A method for preparing a dispersant, wherein the raw materials for preparing the dispersant (at room temperature) include 30% C21 dibasic acid, 15% ricinoleic acid and 55% high molar synthetic 5035 by weight percentage. The preparation method comprises the following steps:
[0040] Step 1: esterifying C21 dibasic acid with ricinoleic acid in the presence of catalyst 1 until the acid value decreases from more than 280 mg / g to less than 180 mg / g to obtain an esterified product;
[0041] That is, C21 dibasic acid, ricinoleic acid and catalyst 1 are added to a 1L four-necked reaction bottle, and the temperature is controlled and heated to 200-220°C under nitrogen and stirring protection conditions. At 200-220°C, the catalyst 1 is completely dissolved. As the esterification reaction proceeds, the acid value of the entire system decreases. When the acid value decreases from more than 280 mg / g to less than 180 mg / g, the heating is stopped. When the temperature drops to less than 60°C, the stirring is stopped to obtain the esterification product. The amount of the catalyst 1 is 0.5‰ of the total mass of the raw materials.
[0042] Step 2: Add alkyl alcohol polyoxyethylene polyoxypropylene ether and catalyst 2 to the esterification product, react at a temperature of 200-220° C. to prepare a final product with an acid value reduced to below 50 mg / g.
[0043] That is, add high-molecular compound 5035 and catalyst 2 to a four-necked reaction flask (or esterification product), heat to 200-220°C during stirring, and completely dissolve catalyst 2. As the reaction proceeds, the acid value of the entire system decreases. When the acid value decreases to below 50 mg / g, stop heating. When the temperature decreases to below 60°C, stop stirring to obtain the final product. The amount of catalyst 2 used is 0.5‰ of the total mass of the raw materials.
[0044] Example 2
[0045] The difference from Example 1 is that the raw material is replaced from high molar compound 5035 to high molar compound 7025; other substances, amounts and preparation methods are the same as those in Example 1.
[0046] Example 3
[0047] The difference from Example 1 is that the raw material is replaced from high molar compound 5035 to high molar compound 9045; other substances, dosages and preparation methods are the same as those in Example 1. The specific preparation method is as follows:
[0048] A method for preparing a dispersant, wherein the raw materials for preparing the dispersant (at room temperature) are 30% by weight of C21 dibasic acid, 15% of ricinoleic acid and 55% of high molar synthetic 9045. The preparation method comprises the following steps:
[0049] Step 1: esterifying C21 dibasic acid with ricinoleic acid in the presence of catalyst 1 until the acid value decreases from more than 280 mg / g to less than 180 mg / g to obtain an esterified product;
[0050] That is, C21 dibasic acid, ricinoleic acid and catalyst 1 are added to a 1L four-necked reaction bottle, and the temperature is controlled and heated to 200-220°C under nitrogen and stirring protection conditions. At 200-220°C, the catalyst 1 is completely dissolved. As the esterification reaction proceeds, the acid value of the entire system decreases. When the acid value decreases from more than 280 mg / g to less than 180 mg / g, the heating is stopped. When the temperature drops to less than 60°C, the stirring is stopped to obtain the esterification product. The amount of the catalyst 1 is 0.5‰ of the total mass of the raw materials.
[0051] Step 2: Add alkyl alcohol polyoxyethylene polyoxypropylene ether and catalyst 2 to the esterification product, react at a temperature of 200-220° C. to prepare a final product with an acid value reduced to below 50 mg / g.
[0052] That is, add high molar compound 9045 and catalyst 2 to the four-mouth reaction bottle (or esterification product), heat to 200-220°C during stirring, and completely dissolve catalyst 2. As the reaction proceeds, the acid value of the entire system decreases. When the acid value decreases to below 50 mg / g, stop heating. When the temperature decreases to below 60°C, stop stirring to obtain the final product. The amount of catalyst 2 is 0.5‰ of the total mass of the raw materials.
[0053] Example 4
[0054] The difference from Example 3 is that the raw material is replaced from high molar compound 9045 to high molar compound 12030; other substances, amounts and preparation methods are the same as those in Example 1.
