CN109400347A - It is a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic support preparation method of spring maize base manure - Google Patents
It is a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic support preparation method of spring maize base manure Download PDFInfo
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- CN109400347A CN109400347A CN201811328806.8A CN201811328806A CN109400347A CN 109400347 A CN109400347 A CN 109400347A CN 201811328806 A CN201811328806 A CN 201811328806A CN 109400347 A CN109400347 A CN 109400347A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
- C05D9/02—Other inorganic fertilisers containing trace elements
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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Abstract
The present invention relates to a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic support preparation method of spring maize base manure, the preparation method include the preparation of humic acid extractant, the preparation of humic acid extracting solution, the preparation of chelated zinc liquid and the preparation of Humic acid synergistic carrier.After Humic acid synergistic carrier of the present invention is in conjunction with phosphorus ammonium, the more commercially available phosphorus ammonium of soil pH in fertile border 1cm reduces by 0.3~1.4 unit, soil Ca2- P and Ca8Average more commercially available phosphorus ammonium improves 22% and 16% to-P respectively.Wheat root weight and vigor improve 35% or more, and relatively control averagely improves 45.7% and 26.2% respectively for maize root system fresh weight and vigor.Compared with commercially available phosphorus ammonium, the wheat yield of humic acid-ammonium phosphate A, B, C of the present invention averagely improve 12.6%, and phosphate fertilizer utilization efficiency improves 9.34 percentage points；Corn yield averagely improves 16.1%, and phosphate fertilizer utilization efficiency improves 10.7 percentage points.
Description
[technical field]
The present invention relates to technical field of fertilizer production.More particularly it relates to which a kind of be suitable for winter wheat or spring maize
The phosphorus ammonium Humic acid synergistic support preparation method of base manure.
[background technique]
The 5.5% of the world phosphor resource reserves Jin Zhan, China gross reserves, the per-capita quantity of the resources is only the 39% of world average level.
Phosphorus ammonium is the most important phosphate fertilizer variety in China, but because its enter soil after easily fixed by metal ions such as calcium, magnesium, iron, aluminium, this season
Utilization rate only 20% or so, causes huge economic loss and the wasting of resources.Soil is only in the case where 6~7 pH, effectively
Phosphorus concentration highest.The calcium and magnesium ion content of basic soil is high, after phosphorus enters soil, 80% or more is fixed in 3 days, cannot
It is absorbed by crops utilization.By greatly improving phosphate fertilizer utilization efficiency, Phosphorus Fertilizer Rates are reduced, are to promote the sustainable benefit of China's phosphate fertilizer resource
With important technology approach.
Wheat In North China and northeast spring maize phosphorus ammonium make base manure application season temperature it is low, phosphorus in the soil activity it is low,
The absorbability of crop root is poor, therefore peasant household guarantees enough supplies of phosphorus nourishing, also result in by increasing phosphorus ammonium dosage
A large amount of phosphorus be fixed to invalid phosphorus in the soil.
Reducing the approach that phosphate fertilizer utilization efficiency was fixed, improved to phosphorus mainly has the metal adjusted in soil pH, reduction phosphorus and soil
Ions binding quantity promotes crop to absorb.The acidic functionalities such as carboxyl rich in, phenolic hydroxyl group in humic acid, can be certain
Phosphorus is reduced in degree to fix, and improves phosphorus amount.1 03274798A of CN discloses a kind of Humic acid synergistic ammonium phosphate and its system
Preparation Method extracts weathered coal/lignite humic acid with sig water, prepares Humic acid synergistic liquid, by it in conjunction with ammonium phosphate production process,
Humic acid synergistic ammonium phosphate is produced, has the function of that inhibiting to reduce phosphorus fixes.But it yet there are no related suitable for winter wheat or spring
Phosphorus the ammonium patent application of Humic acid synergistic carrier and its related data of corn base manure.
Therefore, the present inventor, for technical problem of the existing technology, passes through on the basis for summarizing the prior art
Lot of experiments and analysis work, complete the present invention finally.
[summary of the invention]
[technical problems to be solved]
The object of the present invention is to provide a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic carrier system of spring maize base manure
Preparation Method.
[technical solution]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic support preparation method of spring maize base manure.
