CN102823589A - Pesticide water effervescent dispersible tablet and preparation method thereof - Google Patents

Pesticide water effervescent dispersible tablet and preparation method thereof Download PDF

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CN102823589A
CN102823589A CN2012103555559A CN201210355555A CN102823589A CN 102823589 A CN102823589 A CN 102823589A CN 2012103555559 A CN2012103555559 A CN 2012103555559A CN 201210355555 A CN201210355555 A CN 201210355555A CN 102823589 A CN102823589 A CN 102823589A
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agricultural chemicals
acid
aqueous dispersion
mass parts
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CN102823589B (en
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张惠明
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FIVESTAR (NANTONG) CHEMICAL Co Ltd
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Abstract

The invention discloses a pesticide water effervescent dispersible tablet and a preparation method thereof. According to the pesticide water effervescent dispersible tablet and the preparation method thereof, ammonium hydrogen carbonate is used as a gas source, and an acid source or alkali source is selected according to the physical property of different raw materials, i.e. the acid source and the ammonium hydrogen carbonate are added into the acid-resistant raw materials, and tablets are put into water to produce carbon oxide during use; and the alkali source and the ammonium hydrogen carbonate are added into the alkali-resistant raw materials, and tablets are put into water to produce ammonia gas. The pesticide water effervescent dispersible tablet can rapidly boil and disintegrate in water and therefore avoid the reduction of application effect caused by degradation of effective components of the pesticide effervescent dispersible tablet, so that the pesticide water effervescent dispersible tablet with stable chemical properties is obtained.

Description

A kind of agricultural chemicals aqueous dispersion effervescent tablet and preparation method thereof
Technical field
The present invention relates to a kind of pesticide processing field, relate in particular to soaked dispersion effervescent tablet of a kind of agricultural chemicals and preparation method thereof.
Background technology
Effervescent tablet is a kind of pesticides new formulation of fast development; This tablet is met water can produce a large amount of bubbles rapidly, and foaming boiling, disintegration fast are dispersed in active ingredient in the water uniformly in water; Formation has the solution or the aqueous dispersion of good action effect, and suspensibility is with dispersed higher.
The basic principle of agricultural chemicals aqueous dispersion effervescent tablet is in tablet, to contain acidic materials (acid source; Be generally citric acid, tartaric acid, fumaric acid etc.) and the material of the getting angry (source of getting angry; Be generally the basic salt of carbon containing acid group, like carbonic hydroammonium, sodium carbonate etc.), neutralization reaction takes place with the source of getting angry in acid source after tablet is met water; Discharge carbonic acid gas; Thereby reach foaming boiling, quickly disintegrated effect, agricultural chemicals aqueous dispersion effervescent tablet can directly be shed disintegration diffusion voluntarily in the paddy field in use, also can drop in the sprayer to spray in the crop target after the disintegration dispersion.
The pesticidal preparations of China is mainly missible oil and pulvis at present; Because missible oil uses a large amount of chemical solvent-environment and user are caused very big injury like toluene, xylol etc.; Pulvis is then because its serious drift of flying upward is particularly serious to user's injury, the metering difficulty when these two kinds of formulations also exist packing to use; And the aqueous dispersion effervescent tablet is owing to have given configuration, accurately monolithic weight, solvent-free, nothing drift, easy to use; Having simultaneously foaming boiling, disintegration fast, higher suspension rate and dispersive property again, is a kind of environmentally friendly pesticides new formulation, has become the frontier that current pesticidal preparations develops rapidly.
Agricultural chemicals aqueous dispersion effervescent tablet generally is made up of pesticide original medicine, acid source, carbon dioxide source, surfactant, free-flow agent, binding agent, inert filler etc.; Like the patent No. 00107465.2, described in 200610104832.3; But most Pesticidal products are not to be exactly unstable to alkali to acid, very easily decompose, thereby cause the product poor chemical stability; The active ingredient degraded, result of use descends.
Summary of the invention
Goal of the invention: be the source of getting angry with dual gas supply compound-carbonic hydroammonium, select corresponding acid source or alkali source, obtain a kind of agricultural chemicals aqueous dispersion effervescent tablet of stable chemical performance to different agricultural chemicals rerum naturas.
Another object of the present invention provides the preparation method of this agricultural chemicals aqueous dispersion effervescent tablet.
