CN102405933B - Herbicide complex - Google Patents
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- CN102405933B CN102405933B CN201110373896.4A CN201110373896A CN102405933B CN 102405933 B CN102405933 B CN 102405933B CN 201110373896 A CN201110373896 A CN 201110373896A CN 102405933 B CN102405933 B CN 102405933B
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Abstract
The invention provides a herbicide complex, which is an aqueous solution compounded by using ammonium humate and organic phosphine herbicide, wherein the ammonium humate is prepared by the following processes of: mixing weathered coal and ammonium hydrogen carbonate in a weight ratio of (2-4): 1, performing ammoniation reaction with stirring and rolling at a temperature of between 16 and 35 DEG C, and thus obtaining the ammonium humate, wherein the stirring rate is 30 to 40r/min, the stirring time is 1 to 2 hours, the rolling pressure is 1.6 to 2kg/cm<2>, and the humic acid content of the weathered coal is 30 to 70 percent. The ammonium humate in the herbicide complex provided by the invention has the solubility of over 90 percent and multiple active ingredients, and can promote the exertion of the pesticide effect of the herbicide in the herbicide complex, so that the herbicide complex has good weeding effect.
Description
The application is that the application number of submitting for 21st for 09 month for 2010 is 201010297999.2, the divisional application that denomination of invention is a kind of ammonium humate and its preparation method and application.
Technical field
The present invention relates to a kind of herbicide complex, relate in particular to a kind of solvability that contains and exceed 90% and there is the herbicide complex of the ammonium humate of various active component.
Background technology
Humic acid is the macromolecular organic compound that occurring in nature extensively exists, and has fertilizer synergistic, improves soil, stimulates plant growth, improves the functions such as agricultural product quality.But, the humic acid of occurring in nature is to combine and be the state of mineralizing and exist with calcium, magnesium etc., the humic acid of state of mineralizing can not be absorbed and used by plants, and only has and makes it to become soluble-salt with sodium salt, sylvite and ammonium salt, could be used as the source of manure.The sodium salt of humic acid and sylvite have very strong spread effect to crops root system, need to be controlled concentration, thereby have certain limitation in agricultural application when application.Therefore humic acid ammonium salt is comparison recommendation.
Both at home and abroad researcher has carried out some for humic acid and slaine thereof with mixture of herbicides synergy aspect and has studied, and can prove: humic acid can promote the leaching transfer ability of Herbicide Ethametsulfuron-methyl; Sodium humate mixes with sulfonylurea herbicide to use can obtain fine herbicidal effect; Potassium humate mixes use synergy with weed killer herbicide aryloxy carboxylic acid obvious.Research aspect compound synergic finds, 1, the solvability of humate has remarkable impact; 2, select suitable weed killer herbicide kind to carry out composite, have remarkable impact for herbicidal effect and plant growth.Sodium humate and humic acid potassium illustrate before the impact of crops, although the ammonium salt of humic acid is more conducive to use, but the ammonium humate generally being used is at present to grind the methods such as ammonium and make ammonium humate and make according to traditional mixed-stacking ammonium, Raymond mill, final ammonium humate product solubility is generally on the low side, uses herbicidal effect not good with mixture of herbicides.
How to improve the preparation technology of ammonium humate, prepare a kind of ammonium humate of highly dissoluble, make to obtain a kind of new herbicides complex with good herbicidal effect with mixture of herbicides, become and have problem to be solved.
Summary of the invention
The invention provides a kind of ammonium humate and preparation method thereof, by improvement of production process, make the solvability of ammonium humate exceed 90%, and contain various active component, be beneficial to the composite synergistic to weed killer herbicide.
The present invention also provide above-mentioned ammonium humate with mixture of herbicides synergy aspect application, and described ammonium humate and herbicide complex, the synergy of ammonium humate and weed killer herbicide more promotes the performance of effect of herbicides.
The preparation method of a kind of ammonium humate provided by the invention, is made up of following steps:
By weathered coal with carbonic hydroammonium with 2～4: 1 weight ratio is mixed, under 16 ℃ of-35 ℃ of conditions, maintain stir and roll extrusion carry out ammonium reaction, make ammonium humate,
Wherein, mixing speed is 30～40r/min, and mixing time is 1～2hr; Rolling pressure is 1.6～2kg/cm
2, and the content of described Humic Acid from Weathered Coal is 30～70%.
