CN105191983B - A kind of auxotype copper fungicide and preparation method - Google Patents
A kind of auxotype copper fungicide and preparation method Download PDFInfo
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- CN105191983B CN105191983B CN201510719364.XA CN201510719364A CN105191983B CN 105191983 B CN105191983 B CN 105191983B CN 201510719364 A CN201510719364 A CN 201510719364A CN 105191983 B CN105191983 B CN 105191983B
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Abstract
The present invention relates to a kind of auxotype copper fungicide and preparation method; the trace elements such as boron, zinc, manganese, molybdenum are added in cupric ammine complex; ethylenediamine of the addition with sterilizing function and high-efficiency copper ion chelating agent; add simultaneously and promote the citric acid of tricarboxylic acid cycle be used as chelating agent as complexing agent and addition EDTA etc., composition it is a kind of both with copper protective fungicide and absorbability sterilizing function and meanwhile microelement-supplementing promotion plant growth liquid complex.In this deep blue purple color complex solution, water-insoluble is few, and free copper ion concentration is very low, antimicrobial spectrum is wide, (endogenous and native transmissibility plant diseases) such as preventing and treating crop droop, powdery mildew, early blight works well, and is less prone to poisoning, and and can promotes plant growth volume increase.Production process is simple and easy, and raw material is easy to get, and production cost is relatively low, is easy to promote.
Description
Technical field
The invention mainly relates to a kind of copper fungicide, more particularly to a kind of auxotype with protective effect and systemic action
Copper fungicide and preparation method thereof.
Background technology
Copper fungicide, due to wide sterilization spectrum, the resistance to the action of a drug is not likely to produce, in being widely used agriculturally, with long
History.Traditional basic copper sulfate (Bordeaux mixture etc.) application history existing more than 100 years as protective fungicide, copper ammonia complexation
Thing solution (network ammonia copper) agriculturally prevent and treat crop a variety of germs (such as droop, downy mildew, angular leaf spot, epidemic disease, false smut,
Fruit tree putrefaction disease etc.) it has been a kind of agricultural measures generally used.But the alkalescence of common cupric ammine complex solution it is relatively strong and
The characteristics of free ammonium ion, easily there is poisoning in improper use, limits wider application.Thereafter occur a variety of comparing cuprammonium
The highly efficient complex compound of complex ion, chelate, compound (such as amino acid copper, polyacid copper, ethylenediamine polyacid copper, quinoline
Copper etc.), preventing and treating crop endogeny disease effect is preferable.But the chelating or complexing degree to copper ion are all not reaching to maximization,
Free Cu2+The concentration of ion is not lowered to minimum, and the possibility for poisoning occur still is present.
The content of the invention
It is an object of the invention to provide a kind of highly efficient auxotype copper fungicide, make free Cu therein2+Ion
Concentration further reduces, and use is safer, the absorbability copper fungicide of controlling disease effect promoting, and compounds various crop needs
Trace element and growth regulatory substance, while controlling disease, promote plant growth, improve yield and improving quality.
A kind of auxotype copper fungicide for adding ethylenediamine, is made up of following components by weight：
Wherein, described ethylenediamine is the chelating agent for being different from other complexing agents, chelating agent.
Wherein, other described complexing agents, chelating agent are in citric acid, EDTA, EDETATE SODIUM, DTPA, EDDHA sodium salt etc.
One or more.
Wherein, described micro- salt be zinc sulfate, zinc acetate or zinc nitrate, manganese sulfate, manganese acetate or manganese nitrate,
One or more in ferrous sulfate or iron ammonium sulfate, ammonium molybdate or sodium molybdate, borax, boric acid etc..
Wherein, described surfactant is anion surfactant and nonionic surfactant.
Wherein, described surfactant is selected from AES, lauryl sodium sulfate, lauryl sodium sulfate, detergent alkylate
Sodium sulfonate, tween, Si Pan, OP-10 (APES), peregal, LS (lauroyl sarcosine sodium) one kind or
It is several.
Wherein, described plant growth regulator is stable material in alkalescence, selected from mepiquat chloride, Nafusaku, DA-
6th, the one or more of amino chitosan oligosaccharide, drop-proof agent, compound sodium nitrophenolate, glycine betaine.
Wherein, close copper solution in ammonium and add micro- salt and a variety of chelating agents, complexing agent, surfactant, plant
Growth regulator；Finished product is homogeneous phase solution of the darkviolet to deep blue purple color.