Technical scheme: a kind of agricultural chemicals aqueous dispersion effervescent tablet; It is made up of following mass parts: in pesticide original medicine 5~60 mass parts, dual gas supply compound 10~30 mass parts, the dual gas supply compound and material 10~30 mass parts, surfactant 3~10 mass parts, inert filler 2~70 mass parts, binding agent 1~5 mass parts, free-flow agent 1~5 mass parts, described dual gas supply compound is a carbonic hydroammonium;
Said pesticide original medicine be to the alkali sensitivity to the metastable agricultural chemicals of acid, in the corresponding said dual gas supply compound with material be acid source; Said pesticide original medicine be acid labile to the metastable agricultural chemicals of alkali, in the corresponding said dual gas supply compound with material be alkali source.
As optimization, said is that in cartap or first dimension salt or Nitenpyram or Imidacloprid or Acetamiprid or dimethomorph or thiophene worm piperazine or Fluoxastrobin or kresoxim-methyl or Difenoconazole or carbendazim or cyprodinil or Flusilazole or piperazine humulone or metamitron or atrazine or cyhalofop-butyl or heteroauxin or brassin lactones or the gibberellin one or more are composite to the alkali sensitivity to the metastable agricultural chemicals of acid; Said acid labile is rimsulfuron or nicosulfuron or metsulfuron-methyl or chlorine sulphur is grand or one or more of pyrazosulfuron or bensulfuron-methyl or thifensulfuronmethyl or isoproturon or diuron or penoxsuam or Flumetsulam or two careless ether or Rynaxypyr or indenes worm prestige or pyrrole aphid ketone or fludioxonil or nitrile bacterium azoles or propiconazole or matrine or compound sodium nitrophenolate are composite to the metastable agricultural chemicals of alkali.
As optimization, said acid source is one or more in citric acid or tartaric acid or the fumaric acid; Said alkali source is one or more in potassium hydroxide or sodium hydroxide or sodium carbonate or the potash.
As optimization, said surfactant is one or more in penetrating agent BX or sodium lignin sulfonate or lauryl sodium sulfate or PO-EO block polyether or acrylate homopolymer sodium salt or the naphthalenesulfonate.
As optimization, said inert filler is one or more in corn starch or diatomite or talcum powder or bentonite or the kaolin.
As optimization, said binding agent is the one or more kinds of mixtures among water soluble starch or sodium carboxymethyl starch or polyethylene glycol PEG4000 or the polyethylene glycol PEG6000.
As optimization, said free-flow agent is one or more in white carbon or dolomol or the talcum powder.
The preparation method of said agricultural chemicals aqueous dispersion effervescent tablet may further comprise the steps:
1, to the alkali sensitivity to the metastable agricultural chemicals of acid:
(1) preparation master batch: the pesticide original medicine that will accurately measure, acid source, surfactant, inert filler mix in mixer, through comminution by gas stream it are crushed to more than 500 orders, and powder is collected in another mixer; Adding 10~20% is dissolved with the aqueous solution of binding agent and mediates; Obtain wet granular through extruder grain or wet granulation, dry to moisture content and be less than 1%, whole again grain sieves; Get 30~60 order particles, for use;
(2) compressing tablet: master batch, carbonic hydroammonium, the free-flow agent of above-mentioned (1) preparation that will accurately measure mix in mixer; In tablet press machine, be pressed into the tablet of given configuration; Diameter can selected between 5~40mm; Thickness can be selected between 3~15mm, and monolithic weight is at 0.5~20g.
2, acid labile is to the metastable agricultural chemicals of alkali:
(1) preparation master batch: the pesticide original medicine that will accurately measure, alkali source, surfactant, inert filler mix in mixer, through comminution by gas stream it are crushed to more than 500 orders, and powder is collected in another mixer; Adding 10~20% is dissolved with the aqueous solution of binding agent and mediates; Obtain wet granular through extruder grain or wet granulation, dry to moisture content and be less than 1%, whole again grain sieves; Get 30~60 order particles, for use;
(2) compressing tablet: master batch, carbonic hydroammonium, the free-flow agent of above-mentioned (1) preparation that will accurately measure mix in mixer; In tablet press machine, be pressed into the tablet of given configuration; Tablet diameters can be selected between 5~40mm; Thickness can be selected between 3~15mm, and monolithic weight is at 0.5~20g.