In one embodiment of the present of invention, the preparation method of described ammonium humate, described weathered coal is preferably 50-65% containing humic acid ratio, water content is 15～30% weathered coal, same as the prior art, the present invention's weathered coal used can be leonardite, weathering ub-bituminous coal, weathered bituminite conventionally.
The product of preparation according to the method described above, the present invention is called ammonium humate or rotten ammonium, by the control to ammonium reaction condition and parameter, the ammonium humate product obtaining contains various active composition, and solvability exceedes 90%, and approaching 93～95%, these are, and existing ammonium humate product is difficult to compare.
So the present invention provides the ammonium humate product for preparing according to the method described above and the application of described ammonium humate and mixture of herbicides synergy aspect simultaneously.
The ammonium humate of preparing based on said method, the present invention also provides a kind of herbicide complex, add water formulated by described ammonium humate and organic phosphine class weed killer herbicide,, herbicide complex provided by the invention is the aqueous solution obtaining after a kind of above-mentioned ammonium humate and organic phosphine class mixture of herbicides, can be directly used in the weeding operation in farmland, due to the synergy of ammonium humate, effect of weed killer herbicide is significantly improved.
In above-mentioned herbicide complex, described organic phosphine class weed killer herbicide is preferably glyphosate or two propylamine phosphine.
A kind of herbicide complex is provided in one embodiment of the present of invention, described herbicide complex adds water formulated by described ammonium humate and glyphosate or two propylamine phosphine, in this herbicide complex, the content of described ammonium humate is 0.8～1.5g/L, and the content of described glyphosate or two propylamine phosphines is 6～7g/L.
Based on the synergistic effect of above-mentioned ammonium humate, the present invention also provides another kind of herbicide complex, is the aqueous solution after above-mentioned ammonium humate and sulfonylurea herbicide and phenoxy acetic acid class mixture of herbicides; Due to the highly dissoluble of ammonium humate, described herbicide complex is also a kind of aqueous solution reagent that can directly use.Preferably, described sulfonylurea herbicide can be nicosulfuron, sulfometuronmethyl, Sulfometuron Methyl, ethametsulfuron, bensulfuron-methyl or wherein two kinds of above combinations; Described phenoxy acetic acid class weed killer herbicide can be 2.4-D butyl ester, 2.4D chloro butyl ester, 2.4D fluoro butyl ester or wherein two kinds of above combinations.
Concrete, another kind of herbicide complex provided by the invention can be described ammonium humate, nicosulfuron and the 2.4-D butyl ester aqueous solution after composite, in this herbicide complex, the volume ratio of described nicosulfuron and water is 6～7: 1, the volume ratio of described 2.4D butyl ester and water is 0.5～0.7: 1, and the content of described ammonium humate is 6～7g/L.
The preparation method of ammonium humate of the present invention, specific process conditions are adopted, control the shorter ammonium time, make the ammonium humate that is prepared into not only solvability exceed 90%, and contain terpene gibberellin, IA, the 6-BA basic element of cell division, vitamin PP degradation product, and polyamines, plant hormone (anthocyanidin), the various active components such as fulvic acid, because said components contains phenolic hydroxyl group, hydroxyl, alcoholic extract hydroxyl group, hydroxyquinone, enol base, amino, quinonyl, quinone hydrogen base, the multiple functional group such as methoxyl group, than the ammonium humate of traditional sense, there is stronger cation exchange capacity (CEC), buffer capacity, adsorption capacity and catalytic capability, , show higher physiologically active, thereby while using with mixture of herbicides, be beneficial to the performance that promotes the effect of herbicides in herbicide complex.
Accompanying drawing explanation
Fig. 1 is characteristic group's absworption peak figure of infrared spectroscopic determination ammonium humate of the present invention;
Fig. 2 is the characteristic component absworption peak figure of infrared spectroscopic determination ammonium humate of the present invention;
Fig. 3 is the LC-MS LC-MS analysis figure of ammonium humate of the present invention.Wherein a is liquid-phase chromatographic analysis figure, and b, c are mass spectral analysis figure.