Which use to the very high ethylenediamine of copper ion complex stability as complexing agent.
Ethylenediamine, chemical formula NH2-CH2-CH2-NH2, molecular weight 60.10, colourless or slightly yellow liquid, there is similar ammonia
Smell, there is strong basicity, 8~10 DEG C of fusing point.
Ethylenediamine is very strong to the complexing power of bivalent cupric ion, and its Complex Stability Constants is log β=21.0, not only far
Higher than ammoniacal copper complex ion (log β=13.32), also above copper citrate complex ion (its log β=14.2), higher than EDTA copper (its
Log β=18.8).Its complex mechanism is：The stabilization that ethylenediamine closes copper is because chelating effect.It is dsp3 hydridization that ethylenediamine, which closes copper,
Copper ion forms stable five-membered ring chelate with ethylenediamine.
Ethylenediamine molecular weight is smaller, and the metal ion quantity of its Unit Weight complexing is also higher, so, as long as addition is few
Ethylenediamine can make part copper ion complexation into highly stable water-soluble complex ion.In addition, ethylenediamine is inherently a kind of
Bactericide, bactericidal effect can further enhance after being complexed with copper ion.
As the complexing agent of copper ion it is the outstanding characteristic that has of the present invention present invention employs ethylenediamine.Add ethylenediamine
Afterwards, product is changed into deep blue purple color to darkviolet from navy blue, and maintains homogeneous phase transparent state.
In order that various trace elements (zinc, manganese, iron, molybdenum, boron) ion is all deposited with completely water miscible complexing sequestering properties
In system, be easy to crop efficient absorption utilize, while with the addition of citric acid, amino acid, EDTA (ethylenediamine tetra-acetic acid),
DTPA (diethylene triamine pentacetic acid (DTPA)), EDDHA (the big acetic acid of the salicyl of ethylenediamine two) etc. are as complexing agent, chelating agent.Make body
Metal ion in system is complexed chelating completely, and water-soluble solution state is presented, can be uniformly dispersed quickly when being diluted with water.Add lemon
It is 7.0~10.5 that the acidic materials such as lemon acid have the pH value of regulation system simultaneously, and it is too strong to be unlikely to alkalescence.
In order to improve promotion plant growth, promote crop to absorb nutrient, reasonably with the addition of in system
Surfactant (AES, lauryl sodium sulfate, sodium alkyl benzene sulfonate, OP-10, peregal etc.) and plant growth regulator (contracting
Save amine, Nafusaku, amino chitosan oligosaccharide, drop-proof agent, compound sodium nitrophenolate, glycine betaine etc.).
The citric acid used in system is both the complexing agent of copper ion, is the acidity-basicity regulator of system again, and itself is planted
Thing has the function that to promote plant kerbs tricarboxylic acid cycle again after absorbing, so as to can also promote the growth of crop.
Product of the present invention has good prevention effect to the various bacteria of crop, fungi, Disease.It can fill
Root, foliage-spray and smearing, the utilization rate of copper ion improve, and extension rate is big, and dosage is few, is both acted on protective control,
There is the preventive and therapeutic effect of absorbability conduction again, easy to use, manufacturing process is easy, has promotional value.Product of the present invention after
Test and use on the vegetables on Shanxi, Shaanxi, Hebei and other places, melon, fruit tree and industrial crops over several years, it is withered for preventing and treating watermelon
Wither disease, downy mildew of garpe, green pepper early blight late blight, angular leaf spot of cucumber, canker of apple fruit etc., particularly prevent and treat melon continuous cropping
One of disease droop, achieve obvious prevention effect and yield increasing effect.
It is an advantage of the invention that：Most stable of ethylenediamine copper complexing design at present is employed in the formula of the present invention, is used
In free copper ion high number reduce, the poisoning of copper agent substantially reduces.Product of the present invention is water-soluble very well, and raw material is easy
, simple production process is easy to use, and bin stability etc. is good.Not only with protectiveness but also with uptake and translocation, anti-Zhiduo County
The effect of kind disease is improved, while promotes the significant effect of plant growth.Compared to traditional copper biocide preparation product, use
Work well.With application value.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Material is all from commercially available.Wherein, EDTA be the abbreviation of ethylenediamine tetra-acetic acid, DTPA be diethylene triamine pentacetic acid (DTPA)
Abbreviation, EDDHA are the abbreviations of the big acetic acid of the salicyl of ethylenediamine two.
