CN102823589B - 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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CN102823589B
CN102823589B CN201210355555.9A CN201210355555A CN102823589B CN 102823589 B CN102823589 B CN 102823589B CN 201210355555 A CN201210355555 A CN 201210355555A CN 102823589 B CN102823589 B CN 102823589B
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pesticide
tablet
mass parts
effervescent
water
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CN102823589A (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 pesticide water disperses 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 rapidly a large amount of bubbles, and in water, foaming boiling, disintegration fast, be dispersed in water active ingredient uniformly, formation has solution or the aqueous dispersion of good action effect, and suspensibility and dispersiveness are higher.
It is in tablet, to contain acidic materials (acid source that pesticide water disperses the general principle of effervescent tablet, 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 containing carbonate, as carbonic hydroammonium, sodium carbonate etc.), there is neutralization reaction 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, pesticide water disperses effervescent tablet can directly shed in use disintegration diffusion voluntarily in paddy field, also can drop into disintegration in sprayer and spray in crop target after disperseing.
The pesticidal preparations of China is mainly missible oil and pulvis at present, because missible oil uses a large amount of chemical solvent-as toluene, dimethylbenzene etc. cause very big injury to environment and user, pulvis flies upward drift because it is serious, particularly serious to user's injury, metering difficulty when these two kinds of formulations also exist packaging to use, and aqueous dispersion effervescent tablet is owing to having given configuration, accurately monolithic weight, solvent-free, without drift, easy to use, there is again foaming boiling simultaneously, disintegration fast, higher suspension rate and dispersive property, it is a kind of environmentally friendly pesticides new formulation, become the frontier that current pesticidal preparations develops rapidly.
Pesticide water disperses effervescent tablet to be generally made up of pesticide original medicine, acid source, carbon dioxide source, surfactant, free-flow agent, binding agent, inert filler etc., described in the patent No. 00107465.2,200610104832.3, but most Pesticidal products are not to be exactly unstable to alkali to acid, very easily decompose, thereby cause product poor chemical stability, active ingredient degraded, result of use declines.
Summary of the invention
Goal of the invention: for the source of getting angry, select corresponding acid source or alkali source for different agricultural chemicals physical property with dual gas supply compound-carbonic hydroammonium, a kind of pesticide water that obtains stable chemical performance disperses effervescent tablet.
Another object of the present invention is to provide the preparation method that this pesticide water disperses effervescent tablet.
Technical scheme: a kind of pesticide water disperses 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, 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 carbonic hydroammonium;
Described pesticide original medicine be to alkali sensitivity to the metastable agricultural chemicals of acid, in corresponding described dual gas supply compound and material be acid source; Described pesticide original medicine be acid labile to the metastable agricultural chemicals of alkali, in corresponding described dual gas supply compound and material be alkali source.
As optimization, described is that one or more in cartap or first dimension salt or Nitenpyram or Imidacloprid or Acetamiprid or dimethomorph or Diacloden 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 gibberellin are composite to alkali sensitivity to the metastable agricultural chemicals of acid; Described 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 indoxacarb or pymetrozine 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, described acid source is one or more in citric acid or tartaric acid or fumaric acid; Described alkali source is one or more in potassium hydroxide or sodium hydroxide or sodium carbonate or potash.
As optimization, described 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 naphthalenesulfonate.
As optimization, described inert filler is one or more in corn starch or diatomite or talcum powder or bentonite or kaolin.
As optimization, described binding agent is the one or more kinds of mixtures in water soluble starch or sodium carboxymethyl starch or polyethylene glycol PEG4000 or polyethylene glycol PEG6000.
As optimization, described free-flow agent is one or more in white carbon or dolomol or talcum powder.
Described pesticide water disperses the preparation method of effervescent tablet, comprises the following steps:
1, to alkali sensitivity to the metastable agricultural chemicals of acid:
(1) prepare master batch: good accurate-metering pesticide original medicine, acid source, surfactant, inert filler are mixed in mixer, more than being crushed to 500 orders by air-flow crushing, powder is collected in another mixer, add 10~20% aqueous solution that are dissolved with binding agent to mediate, obtain wet granular through extruder grain or wet granulation, dry to moisture content and be less than 1%, more whole grain sieves, get 30~60 order particles, stand-by;
(2) compressing tablet: master batch, carbonic hydroammonium, free-flow agent prepared by good accurate-metering above-mentioned (1) 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) prepare master batch: good accurate-metering pesticide original medicine, alkali source, surfactant, inert filler are mixed in mixer, more than being crushed to 500 orders by air-flow crushing, powder is collected in another mixer, add 10~20% aqueous solution that are dissolved with binding agent to mediate, obtain wet granular through extruder grain or wet granulation, dry to moisture content and be less than 1%, more whole grain sieves, get 30~60 order particles, stand-by;
(2) compressing tablet: master batch, carbonic hydroammonium, free-flow agent prepared by good accurate-metering above-mentioned (1) 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 by 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 as follows:
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 acid source, and AOH is alkali source.