Embodiment
For making object of the present invention, technical scheme and technique effect clearer; below in conjunction with the specific embodiment of the invention and respective drawings; technical scheme in the embodiment of the present invention is clearly and completely described; but following examples can not be interpreted as restriction that can practical range of the present invention; based on the embodiment in the present invention; all other embodiment that those of ordinary skills obtain under the prerequisite of not making creative work, belong to the scope of protection of the invention.
In following examples, adopt the leonardite in Shanxi, purchased from Xiangning County of Shanxi Province, Linfen, from the coal mining Co., Ltd in the counties such as stone, Jincheng, Xinzhou; Nicosulfuron is purchased from Dezhou biochemical Co., Ltd of auspicious dragon, and wherein nicosulfuron has another name called beautiful rule, active ingredient 40 grams per liters; 2.4-D butyl ester is purchased from Shandong Qiaochang Chemical Co., Ltd, and 2.4-D butyl ester active ingredient is 57%.
IR spectrometer model: Nicolet 6700, is determined at Institute of Analysis of East China University of Science and completes; HPLC (high performance liquid chromatography) chromatograph model: Agilent 1100, LC-MS liquid chromatography-mass spectrography model: Agilent11100-Finnigan LCQ Deca XP, is determined at biotechnology key lab of country of East China University of Science and completes.
Embodiment mono-
Illustrate ammonium humate provided by the invention and preparation method thereof by the present embodiment.The preparation method of ammonium humate of the present invention comprises:
Leonardite is processed into powder, measures wherein water content and be approximately 20wt%, in this leonardite powder, the content of humic acid is approximately 55.21%;
Above-mentioned leonardite powder is mixed with the ratio of 70: 30 with carbonic hydroammonium in the reactor with stirring and rolling device, under 15～20KW motor driven, utilize interval to be welded on agitating plate and the milling roller on the turning cylinder circumference in reactor, keep the temperature of weathered coal powder and bicarbonate mixture at 16-35 ℃, speed with 30r/min stirs, roll extrusion 1hr obtains ammonium humate of the present invention, wherein, milling roller is the milling roller that can apply 1.6～2kg rolling pressure in unit are, above-mentioned spaced agitating plate and milling roller can make leonardite powder and the bicarbonate mixture in reactor alternately be stirred within 1hr, roll extrusion.
The solubility that the ammonium humate of being made up of said method is tested in water tumbler reaches 95%.Concrete method of testing is as follows:
Claim 100g above-mentioned ammonium humate, the weight of putting into after the extremely basic constant weight of drying machine drying is 80g, can think that the water content of above-mentioned ammonium humate is 20%.Dried above-mentioned ammonium humate is put into 2000ml distilled water water, fully stir 10min, make large portion humic acid soluble in water, then precipitate 30min, make insoluble matter precipitation bottom, remove most of aqueous solution with siphonage.In remaining sediment, then add 2000ml distilled water, fully stir 10min, precipitation half an hour, remove the large portion aqueous solution with siphonage.By remaining insoluble matter, with putting into drying machine drying after Filter paper filtering, then to weigh heavy remaining insoluble matter weight in the balance be 4g.So, with calculating solubility index, its account form is as follows:
Solubility=95%
The ammonium humate that said method is prepared into adopts its characteristic group of infrared spectroscopic determination and characteristic component; As shown in Figure 1, the characteristic group of ammonium humate has measurement result: carboxyl (1510cm
-1), hydroxyl (3300-3340cm
-1), amide groups (1620-1650cm
-1), in alicyclic ring-flexible (1100-1030cm of C-O
-1), n methine (725cm
-1) etc.; Fig. 2 is the characteristic component peak of absorption intensity above-mentioned ammonium humate while being 50%, and as can be seen from the figure the characteristic component in above-mentioned ammonium humate has cellulose polysaccharide, inorganic ash content, humic acid degradation product, C
21h
47n
3o
10, ammonium polyphosphate etc.