The step of preparation method, is as follows:
A, prepared by humic acid extractant
20~50 parts by weight hydramine, 5~10 parts by weight dimethylformamides and 5~10 parts by weight ethylene glycol are added to 1000
In the water that~2000 parts by weight temperature are 60~70 DEG C, stirring and dissolving is cooling, obtains the humic acid extractant；
B, prepared by humic acid extracting solution
100 parts by weight humic acid minerals raw materials are added to 800~1500 parts by weight to extract in the humic acid that step A is obtained
In agent, its temperature is then gradually increased to 90 DEG C under stiring, and keeps 40~60min at this temperature, is then cooled to
Room temperature, centrifuge separation, sediment discard, and obtain the humic acid extracting solution；
C, prepared by chelated zinc liquid
By 100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine and 30 parts by weight of glycerin
It is added in the water that 1000 parts by weight temperature are 50 DEG C, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature
80 DEG C of degree, stirring and dissolving obtain the chelated zinc liquid；
D, prepared by Humic acid synergistic carrier
10~20 parts by weight benzene carboxylic acids and 0.02~0.10 parts by weight polyethylene glycol are added to 100 parts by weight in step B
In obtained humic acid extracting solution, it is heated to temperature 50 C, 2~3 parts by weight cumyl peroxides is added, is then heated to
100 DEG C of temperature, 60~120min is reacted at this temperature, adds 3~8 parts by weight of polyoxyethylene ethers and 0.5~2.0 weight
Part O-phthalic alkanol amides, cooling, its pH value is adjusted to 4.5~5.5 by used phosphate aqueous solution, is obtained a kind of suitable for the winter
The phosphorus ammonium Humic acid synergistic carrier of wheat or summer corn base manure.
A preferred embodiment of the invention, in step, the hydramine are one or more to be selected from a second
Hydramine, diethanol amine, triethanolamine or N methyldiethanol amine hydramine.
It according to another preferred method of implementation of the present invention, in step, will be under conditions of 60~240rpm of revolving speed
The solution that stirring and dissolving obtains is cooled to 40 DEG C of temperature or less.
According to another preferred method of implementation of the present invention, in step, hydramine, dimethylformamide, ethylene glycol and water
Weight ratio be 28~42:6~9:6~9:1200~1800.
According to another preferred method of implementation of the present invention, in stepb, the humic acid minerals raw material is weathered coal
Or lignite,
According to another preferred method of implementation of the present invention, in stepb, the granularity of the humic acid minerals raw material is
150~300 mesh.
According to another preferred method of implementation of the present invention, in stepb, under the conditions of 1000~5000rpm of revolving speed from
The heart separates 5~30min.
According to another preferred method of implementation of the present invention, in step D, the benzene carboxylic acid be benzoic acid, phenylacetic acid,
Salicylic acid or acetylsalicylic acid.
According to another preferred method of implementation of the present invention, in step D, the concentration of the peroxophosphoric acid aqueous solution be 1~
5mol/L。
According to another preferred method of implementation of the present invention, in step D, polyoxyethylene ether and phthalic acid alkane is added
Its solution is cooled to 10~40 DEG C of temperature after base amide.
The present invention is described in more detail below.
The present invention relates to a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic support preparation method of spring maize base manure.
The step of preparation method, is as follows:
A, the preparation of humic acid extractant
20~50 parts by weight hydramine, 5~10 parts by weight dimethylformamides and 5~10 parts by weight ethylene glycol are added to 1000
In the water that~2000 parts by weight temperature are 60~70 DEG C, stirring and dissolving is cooling, obtains the humic acid extractant.
The hydramine that the present invention uses is a kind of using the nitrogen-atoms of ammonia as core, and the chemical combination that the hydrogen atom of ammonia is replaced by alcohol
Object, it can be chelated with calcium, magnesium, the iron plasma in humic acid minerals raw material, the water solubility of this raw material be improved, to facilitate
Improve the recovery rate that humic acid is extracted from humic acid minerals raw material.
The hydramine that the present invention uses is one or more selected from monoethanolamine, diethanol amine, triethanolamine or N- methyl two
The hydramine of ethanol amine.The hydramine is all current market sales of product, for example, by Shanghai Min Chen Chemical Co., Ltd. with
Trade name monoethanolamine (MEA) sale product, by Chemical Co., Ltd., Guoan, Zouping County with trade name N methyldiethanol amine
(MDEA) product sold.
In the present invention, when other raw material dosages are in the range, if the dosage of hydramine is lower than 20 parts by weight
When, then it can reduce humic acid recovery rate；If the dosage of hydramine is higher than 50 parts by weight, humic acid extractant liquid gas will lead to
Bubble is excessive, and tiny impurity is mixed in humic acid liquid, the humic acid liquid purity decline of extraction；Therefore, the dosage of hydramine is
20~50 parts by weight are suitable, preferably 28~42 parts by weight, more preferably 30~36 parts by weight.
