Diflufenican-containing compound and processing technology thereof

Abstract

The invention discloses a diflufenican-containing compound and a processing technology thereof, and relates to the technical field of agriculture. The diflufenican-containing compound agent is prepared from the following components in percentage by mass: 10 to 20 percent of diflufenican, 8 to 12 percent of isoproturon, 8 to 12 percent of florasulam, 0.5 to 1 percent of an anti-freezing agent, 0.5 to 1 percent of a de-foaming agent, 1.5 to 2.5 percent of a cosolvent, 1 to 3 percent of a wetting agent, 0.5 to 1 percent of a preservative, 1.5 to 3.5 percent of a dispersing agent and the balance of water. The defoaming agent is prepared from butynediol diethoxy ether grafted with low-hydrogen polydimethylsiloxane, and the defoaming agent is prepared from the butynediol diethoxy ether grafted with low-hydrogen polydimethylsiloxane; the dispersing agent is prepared from polyether amine bridging modified sodium lignin sulfonate. The pesticide is loaded on the nano silicon dioxide, so that the pesticide has good release performance and stability, the utilization rate of the pesticide is improved, the nano pesticide is small in size, the pesticide can better permeate into plant tissues, and a better prevention and treatment effect is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of agriculture, and in particular to a diflufenicol-containing compound agent and a processing technology thereof. Background Art

[0002] Applying chemical herbicides is the most effective way to remove weeds in farmland, but long-term application of chemical herbicides of a single variety or mode of action will cause problems such as herbicide residues, weed resistance, and environmental pollution. The development of new varieties of herbicides is costly and wasteful. In contrast, the development of compound herbicides requires less investment, has a shorter R&D cycle, and has higher economic benefits.

[0003] Flufenacet is a carotenoid biosynthesis inhibitor that destroys chlorophyll and cells, leading to plant death. It is suitable for control in barley and wheat fields. When applied before or after weed germination, it can form a leaching-resistant drug layer on the soil surface, which remains active during crop growth. When weeds germinate, they absorb the drug, resulting in a decrease in the carotenoid content in the weed plants, chlorophyll destruction, cell membrane rupture, and weed wilt and die.

[0004] The use of compound herbicides can improve the control effect, reduce residues, and delay the occurrence and development of weed resistance and drug resistance. Therefore, we propose a compound agent containing diflufenicol and its processing technology. Summary of the invention

[0005] The object of the present invention is to provide a diflufenicol-containing compound and a processing technology thereof, so as to solve the problems raised in the prior art.

[0006] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a compound containing diflufenicol, comprising the following mass components: in mass percentage, 10-20% diflufenicol, 8-12% isoproturon, 8-12% bispyribac, 0.5-1% antifreeze, 0.5-1% defoamer, 1.5-2.5% cosolvent, 1-3% wetting agent, 0.5-1% preservative, 1.5-3.5% dispersant, and the rest is water.

[0007] In the above technical scheme, difluanid is suitable for controlling various broad-leaved weeds such as cleaver, purslane, Amaranthus retroflexus, wild pea, Artemisia selengensis and bindweed in barley and wheat fields; isoproturon is suitable for controlling annual weeds such as alopecuroides and crabgrass in tomato and potato fields; and bispyribac is mainly used for controlling broad-leaved weeds in winter wheat.

[0008] Furthermore, the antifreeze agent is one or a mixture of ethylene glycol and calcium chloride;

[0009] The wetting agent is one or a mixture of fatty alcohol polyoxyethylene ether, sodium dodecyl sulfate, and calcium dodecylbenzene sulfonate;

[0010] The cosolvent is one or a mixture of propylene glycol, ethylene glycol and glycerin;

[0011] The preservative is one or a mixture of formaldehyde, benzoic acid, sodium benzoate and potassium sorbate.

[0012] Furthermore, the defoaming agent is prepared by grafting butynediol diethoxy ether with low-hydrogen polydimethylsiloxane.

[0013] Furthermore, the dispersant is prepared by polyetheramine bridge-modified sodium lignin sulfonate.