Embodiment 1
(1) preparation of copper ammon solution
25 parts of copper sulphate, 35 parts of ammonium hydrogen carbonate are added in 40 parts of water, heating and stirring reaction at 70 DEG C, release two
Carbon oxide gas, it is copper ammon solution after being cooled down after dissolving, cupric about 7.5%, sampling analysis is standby；
(2) preparation of auxotype copper fungicide：40Kg copper ammon solutions are taken, add zinc sulfate 3kg, manganese sulfate under agitation
3kg, citric acid 3kg, ethylenediamine tetra-acetic acid (EDTA) 5kg, borax 3kg, iron ammonium sulfate 0.5kg, sodium molybdate 0.2kg, stirring
It is uniformly dispersed, is slowly added to ethylenediamine 5kg, exothermic heat of reaction, stirs more than 30 minutes.After chelating dissolving completely, add under agitation
Enter AES ammonium surfactant 0.8kg, add methyl α-naphthyl acetate 0.5kg, add water 36kg, stir, inspection by sampling, produce nutrition
Type copper fungicide.
Embodiment 2
(1) preparation of copper ammon solution
25 parts of copper sulphate are added in 20 parts of water, about 60 parts of the ammoniacal liquor of lower dropwise addition 26% is stirred, reaches 10.5 to pH value
~11.0, and present and be completely dissolved state, both obtain copper ammon solution.Cupric about 6.2%, sampling analysis is standby；
(2) preparation of auxotype copper fungicide：Above-mentioned 60kg copper ammon solutions are taken, add zinc nitrate 4kg, sulfuric acid under agitation
Manganese 3kg, citric acid 2.5kg, ethylenediamine tetra-acetic acid (EDTA) 5kg, borax 4kg, ferrous sulfate 0.4kg, sodium molybdate 0.1kg, are stirred
Mix uniformly, be slowly added to ethylenediamine 4kg, exothermic heat of reaction, stir more than 30 minutes.Chelating completely after, under agitation add tween-
80 surfactant 0.8kg, compound sodium nitrophenolate 0.5kg is added, water 15.7kg to total amount 100kg is added, stirs, sampling inspection
Test, produce auxotype copper fungicide.
Embodiment 3
(1) preparation of copper ammon solution
23 parts of copper nitrates are added in 22 parts of water, about 60 parts of the ammoniacal liquor of lower dropwise addition 26% is stirred, reaches 10.5 to pH value
~11.0, and present and be completely dissolved state, both obtain copper ammon solution.Cupric about 5.9%, sampling analysis is standby；
(2) preparation of auxotype copper fungicide：Above-mentioned 64kg copper ammon solutions are taken, add zinc sulfate 2kg, nitric acid under agitation
Manganese 3.0kg, citric acid 4kg, ethylenediamine tetra-acetic acid (EDTA) 5kg, the big sodium acetate of the salicyl of ethylenediamine two (EDDHANa) 2kg,
Boric acid 4kg, ferrous sulfate 1.5kg, ammonium molybdate 0.5kg, stir, be slowly added to ethylenediamine 9kg, exothermic heat of reaction, stirring 30
More than minute.After chelating is complete, OP-10 surfactant 1.0kg are added under agitation, are added DA-61.5kg, are added water
2.5kg to total amount 100kg, stirs, inspection by sampling, produces auxotype copper fungicide and (contains Cu:3.77%).
Embodiment 4
(1) preparation of copper ammon solution：The ammino copper crystal 28kg of sulfuric acid monohydrate four is taken, is dissolved into 67kg water, adds in right amount
Ammoniacal liquor 5kg, stirs, and both obtains copper ammon solution.Cupric about 7.2%, sampling analysis is standby；
(2) preparation of auxotype copper fungicide：Above-mentioned 70kg parts copper ammon solution is taken, adds zinc acetate 2.0kg under agitation,
Manganese nitrate 1.5kg, citric acid 3kg, ethylenediamine tetra-acetic acid (EDTA) 3kg, boric acid 4kg, ferrous sulfate 0.2kg, sodium molybdate
0.3kg, stir, be slowly added to ethylenediamine 8kg, exothermic heat of reaction, stir more than 30 minutes.After chelating is complete, under agitation
LS (lauroyl sarcosine sodium) surfactant 1.5kg is added, glycine betaine 5.0kg is added, adds water 1.5kg to total amount
100kg, stir, inspection by sampling, produce auxotype copper fungicide.