[0055] Comparative Example 1
[0056] Comparative Example 1 is compared with Example 3, except that the high molar synthetic compound 9045 in the raw material is replaced by lactic acid, the other substances, amounts and preparation methods are the same as those in Example 3.
[0057] Comparative Example 2
[0058] Compared with Example 3, Comparative Example 2 differs from Example 3 in that, except for "the acid value is reduced to below 80 mg / g and heating is stopped" in step 2, the remaining prepared materials, amounts and preparation methods are the same as those in Example 3.
[0059] Comparative Example 3
[0060] The difference from Example 3 is that "the preparation raw materials are 15% C21 dibasic acid, 40% ricinoleic acid and 45% high molar synthetic compound 9045 by weight at room temperature", and the other substances, amounts and preparation methods are the same as those in Example 3.
[0061] Comparative Example 4
[0062] The difference from Example 3 is that the raw material is replaced from high molar compound 9045 to high molar compound 7045. The other substances, amounts and preparation methods are the same as those in Example 3.
[0063] Comparative Example 5
[0064] The difference from Example 3 is that the high molar compound 9045 in the raw material is replaced with polyethylene glycol (M W =500-3000), the remaining substances, amounts and preparation methods are the same as those in Example 3.
[0065] Comparative Example 6
[0066] The difference from Example 3 is that the high molar compound 9045 in the raw material is replaced by polyethylene glycol monomethyl ether, and the other substances, amounts and preparation methods are the same as those in Example 3.
[0067] Comparative Example 7
[0068] The difference from Example 3 is that the high molar compound 9045 in the raw material is replaced by a polyethylene oxide-propylene oxide block copolymer (MW=500-3000). The other substances, amounts and preparation methods are the same as those in Example 3.
[0069] Comparative Example 8
[0070] The difference from Example 3 is that the high molar compound 9045 in the raw material is replaced by a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (MW=500-3000). The other substances, amounts and preparation methods are the same as those in Example 3.
[0071] Comparative Example 9
[0072] A method for preparing a dispersant, wherein the raw materials for preparing the dispersant include 30% C21 dibasic acid, 15% ricinoleic acid and 55% high molar synthetic compound 9045 by weight at room temperature. The preparation method comprises the following steps:
[0073] Step 1: Add C21 dibasic acid, ricinoleic acid and catalyst 1 to a 1L four-necked reaction bottle, under nitrogen and stirring protection conditions, control the temperature to 20-40°C, stir at 20-40°C for 1 hour to mix the substances evenly, and obtain a mixture 1. The amount of the catalyst 1 is 0.5‰ of the total mass of the raw materials.
[0074] Step 2: Add high molar compound 9045 and catalyst 2 to mixture 1, control the temperature to 20-40°C, stir at 20-40°C for 1 hour to mix all substances evenly to obtain the final product.
[0075] Application of the final products described in Examples 1-4 and Comparative Examples 1-9
[0076] A pesticide dispersible oil suspension comprises the above-prepared dispersant, and the mass percentage of the dispersant in the pesticide dispersible oil suspension is 2-4%.
[0077] Preferably, the pesticide dispersible oil suspension is an insecticide or a herbicide, and the herbicide or the pesticide comprises the following components by mass percentage: 30-40% of the original drug, 4% of the final product prepared by any one of Examples 1-4 or any one of Comparative Examples 1-9, 15% of the emulsifier, 3-7% of the stabilizer, and the balance is vegetable oil. The total mass percentage of each component is 100%.
[0078] The specific raw materials and dosage of the insecticide are shown in Table 1, wherein the final product of the insecticide in Application Example 1 is the final product prepared by Examples 1-4 and Comparative Examples 1-9, respectively, and the final product of Application Example 2 is the final product prepared by Example 3.