[0014] A processing technology of a difluanid-containing compound comprises the following steps:

[0015] Add diflufenac, isoproturon, bispyribac, cosolvent and water to a batching kettle, stir for 1 to 1.5 hours to form a slurry, send the resulting slurry to a grinder, grind it coarsely for 1.5 to 2.5 hours to obtain a coarse abrasive, then send the coarse abrasive to a sand mill for sand grinding for 2.5 to 3.5 hours, then transport it to a mixing kettle, add antifreeze, defoamer, wetting agent, preservative and dispersant, stir for 0.5 to 1.5 hours, then add nano silicon dioxide, stir for 6 to 8 hours to obtain a compound containing diflufenac.

[0016] Furthermore, the compound containing difluanid includes the following mass components: in mass percentage, 10-20% difluanid, 8-12% isoproturon, 8-12% bispyribac, 0.5-1% antifreeze, 0.5-1% defoamer, 1.5-2.5% solubilizer, 1-3% wetting agent, 0.5-1% preservative, 1.5-3.5% dispersant, 1-5% nano silicon dioxide, and the balance is water.

[0017] Further, diflufenicol CAS number: 83164-33-4, from Jiangsu Heyutai Chemical Co., Ltd.;

[0018] Isoproturon CAS number: 34123-59-6, from Jiangsu Heyutai Chemical Co., Ltd.;

[0019] Bispyribac CAS number: 145701-23-1, from Jiangsu Heyutai Chemical Co., Ltd.;

[0020] Furthermore, nano silicon dioxide CAS number: 7440-21-3, diameter: 1-50 nm, comes from Jiangsu Xianfeng Nanomaterials Co., Ltd.

[0021] Furthermore, the defoamer is prepared by grafting butynediol diethoxy ether with low hydrogen polydimethylsiloxane, and the specific process is as follows:

[0022] Add low hydrogen polydimethylsiloxane, butynediol diethoxy ether, isopropanol and Speier catalyst into a reaction kettle, heat to 85-90°C within 30 minutes under a nitrogen atmosphere, react for 5-6 hours, and after the reaction is completed, distill under reduced pressure and dry in vacuum to obtain a defoaming agent.

[0023] Furthermore, the mass ratio of low hydrogen polydimethylsiloxane, butynediol diethoxy ether, isopropanol and Speier catalyst is (0.5-1): (0.5-1): (1-2): (0.11-0.21).

[0024] Furthermore, the temperature of the reduced pressure distillation is 40-45° C., and the time is 1-2 h.

[0025] Furthermore, the process conditions of vacuum drying are: temperature: 35-45°C, time: 31-36h.

[0026] Furthermore, the Speier catalyst is a chloroplatinic acid-isopropanol solution with a mass fraction of 2%;

[0027] Chloroplatinic acid CAS number: 18497-13-7, from Jiangsu Jinwo New Materials Co., Ltd.;

[0028] Isopropyl alcohol CAS number: 67-63-0, from Wuxi Changyu Chemical Raw Materials Co., Ltd.

[0029] Furthermore, butynediol diethoxy ether CAS number: 112-34-5, purity: 99%, comes from Wuhan Yalong New Materials Co., Ltd.

[0030] Further, low hydrogen polydimethylsiloxane is prepared by the following process:

[0031] Add high hydrogen polydimethylsiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane to a three-necked flask, heat in a water bath to 30-35°C, add methylsulfonic acid, stir at constant temperature for 18-20 hours, then add NaHCO3 aqueous solution, wait for the mixed solution to be heated to 30-35°C, transfer to a split funnel, wash with water until the lower layer is neutral, and distill under reduced pressure to obtain low hydrogen polydimethylsiloxane.

[0032] Furthermore, the mass ratio of high hydrogen polydimethylsiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and NaHCO3 aqueous solution is (2-4): (2-4): 1: (0.5-1).

[0033] Furthermore, the temperature of the reduced pressure distillation is 40-45° C., and the time is 1-2 h.