The present invention realizes through the following principles of chemistry:
Dual gas supply compound carbonic hydroammonium is met acid or is met alkali release of carbon dioxide or ammonia respectively, and its reaction equation is following:
Acidolysis reaction: NH 4HCO 3+ R 1COOH=R 1COONH 4+ H 2O+CO 2↑;
Alkaline hydrolysis reaction: NH 4HCO 3+ AOH=AHCO 3+ H 2O+NH 3↑;
Wherein, R 1COOH is an acid source, and AOH is an alkali source.
The invention has the advantages that: the agricultural chemicals aqueous dispersion effervescent tablet of the present invention disintegration of in water, seething with excitement rapidly, can avoid the degraded of agricultural chemicals aqueous dispersion effervescent tablet active ingredient, result of use descends, thereby obtains the agricultural chemicals aqueous dispersion effervescent tablet of stable chemical performance.
The preparation method of agricultural chemicals aqueous dispersion effervescent tablet of the present invention can be used for producing like cartap; First dimension salt; Nitenpyram; Imidacloprid; Acetamiprid; Dimethomorph; Thiophene worm piperazine; Fluoxastrobin; Kresoxim-methyl; Difenoconazole; Carbendazim; Cyprodinil; Flusilazole; The piperazine humulone; Metamitron; Atrazine; Cyhalofop-butyl; Heteroauxin; Brassin lactones; Gibberellin; Rimsulfuron; Nicosulfuron; Metsulfuron-methyl; Chlorine sulphur is grand; Pyrazosulfuron; Bensulfuron-methyl; Thifensulfuronmethyl; Isoproturon; Diuron; Penoxsuam; Flumetsulam; Two careless ethers; Rynaxypyr; Indenes worm prestige; Pyrrole aphid ketone; Fludioxonil; Nitrile bacterium azoles; Propiconazole; Matrine; Aqueous dispersion effervescent tablets such as compound sodium nitrophenolate.
Embodiment
Below in conjunction with embodiment the present invention is described further:
Embodiment 1
5% emamectin benzoate water disperses the preparation (percentage composition in the present embodiment is mass percent) of effervescent tablet:
(1) preparation 6.17% first dimension salt master batch: the former medicine 8.8kg of 70% first dimension salt, tartaric acid 12kg, the sodium lignin sulfonate 2kg that will accurately measure, naphthalene sulfonate 6kg, corn starch 25kg, kaolin 44.7kg mixes in mixer; Through comminution by gas stream it is crushed to more than 500 orders; Powder is collected in another mixer, adds the aqueous solution kneading that 15.5kg is dissolved with 10% sodium carboxymethyl starch, obtains the column wet granular through extruder grain; Dry to moisture content and be less than 1%; Sieve by the whole grain of pelletizing machine vibratory sieve again, get 30~60 order particles, for use;
(2) compressing tablet: master batch 81kg, carbonic hydroammonium 18kg, the white carbon 1kg of above-mentioned (1) preparation that will accurately measure mix in mixer, in tablet press machine, are pressed into circular tablet, diameter 12mm, and thickness 3.5mm, monolithic weight is about 1.0g;
(3) performance test: active ingredient: 5.06%, 30 ℃ of heat storage was 5.05% after 30 days; Disintegration time: 74s; Suspensibility: 91.4%, pH value: 3.7 (1% aqueous solution);
(4) application test:
Present embodiment is applied to prevent and treat rice leaf folder, and the result shows that effect is better than commercially available 5% emamectin benzoate water dispersible granule and 40% chlorpyrifos ec, can not only effective insecticidal, and also also lower to the loss of leaf.See the following form:
Figure 807873DEST_PATH_IMAGE001
Embodiment 2
The preparation of 40% Acetamiprid aqueous dispersion effervescent tablet (percentage composition in the present embodiment is mass percent):
(1) preparation 49.4% Acetamiprid master batch: the former medicine 51.5kg of 96% Acetamiprid that will accurately measure, citric acid 12kg, acrylate homopolymer sodium salt 2kg, naphthalene sulfonate 8kg, corn starch 15kg, talcum powder 9.8kg mixes in mixer; Through comminution by gas stream it is crushed to more than 500 orders; Powder is collected in another mixer, adds the aqueous solution kneading that 17kg is dissolved with 10% PEG6000, obtains irregular wet granular through wet granulation; Dry to moisture content and be less than 1%; Sieve by the whole grain of pelletizing machine vibratory sieve again, get 30~60 order particles, for use;