[0079] Table 1
[0080] Application Example 1 Application Example 2 raw material Mass percentage / % Mass percentage / % use Dinotefuran 15 15 Technical drug Spirotetramat 15 15 Technical drug Final product 4 2 Dispersants OD-2 4 4 Emulsifier 0D-7 11 11 Emulsifier Organic soil 1 1 Stabilizer White Carbon Black 2 2 Stabilizer Vegetable oil Residue Residue Oil-based
[0081] The preparation method of the insecticide described in Table 1 is:
[0082] Add vegetable oil, emulsifier (OD-2 and 0D-7) and the final product into a sand mill, stir evenly, then add organic soil, white carbon black, technical drug (dinotefuran, spirotetramat), stir evenly again, sand mill for about 2 hours, and measure the suspension rate and emulsification when the particle size is D90≤5μm.
[0083] “Adding vegetable oil, emulsifier and final product into the sand mill” means that vegetable oil is first added into the sand mill, and then emulsifier and final product are added into the sand mill.
[0084] The specific raw materials and dosage of the herbicides are shown in Table 2. The final product of the herbicide in Application Example 3 is the final product prepared by using Examples 1-4 and Comparative Examples 1-9 respectively. Application Example 3 contains 13 herbicides, and the final product used in Application Example 4 is one herbicide made from the final product prepared in Example 3.
[0085] Table 2
[0086] Application Example 3 Application Example 4 Element Mass percentage / % Mass percentage / % use Nicosulfuron 4 4 Technical drug Mesotrione 12 12 Technical drug Atrazine 24 24 Technical drug Final product 4 2 Dispersants OD-7 11 11 Emulsifier OD-2 4 4 Emulsifier BHT (Butylated Hydroxytoluene) 1 1 Stabilizer Organic soil 1 1 Stabilizer White Carbon Black 1 1 Stabilizer Vegetable oil Residue Residue Oil-based
[0087] The preparation process of the above-mentioned herbicide is as follows: vegetable oil, emulsifier (OD-2 and OD-7), final product, and BHT are added to a sand mill, stirred evenly, and then organic soil, white carbon black, and technical drugs (nicosulfuron, mesotrione, and atrazine) are added. After stirring evenly again, the mixture is sand milled for about 2 hours, and the particle size is D90≤5μm. The suspension rate and emulsification properties are measured.
[0088] “Add vegetable oil, emulsifiers (OD-2 and OD-7), the final product and BHT into the sand mill” means first adding vegetable oil into the sand mill, and then adding emulsifiers OD-2, OD-7, the final product and BHT into the sand mill.
[0089] The test methods for the various properties of the pesticides in Table 1 and the herbicides in Table 2 are as follows:
[0090] 1. Storage stability at room temperature: refer to the standard NYT1427-2007 General Rules for Storage Stability Test of Pesticides at Room Temperature. The sample has no solid or oily precipitation after 3 months at room temperature;
[0091] 2. Low temperature storage stability: refer to the national standard GB / T 19137-2003 pesticide low temperature stability determination method, the sample is at 0℃, no solid or oily matter is precipitated after 7 days;
[0092] 3. High temperature storage stability: refer to the national standard GB / T 19136-2003 Pesticide thermal storage stability determination method. The sample is stored at 54°C for 14 days without solid or oily precipitation, and the decomposition rate of the active ingredient is ≤10%.
[0093] 4. Particle size: refer to the LS-POPCP laser particle size analyzer for particle size detection. The particle size growth rate before and after thermal storage is ≤20%;
[0094] 5. Suspension rate test method: refer to GBT 14825-2006 Pesticide suspension rate determination method.
[0095] 6. Emulsification performance test method: refer to GB / T 3776.3-1983 Pesticide emulsifier emulsification performance test method.
[0096] 7. Wet sieving test method: refer to GB / T 16150-1995.
[0097] 8. Persistent foaming test method: refer to GB / T 28137-2011.
[0098] 9. Tipping test method: refer to GB / T 31737-2015.
[0099] The test results are shown in Table 3 and Table 4. Examples 1-4 and Comparative Examples 1-9 in Table 3 are insecticides prepared using the final products prepared in Examples 1-4 and Comparative Examples 1-9 in Application Example 1 (the dosage of the final product is 4%), and Application Example 2 is an insecticide prepared using the final product prepared in Example 3 (the dosage of the final product is 2%).
