Summary of the invention
The purpose of this invention is to provide a kind of preparation method and application of copper rosinate, there is the method complexity in the preparation that the invention solves present copper rosinate, is difficult for implementing the problem of not environmental protection, and the narrow problem of range of application of present copper rosinate.
The preparation method of copper rosinate mixes mantoquita and alkali lye earlier among the present invention, stir into symmetric suspension, slowly splash in the solution of rosin and solvent again, solution colour gradually becomes green by blueness in the dropping process, and there is exothermic phenomenon to produce, to in time cool off, dripped off in general 20-40 minute, drip off, be warming up to 70-90 ℃, and carry out the normal pressure dehydration reaction, after dehydration finishes with water trap (100L), filter the 20%-50% solution that obtains copper rosinate, the content of analyzing and testing product with standard filter paper.
Among the preparation method of copper rosinate, the molar ratio scope of rosin and mantoquita, alkali lye is (1-4): (0.5-1.5) among the present invention: (1-4), the optimum proportion scope is (2-3): (0.8-1.2): (2-4); The mass ratio range of rosin and solvent is 1: (3-6), the optimum proportion scope is 1: (3-4.5).
Among the present invention among the preparation method of copper rosinate, used solvent is the mixture of a kind of of methyl alcohol, ethanol, butanols, toluene, dimethylbenzene, solvent oil, dimethyl formamide, acetone, butanone or pimelinketone or at least two kinds.
Among the present invention among the preparation method of copper rosinate, used alkali lye is the mixture of a kind of of sodium hydroxide, potassium hydroxide, ammoniacal liquor, thanomin, diethanolamine, trolamine, methylamine, ethamine or triethylamine or at least two kinds.
Among the present invention among the preparation method of copper rosinate, used mantoquita is the mixture of a kind of of copper sulfate, cupric sulfate pentahydrate, cupric chloride, cupric nitrate, cupric tartrate sodium, neutralized verdigris, oxine mantoquita, chitosan mantoquita, Cuprocitrol, EDTA mantoquita or ammoniacal copper complex ion or at least two kinds.
The application of copper rosinate of the present invention is: the copper rosinate of method for preparing cooperates with medicament, is used to prevent and treat diseases and pests of agronomic crop.
The application of copper rosinate of the present invention, the medicament composite with copper rosinate is: sterilant, antibiotics or other sterilant such as triazole species, amides, miazines, methoxy acrylic, Evil (miaow) azole, thiazoles, morpholine class, pyridines, quinoline, pyroles, amino formate, organic phosphates.
Wherein, triazole species comprises: difenoconazole, Wocosin 50TK, tricyclazole, tebuconazole, own azoles alcohol, cyproconazole, alkene azoles alcohol, fluorine ring azoles, fluzilazol, flutriafol, nitrile bacterium azoles or triadimenol;
Amides comprises: flumorph, dimethomorph, efficient metaxanin, fultolanil, cyflufenamid or fenfuram;
Miazines comprises: phonetic mould amine, mepanipyrim, cyprodinil;
Methoxy acrylic comprises: Azoxystrobin, ether bacterium amine, kresoxim-methyl, SSF 126 or ZEN 90160;
Evil (miaow) azole comprises: thiabendazole, efficiently press down mould azoles, press down mould azoles, prochloraz, cyanogen frost azoles, pefurazoate or dislike mould spirit;
Thiazoles comprises: Guardian;
The morpholine class comprises: dodemorph or tridemorph;
Pyridines comprises: fluazinam;
Quinoline comprises: hydroxyquinoline;
Pyroles comprises: the bacterium cyanogen of chuckleing of dressing seed
Amino formate comprises: mould prestige of second or Propamocarb;
Organic phosphates comprises: iprobenfos, edifenphos;
Antibiotics comprises: kasugamycin, polyoxin or jingganmycin;
Other sterilant comprises: metaxanin, derosal, thiophanate_methyl, triazolone, m-tetrachlorophthalodinitrile, isoprothiolane, thiram, zinc manganese ethylenebisdithiocarbamate, zinc 1,2-propylene bisdithiocarbamate, sulphur, Acibenzolar or white urea cyanogen.