(2) compressing tablet: master batch 81kg, carbonic hydroammonium 18kg, the dolomol 1kg of above-mentioned (1) preparation that will accurately measure mix in mixer, in tablet press machine, are pressed into circular tablet, diameter 24mm, and thickness 5mm, monolithic weight is about 2g;
(3) performance test: active ingredient: 40.38%, 30 ℃ of heat storage was 40.40% after 30 days; Disintegration time: 82s; Suspensibility: 92.6%, pH value: 4.1 (1% aqueous solution);
(4) application test:
Present embodiment is applied to prevent and treat cabbage aphid, and the result shows that quick-acting is superior to 3% acetamiprid EC, sees the following form:
Embodiment 3
The preparation of 10% penoxsuam aqueous dispersion effervescent tablet (percentage composition in the present embodiment is mass percent):
(1) preparation 14.0% penoxsuam master batch: the former medicine 14.7kg of 95% penoxsuam that will accurately measure, potash 49kg, acrylate homopolymer sodium salt sodium 3kg, naphthalene sulfonate 8kg, corn starch 15kg; Diatomite 8.7kg mixes in mixer, through comminution by gas stream it is crushed to more than 500 orders, and powder is collected in another mixer; Adding 16kg is dissolved with the aqueous solution of 7% sodium carboxymethyl starch and 3% PEG4000 and mediates; Obtain irregular wet granular through wet granulation, dry to moisture content and be less than 1%, sieve by the whole grain of pelletizing machine vibratory sieve again; Get 30~60 order particles, for use;
(2) compressing tablet: master batch 71.5kg, carbonic hydroammonium 27kg, white carbon 1kg, the talcum powder 0.5kg of above-mentioned (1) preparation that will accurately measure mix in mixer; In tablet press machine, be pressed into circular tablet; Diameter 12mm, thickness 3.5mm, monolithic weight is about 1.0g;
(3) performance test: active ingredient: 10.3%, 30 ℃ of heat storage was 10.21% after 30 days; Disintegration time: 80s; Suspensibility: 88.7%, pH value: 8.7 (1% aqueous solution);
(4) application test:
Present embodiment carries out the living test of indoor weeding to be tested, and it is consistent that the result is shown in 2.5% oil suspending agent effect, sees the following form:
Figure 442434DEST_PATH_IMAGE003
Embodiment 4
The preparation of 20% Rynaxypyr aqueous dispersion effervescent tablet (percentage composition in the present embodiment is mass percent):
(1) preparation 27.8% Rynaxypyr master batch: the former medicine 30.2kg of 92% Rynaxypyr that will accurately measure, sodium carbonate 38kg, PO-EO block polyether 2kg, penetrating agent BX 4kg, lauryl sodium sulfate 5kg, corn starch 15kg; Bentonite 4.2kg mixes in mixer, through comminution by gas stream it is crushed to more than 500 orders, and powder is collected in another mixer; Adding 16kg is dissolved with the aqueous solution of 7% water soluble starch and 3% PEG6000 and mediates; Obtain the column wet granular through extruder grain, dry to moisture content and be less than 1%, sieve by the whole grain of pelletizing machine vibratory sieve again; Get 30~60 order particles, for use;
(2) compressing tablet: master batch 72kg, carbonic hydroammonium 27kg, the white carbon 1kg of above-mentioned (1) preparation that will accurately measure mix in mixer, in tablet press machine, are pressed into circular tablet, diameter 24mm, and thickness 8mm, monolithic weight is about 5.0g;
(3) performance test: active ingredient: 20.1%; Disintegration time: 93s; Suspensibility: 90.6%, pH value: 8.7 (1% aqueous solution);
(4) application test:
Be that suspending agent and tablet are prevented and treated leaf-roller effect comparison table in paddy rice below, the result shows tablet and suspending agent action effect no significant difference:
Figure 837643DEST_PATH_IMAGE004
Embodiment 5
The preparation of 20% Difenoconazole aqueous dispersion effervescent tablet (percentage composition in the present embodiment is mass percent):