[0034] Further, high hydrogen polydimethylsiloxane CAS number: 63148-62-9, hydrogen content: 0.13%, from Foshan Guirunbao Biotechnology Co., Ltd.;

[0035] Octamethylcyclotetrasiloxane CAS number: 556-67-2, purity: 99%, from Merck reagent;

[0036] Hexamethyldisiloxane CAS number: 107-46-0, purity: 99%, from Merck reagent;

[0037] Methanesulfonic acid CAS number: 75-75-2, from Shandong Tianshili Biotechnology Co., Ltd.

[0038] Furthermore, the mass fraction of NaHCO3 aqueous solution is 10%, NaHCO3, CAS No.: 144-55-8, sourced from Tianjin Biboyuan Technology Development Co., Ltd.

[0039] In the above technical scheme, low hydrogen polydimethylsiloxane has good appearance fluidity and water dispersibility, low surface tension, and excellent defoaming and antifoaming properties. The present invention introduces the acetylenic group and alcoholic hydroxyl group of butynediol diethoxy ether into the low hydrogen polydimethylsiloxane to undergo hydrosilylation, so that the product has excellent defoaming and antifoaming properties and good wetting and spreading properties.

[0040] Furthermore, the dispersant is prepared by polyetheramine bridged modified sodium lignin sulfonate, and the specific process is as follows:

[0041] The sodium lignin sulfonate aqueous solution is heated to 85-95° C., then mixed with polyetheramine, stirred evenly, and then formaldehyde aqueous solution is added to react at a constant temperature, and then cooled to 20-30° C. to obtain modified sodium lignin sulfonate.

[0042] Furthermore, the mass ratio of the sodium lignin sulfonate aqueous solution, the polyetheramine, and the formaldehyde aqueous solution is 1:(0.3-0.5):(0.2-0.4).

[0043] Furthermore, the constant temperature is 85-95° C., and the reaction time is 1-1.5 h.

[0044] Furthermore, the mass fraction of the sodium lignin sulfonate aqueous solution is 25%, and the CAS number of sodium lignin sulfonate is 8061-51-6; it comes from Yingxin Laboratory;

[0045] The mass fraction of formaldehyde aqueous solution is 10%, formaldehyde CAS number: 50-00-0, derived from pre-derivative chemistry;

[0046] Polyetheramine CAS number: 9046-10-0, from Jinan Jinyu Chemical Co., Ltd.

[0047] In the above technical scheme, sodium lignin sulfonate achieves the purpose of dispersion through electrostatic repulsion and steric hindrance to maintain the stability of the system. Its electrostatic repulsion comes from the sulfonic acid group as a strong electrolyte, and the sulfonic acid group will affect the solubility of sodium lignin sulfonate in water. The complex spatial structure of sodium lignin sulfonate will affect the steric hindrance, and the spatial structure is related to the molecular weight. Therefore, the present invention uses sodium lignin sulfonate as a raw material, formaldehyde as an initiator, and a bridging reaction with polyetheramine to obtain modified sodium lignin sulfonate, change its sulfonic acid group content and molecular weight, and improve the dispersion performance of sodium lignin sulfonate while maintaining the stability of the system.

[0048] Compared with the prior art, the present invention has the following beneficial effects:

[0049] 1. By modifying low-hydrogen polydimethylsiloxane, the acetylene group and alcoholic hydroxyl group of butynediol diethoxy ether are introduced into low-hydrogen polydimethylsiloxane, and hydrosilylation occurs, so that the product has excellent defoaming and anti-foaming properties and good wetting and spreading properties; at the same time, nano-silica acts as a functional additive and synergizes with the modified polydimethylsiloxane to further improve the performance of the defoamer.

[0050] 2. Modified sodium lignin sulfonate is obtained by bridging polyetheramine with sodium lignin sulfonate, changing its sulfonic acid group content and molecular weight, thereby improving the dispersion performance of sodium lignin sulfonate while maintaining the stability of the system.

[0051] 3. The present invention loads pesticides onto nano-silicon dioxide, so that the pesticides have good release performance and stability, and improve the utilization rate of the pesticides. In addition, the small size of the nano-pesticides helps the pesticides to better penetrate into plant tissues, thereby achieving better control effects. DETAILED DESCRIPTION

[0052] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0053] In the following specific implementations,

[0054] The antifreeze agent is ethylene glycol, CAS number: 107-21-1; the cosolvent is propylene glycol, CAS number: 57-55-6; the purity is 99%, and they are from Jinan Deying Chemical Co., Ltd.