The invention has the advantages that: pesticide water of the present invention disperses the effervescent tablet disintegration of seething with excitement rapidly in water, can avoid pesticide water to disperse the degraded of effervescent tablet active ingredient, and result of use declines, thereby the pesticide water that obtains stable chemical performance disperses effervescent tablet.
Pesticide water of the present invention disperses the preparation method of effervescent tablet to can be used for producing as cartap, first dimension salt, Nitenpyram, Imidacloprid, Acetamiprid, dimethomorph, Diacloden, Fluoxastrobin, kresoxim-methyl, Difenoconazole, carbendazim, cyprodinil, Flusilazole, 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 ether, Rynaxypyr, indoxacarb, pymetrozine, fludioxonil, nitrile bacterium azoles, propiconazole, matrine, the aqueous dispersion effervescent tablets such as compound sodium nitrophenolate.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
5% emamectin benzoate water disperses the preparation (percentage composition in the present embodiment is mass percent) of effervescent tablet:
(1) prepare 6.17% first dimension salt master batch: by good the accurate-metering former medicine 8.8kg of 70% first dimension salt, tartaric acid 12kg, sodium lignin sulfonate 2kg, naphthalene sulfonate 6kg, corn starch 25kg, kaolin 44.7kg mixes in mixer, more than being crushed to 500 orders by air-flow crushing, powder is collected in another mixer, the aqueous solution that adds 15.5kg to be dissolved with 10% sodium carboxymethyl starch is mediated, obtain column wet granular through extruder grain, dry to moisture content and be less than 1%, sieved by the whole grain of pelletizing machine vibratory sieve again, get 30~60 order particles, stand-by;
(2) compressing tablet: master batch 81kg, carbonic hydroammonium 18kg, white carbon 1kg prepared by good accurate-metering above-mentioned (1) mix in mixer, are pressed into circular tablet in tablet press machine, diameter 12mm, thickness 3.5mm, monolithic weight is in 1.0g left and right;
(3) performance test: active ingredient: 5.06%, 30 DEG C of heat storage was 5.05% after 30 days; Disintegration time: 74s; Suspensibility: 91.4%, pH value: the 3.7(1% aqueous solution);
(4) application test:
The present embodiment is applied to control rice leaf folder, and result shows that effect is better than commercially available 5% emamectin benzoate water dispersible granule and 40% chlorpyrifos ec, effectively desinsection, and also also lower to the loss of leaf.See the following form:
Figure 807873DEST_PATH_IMAGE001
Embodiment 2
The preparation (percentage composition in the present embodiment is mass percent) of 40% Acetamiprid aqueous dispersion effervescent tablet:
(1) prepare 49.4% Acetamiprid master batch: by good the accurate-metering former medicine 51.5kg of 96% Acetamiprid, citric acid 12kg, acrylate homopolymer sodium salt 2kg, naphthalene sulfonate 8kg, corn starch 15kg, talcum powder 9.8kg mixes in mixer, more than being crushed to 500 orders by air-flow crushing, powder is collected in another mixer, the aqueous solution that adds 17kg to be dissolved with 10% PEG6000 is mediated, obtain irregular wet granular through wet granulation, dry to moisture content and be less than 1%, sieved by the whole grain of pelletizing machine vibratory sieve again, get 30~60 order particles, stand-by;
(2) compressing tablet: master batch 81kg, carbonic hydroammonium 18kg, dolomol 1kg prepared by good accurate-metering above-mentioned (1) mix in mixer, are pressed into circular tablet in tablet press machine, diameter 24mm, thickness 5mm, monolithic weight is in 2g left and right;
(3) performance test: active ingredient: 40.38%, 30 DEG C of heat storage was 40.40% after 30 days; Disintegration time: 82s; Suspensibility: 92.6%, pH value: the 4.1(1% aqueous solution);
(4) application test:
The present embodiment is applied to control cabbage aphid, and result shows that quick-acting is better than 3% acetamiprid EC, sees the following form:
Embodiment 3
The preparation (percentage composition in the present embodiment is mass percent) of 10% penoxsuam aqueous dispersion effervescent tablet:
(1) prepare 14.0% penoxsuam master batch: by the former medicine 14.7kg of 95% penoxsuam good accurate-metering, potash 49kg, acrylate homopolymer sodium salt sodium 3kg, naphthalene sulfonate 8kg, corn starch 15kg, , diatomite 8.7kg mixes in mixer, more than being crushed to 500 orders by air-flow crushing, powder is collected in another mixer, the aqueous solution that adds 16kg to be dissolved with 7% sodium carboxymethyl starch and 3% PEG4000 is mediated, obtain irregular wet granular through wet granulation, dry to moisture content and be less than 1%, sieved by the whole grain of pelletizing machine vibratory sieve again, get 30~60 order particles, stand-by,
(2) compressing tablet: master batch 71.5kg, carbonic hydroammonium 27kg, white carbon 1kg, talcum powder 0.5kg prepared by good accurate-metering above-mentioned (1) mix in mixer, in tablet press machine, be pressed into circular tablet, diameter 12mm, thickness 3.5mm, monolithic weight is in 1.0g left and right;