(1) preparation 27.8% Difenoconazole master batch: 96% difenoconazole technical material 29kg, fumaric acid 12.5kg, the lauryl sodium sulfate 3kg that will accurately measure, naphthalene sulfonate 8kg, corn starch 41.7kg, kaolin 4.2kg mixes in mixer; Through comminution by gas stream it is crushed to more than 500 orders; Powder is collected in another mixer, adds the aqueous solution kneading that 16kg is dissolved with 10% water soluble starch, obtains irregular wet granular through wet granulation; Dry to moisture content and be less than 1%; Sieve by the whole grain of pelletizing machine vibratory sieve again, get 30~60 order particles, for use;
(2) compressing tablet: master batch 72kg, carbonic hydroammonium 27kg, the dolomol 1kg of above-mentioned (1) preparation that will accurately measure mix in mixer, in tablet press machine, are pressed into circular tablet, diameter 24mm, and thickness 8mm, monolithic weight is about 5.0g;
(3) performance test: active ingredient: 20.3%; Disintegration time: 87s; Suspensibility: 91.4%, pH value: 5.8 (1% aqueous solution);
(4) application test:
20% Difenoconazole aqueous dispersion effervescent tablet is consistent with water dispersible granules to the control efficiency of citrus (granulated sugar tangerine) anthracnose, sees the following form:

Claims (8)

1. agricultural chemicals aqueous dispersion effervescent tablet; It is characterized in that: it is made up of following mass parts: in pesticide original medicine 5~60 mass parts, dual gas supply compound 10~30 mass parts, the dual gas supply compound and material 10~30 mass parts, surfactant 3~10 mass parts, inert filler 2~70 mass parts, binding agent 1~5 mass parts, free-flow agent 1~5 mass parts, described dual gas supply compound is a carbonic hydroammonium; Said pesticide original medicine is to the metastable agricultural chemicals of acid to the alkali sensitivity; Be acid source with material in the corresponding said dual gas supply compound; Said pesticide original medicine be acid labile to the metastable agricultural chemicals of alkali, in the corresponding said dual gas supply compound with material be alkali source.
2. agricultural chemicals aqueous dispersion effervescent tablet according to claim 1 is characterized in that: said is that in cartap or first dimension salt or Nitenpyram or Imidacloprid or Acetamiprid or dimethomorph or thiophene worm piperazine or Fluoxastrobin or kresoxim-methyl or Difenoconazole or carbendazim or cyprodinil or Flusilazole or piperazine humulone or metamitron or atrazine or cyhalofop-butyl or heteroauxin or brassin lactones or the gibberellin one or more are composite to the alkali sensitivity to the metastable agricultural chemicals of acid; Said acid labile is rimsulfuron or nicosulfuron or metsulfuron-methyl or chlorine sulphur is grand or one or more of pyrazosulfuron or bensulfuron-methyl or thifensulfuronmethyl or isoproturon or diuron or penoxsuam or Flumetsulam or two careless ether or Rynaxypyr or indenes worm prestige or pyrrole aphid ketone or fludioxonil or nitrile bacterium azoles or propiconazole or matrine or compound sodium nitrophenolate are composite to the metastable agricultural chemicals of alkali.
3. agricultural chemicals aqueous dispersion effervescent tablet according to claim 1 is characterized in that: said acid source is one or more in citric acid or tartaric acid or the fumaric acid; Said alkali source is one or more in potassium hydroxide or sodium hydroxide or sodium carbonate or the potash.
4. agricultural chemicals aqueous dispersion effervescent tablet according to claim 1 is characterized in that: said surfactant is one or more in penetrating agent BX or sodium lignin sulfonate or lauryl sodium sulfate or PO-EO block polyether or acrylate homopolymer sodium salt or the naphthalenesulfonate.
5. agricultural chemicals aqueous dispersion effervescent tablet according to claim 1 is characterized in that: said inert filler is one or more in corn starch or diatomite or talcum powder or bentonite or the kaolin.
6. agricultural chemicals aqueous dispersion effervescent tablet according to claim 1 is characterized in that: said binding agent is the one or more kinds of mixtures among water soluble starch or sodium carboxymethyl starch or polyethylene glycol PEG4000 or the polyethylene glycol PEG6000.