Embodiment 5
(1) preparation of copper ammon solution：It is same as Example 4.
(2) preparation of auxotype copper fungicide：Above-mentioned 35kg copper ammon solutions are taken, add zinc acetate 4kg, acetic acid under agitation
Manganese 4kg, citric acid 6kg, ethylenediamine tetra-acetic acid (EDTA) 4kg, the big sodium acetate of the salicyl of ethylenediamine two (EDDHANa) 4kg, boron
Sand 5kg, ferrous sulfate 1.5kg, sodium molybdate 0.5kg, stir, be slowly added to ethylenediamine 4kg, exothermic heat of reaction, stir 30 points
It is more than clock.After chelating is complete, the surfactant 1.0kg of paregal O -15 is added under agitation, adds amino-oligosaccharide 2.0kg,
Water 29kg to total amount 100kg is added, is stirred, inspection by sampling, produces auxotype copper fungicide.
Embodiment 6
(1) preparation of copper ammon solution：It is same as Example 1.
(2) preparation of auxotype copper fungicide：Above-mentioned 36kg copper ammon solutions are taken, add zinc acetate 4kg, acetic acid under agitation
Manganese 4kg, citric acid 3kg, kilnitamin 6kg, the big sodium acetate of the salicyl of ethylenediamine two (EDDHANa) 3kg, boric acid 5kg, sulphur
Sour ferrous ammonium 1.5kg, sodium molybdate 0.5kg, stirs, and is slowly added to ethylenediamine 10kg, exothermic heat of reaction, stirring 30 minutes with
On.After chelating is complete, AES surfactant 1.5kg are added under agitation, are added mepiquat chloride 2.5kg, are added water 23kg to total amount
100kg, stir, inspection by sampling, produce auxotype copper fungicide.
Embodiment 7
The present invention prevents and treats withered watermelon and withered the effect of disease sickle-like bacteria：
(1) protection effect comparative test is done into the network ammonia copper water agent of 1~embodiment of embodiment 6 and 22%.
(2) trial crops：Watermelon.
(3) germ：Fusarium wilt.
(4) apply：Germ is inoculated with after spraying decoction within 24 hours.
(5) serial dilutions are selected, so as to observing effect.
(6) effect experiment (sickle-like bacteria inhibiting rate) records：
For the present composition in the case where dosage (in terms of copper ion %) is reduced, the effect for preventing and treating watermelon blight is good
It is good.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (6)
- A kind of 1. auxotype copper fungicide, it is characterised in that：It is made up of following component as mass fraction：Wherein, other described complexing agents or chelating agent are one in citric acid, EDTA, EDETATE SODIUM, DTPA, EDDHA sodium salt Kind is several；Described micro- salt is zinc sulfate, zinc acetate or zinc nitrate, manganese sulfate, manganese acetate or manganese nitrate, ferrous sulfate Or the one or more in iron ammonium sulfate, ammonium molybdate or sodium molybdate, borax, boric acid；Described surfactant is anion surfactant and nonionic surfactant；Described plant growth regulator is stable material in alkalescence, selected from mepiquat chloride, Nafusaku, DA-6, amino shell Oligosaccharides, drop-proof agent, compound sodium nitrophenolate, the one or more of glycine betaine.
- A kind of 2. auxotype copper fungicide as claimed in claim 1, it is characterised in that：By following component as mass fraction Composition：Wherein, other described complexing agents or chelating agent are one in citric acid, EDTA, EDETATE SODIUM, DTPA, EDDHA sodium salt Kind is several；Described micro- salt is zinc sulfate, zinc acetate or zinc nitrate, manganese sulfate, manganese acetate or manganese nitrate, ferrous sulfate Or the one or more in iron ammonium sulfate, ammonium molybdate or sodium molybdate, borax, boric acid；Described surfactant is anion surfactant and nonionic surfactant；Described plant growth regulator is stable material in alkalescence, selected from mepiquat chloride, Nafusaku, DA-6, amino shell Oligosaccharides, drop-proof agent, compound sodium nitrophenolate, the one or more of glycine betaine.
- A kind of 3. auxotype copper fungicide as claimed in claim 1 or 2, it is characterised in that：The ethylenediamine is a kind of copper Chelating agent.