Dimethylformamide is a kind of organic base, it is reacted with acidic-groups such as carboxyl, phenolic hydroxyl groups in humic acid,
Humic acid is set to become a kind of water-soluble humic acid, so as to from containing extracting humic acid in humic acid material, and it is also
It can increase methyl, methoxy functional mass contg in humic acid.The dimethylformamide that the present invention uses is currently on the market
The product of sale, such as the product sold by Nanjing Ke Zheng Chemical Co., Ltd. with trade name n,N-Dimethylformamide (DMF).
In the present invention, when other raw material dosages are in the range, if the dosage of dimethylformamide is lower than 5 weights
When measuring part, then humic acid recovery rate can be reduced；If the dosage of dimethylformamide is higher than 10 parts by weight, rotten plant will lead to
Liquid bubble is excessive in sour extraction process, and tiny impurity is mixed in humic acid liquid, the humic acid purity decline of extraction；Cause
This, the dosage of dimethylformamide is that 5~10 parts by weight are suitable, preferably 6~8 parts by weight.
Ethylene glycol can enhance due to the good intersolubility of water and low temperature resistance humic acid extractant liquid stability and
Mobility.The ethylene glycol that the present invention uses is current market sales of product, such as the limited public affairs of chemical products are just being risen by Zhengzhou
Take charge of the product sold with trade name anti-icing fluid spent glycol.
In the present invention, when other raw material dosages are in the range, if the dosage of ethylene glycol is lower than 5 parts by weight
When, then it is unobvious that humic acid liquid stabilizing effect is improved when can be to low temperature；If the dosage of ethylene glycol is higher than 10 parts by weight,
Then can be higher because of hydroxyl, it may cause part humic acid precipitating with storage time extension, therefore, the dosage of ethylene glycol is 5~10
Parts by weight are suitable, preferably 6~9 parts by weight.
When other raw material dosages are in the range, if the dosage of water is lower than 1000 parts by weight, it can be planted because of corruption
Acid extractant excessive concentration, water content is low, and solubility is limited, then extracts the decline of humic acid efficiency；If the dosage of water is higher than
, then can be too low because of humic acid Extractant concentration when 2000 parts by weight, also result in the decline of humic acid recovery rate；Therefore, the use of water
Amount is that 1000~2000 parts by weight are suitable, preferably 1200~1800 parts by weight, more preferably 1400~1600 weight
Measure part.
Preferably, the weight ratio of hydramine, dimethylformamide, ethylene glycol and water be 28~42:6~9:6~9:1200~
1800。
In this step, the solution that stirring and dissolving obtains under conditions of 60~240rpm of revolving speed is cooled to temperature 40
DEG C hereinafter, main purpose be guarantee humic acid extractant stability and quantifying it is standby.
B, the extraction of humic acid
100 parts by weight humic acid minerals raw materials are added to 800~1500 parts by weight to extract in the humic acid that step A is obtained
In agent, its temperature is then gradually increased to 90 DEG C under stiring, and keeps 40~60min at this temperature, is then cooled to
Room temperature, centrifuge separation, sediment discard, and obtain the humic acid extracting solution.
According to the present invention, the humic acid minerals raw material is weathered coal or lignite.
Weathered coal be earth's surface or shallow-layer lignite, bituminous coal and anthracite be subjected to for a long time atmosphere, sunlight, sleet, underground water with
And the product of the comprehensive functions such as minerals erosion.Weathered coal humic acid total content is usually 30~70%, reach as high as 80% with
On.
Lignite is the minimum pit coal of degree of coalification, a kind of brownish black between peat and pitch coal, lacklustre
Rudimentary coal.
According to the present invention, weathered coal or lignite are crushed using existing conventional crushing plant, collect granularity be 150~
The humic acid minerals raw material of 300 mesh carries out preparing humic acid extracting solution.
In the present invention, when humic acid minerals raw material is 100 parts by weight, if humic acid described in the humic acid extractant
Extractant dosage is lower than 800 parts by weight, then will lead to that liquid is thick to be difficult to carry out subsequent centrifugal treating；If the humic acid mentions
It takes agent dosage to be higher than 1500 parts by weight, then will lead to the humic acid liquid water content of extraction, influence the application in urea.Cause
This, the humic acid extractant dosage is that 800~1500 parts by weight are appropriate.