[0055] The wetting agent is sodium dodecyl sulfate, CAS number: 151-21-3, purity 94%, from Anhui Fengzhen Environmental Protection Technology Co., Ltd.;

[0056] The preservative is formaldehyde, CAS number: 50-00-0, derived from pre-derivative chemistry;

[0057] Difluanid CAS number: 83164-33-4, from Jiangsu Heyutai Chemical Co., Ltd.;

[0058] Isoproturon CAS number: 34123-59-6, from Jiangsu Heyutai Chemical Co., Ltd.;

[0059] Bispyribac CAS number: 145701-23-1, from Jiangsu Heyutai Chemical Co., Ltd.;

[0060] Nano-silicon dioxide CAS number: 7440-21-3, diameter: 1-50nm, from Jiangsu Xianfeng Nanomaterials Co., Ltd.

[0061] The mass fraction of NaHCO3 aqueous solution is 10%, NaHCO3, CAS No.: 144-55-8, from Tianjin Biboyuan Technology Development Co., Ltd.;

[0062] High hydrogen polydimethylsiloxane CAS number: 63148-62-9, purity: 99%, from Foshan Guirunbao Biotechnology Co., Ltd.

[0063] Octamethylcyclotetrasiloxane CAS number: 556-67-2, purity: 99%, from Merck reagent;

[0064] Hexamethyldisiloxane CAS number: 107-46-0, purity: 99%, from Merck reagent;

[0065] Methanesulfonic acid CAS number: 75-75-2, from Shandong Tianshili Biotechnology Co., Ltd.

[0066] Butynediol diethoxy ether CAS number: 112-34-5, purity: 99%, from Wuhan Yalong New Materials Co., Ltd.;

[0067] The Speier catalyst is chloroplatinic acid-isopropanol solution with a mass fraction of 2%;

[0068] Chloroplatinic acid CAS number: 18497-13-7, from Jiangsu Jinwo New Materials Co., Ltd.;

[0069] Isopropyl alcohol CAS number: 67-63-0, from Wuxi Changyu Chemical Raw Materials Co., Ltd.

[0070] The mass fraction of sodium lignin sulfonate aqueous solution is 25%, CAS number of sodium lignin sulfonate: 8061-51-6; from Yingxin Laboratory;

[0071] The mass fraction of formaldehyde aqueous solution is 10%, formaldehyde CAS number: 50-00-0, derived from pre-derivative chemistry;

[0072] Polyetheramine CAS number: 9046-10-0, from Jinan Jinyu Chemical Co., Ltd.

[0073] Embodiment 1: A compound containing diflufenicol and a processing technology thereof, comprising the following steps:

[0074] Step (1) Preparation of defoamer:

[0075] Add high hydrogen polydimethylsiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane in a mass ratio of 2:2:1 into a three-necked flask, heat to 30°C in a water bath, add methylsulfonic acid, stir at constant temperature for 18h, then add NaHCO3 aqueous solution, wait for the mixed solution to be heated to 30°C, transfer to a split funnel, wash with water until the lower layer is neutral, and distill under reduced pressure to obtain low hydrogen polydimethylsiloxane; the mass ratio of hexamethyldisiloxane to NaHCO3 aqueous solution is 1:0.5;

[0076] Add low hydrogen polydimethylsiloxane, butynediol diethoxy ether, isopropanol and Speier catalyst into the reaction kettle in a mass ratio of 0.5:0.5:1:0.11, heat to 85°C within 30 minutes under nitrogen atmosphere, react for 5 hours, and after the reaction is completed, distill under reduced pressure, and then vacuum dry at 35°C for 31 hours to obtain a defoaming agent; distill under reduced pressure for 1 hour at 40°C; hydrogen content of high hydrogen polydimethylsiloxane: 0.13%;

[0077] Step (2) Preparation of dispersant:

[0078] The sodium lignin sulfonate aqueous solution is heated to 85°C, and then mixed with polyetheramine at a mass ratio of 1:0.3, stirred evenly, and then added with a 10% formaldehyde aqueous solution, kept at a constant temperature of 85°C for 1 hour, and then cooled to 20°C to obtain a dispersant; the mass fraction of the sodium lignin sulfonate aqueous solution is 25%; the mass ratio of the sodium lignin sulfonate and formaldehyde aqueous solution is 1:0.2;

[0079] Step (3) Preparation of compound:

[0080] Add diflufenac, isoproturon, bispyribac, cosolvent and water into a batching kettle in a mass ratio of 10:8:8:1.5:67.5, stir for 1 hour, and form slurry. The obtained slurry is sent to a grinder and coarsely ground for 1.5 hours to obtain a coarse abrasive. The coarse abrasive is then sent to a sand mill and sand-milled for 2.5 hours. It is then transported to a mixing kettle, and antifreeze, defoamer, wetting agent, preservative and dispersant are added and stirred for 0.5 hours. Nano-silicon dioxide is then added and stirred for 6 hours to obtain a compound containing diflufenac. The mass ratio of antifreeze, defoamer, wetting agent, preservative, dispersant and nano-silicon dioxide is 0.5:0.5:1:0.5:1.5:1.

[0081] Embodiment 2: A compound containing diflufenicol and its processing technology, comprising the following steps:

[0082] Step (1) Preparation of defoamer:

[0083] Add high hydrogen polydimethylsiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane in a mass ratio of 3:3:1 into a three-necked flask, heat to 32°C in a water bath, add methylsulfonic acid, stir at constant temperature for 19h, then add NaHCO3 aqueous solution, wait for the mixed solution to be heated to 33°C, transfer to a split funnel, wash with water until the lower layer is neutral, and distill under reduced pressure to obtain low hydrogen polydimethylsiloxane; the mass ratio of hexamethyldisiloxane to NaHCO3 aqueous solution is 1:0.7;

[0084] Low hydrogen polydimethylsiloxane, butynediol diethoxy ether, isopropanol and Speier catalyst were added to the reactor in a mass ratio of 0.7:0.7:1.5:0.16, and heated to 87°C within 30 minutes under nitrogen atmosphere, and reacted for 5.5 hours. After the reaction was completed, it was distilled under reduced pressure, and then vacuum dried at 40°C for 33 hours to obtain a defoaming agent; distilled under reduced pressure for 1.5 hours at a temperature of 43°C; hydrogen content of high hydrogen polydimethylsiloxane: 0.13%;

[0085] Step (2) Preparation of dispersant:

[0086] The sodium lignin sulfonate aqueous solution is heated to 90°C, and then mixed with polyetheramine at a mass ratio of 1:0.4, stirred evenly, and then added with a 10% formaldehyde aqueous solution, and reacted at a constant temperature of 90°C for 1.3 hours, and then cooled to 25°C to obtain a dispersant; the mass fraction of the sodium lignin sulfonate aqueous solution is 25%; the mass ratio of the sodium lignin sulfonate and formaldehyde aqueous solution is 1:0.3;

[0087] Step (3) Preparation of compound:

[0088] Add diflufenac, isoproturon, bispyribac, cosolvent and water into a batching kettle in a mass ratio of 15:10:10:2:53, stir for 1.3 hours, and form slurry. The obtained slurry is sent to a grinder and coarsely ground for 2 hours to obtain a coarse abrasive. The coarse abrasive is then sent to a sand mill and sand-milled for 3 hours. It is then transported to a mixing kettle, and antifreeze, defoamer, wetting agent, preservative and dispersant are added and stirred for 1 hour. Nano-silicon dioxide is then added and stirred for 7 hours to obtain a compound containing diflufenac. The mass ratio of antifreeze, defoamer, wetting agent, preservative, dispersant and nano-silicon dioxide is 0.7:0.7:2:0.6:2.5:3.5.