- A kind of 4. auxotype copper fungicide as claimed in claim 1 or 2, it is characterised in that：Described surfactant is selected from AES, lauryl sodium sulfate, lauryl sodium sulfate, neopelex, tween, Si Pan, OP-10, the one of peregal Kind is several.
- A kind of 5. auxotype copper fungicide preparation method, it is characterised in that：1) copper ammon solution is prepared, copper sulphate, ammonium hydrogen carbonate are added to the water, heating and stirring reaction at 70 DEG C, releases two Carbon oxide gas, it is copper ammon solution after being cooled down after dissolving；2) auxotype copper fungicide is prepared, takes copper ammon solution obtained above, stirs the lower micro- salt of addition, other complexings Agent or chelating agent, it is dispersed with stirring uniformly, is slowly added to ethylenediamine, stirs more than 30 minutes；After chelating dissolving completely, under agitation Surfactant and plant growth regulator are added, is stirred, obtains auxotype copper fungicide, finished product is darkviolet to dark blue The solution of purple, in auxotype copper fungicide is prepared, percentage by weight is as follows shared by each component：Wherein, other described complexing agents or chelating agent are one in citric acid, EDTA, EDETATE SODIUM, DTPA, EDDHA sodium salt Kind is several；Described micro- salt is zinc sulfate, zinc acetate or zinc nitrate, manganese sulfate, manganese acetate or manganese nitrate, ferrous sulfate Or the one or more in iron ammonium sulfate, ammonium molybdate or sodium molybdate, borax, boric acid；Described surfactant is anion surfactant and nonionic surfactant；Described plant growth regulator is stable material in alkalescence, selected from mepiquat chloride, Nafusaku, DA-6, amino shell Oligosaccharides, drop-proof agent, compound sodium nitrophenolate, the one or more of glycine betaine.
- A kind of 6. preparation method of auxotype copper fungicide as claimed in claim 5, it is characterised in that：Preparing auxotype copper In bactericide, percentage by weight is as follows shared by each component：Wherein, other described complexing agents or chelating agent are one in citric acid, EDTA, EDETATE SODIUM, DTPA, EDDHA sodium salt Kind is several；Described micro- salt is zinc sulfate, zinc acetate or zinc nitrate, manganese sulfate, manganese acetate or manganese nitrate, ferrous sulfate Or the one or more in iron ammonium sulfate, ammonium molybdate or sodium molybdate, borax, boric acid；Described surfactant is anion surfactant and nonionic surfactant；Described plant growth regulator is stable material in alkalescence, selected from mepiquat chloride, Nafusaku, DA-6, amino shell Oligosaccharides, drop-proof agent, compound sodium nitrophenolate, the one or more of glycine betaine.
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| CN107337503A (en) * | 2017-06-06 | 2017-11-10 | 重庆金满地肥料有限公司 | A kind of preparation method of cupric medicine fertilizer and its pulvis |
| CN107445741A (en) * | 2017-09-28 | 2017-12-08 | 惠州市欧野科技有限公司 | A kind of watermelon mill water culture nutrient solution |
| CN113439759A (en) * | 2021-08-04 | 2021-09-28 | 李安民 | Copper citrate and bacillus polymyxa root sterilization composition and preparation method thereof |
| CN113767931A (en) * | 2021-09-09 | 2021-12-10 | 广西太美生物科技股份有限公司 | Plant immunizing agent containing phosphorous acid and copper ions and preparation method thereof |
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|---|---|---|---|---|
| CN1033230A (en) * | 1987-11-24 | 1989-06-07 | 山西省临猗县精细化工厂 | Anti-wither chemical and preparation method thereof |
| CN1077338A (en) * | 1993-04-02 | 1993-10-20 | 康朝阳 | Composite agriculture chemical and synthetic method thereof |
| CN101322499A (en) * | 2008-07-28 | 2008-12-17 | 李海涛 | Zinc-cupric-amminium complexion composite plant acid bactericidal agent |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033230A (en) * | 1987-11-24 | 1989-06-07 | 山西省临猗县精细化工厂 | Anti-wither chemical and preparation method thereof |
| CN1077338A (en) * | 1993-04-02 | 1993-10-20 | 康朝阳 | Composite agriculture chemical and synthetic method thereof |
| CN101322499A (en) * | 2008-07-28 | 2008-12-17 | 李海涛 | Zinc-cupric-amminium complexion composite plant acid bactericidal agent |
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