CN105284814B - Quinclorac solid preparation and preparation method thereof - Google Patents
Quinclorac solid preparation and preparation method thereof Download PDFInfo
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- CN105284814B CN105284814B CN201510824932.2A CN201510824932A CN105284814B CN 105284814 B CN105284814 B CN 105284814B CN 201510824932 A CN201510824932 A CN 201510824932A CN 105284814 B CN105284814 B CN 105284814B
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Abstract
The invention provides a quinclorac solid preparation, which comprises the following components in percentage by weight: 30 to 70 weight percent of quinclorac; 2 wt% -10 wt% of synergist; 1 to 3 weight percent of thickening agent; 2 wt% -8 wt% of wetting agent; 2 to 10 weight percent of dispersant and the balance of filler. The invention mixes the components and then crushes the components to obtain the quinclorac solid preparation. In actual use, the quinclorac solid preparation prepared by the invention has short wetting time, high suspension rate, easy spraying, uniform dispersion and difficult generation of local phytotoxicity; on the basis of meeting the control requirement of crop phytotoxicity, the pesticide composition has less dosage, does not have the phytotoxicity problem to crops, and is environment-friendly.
Description
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to a quinclorac solid preparation and a preparation method thereof.
Background
The quinclorac is a specific selective herbicide for preventing and killing barnyard grass in a rice field, belongs to a hormone-type quinoline carboxylic acid herbicide, is mainly used for preventing and controlling the barnyard grass, and has a long working life and an effect in 1-7 leaf periods. The weed poisoning symptom is similar to the action symptom of auxin substances, the tender leaves of the injured barnyard grass have slight green loss, the leaves have longitudinal stripes and are bent, and the green loss of the leaves of the injured barnyard grass filled with the barnyard grass is changed into purple brown to wither. The typical symptoms of the damaged seedlings are that the seedlings have onion heart seedlings and the leaf color is normal; the new leaf can not be drawn out because the upper tissue is healed, the stem is stripped, and the new leaf is curled in the new leaf. The heart leaves of the seriously damaged seedlings are curled into scallion tubular shape to be upright and are generally withered after being transplanted to a field; if the seedlings survive, the formed tillering seedlings are also malformed, and some rice plants even die of the whole cluster. In the seedlings with light phytotoxicity, the stem base is expanded, becomes hard and brittle, and the heart leaves become narrow and twisted into malformation.
At present, the herbicide for paddy fields is limited by the safety of crops, and the weed control spectrum is also limited. The method for preventing and treating agricultural diseases, insect pests and weeds by mixing different pesticide varieties is a common method for preventing and treating agricultural diseases, insect pests and weed pests, but the properties and pesticide effects of different pesticides are different, and if the effective components and the mixture ratio of the pesticides in the mixed pesticides are not properly selected, in the actual use, the pesticide cannot well prevent and treat specific diseases, insect pests and weed pests, and the ideal prevention and treatment effect of the diseases, insect pests and weed pests cannot be achieved, or the pesticide damage is caused to current crops and even later crops. In the prior art, a single quinclorac herbicide can be used for controlling weeds in a targeted manner, but strict limitations are imposed on the dosage and application operation of the herbicide, and if the dosage is improper or the application is not uniform, the effect of controlling the weeds is poor or the weeds are damaged by current crops or even later crops.
Disclosure of Invention
The invention aims to provide a quinclorac solid preparation and a preparation method thereof, and the quinclorac solid preparation provided by the invention has the advantages of short wetting time, high suspension rate, easy spraying, uniform dispersion and difficult generation of local phytotoxicity in actual use; on the basis of meeting the control requirement of crop phytotoxicity, the pesticide composition has less dosage, does not have the phytotoxicity problem to crops, and is environment-friendly.
The technical scheme of the invention is as follows:
in the present invention, the percentages used are mass percentages unless otherwise specified.
The invention provides a quinclorac solid preparation, which comprises the following components in percentage by weight:
30 to 70 weight percent of quinclorac;
2 wt% -10 wt% of synergist;
1 to 3 weight percent of thickening agent;
2 wt% -8 wt% of wetting agent;
2 to 10 weight percent of dispersant;
the balance of filler.
Preferably, the quinclorac solid preparation comprises the following components:
40 to 60 weight percent of quinclorac;
4 wt% -8 wt% of synergist;
1.5 wt% -2.5 wt% of thickening agent;
3 wt% -6 wt% of wetting agent;
4 to 7 weight percent of dispersant;
the balance of filler.