[0089] Embodiment 3: A compound containing diflufenicol and its processing technology, comprising the following steps:

[0090] Step (1) Preparation of defoamer:

[0091] Add high hydrogen polydimethylsiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane in a mass ratio of 4:4:1 into a three-necked flask, heat to 35°C in a water bath, add methylsulfonic acid, stir at constant temperature for 20 hours, then add NaHCO3 aqueous solution, wait for the mixed solution to be heated to 35°C, transfer to a split funnel, wash with water until the lower layer is neutral, and distill under reduced pressure to obtain low hydrogen polydimethylsiloxane; the mass ratio of hexamethyldisiloxane to NaHCO3 aqueous solution is 1:1;

[0092] Add low hydrogen polydimethylsiloxane, butynediol diethoxy ether, isopropanol and Speier catalyst into the reaction kettle in a mass ratio of 1:1:2:0.21, heat to 90°C within 30 minutes under nitrogen atmosphere, react for 6 hours, and after the reaction is completed, distill under reduced pressure, and then vacuum dry at 45°C for 36 hours to obtain a defoaming agent; distill under reduced pressure for 2 hours at a temperature of 45°C; hydrogen content of high hydrogen polydimethylsiloxane: 0.13%;

[0093] Step (2) Preparation of dispersant:

[0094] The sodium lignin sulfonate aqueous solution is heated to 95°C, and then mixed with polyetheramine at a mass ratio of 1:0.5, stirred evenly, and then a 10% formaldehyde aqueous solution is added, and the reaction is carried out at a constant temperature of 95°C for 1.5 hours, and then cooled to 30°C to obtain a dispersant; the mass fraction of the sodium lignin sulfonate aqueous solution is 25%; the mass ratio of the sodium lignin sulfonate and formaldehyde aqueous solution is 1:0.4;

[0095] Step (3) Preparation of compound:

[0096] Add diflufenac, isoproturon, bispyribac, cosolvent and water into a batching kettle in a mass ratio of 20:12:12:2.5:39, stir for 1.5 hours, and form slurry. The obtained slurry is sent to a grinder and coarsely ground for 2.5 hours to obtain a coarse abrasive. The coarse abrasive is then sent to a sand mill and sand-milled for 3.5 hours. It is then transported to a mixing kettle, and antifreeze, defoamer, wetting agent, preservative and dispersant are added and stirred for 1.5 hours. Nano-silicon dioxide is then added and stirred for 8 hours to obtain a compound containing diflufenac. The mass ratio of antifreeze, defoamer, wetting agent, preservative, dispersant and nano-silicon dioxide is 1:1:3:1:3.5:5.

[0097] Comparative Example 1: Taking Example 1 as a control, the defoamer uses high hydrogen polydimethylsiloxane, a compound containing diflufenicol and its processing technology, comprising the following steps:

[0098] Step (1) Preparation of dispersant: same as in Example 1;

[0099] Step (2) Preparation of compound:

[0100] Add diflufenac, isoproturon, bispyribac, cosolvent and water into a batching kettle in a mass ratio of 10:8:8:1.5:56, stir for 1 hour, and form slurry. The obtained slurry is sent to a grinder and coarsely ground for 1.5 hours to obtain a coarse abrasive. The coarse abrasive is then sent to a sand mill and sand-milled for 2.5 hours. It is then transported to a mixing kettle, and high hydrogen polydimethylsiloxane, antifreeze, wetting agent, preservative and dispersant are added and stirred for 0.5 hours. Nano-silica is then added and stirred for 6 hours to obtain a diflufenac-containing compound. The mass ratio of antifreeze, high hydrogen polydimethylsiloxane, wetting agent, preservative, dispersant and nano-silica is 0.5:0.5:1:0.5:1.5:1.