On the basis of HPLC efficient liquid phase chromatographic analysis, the ammonium humate that said method is prepared into has carried out LC-MS LC-MS analysis, result shows to contain the terpene gibberellin that the more molecular weight of relative amount is 317.02 by the ammonium humate of the present embodiment, and (existing known gibberellin has 125 kinds, typical gibberellin molecular weight is 343), molecular weight is 222.31 the 6-BA basic element of cell division (the 6-BA basic element of cell division, formal name used at school: 6-benzyl aminopurine, typical 6-BA basic element of cell division molecular weight 225.3), molecular weight is 102.24 vitamin PP degradation product (standard vitamin PP molecular weight 122.13), the polyamines of molecular weight between 401-752, plant hormone (steroid class, anthocyanidin), fulvic acid.The LC-MS liquid chromatography-mass spectrography figure of ammonium humate prepared by the present embodiment method is shown in Fig. 3.
Embodiment bis-
Illustrate another kind of ammonium humate provided by the invention and preparation method thereof by the present embodiment.The preparation method of the ammonium humate of the present embodiment comprises:
Leonardite is processed into powder, measures wherein water content and be approximately 20wt%, in this leonardite powder, the content of humic acid is approximately 55.21%;
After above-mentioned leonardite powder is mixed with the ratio of 75: 25 with carbonic hydroammonium, under 15～20KW motor driven, utilize interval to be welded on agitating plate and the milling roller on turning cylinder circumference, keep the temperature of weathered coal powder and bicarbonate mixture at 16-35 ℃, speed with 30r/min stirs, roll extrusion 1.5hr obtains ammonium humate of the present invention, wherein, milling roller is the milling roller that can apply 1.6～2kg rolling pressure in unit are, above-mentioned spaced agitating plate and milling roller can make the leonardite powder of each point and bicarbonate mixture alternately be stirred within 1.5hr, roll extrusion.
The solubility that the ammonium humate of being made up of said method is tested in water tumbler reaches 94%.Concrete method of testing is with embodiment mono-.Ammonium humate employing its characteristic group of infrared spectroscopic determination that the present embodiment method is prepared into and characteristic component and LC-MS liquid chromatography-mass spectrography figure result and embodiment mono-are basic identical, do not repeat them here.
Embodiment tri-
Illustrate herbicide complex provided by the present invention and herbicidal methods thereof by the present embodiment.
A kind of herbicide complex, the ammonium humate being obtained by embodiment mono-method and glyphosate add water formulated, and the content of described ammonium humate is 1g/L, and the content of described glyphosate is 5.5g/L.
Use sprayer to spray weeding described herbicide complex solution.Use respectively the glyphosate aqueous solution 1 (content of glyphosate is 5.5g/L) in contrast 1 that does not add ammonium humate, and the glyphosate aqueous solution 2 (content of glyphosate is 20g/L) that does not add ammonium humate in contrast 2, promote weed killer herbicide herbicidal effect to verify to ammonium humate of the present invention.
Test site: Dalate Banner, the Inner Mongol, the woods are called Wu Gudi village, town together.
Experimental field situation: be located at farmland motor-pumped well limit uncultivated area, main weeds kind has: lamb's-quarters (Chenopodium album L.), puncture vine (Tribulus terrestris L.), Amaranthus retroflexus (Amaranthus retroflexus.L), chickweed (Stellaria media (L.) cyr), pivot holds (Polygonum aviculare L.), Siberian cocklebur (Xanthium sibiricum patriun), black nightshade (Solanum nigrum L.), before car (Plantago asiatica L.), smelly wormwood artemisia (Artemisia hedinii ostenf) etc.Weeds are banded or bunch shape distributes, and cover ratio is 50% left and right, 200-500 gram/m of weeds fresh weight
2, most of weeds are in growth animated period, as larger in lamb's-quarters up to 30cm, have multiple branches, and Amaranthus retroflexus, wormwood artemisia are also more than 25cm, and the puncture vine growth of crawling, has opened chrysanthemum, and tall and big in 5cm, little careless ratio is few, has no narrow leaf grass.
Sprayer: 3WBS-16A knapsack sprayer.
Administration time and application method: fine day, spray when 6-7 afternoon, spray area 220m
2, wherein, the herbicide complex solution of the present embodiment and contrast 1,2 solution spray respectively wherein 1/3 area, and the herbicide complex solution of controlling unit are sprinkling is identical with the amount of contrast 1, contrast 2 solution, is about 45～50ml/m
2.