Preferably, the particle size of the quinclorac solid preparation is less than 25 μm.
Preferably, the quinclorac comprises quinclorac bulk drug, quinclorac sodium salt or quinclorac potassium salt.
Preferably, the synergist comprises a methylated vegetable oil, an ethoxylated fatty alcohol and an anionic alkyl glycoside derivative, wherein the mass ratio of the methylated vegetable oil to the ethoxylated fatty alcohol to the anionic alkyl glycoside derivative is preferably (2-4): (0.5-1.5): (5-7).
Preferably, the thickening agent comprises one or more of sodium carboxymethyl cellulose, polyvinyl alcohol and Arabic gum.
Preferably, the wetting agent comprises one or more of sodium dodecyl sulfate, alkyl succinic acid sulfonate and alkyl naphthalene sulfonate.
Preferably, the dispersant comprises one or more of lignosulfonate, sodium methylene dinaphthalene sulfonate and polycarboxylate.
Preferably, the filler comprises one or more of diatomite, white carbon black, light calcium carbonate, kaolin and starch.
The invention provides a preparation method of a quinclorac solid preparation in the technical scheme, which comprises the following steps:
(1) mixing quinclorac, a synergist, a thickener, a wetting agent, a dispersant and a filler to obtain a mixed material;
(2) and (2) crushing and mixing the mixed material obtained in the step (1) to obtain the quinclorac solid preparation.
The invention provides a quinclorac solid preparation, which comprises the following components in percentage by weight: 30 to 70 weight percent of quinclorac; 2 wt% -10 wt% of synergist; 1 to 3 weight percent of thickening agent; 2 wt% -8 wt% of wetting agent; 2 to 10 weight percent of dispersant and the balance of filler. The invention mixes the components and then crushes the components to obtain the quinclorac solid preparation. The suspending agent is more quickly dissolved in water, has high suspension rate, is easy to spray and uniformly dispersed, and is not easy to generate local phytotoxicity; on the basis of meeting the control requirement of crop phytotoxicity, the pesticide composition has less dosage, does not have the phytotoxicity problem to crops, and is environment-friendly.
The wetting time of the quinclorac solid preparation provided by the invention is as low as 38s, the suspension rate can reach 98%, and under the condition that the application dose is 50 g/mu, the pesticide effects for preventing and removing barnyard grass in the paddy field in 15 days, 30 days and 45 days after the application are respectively 93.00%, 92.30% and 91.12%.
Detailed Description
The invention provides a quinclorac solid preparation, which comprises the following components in percentage by weight:
30 to 70 weight percent of quinclorac;
2 wt% -10 wt% of synergist;
1 to 3 weight percent of thickening agent;
2 wt% -8 wt% of wetting agent;
2 to 10 weight percent of dispersant;
the balance of filler.
The quinclorac solid preparation provided by the invention has the advantages of short wetting time, high suspension rate, easy spraying, uniform dispersion and difficult generation of local phytotoxicity; on the basis of meeting the control requirement of crop phytotoxicity, the pesticide composition has less dosage, does not have the phytotoxicity problem to crops, and is environment-friendly.
The quinclorac solid preparation provided by the invention comprises 30-70 wt% of quinclorac, preferably 40-60 wt%, and more preferably 45-55 wt%. In the present invention, the source of the quinclorac is not particularly limited, and quinclorac known to those skilled in the art can be used. In the present invention, the quinclorac preferably comprises quinclorac bulk drug, quinclorac sodium salt or quinclorac potassium salt.
The quinclorac solid preparation provided by the invention comprises 2-10 wt% of synergist, preferably 4-8 wt%. In the invention, the synergist has excellent wettability, very outstanding affinity to plant bodies and good adhesiveness, can greatly reduce the loss of liquid medicine components, accelerates the transmission of effective components in a target body, greatly improves the pesticide effect and reduces the pesticide damage. In the present invention, the synergist preferably comprises methylated vegetable oil, ethoxylated fatty alcohol and anionic alkyl glycoside derivative. In the invention, the mass ratio of the methylated vegetable oil, the ethoxylated fatty alcohol and the anionic alkyl glycoside derivative is preferably (2-4): (0.5-1.5): (5-7), more preferably 3: 1: 6. specifically, in embodiments of the invention, the potentiator can be an AG/LR-0992 clear microemulsion provided by Nippondi Italy group.