[0101] Comparative Example 2: Taking Example 1 as a control, without modifying the sodium lignin sulfonate, a compound agent containing diflufenicol and a processing technology thereof include the following steps:

[0102] Step (1) Preparation of defoaming agent: same as in Example 1;

[0103] Step (2) Preparation of compound:

[0104] Add diflufenac, isoproturon, bispyribac, cosolvent and water into a batching kettle in a mass ratio of 10:8:8:1.5:56, stir for 1 hour, and form slurry. The obtained slurry is sent to a grinder and coarsely ground for 1.5 hours to obtain a coarse abrasive. The coarse abrasive is then sent to a sand mill and sand-milled for 2.5 hours. It is then transported to a mixing kettle, and a defoamer, an antifreeze agent, a wetting agent, a preservative and sodium lignin sulfonate are added and stirred for 0.5 hours. Nano-silicon dioxide is then added and stirred for 6 hours to obtain a compound containing diflufenac. The mass ratio of the antifreeze agent, the defoamer, the wetting agent, the preservative, the sodium lignin sulfonate and the nano-silicon dioxide is 0.5:0.5:1:0.5:1.5:1.

[0105] Comparative Example 3: Taking Example 1 as a control, nano silicon dioxide is not added during the preparation of the compound, a compound containing diflufenicol and a processing technology thereof, comprising the following steps:

[0106] Step (1) Preparation of defoaming agent: same as in Example 1;

[0107] Step (2) Preparation of dispersant: same as in Example 1;

[0108] Step (3) Preparation of compound:

[0109] Add diflufenac, isoproturon, bispyribac, cosolvent and water into a batching kettle in a mass ratio of 10:8:8:1.5:56, stir for 1 hour, and form slurry. The obtained slurry is sent to a grinder and coarsely ground for 1.5 hours to obtain a coarse abrasive. The coarse abrasive is then sent to a sand mill and sand-milled for 2.5 hours. It is then transported to a mixing kettle, and antifreeze, defoamer, wetting agent, preservative and dispersant are added and stirred for 0.5 hours to obtain a compound containing diflufenac; the mass ratio of antifreeze, defoamer, wetting agent, preservative and dispersant is 0.5:0.5:1:0.5:1.5.

[0110] experiment:

[0111] The compound preparations obtained in Examples 1 to 3 and Comparative Examples 1 to 3 were used to conduct efficacy tests on weeds in wheat fields to determine the control effects:

[0112] Field efficacy test:

[0113] Select wheat fields with more weeds such as Alopecuroides, Digitaria, and Chenopodium album. Refer to the "Guidelines for Field Efficacy Tests of Pesticides" of the Ministry of Agriculture and Rural Affairs, apply pesticides according to the designed dosage, use 20g of compound agent diluted with water to 30kg, spray evenly over the whole field, and test the control effect 15 days and 30 days after application;

[0114] Control effect (%) = (number of weeds in the blank control area - number of weeds in the treatment area) / number of weeds in the blank control area × 100%;

[0115] Meteorological data during the test period:

[0116]

[0117] Table 1 Meteorological data

[0118] The experimental results are shown in the following table:

[0119]

[0120] Table 2 Prevention data

[0121] Defoaming performance measurement: According to GB / T26527-2011 "Silicone Defoamer", a foaming liquid was prepared, and the performance of the defoamers in Examples 1 to 3 and Comparative Examples 1 to 3 was measured, and the foaming power and anti-foaming performance were measured using a circulating bubbler;

[0122] Defoaming time / s Foam suppression height / mL Example 1 7 350 Example 2 6 340 Example 3 6 335 Comparative Example 1 10 430 Comparative Example 2 7 345 Comparative Example 3 7 340

[0123] Table 3 Defoaming performance data

[0124] According to the data in the above table, we can clearly draw the following conclusions:

[0125] The compounding agents obtained in Examples 1 to 3 are compared with the compounding agents obtained in Comparative Examples 1 to 3. The test results show that:

[0126] Compared with Comparative Example 1, the compound agents obtained in Examples 1 to 3 have better control effects on Alopecurus mume, Digitaria sanguinea, and Chenopodium album, and the defoamers in Examples 1 to 3 have better defoaming and foam-inhibiting properties, which fully demonstrates that in the present invention, the addition of nano-silicon dioxide, the modification of sodium lignin sulfonate, and the modification of high-hydrogen polydimethylsiloxane achieve the improvement of the weed control effect and defoaming and foam-inhibiting properties of the compound agent.