[0100] Examples 1-4 and Comparative Examples 1-9 in Table 4 are herbicides prepared using the final products prepared in Examples 1-4 and Comparative Examples 1-9 in Application Example 3 (the dosage of the final product is 4%), and Application Example 4 is a herbicide prepared using the final product prepared in Example 3 (the dosage of the final product is 2%).
[0101] Table 3
[0102]
[0103]
[0104] Table 4
[0105]
[0106]
[0107] It can be seen from the data in Tables 3 and 4 that when the dispersant prepared by any one of Examples 1-4 of the present invention is used to prepare the pesticide or herbicide, the system can be kept from agglomerating during the grinding process, the suspension rate is high, the emulsification performance is good, and the obtained pesticide or herbicide is thermally stable at room temperature, low temperature, and high temperature.
[0108] The pesticide and herbicide provided by the present invention, the samples are stored in hot storage (high temperature storage), cold storage (low temperature storage) and room temperature for two years, and still maintain good stability and fluidity, and all indicators are qualified. This shows that the dispersant of the present invention has a good dispersing effect, and can make the pesticide and herbicide prepared by using the dispersant have good storage stability.
[0109] The production process of the dispersant of the present invention is safe and environmentally friendly, the sample has uniform appearance at room temperature, good fluidity, convenient production and operation, stable quality and performance, and small batch difference; the dispersant of the present invention has good general performance and environmental performance.
[0110] At the same time, when the dispersant of the present invention is applied to the herbicide or insecticide of the present invention, only 2-4% is used to form an insecticide or herbicide with good stable effect. This may be because the structure of the hydrophilic and lipophilic segments is more suitable for vegetable oils and the original drug of the present invention, resulting in unexpected technical effects.
[0111] In the examples and comparative examples, the stirring speed may be 200-250 r / min. In examples 1-4, "30% C21 dibasic acid, 15% ricinoleic acid and 55% high molar synthetic compound" may be 60 g C21 dibasic acid, 30 g ricinoleic acid and 110 g high molar synthetic compound. In step 1 and step 2, adding a certain substance means adding all of the substance.
[0112] It should be noted that in Table 1 and Table 2, the sum of the mass percentages of the various components after supplementation is 100%.
[0113] SEC0L-EP-5035 can also be called high mole compound 5035, SEC0L-EP-7025 can also be called high mole compound 7025, SEC0L-EP-7045 can also be called high mole compound 7045, SEC0L-EP-9050 can also be called high mole compound 9050, and SEC0L-EP-12030 can also be called high mole compound 12030.
[0114] In SECOL-EP-5035, SECOL-EP-7025, SECOL-EP-7045, SECOL-EP-9050 and SECOL-EP-12030, the general molecular structural formula of the main components is:
[0115] in,
[0116] In SEC0L-EP-5035, m is 5 and n is 3.5.
[0117] In SEC0L-EP-7025, m is 7 and n is 2.5.
[0118] In SEC0L-EP-7045, m is 7 and n is 4.5.
[0119] In SEC0L-EP-9050, m is 9 and n is 5.
[0120] In SEC0L-EP-12030, m is 12 and n is 3.
[0121] Emulsifiers OD-2 and OD-7 can be sold by Fuzhou Sugest New Material Technology Co., Ltd.
[0122] The preparation raw material described in the present invention does not contain catalyst 1 and catalyst 2.
[0123] The main component of the organic tin is dibutyltin dilaurate, with a CAS number of 77-58-7, which can be sold by Jinan Century Tongda Chemical Co., Ltd.
[0124] The above is only a preferred embodiment of the present invention, and it cannot be used to limit the scope of the present invention. That is, all simple equivalent changes and modifications made according to the contents recorded in the claims and the invention specification are still within the scope of the claims of the present invention. In addition, the abstract and title are only used to assist in searching patent documents, and are not used to limit the scope of the rights of the present invention.