The quinclorac solid preparation provided by the invention comprises 1 to 3 weight percent of thickening agent, preferably 1.5 to 2.5 weight percent. In the invention, the thickening agent preferably comprises one or more of sodium carboxymethyl cellulose, polyvinyl alcohol and Arabic gum. The source of the thickener in the present invention is not particularly limited, and commercially available products of the above thickener known to those skilled in the art may be used.
The quinclorac solid preparation provided by the invention comprises 2-8 wt% of wetting agent, preferably 3-6 wt%. In the present invention, the wetting agent preferably comprises one or more of sodium lauryl sulfate, alkyl succinic acid sulfonate, alkyl naphthalene sulfonate and detergent. The source of the wetting agent is not particularly limited in the present invention, and commercially available products of the above wetting agents known to those skilled in the art may be used.
The quinclorac solid preparation provided by the invention comprises 2-10 wt% of dispersant, preferably 4-7 wt%. In the present invention, the dispersant preferably comprises one or a combination of several of lignosulfonate, sodium methylene dinaphthalene sulfonate and polycarboxylate. The source of the dispersant in the present invention is not particularly limited, and commercially available dispersants known to those skilled in the art may be used.
The quinclorac solid preparation provided by the invention comprises the rest of filler. The source of the filler is not particularly limited in the present invention, and a filler known to those skilled in the art may be used. In the invention, the filler preferably comprises one or a combination of more of diatomite, white carbon black, light calcium carbonate, kaolin and starch.
The particle size of the quinclorac solid preparation provided by the invention is preferably less than 25 mu m.
The invention provides a preparation method of a quinclorac solid preparation in the technical scheme, which comprises the following steps:
(1) mixing quinclorac, a synergist, a thickener, a wetting agent, a dispersant and a filler to obtain a mixed material;
(2) and (2) crushing and mixing the mixed material obtained in the step (1) to obtain the quinclorac solid preparation.
The invention mixes quinclorac, synergist, thickener, wetting agent, dispersant and filler to obtain a mixed material. In the present invention, there is no special requirement for the mixing mode, mixing equipment and feeding sequence of the above components, and the mixing technical scheme known to those skilled in the art can be adopted. In the present invention, the quinclorac, the synergist, the thickener, the wetting agent, the dispersant and the filler are preferably mixed using a double helix conical mixer. In the present invention, the mixing time is preferably 0.5 to 1.5 hours, and more preferably 1 hour.
The invention crushes the obtained mixed materials. In the invention, the method for crushing the mixed material and the crushing equipment have no special requirements, and the technical scheme of crushing which is well known by the technical personnel in the field can be adopted. In the present invention, it is preferable to pulverize the mixed material using a fluidized bed jet mill. In the invention, the grinding pressure is preferably 8.5-9.5 Mpa, and the grinding revolution is preferably 3000-5000 r/min.
The invention completes the crushing and then mixes to obtain the quinclorac solid preparation. In the present invention, there is no special requirement for the mixing mode and mixing equipment, and the mixing technical scheme known to those skilled in the art can be adopted. In the present invention, it is preferable to mix the pulverized material using a gravity-free mixer. In the present invention, the mixing time is preferably 0.5 to 1.5 hours, and more preferably 1 hour.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In an embodiment of the invention, the synergist is AG/LR-0992 clear microemulsion provided by Nippody group, Italy.
Example 1:
preparation of 30% Quinclorac solid preparation
350kg of quinclorac original drug (content is 85%), 60kg of synergist, 20kg of sodium carboxymethylcellulose, 20kg of sodium dodecyl sulfate, 40kg of sodium lignosulfonate, 60kg of white carbon black and 450kg of diatomite are put into a double-helix conical mixer and mixed for 0.5h to obtain a mixed material, then the mixed material is crushed by a fluidized bed jet mill under the conditions of 8.5MPa and 5000r/min, and is stirred and mixed for 1h by a gravity-free mixer to obtain a 30% quinclorac solid preparation.