[0127] Compared with Example 1, Comparative Example 1 uses high hydrogen polydimethylsiloxane, which has poor water dispersibility, affecting its defoaming and antifoaming performance. Comparative Example 2 does not modify the sodium lignin sulfonate, the sulfonic acid group content and the molecular weight have not changed, the dispersibility has not been improved, and the control effect of the compound agent is reduced. Comparative Example 3 does not add nano silicon dioxide, and there is no nano silicon dioxide as a carrier, and the control effect of the compound agent is reduced. It can be seen that the setting of the process and the materials used in this application can promote the improvement of the control effect and defoaming performance of the prepared compound agent.

[0128] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

Claims

1. A compound containing diflufenicol, characterized in that: The invention comprises the following mass components: by mass percentage, 10-20% of diflufenicol, 8-12% of isoproturon, 8-12% of bispyribac, 0.5-1% of antifreeze agent, 0.5-1% of defoamer, 1.5-2.5% of cosolvent, 1-3% of wetting agent, 0.5-1% of preservative, 1.5-3.5% of dispersant, and the rest is water; The defoamer is prepared by grafting butynediol diethoxy ether with low-hydrogen polydimethylsiloxane.

2. A compound formulation containing diflufenicol according to claim 1, characterized in that: The low hydrogen polydimethylsiloxane is prepared from high hydrogen polydimethylsiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and methanesulfonic acid.

3. The compound formulation containing diflufenicol according to claim 1, characterized in that: The dispersant is prepared from polyetheramine bridge-modified sodium lignin sulfonate.

4. A processing technology for a compound containing diflufenicol, characterized in that: Including the following processes: Add diflufenac, isoproturon, bispyribac, cosolvent and water to a batching kettle, stir for 1 to 1.5 hours to form a slurry, send the resulting slurry to a grinder, grind it coarsely for 1.5 to 2.5 hours to obtain a coarse abrasive, then send the coarse abrasive to a sand mill for sand grinding for 2.5 to 3.5 hours, then transport it to a mixing kettle, add antifreeze, defoamer, wetting agent, preservative and dispersant, stir for 0.5 to 1.5 hours, then add nano silicon dioxide, stir for 6 to 8 hours to obtain a compound containing diflufenac.

5. The processing technology of a difluanid-containing compound according to claim 4, characterized in that: The defoamer is made by the following process: Add low hydrogen polydimethylsiloxane, butynediol diethoxy ether, isopropanol and Speier catalyst into a reaction kettle, heat to 85-90°C within 30 minutes under a nitrogen atmosphere, react for 5-6 hours, and after the reaction is completed, distill under reduced pressure and dry in vacuum to obtain a defoaming agent.

6. The processing technology of the difluanid-containing compound according to claim 5, characterized in that: The low hydrogen polydimethylsiloxane is prepared by the following process: Add high hydrogen polydimethylsiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane to a three-necked flask, heat in a water bath to 30-35°C, add methylsulfonic acid, stir at constant temperature for 18-20 hours, then add NaHCO3 aqueous solution, wait for the mixed solution to be heated to 30-35°C, transfer to a split funnel, wash with water until the lower layer is neutral, and distill under reduced pressure to obtain low hydrogen polydimethylsiloxane.

7. The processing technology of the difluanid-containing compound according to claim 4, characterized in that: The dispersant is prepared by the following process: The sodium lignin sulfonate aqueous solution is heated to 85-95° C., then mixed with polyetheramine, stirred evenly, and then formaldehyde aqueous solution is added to react at a constant temperature, and then cooled to 20-30° C. to obtain modified sodium lignin sulfonate.

8. The processing technology of the difluanid-containing compound according to claim 5, characterized in that: The process conditions of reduced pressure distillation are: temperature: 40-45°C, time: 1-2h.

9. The processing technology of the difluanid-containing compound according to claim 6, characterized in that: The mass ratio of high hydrogen polydimethylsiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and NaHCO3 aqueous solution is (2-4): (2-4): 1: (0.5-1).

10. The processing technology of the difluanid-containing compound according to claim 7, characterized in that: The mass ratio of the sodium lignin sulfonate aqueous solution, the polyetheramine and the formaldehyde aqueous solution is 1:(0.3-0.5):(0.2-0.4).

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