Claims
1. A method for preparing a dispersant, characterized in that: The raw materials for its preparation include dibasic acid, ricinoleic acid and alkyl alcohol polyoxyethylene polyoxypropylene ether; and the preparation method thereof includes the following steps: Step 1: conducting an esterification reaction between a dibasic acid and ricinoleic acid in the presence of a catalyst 1 until the acid value decreases from more than 280 mg / g to less than 180 mg / g to obtain an esterified product; Step 2: adding alkyl alcohol polyoxyethylene polyoxypropylene ether and catalyst 2 to the esterification product, reacting at a temperature of 200-220° C. to prepare a final product having an acid value reduced to below 50 mg / g; The molecular structure formula of the alkyl alcohol polyoxyethylene polyoxypropylene ether includes: R-0-(CH2CH2O)m-(CH2(CH3)CH2O)nH; R is a normal alkyl group containing 12-14 carbon atoms; wherein m is an integer of 5-12, and n is 2.5-5.0; and the dibasic acid is a dibasic acid containing 19-22 carbon atoms.
2. The method for preparing a dispersant according to claim 1, characterized in that: The raw materials for preparation include 30% dibasic acid, 15% ricinoleic acid and 55% alkyl alcohol polyoxyethylene polyoxypropylene ether; the amount of catalyst 1 and catalyst 2 is 0.5‰ of the amount of the raw materials for preparation; the catalyst 1 and catalyst 2 are both organic tin; the dibasic acid containing 19-22 carbon atoms is a dibasic acid containing 21 carbon atoms, and its molecular structure formula is: X+Y=12, X and Y are integers and X≥0, Y≥0; one of R1 and R2 is a carboxyl group and the other is hydrogen.
3. The method for preparing a dispersant according to claim 1, characterized in that: The preparation method of step 1 comprises: adding dibasic acid, ricinoleic acid and catalyst 1 into a reaction device, heating to 200-220° C. under nitrogen protection and stirring conditions, carrying out esterification reaction at 200-220° C., stopping heating when the acid value decreases from more than 280 mg / g to less than 180 mg / g; and stopping stirring when the temperature decreases to less than 60° C. to obtain an esterification product; the dispersant is a pesticide dispersible oil suspension dispersant.
4. The method for preparing a dispersant according to claim 1, characterized in that: The reactions of step 1 and step 2 are all carried out under nitrogen protection; the alkyl alcohol polyoxyethylene polyoxypropylene ether is a product sold by Jiangsu Secco Chemical Co., Ltd. under the trade names of SECOL-EP-5035, SECOL-EP-7025, SECOL-EP-9050, and SECOL-EP-12030; the molecular structural formula of the alkyl alcohol polyoxyethylene polyoxypropylene ether comprises the following structural formula: Wherein, m is an integer of 5-12, n is 2.5-5.0, and when m is 7, n is not 4.
5.
5. A dispersant, characterized in that: The dispersant is prepared by the preparation method of the dispersant according to any one of claims 1 to 4.
6. A pesticide dispersible oil suspension, characterized in that: It comprises the dispersant according to claim 5, The mass percentage of the dispersant in the pesticide dispersible oil suspension is 2-4%.
7. A pesticide dispersible oil suspension according to claim 6, characterized in that: The pesticide dispersible oil suspension comprises the following components by mass percentage: 30-40% of the original drug, 2-4% of the dispersant according to claim 6, 15% of the emulsifier, 3% of the stabilizer, and the balance is vegetable oil.
8. The pesticide dispersible oil suspension according to claim 6, characterized in that: The pesticide dispersible oil suspension is an insecticide, which contains the following components by mass percentage: 15% of dinotefuran, 15% of spirotetramat, 2-4% of the dispersant according to claim 6, OD-24%, 0D-711%, 1% of organic soil, 2% of white carbon black, and the balance is vegetable oil.
9. The pesticide dispersible oil suspension according to claim 6, characterized in that: The pesticide dispersible oil suspension is a herbicide, which comprises the following components by mass percentage: 4% nicosulfuron, 12% mesotrione, 24% atrazine, 2-4% of the dispersant according to claim 4, 11% OD-7, 4% OD-2, 1% BHT, 1% organic soil, 1% white carbon black, the balance is vegetable oil.