Example 2:
preparation of 30% Quinclorac sodium salt solid preparation
410kg of quinclorac sodium salt (with the content of 73%), 80kg of synergist, 20kg of polyvinyl alcohol, 45kg of alkyl succinic acid sulfonate, 50kg of sodium methylene dinaphthalene sulfonate, 70kg of light calcium carbonate and 325kg of kaolin are put into a double-helix conical mixer and mixed for 1h to obtain a mixed material, then the mixed material is crushed by a fluidized bed jet mill under the conditions of 9.5MPa and 3000r/min and is stirred and mixed for 0.5h by a gravity-free mixer to obtain a 30% quinclorac sodium salt solid preparation.
Example 3:
preparation of 30% Quinclorac Potassium salt solid preparation
425kg of quinclorac potassium salt (with the content of 70 percent), 100kg of synergist, 20kg of Arabic gum, 20kg of sodium dodecyl sulfate, 10kg of alkyl naphthalene sulfonate, 40kg of sodium lignosulfonate, 10kg of polycarboxylate, 60kg of white carbon black, 200kg of diatomite and 115kg of starch are put into a double-helix conical mixer and mixed for 1.5 hours to obtain a mixed material, then the mixed material is crushed by a fluidized bed jet mill under the conditions of 9.0MPa and 4000r/min, and is stirred and mixed for 0.5 hour by a gravity-free mixer to obtain a 30 percent quinclorac potassium salt solid preparation.
Example 4:
preparation of 50% Quinclorac solid preparation
590kg of quinclorac original drug (content is 85%), 60kg of synergist, 20kg of sodium carboxymethylcellulose, 30kg of sodium dodecyl sulfate, 30kg of sodium lignosulfonate, 60kg of white carbon black and 210kg of diatomite are put into a double-helix conical mixer and mixed for 1h to obtain a mixed material, then the mixed material is crushed by a fluidized bed jet mill under the conditions of 8.5MPa and 5000r/min, and is stirred and mixed for 1.5h by a gravity-free mixer to obtain a 50% quinclorac original drug solid preparation.
Example 5:
preparation of 50% Quinclorac sodium salt solid preparation
700kg of quinclorac sodium salt (with the content of 73 percent), 80kg of synergist, 20kg of polyvinyl alcohol, 45kg of alkyl succinic acid sulfonate, 50kg of sodium methylene dinaphthalene sulfonate, 70kg of white carbon black and 80kg of diatomite are put into a double-helix conical mixer and mixed for 0.5h to obtain a mixed material, then the mixed material is crushed by a fluidized bed jet mill under the conditions of 9.0MPa and 4000r/min, and is stirred and mixed for 1h by a gravity-free mixer to obtain the 50 percent quinclorac sodium salt solid preparation.
Example 6:
preparation of 50% Quinclorac Potassium salt solid preparation
715kg of quinclorac potassium salt (with the content of 70 percent), 50kg of synergist, 20kg of Arabic gum, 20kg of sodium dodecyl sulfate, 10kg of alkyl naphthalene sulfonate, 40kg of sodium lignosulfonate, 10kg of polycarboxylate, 60kg of white carbon black and 75kg of light calcium carbonate are put into a double-helix conical mixer and mixed for 1h to obtain a mixed material, then the mixed material is crushed by a fluidized bed airflow crusher under the conditions of 9.5MPa and 3000r/min and is stirred and mixed for 0.5h by a gravity-free mixer to obtain the 50 percent quinclorac sodium salt solid preparation.
In the invention, a commercially available 50% quinclorac solid preparation (comparative example) and 50% quinclorac solid preparations prepared in the embodiments 4 to 6 of the invention are used as the quinclorac solid preparation to be tested, and a wetting time and a suspension rate measurement test are carried out. According to the method specified in GB/T5451-2001, a wetting time test is carried out on the quinclorac solid preparation to be tested; the suspension rate test of the quinclorac solid preparation to be tested was carried out according to the method specified in GB/T14825-2006. The results are shown in Table 1.
TABLE 1 Quinclorac solid formulation wetting time and suspension test
| Quinclorac solid preparation for test | Wetting time(s) | Suspension Rate (%) |
| Example 4 | 50 | 95 |
| Example 5 | 42 | 97 |
| Example 6 | 38 | 98 |
| Comparative example | 65 | 90 |
The test results show that compared with the commercially available quinclorac solid preparation in the comparative example, the quinclorac solid preparation prepared by the invention has the advantages of higher dissolution speed and higher suspension rate, and can ensure that the pesticide is more uniformly dispersed in water and the spraying concentration is more uniform in the actual use process of the quinclorac solid preparation, so that the local phytotoxicity is not easy to generate.