Spraying in after 2 solution 16 days of above-mentioned herbicide complex solution, contrast 1, contrast, medication effect is added up, wherein, after medication, the poisoning intensity grade of main weeds is :-there is no a poisoning; + slight poisoning; ++ medium poisoning; +++ serious poisoning; The serious poisoning of ++++very; D death; Result is as shown in table 1:
As can be seen from the above table, after medication, main weeds poisoning intensity grade is with the variation of number of days, and herbicide complex is approximately to rise one-level or half grade average every day; Contrast 1 is approximately on average within every two days, to rise one-level or half grade; Contrast and rise one-level 2 average every days.The glyphosate of same dosage, the drug effect reaction of the herbicide complex that contains ammonium humate does not add the contrast 1 fast 2-5 days (various weeds differ) of ammonium humate, approach with the herbicidal effect that contrasts 2 high dose glyphosates, and the dosage of contrast 2 glyphosates far exceedes the dosage range of the glyphosate that this area normally applies, further can illustrate that herbicide complex weeding drug effect of the present invention improves significantly.In addition, weed killer herbicide spray rear various weeds to compound of weed killer reactions vary, in various weeds, lamb's-quarters is more responsive, smelly wormwood artemisia relatively has resistance, puncture vine resistance maximum is reacted the slowest.
Therefore, ammonium humate prepared by the inventive method can promote the performance of the drug effect of glyphosate, shortens weeds reaction time 2-5 days, can be used to reduce glyphosate consumption, reduces the pollution to environment.
Embodiment tetra-
Illustrate another kind of herbicide complex provided by the present invention and herbicidal methods thereof by the present embodiment.
A kind of herbicide complex, the ammonium humate being obtained by embodiment mono-method and nicosulfuron and 2.4-D butyl ester add water to configure and form, the volume ratio of described nicosulfuron and water is 6.7: 1, the volume ratio of described 2.4-D butyl ester and water is 0.67: 1, and the content of described ammonium humate is 0.67 grams per liter water.
In contrast, use and do not add the nicosulfuron of ammonium humate and the 2.4-D butyl ester solution that configuration forms that adds water, the volume ratio of wherein said nicosulfuron and water is 6.7: 1, the volume ratio of described 2.4-D butyl ester and water is 0.67: 1, and the herbicidal effect of the herbicide complex to the present embodiment is verified.
Experiment place: corn field.
Sample plot situation: native boundary is husky boundary soil, and base fertilizer is sheep excrement, has crop corn in ground when medication, the high 18-22cm of corn, kind: directly restrain No. 7.In ground, main weeds has: lamb's-quarters (Chenopodium album L.), puncture vine (Tribulus terrestris L.), Siberian cocklebur (Xanthium sibiricum patrin), Amaranthus retroflexus (Amaranthus retroflexus.L), lady's-grass (Digitaria sanguinalis (L.) scop), green foxtail (Setaria viridis (L.) Beauv), wild oat (Avena fatua L.), wild broomcorn millet (Eriochola villosa (Thunb) Kunth), smelly wormwood artemisia (Artemisia hedinii ostenf), pivot holds (Polygonum aviculare L.), drought barnyard grass (Echinochloa crusgall:(L.) Beauv.var.hispidula (Retz) Hack etc., 100-300 gram/m of weeds fresh weight
2, weeds mean height 5-10cm, weeds are in the same size, only have ridge, limit weeds slightly large.
Sprayer: 3WBS-16A knapsack sprayer.
Administration time and application method: fine day, 9 o'clock-10 o'clock morning.Spray area 667m
2, wherein the wherein area of half is sprayed respectively in herbicide complex and contrast, and the amount of controlling the herbicide complex solution of unit are sprinkling and the solution of contrast is identical, is about 20～25ml/m
2.
In 16 days that spray above-mentioned herbicide complex solution, contrast solution, medication effect is added up, wherein, after medication, the poisoning intensity grade of main weeds is :-there is no a poisoning; + slight poisoning; ++ medium poisoning; +++ serious poisoning; The serious poisoning of ++++very; D death; Result is as shown in table 2.