Preparation with copper rosinate and above composite reagent among the present invention is microemulsion, aqueous emulsion, missible oil, suspension agent, wettable powder, suspension emulsion or dosage form of water dispersible granule.
In the application of copper rosinate of the present invention, the mass ratio range of copper rosinate and other many composite reagent is (1-25%): (1-40%).
Copper rosinate is applied among the present invention, and the compound preparation of copper rosinate and other many medicament is used to prevent and treat crop pest kind and the method for preventing and treating and is respectively:
Paddy rice: bacterial leaf-blight, banded sclerotial blight, rice blast or Gerlachia oryaae; Prevent and treat method: at the initial stage of a disease or young panicle formation stage to boot stage, 1000-1200 doubly sprays, boot stage and heading stage each the spray once;
Cotton soybean wheat tobacco: verticillium, root rot, black spot, brown spot, red-star like disease, stem wilt, mashed bell disease, rust, leaf blight or Powdery Mildew; Prevent and treat method: in seedling stage, early flowering season, 1200-1500 doubly sprays, and every spraying in 7-10 days once, sprays 3-4 time altogether;
Cucumber muskmelon watermelon hami melon summer squash balsam pear: bacterial angular leaf spot, spot disease, leaf blight, marginal leaf blight, yellowtop, oidium, macula disease; Prevent and treat method: begin medication at the initial stage of a disease, 1000-1200 doubly converts water spray, every spraying in 7-10 days once, uses 4-6 time continuously;
Chinese cabbage citrus grape: bacterial leaf spot, black spot, soft rot, Peptic Ulcers, anthrax, anthrachose of grape, Powdery Mildew, white eqpidemic disease, white rot; Prevent and treat method: begin medication at the initial stage of a disease, 1000-1200 doubly sprays, and every 10-15 days spray medicines once, sprays 5-8 time altogether;
Eggplant capsicum: bacterial black rot, bacterial wilt, cotton disease, yellows, gray mold, brown spot soft rot, streak virus, macula disease; Prevent and treat method: at the initial stage of a disease, 1000 times of spray medicines every 7-10 days spray medicines once, spray 2-3 time altogether;
Tomato: muscle is rotten sick, rascal is sick, bacterial wilt, macula disease; Prevent and treat method: at the initial stage of a disease, 1000-1200 doubly sprays medicine, every 7-10 days spray medicines once, sprays 2-3 time altogether;
Green onion garlic ginger potato taro: bacterial wilt of ginger, leaf spot, yellowtop, canker; Prevent and treat method: at the initial stage of a disease, 1000 times of spray medicines every 7-10 days spray medicines once, spray 2-3 time altogether;
Kidney bean sponge gourd fresh kidney beans reed wormwood artemisia: bacterial angular leaf spot, leaf spot, rust, black spot; Prevent and treat method: at the initial stage of a disease, 1000-1200 doubly sprays medicine, every 7-10 days spray medicines once, sprays 2-3 time altogether;
Strawberry celery radish asparagus: bacterial leaf spot, black spot, stem wilt, fruit rot; Prevent and treat method: at the initial stage of a disease, 1000 times of spray medicines every 7-10 days spray medicines once, spray 2-3 time altogether;
Longan: sour rot, damping-off, anthrax, leaf blight, mildew, leaf spot; Prevent and treat method: at the initial stage of a disease, 1200-1500 doubly sprays medicine, every 7-10 days spray medicines once, sprays 2-3 time altogether;
Lichee: anthrax, leaf spot, white eqpidemic disease, sour rot, root rot; Prevent and treat method: at the initial stage of a disease, 1000-1200 doubly sprays medicine, every 10-15 days spray medicines once, sprays 4-6 time altogether;
Loquat: eqpidemic disease, dirty leaf disease, grey brown spot, anthrax, sooty mold, bud blight; Prevent and treat method: at the initial stage of a disease, 1000 times of spray medicines every 7-10 days spray medicines once, spray 2-3 time altogether;
Banana: the rotten disease of sudden scab, black spot, any of several broadleaf plants, anthrax, yellow secret note leaf spot, the bacillary accent disease of withering; Prevent and treat method: at the initial stage of a disease, 1000-1200 doubly sprays medicine, every 7-10 days spray medicines once, sprays 2-3 time altogether;
Shaddock orange: yellow twig, shot hole, gummosis, Peptic Ulcers, penicilliosis; Prevent and treat method: at the initial stage of a disease, 1200-1500 doubly sprays medicine, every 10-15 days spray medicines once, sprays 4-5 time altogether;
Mango: peronospora tabacina, anthrax, witches' broom disease, felt disease; Prevent and treat method: at the initial stage of a disease, 1000-1200 doubly sprays medicine, every 7-10 days spray medicines once, sprays 2-3 time altogether.