7. agricultural chemicals aqueous dispersion effervescent tablet according to claim 1 is characterized in that: said free-flow agent is one or more in white carbon or dolomol or the talcum powder.
8. preparation method of agricultural chemicals aqueous dispersion effervescent tablet according to claim 1 is characterized in that: may further comprise the steps:
(1) preparation master batch: in the pesticide original medicine that will accurately measure, the dual gas supply compound and material, surfactant, inert filler in mixer, mix, through comminution by gas stream it is crushed to more than 500 orders, powder is collected in another mixer; Adding 10~20% is dissolved with the water of binding agent and mediates; Obtain wet granular through extruder grain or wet granulation, dry to moisture content and be less than 1%, whole again grain sieves; Get 30~60 order particles, for use;
(2) compressing tablet: master batch, dual gas supply compound, the free-flow agent of the above-mentioned steps that will accurately measure (1) preparation mix in mixer; In tablet press machine, be pressed into the tablet of given configuration; Diameter is selected between 5~40mm; Thickness is selected between 3~15mm, and monolithic weight is at 0.5~20g.
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CN103098802A (en) * 2013-02-02 2013-05-15 广东中迅农科股份有限公司 Penoxsulam effervescent tablet and preparation method thereof
CN103109829A (en) * 2013-02-02 2013-05-22 广东中迅农科股份有限公司 Effervescent tablet of pymetrozine and isoprocarb and preparation method thereof
CN103155940A (en) * 2013-03-22 2013-06-19 青岛瀚生生物科技股份有限公司 Thiamethoxam and azoxystrobin compounded suspended seed coating and preparation method thereof
CN103329898A (en) * 2013-06-04 2013-10-02 广东中迅农科股份有限公司 Pymetrozine effervescent tablet and preparation method therefor
CN103380775A (en) * 2013-07-03 2013-11-06 发事达(南通)化工有限公司 Matrine-brassinolide suspension seed coating agent and preparation method thereof
CN103503887A (en) * 2012-06-18 2014-01-15 张长平 Complex insecticidal bactericide used for controlling paddy rice insect disease
CN103609588A (en) * 2013-11-26 2014-03-05 广西安泰化工有限责任公司 Insecticide containing brassinolide and thiamethoxam
CN103918665A (en) * 2014-05-05 2014-07-16 河北双吉化工有限公司 Insecticide composition containing nitenpyram, pymetrozine and compound sodium nitrophenolate
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US11247944B2 (en) 2019-04-12 2022-02-15 Jeffrey Hanson Robbins Potassium citrate mixture formed from a dry fertilizer and methods thereof
US11254619B2 (en) 2019-04-12 2022-02-22 Jeffrey Hanson Robbins Dry composition including effervescent agents, biostimulant, and plant nutrient
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CN103503887A (en) * 2012-06-18 2014-01-15 张长平 Complex insecticidal bactericide used for controlling paddy rice insect disease
CN103109829A (en) * 2013-02-02 2013-05-22 广东中迅农科股份有限公司 Effervescent tablet of pymetrozine and isoprocarb and preparation method thereof
CN103098802B (en) * 2013-02-02 2016-05-11 广东中迅农科股份有限公司 penoxsuam effervescent tablet and preparation method thereof
CN103098802A (en) * 2013-02-02 2013-05-15 广东中迅农科股份有限公司 Penoxsulam effervescent tablet and preparation method thereof
CN103155940B (en) * 2013-03-22 2014-07-16 青岛瀚生生物科技股份有限公司 Thiamethoxam and azoxystrobin compounded suspended seed coating and preparation method thereof
CN103155940A (en) * 2013-03-22 2013-06-19 青岛瀚生生物科技股份有限公司 Thiamethoxam and azoxystrobin compounded suspended seed coating and preparation method thereof
CN103329898A (en) * 2013-06-04 2013-10-02 广东中迅农科股份有限公司 Pymetrozine effervescent tablet and preparation method therefor
CN103380775B (en) * 2013-07-03 2015-11-18 发事达(南通)化工有限公司 A kind of matrine-brassin lactones suspension seed-coating agent and preparation method thereof
CN103380775A (en) * 2013-07-03 2013-11-06 发事达(南通)化工有限公司 Matrine-brassinolide suspension seed coating agent and preparation method thereof
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