Meanwhile, the invention takes a commercially available 50% quinclorac solid preparation (a comparative example) and 50% quinclorac solid preparations prepared in the embodiments 4 to 6 of the invention as the quinclorac solid preparation to be tested, and the drug effect of preventing and killing the barnyard grass in the paddy field is tested. The results are shown in Table 1.
TABLE 2 Quinclorac solid preparation drug efficacy test for preventing and killing barnyard grass in paddy field
The test results show that the quinclorac solid preparation prepared by the invention has better control effect on the barnyard grass in the paddy field under the condition of the same application dosage compared with the quinclorac solid preparation sold in the control example. The application amount of the quinclorac solid preparation prepared by the invention is relatively reduced under the condition of meeting the requirement of controlling the crop pests to the same extent, and the quinclorac solid preparation is environment-friendly.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The quinclorac solid preparation comprises the following components in percentage by weight:
30 to 70 weight percent of quinclorac;
2 wt% -10 wt% of synergist;
1 to 3 weight percent of thickening agent;
2 wt% -8 wt% of wetting agent;
2 to 10 weight percent of dispersant;
the balance of filler;
the synergist comprises methylated vegetable oil, ethoxylated fatty alcohol and anionic alkyl glycoside derivative;
the mass ratio of the methylated vegetable oil to the ethoxylated fatty alcohol to the anionic alkyl glycoside derivative is (2-4): (0.5-1.5): (5-7);
the thickening agent comprises one or more of sodium carboxymethylcellulose, polyvinyl alcohol and acacia.
2. The quinclorac solid preparation of claim 1, which comprises the following components:
40 to 60 weight percent of quinclorac;
4 wt% -8 wt% of synergist;
1.5 wt% -2.5 wt% of thickening agent;
3 wt% -6 wt% of wetting agent;
4 to 7 weight percent of dispersant;
the balance of filler.
3. The quinclorac solid formulation of claim 1, wherein the particle size of the quinclorac solid formulation is less than 25 μm.
4. The quinclorac solid formulation of claim 1, wherein the quinclorac comprises quinclorac prodrug, quinclorac sodium salt, or quinclorac potassium salt.
5. The quinclorac solid preparation of claim 1, wherein the wetting agent comprises one or more of sodium dodecyl sulfate, alkyl succinic acid sulfonate and alkyl naphthalene sulfonate.
6. The quinclorac solid preparation of claim 1, wherein the dispersant comprises one or more of lignosulfonate, sodium methylene dinaphthalene sulfonate and polycarboxylate.
7. The quinclorac solid preparation of claim 1, wherein the filler comprises one or more of diatomite, white carbon black, light calcium carbonate, kaolin and starch.
8. The method for preparing the quinclorac solid preparation of any one of claims 1 to 7, comprising the following steps:
(1) mixing quinclorac, a synergist, a thickener, a wetting agent, a dispersant and a filler to obtain a mixed material;
(2) and (2) crushing and mixing the mixed material obtained in the step (1) to obtain the quinclorac solid preparation.
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| JP2567560B2 (en) * | 1993-05-24 | 1996-12-25 | 鹿島建設株式会社 | Bridge construction method using precast girders |
| CN1915031A (en) * | 2005-08-16 | 2007-02-21 | 沈阳化工研究院 | Auxiliary agent of weedicide, and method of use |
| CN1330237C (en) * | 2006-01-20 | 2007-08-08 | 浙江新安化工集团股份有限公司 | Dichlorquinolinic acid solid preparation |
| CN101449675B (en) * | 2008-11-19 | 2011-09-07 | 东北农业大学 | Preparation method of herbicide methylated vegetable oil adjuvants |
| CN104262419B (en) * | 2014-09-15 | 2017-06-13 | 上海发凯化工有限公司 | A kind of APG and its dealcoholysis technique |
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Effective date of registration: 20200921 Address after: Taiping Street Yaojia community, Pulandian District, Dalian City, Liaoning Province Patentee after: Dalian renbang Agricultural Technology Group Co., Ltd Address before: 116200 Yao village, Taiping Office, Dalian, Liaoning, Pulandian Patentee before: DALIAN GUANGDA PESTICIDE Co.,Ltd. |