As can be seen from Table 2, after medication, main weeds poisoning intensity grade is with the variation of number of days, and herbicide complex is approximately to rise one-level or half grade average every day; Contrast is approximately on average within every two days, to rise one-level or half grade; Nicosulfuron and the 2.4-D butyl ester of same dosage, add ammonium humate (herbicide complex) than the fast 3-5 days of herbicidal effect that does not add ammonium humate (contrast), the herbicidal effect that the herbicide complex of interpolation ammonium humate is improved, add ammonium humate can reduce nicosulfuron and 2.4-D butyl ester usage amount, thereby reduce the pollution to environment to weed killer herbicide.And various weeds are had various reactions to compound of weed killer, and in various weeds, lamb's-quarters is more responsive, and Amaranthus retroflexus relatively has resistance, and the resistance maximum of wild broomcorn millet is reacted the slowest.
In addition, the advantage that adds the herbicide complex of ammonium humate is also embodied in that to spray droplet moisture capacity strong, loss, volatile ratio contrast will be lacked, especially can find out that at fine day the herbicide complex liquid of sprinkling is slightly long in blade face retention time, can reduce like this weed killer herbicide because of drift or volatilize the other weed killer herbicide of the impact of environment is combined with humic acid and can be retrained weed killer herbicide moving freely in native boundary, thereby reduce intrusion and the injury of weed killer herbicide to non-object, further promote the performance of effect of herbicides, and reduce to greatest extent to the greatest extent the pollution to environment.Observe the reaction of various weeds to herbicide complex, little careless strong reaction, just bowed, turnup some same day; After large careless 2-3 days, also reaction is accelerated, and dehydration is withered fast; After the medication of narrow leaf grass, stop growing, dehydration drying shrinkage is accelerated.This feature, can reduce weeds rehabilitation, bounce-back, and reduces the procreation of long disease bacterium of causing of rotten time of weeds, fully demonstrates the close combination of chemical weed control and the ecological agriculture.
In addition, because nicosulfuron and 2.4-D butyl ester are selective herbicides, crop is safe from harm, therefore, in the time of humic acid amine of the present invention use composite with it, in improving weed killer herbicide herbicidal effect, also there is the effect that promotes plant growth.In the time spraying the herbicide complex of the present embodiment, corn crop is sprayed simultaneously, observed result: after spraying herbicide complex the 3rd day, can obviously find out corn than bud green before spraying, strong drought resistance, there is no obvious wilting phenomenon, and corn after control treatment occurs that wilting phenomenon, leaf roll, look grayish green, waters and just recover after 7 days; Simultaneously herbicide complex corn after treatment than with control treatment after corn growth fast, the two is more than height difference 3cm, growth differences is fairly obvious.In herbicide complex corn growth state after treatment, drought resistance, be obviously better than the corn of control treatment, illustrate that ammonium humate and nicosulfuron and the composite use of 2.4-D butyl ester given full play to again growth potential and the drought resisting function of corn in improving weed killer herbicide performance drug effect.
Claims (3)
1. a herbicide complex, is characterized in that, this herbicide complex is the aqueous solution being exceeded after 90% ammonium humate and organic phosphine class mixture of herbicides by water-soluble, and described ammonium humate is made up of following methods:
Weathered coal is mixed with the weight ratio of 2～4:1 with carbonic hydroammonium, under 16 ℃ of-35 ℃ of conditions, maintains stirring and roll extrusion and carry out ammonium reaction, make ammonium humate,
Wherein mixing speed is 30～40r/min, and mixing time is 1～2hr, and rolling pressure is 1.6～2kg/cm
2, the content of described Humic Acid from Weathered Coal is 30～70%.
2. herbicide complex according to claim 1, is characterized in that, described organic phosphine class weed killer herbicide is glyphosate or two propylamine phosphine.
3. herbicide complex according to claim 1 and 2, it is characterized in that, described herbicide complex adds water formulated by described ammonium humate and glyphosate or two propylamine phosphine, in this herbicide complex, the content of described ammonium humate is 0.8～1.5g/L, and the content of described glyphosate or two propylamine phosphines is 6～7g/L.
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