(3) performance test: active ingredient: 10.3%, 30 DEG C of heat storage was 10.21% after 30 days; Disintegration time: 80s; Suspensibility: 88.7%, pH value: the 8.7(1% aqueous solution);
(4) application test:
The present embodiment carries out the raw test of indoor weeding to be tested, and it is consistent that result is shown in 2.5% oil suspending agent effect, sees the following form:
Figure 442434DEST_PATH_IMAGE003
Embodiment 4
The preparation (percentage composition in the present embodiment is mass percent) of 20% Rynaxypyr aqueous dispersion effervescent tablet:
(1) prepare 27.8% Rynaxypyr master batch: by the former medicine 30.2kg of 92% Rynaxypyr good accurate-metering, 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, more than being crushed to 500 orders by air-flow crushing, powder is collected in another mixer, the aqueous solution that adds 16kg to be dissolved with 7% water soluble starch and 3% PEG6000 is mediated, obtain column wet granular through extruder grain, dry to moisture content and be less than 1%, sieved by the whole grain of pelletizing machine vibratory sieve again, get 30~60 order particles, stand-by,
(2) compressing tablet: master batch 72kg, carbonic hydroammonium 27kg, white carbon 1kg prepared by good accurate-metering above-mentioned (1) mix in mixer, are pressed into circular tablet in tablet press machine, diameter 24mm, thickness 8mm, monolithic weight is in 5.0g left and right;
(3) performance test: active ingredient: 20.1%; Disintegration time: 93s; Suspensibility: 90.6%, pH value: the 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, result shows tablet and suspending agent action effect no significant difference:
Figure 837643DEST_PATH_IMAGE004
Embodiment 5
The preparation (percentage composition in the present embodiment is mass percent) of 20% Difenoconazole aqueous dispersion effervescent tablet:
(1) prepare 27.8% Difenoconazole master batch: by 96% good accurate-metering difenoconazole technical material 29kg, fumaric acid 12.5kg, lauryl sodium sulfate 3kg, naphthalene sulfonate 8kg, corn starch 41.7kg, kaolin 4.2kg mixes in mixer, more than being crushed to 500 orders by air-flow crushing, powder is collected in another mixer, the aqueous solution that adds 16kg to be dissolved with 10% water soluble starch is mediated, obtain irregular wet granular through wet granulation, dry to moisture content and be less than 1%, sieved by the whole grain of pelletizing machine vibratory sieve again, get 30~60 order particles, stand-by,
(2) compressing tablet: master batch 72kg, carbonic hydroammonium 27kg, dolomol 1kg prepared by good accurate-metering above-mentioned (1) mix in mixer, are pressed into circular tablet in tablet press machine, diameter 24mm, thickness 8mm, monolithic weight is in 5.0g left and right;
(3) performance test: active ingredient: 20.3%; Disintegration time: 87s; Suspensibility: 91.4%, pH value: the 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:
Figure 25917DEST_PATH_IMAGE005

Claims (6)

1. a pesticide water disperses 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, 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 carbonic hydroammonium; Described pesticide original medicine 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 indoxacarb or pymetrozine or fludioxonil or nitrile bacterium azoles or propiconazole or matrine or compound sodium nitrophenolate are composite, in corresponding described dual gas supply compound and material be one or more in potassium hydroxide or sodium hydroxide or sodium carbonate or potash.
2. pesticide water according to claim 1 disperses effervescent tablet, it is characterized in that: described 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 naphthalenesulfonate.
3. pesticide water according to claim 1 disperses effervescent tablet, it is characterized in that: described inert filler is one or more in corn starch or diatomite or talcum powder or bentonite or kaolin.
4. pesticide water according to claim 1 disperses effervescent tablet, it is characterized in that: described binding agent is the one or more kinds of mixtures in water soluble starch or sodium carboxymethyl starch or polyethylene glycol PEG4000 or polyethylene glycol PEG6000.
5. pesticide water according to claim 1 disperses effervescent tablet, it is characterized in that: described free-flow agent is one or more in white carbon or dolomol or talcum powder.
6. pesticide water disperses the preparation method of effervescent tablet as claimed in claim 1, it is characterized in that: comprise the following steps:
(1) prepare master batch: by pesticide original medicine good accurate-metering, dual gas supply compound and material, surfactant, inert filler in mixer, mix, more than being crushed to 500 orders by air-flow crushing, powder is collected in another mixer, add 10~20% water that are dissolved with binding agent to mediate, obtain wet granular through extruder grain or wet granulation, dry to moisture content and be less than 1%, more whole grain sieves, get 30~60 order particles, stand-by;
(2) compressing tablet: master batch, dual gas supply compound, free-flow agent prepared by the good above-mentioned steps of accurate-metering (1) 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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