The preparation method of copper rosinate of the present invention, copper rosinate is by rosin, mantoquita, alkali lye under the condition of solvent refluxing by the synthetic system of one kettle way, easy, the easy row of method, environmental protection.Cooperating of copper rosinate of the present invention with other medicament, can prevent and treat the multiple kinds of crops disease and pest, have wide range of applications.
Embodiment
With illustrated embodiments the present invention is done detailed explanation below.
Embodiment 1:
In the enamel reaction still of 4000L, add 620Kg rosin, 2200Kg toluene, stirring is dissolved rosin fully, and the unit for uniform suspension that will contain 125Kg cupric sulfate pentahydrate, 160Kg sodium hydroxide, 400Kg water again was added drop-wise in the rosin solution in 30 minutes, and it is green that the reaction solution color gradually becomes, dropwise, be warmed up to reflux temperature, dehydration reaction is after dehydration finishes, the cooling reaction solution, refilter out decon, obtain the toluene solution of copper rosinate, detection level is 38%.
Embodiment 2:
In the enamel reaction still of 2000L, add 300Kg rosin, the 1000Kg pimelinketone, stirring is dissolved rosin fully, and the unit for uniform suspension that will contain 60Kg cupric chloride, 168Kg potassium hydroxide, 200Kg water again was added drop-wise in the rosin solution in 30 minutes, and it is green that the reaction solution color gradually becomes, dropwise, be warmed up to reflux temperature, dehydration reaction is after dehydration finishes, the cooling reaction solution, refilter out decon, obtain the pimelinketone solution of copper rosinate, detection level is 33%.
Embodiment 3:
In the enamel reaction still of 1000L, add 160Kg rosin, the 480Kg propyl carbinol, stirring is dissolved rosin fully, and the unit for uniform suspension that will contain 40Kg Cuprocitrol, 25Kg ammoniacal liquor, 80Kg water again was added drop-wise in the rosin solution in 30 minutes, and it is green that the reaction solution color gradually becomes, dropwise, be warmed up to reflux temperature, dehydration reaction is after dehydration finishes, the cooling reaction solution, refilter out decon, obtain the butanol solution of copper rosinate, detection level is 45%.
Embodiment 4:
In the enamel reaction still of 5000L, add 750Kg rosin, the 2600Kg dimethyl formamide, stirring is dissolved rosin fully, and the unit for uniform suspension that will contain 200KgEDTA copper, 160Kg methylamine, 1200Kg water again was added drop-wise in the rosin solution in 50 minutes, and it is green that the reaction solution color gradually becomes, dropwise, be warmed up to reflux temperature, dehydration reaction is after dehydration finishes, the cooling reaction solution, refilter out decon, obtain the dimethyl formamide solution of copper rosinate, detection level is 40%.
Embodiment 5:
In the enamel reaction still of 6000L, add 900Kg rosin, the 3300Kg dimethyl formamide, stirring is dissolved rosin fully, and the unit for uniform suspension that will contain 273Kg neutralized verdigris, 600Kg triethylamine, 1200Kg water again was added drop-wise in the rosin solution in 60 minutes, and it is green that the reaction solution color gradually becomes, dropwise, be warmed up to reflux temperature, dehydration reaction is after dehydration finishes, the cooling reaction solution, refilter out decon, obtain the dimethyl formamide solution of copper rosinate, detection level is 28%.
Embodiment 6:
Copper rosinate can be prevented and treated rice seedling blight with the mould spirit of evil by 10%: 20%, was specially: copper rosinate 10%, dislike mould clever 20%, triphenyl phenol polyethenoxy ether 8%, calcium dodecylbenzene sulphonate 2%, the dimethylbenzene surplus is made missible oil, 1000-1200 doubly, convert water and be sprayed on seedbed or the raising box, and then sowing, spray again once with identical dose before transplanting, can prevent and treat rice seedling blight, prevention effect reaches more than 90%.
Embodiment 7:
Copper rosinate and Wocosin 50TK can be prevented and treated wheat powdery mildew, leaf rust by 15%: 10%; Uncinula necator, anthrax; Sigatoka etc.Be specially: copper rosinate 15%, Wocosin 50TK 10%, castor oil polyoxyethylene ether 2%, polyoxyethylene octylphenol ether sulfonate 4%, dimethylbenzene 15%, water surplus is made aqueous emulsion through shearing.Control wheat powdery mildew, leaf rust, their early stage again, medicament is converted water 1200-1500 and is doubly sprayed, and every 7-10 days spray medicines once, sprays 3-4 time altogether; Control uncinula necator, anthrax, if be used for the protectiveness control at the initial stage of a disease, 1500 times of sprayings, if fall ill mid-term, 1200 times of sprayings, spraying in 10-15 days is once sprayed 3-4 time altogether; Prevent and treat sigatoka, at the initial stage of a disease, medicament is converted water 1000-1200 and is doubly sprayed, and 10-15 days at interval, according to the development of the state of an illness, can consider to spray continuously for the second time.
Embodiment 8:
Copper rosinate and flumorph can be prevented and treated oidium such as cucumber, Chinese cabbage, grape by 10%: 15%, tomato, the late blight of potato etc.Be specially: copper rosinate 10%, flumorph 15%, phenyl Soxylat A 25-7 3%, polyoxyethylene octylphenol ether sulfonate 3%, calcium dodecylbenzene sulphonate 2%, dimethylbenzene 5%, water surplus is made suspension emulsion through shearing.Preventing and treating oidium, is to spray medicine at the initial stage of a disease, and medicament is converted water 1000-1200 and doubly sprayed, and sprays medicine once in 10-13 days at interval on the grape, and vegetables 7-10 such as cucumber, Chinese cabbage days once, 3-4 time altogether; Tomato, the late blight of potato all are to convert water 1000-1200 doubly to spray, and 7-10 sprays once, 3-4 time altogether; If fall ill mid-term, need 1000 times of sprayings.
Embodiment 9:
Copper rosinate and Azoxystrobin can be prevented and treated rice blast, downy mildew of garpe, fruit tree rust, black spot, vegetables Powdery Mildew etc. by 25%: 15%.Be specially: copper rosinate 15%, Azoxystrobin 10%, polyoxyethylene octylphenol ether sulfonate 3%, sodium lauryl sulphate 2%, ethylene glycol 3%, defoamer 0.5%, water surplus is made suspension agent through sand milling.Prevent and treat above disease, all dispensers at the initial stage of a disease, 1200-1500 doubly, fruit tree at interval 10-15 days once, other all be 7-10 days once, spray 3-4 time altogether, imitation all can reach more than 85%.
Embodiment 10:
Copper rosinate and m-tetrachlorophthalodinitrile can be prevented and treated diseases such as grey mould fruit rot of strawberry, leaf blight, bitter rot or anthracnose of grape, Powdery Mildew, celery leaf spot, Kidney bean rust, black spot of cabbage by 5%: 40%.Be specially copper rosinate 5%, m-tetrachlorophthalodinitrile 40%, methyl naphthalene sulfonic acid salt 3%, sodium lauryl sulphate 2%, the kaolin surplus is made wettable powder through comminution by gas stream.Prevent and treat above disease, all dispensers at the initial stage of a disease, 1000-1200 doubly, fruit tree at interval 10-15 days once, other all be 7-10 days once, spray 3-4 time altogether, imitation all can reach more than 85%.