In this step, humic acid minerals raw material and humic acid are extracted in the case where revolving speed is the stirring of 100~200rpm
The temperature of agent composition is gradually increased to 90 DEG C, and keeps 40~60min at this temperature.Its Extracting temperature and extraction time are super
It is worthless for crossing the range.If extraction time is shorter than 40min, humic acid is extracted not exclusively, and humic acid is caused to lose；
If extraction time is more than 60min, the energy consumption for extracting humic acid is caused to increase, increased costs.Therefore, humic acid extraction time
It is feasible for 40~60min.
According to the present invention, the extract being cooled to room temperature using centrifuge under conditions of 1000~5000rpm of revolving speed from
The heart separates 5~30min.The centrifuge is the product sold on existing market, such as by ShangHai City centrifugal Machine Institute
Co., Ltd separates the product of sleeping spiral shell sedimentation centrifuge sale with trade name two-phase.
C, chelated zinc liquid
By 100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine and 30 parts by weight of glycerin
It is added in the water that 1000 parts by weight temperature are 50 DEG C, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature
80 DEG C of degree, stirring and dissolving obtain the chelated zinc liquid.
D, the preparation of Humic acid synergistic carrier
10~20 parts by weight benzene carboxylic acids and 0.02~0.10 parts by weight polyethylene glycol are added to 100 parts by weight in step B
In obtained humic acid extracting solution, it is heated to temperature 50 C, 2~3 parts by weight cumyl peroxides is added, is then heated to
100 DEG C of temperature, 60~120min is reacted at this temperature, adds 3~8 parts by weight of polyoxyethylene ethers and 0.5~2.0 weight
Part O-phthalic alkanol amides, cooling, its pH value is adjusted to 4.5~5.5, adds 100 weight by used phosphate aqueous solution
Chelated zinc liquid made from part step C obtains a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic carrier of summer corn base manure.
In the present invention, in the presence of with cumyl peroxide initiator and polyglycol surfactants, benzene carboxylic
The humic acid in humic acid extracting solution that acid is obtained with step B carries out graft reaction, then further increases the acidity of humic acid
Functional group's type and quantity, the purpose is to even closer with the amino reaction bonded in phosphorus ammonium molecule, hence it is evident that delay phosphorus ammonium in soil
Decomposition rate in earth.
In the present invention, the benzene carboxylic acid is benzoic acid, phenylacetic acid, salicylic acid or acetylsalicylic acid；They are all mesh
Preceding product available on the market, such as the product sold with trade name benzoic acid by Jiangsu Shun Feng Chemical Co., Ltd., Shandong are new
Product that Hua Longxin Chemical Co., Ltd. is sold with trade name sublimed salicylic acid, by Zhengzhou Jia Hong Chemical Co., Ltd. with trade name
The product of acetylsalicylic acid sale.
In the present invention, when other raw material dosages are in the range, if benzene carboxylic acid dosage is lower than 10 parts by weight,
Meeting benzene carboxyl functional group incrementss are relatively low；If benzene carboxylic acid dosage is higher than 20 parts by weight, part humic acid can be caused to precipitate；Cause
This, benzene carboxylic acid dosage is that 10~20 parts by weight are appropriate；
It, can be because of dispersion if polyethylene glycol dosage is lower than 0.02 parts by weight when other raw material dosages are in the range
Property is low, and graft effect is undesirable；If polyethylene glycol dosage is higher than 0.1 parts by weight, graft effect will affect；Therefore, benzene carboxylic
Sour dosage is that 0.02~0.1 parts by weight are feasible；
When other raw material dosages are in the range, if cumyl peroxide dosage is lower than 2 parts by weight, it will lead to
Grafting efficiency is low；If cumyl peroxide dosage is higher than 3 parts by weight, it is too fast to will lead to reaction；Therefore, peroxidating two is different
Propyl benzene dosage is that 2~3 parts by weight are appropriate；
This reaction carries out 60~120min at 100 DEG C of temperature, if the reaction time is shorter than 60 min, benzene carboxylic acid
It is inadequate with humic acid combination stability；If the reaction time is longer than 120min, energy consumption increases obvious.Therefore, this is reacted
Time is that 60~120min is feasible.
Polyoxyethylene ether has both resin and nonionic surfactant performance in the present invention, it can not only be used for stationary phase into
The metal ion that one step slows down, reduces in the soil liquid is contacted with phosphorus ammonium.Peroxophosphoric acid is that one kind contains phosphoric acid and several polyphosphoric acids
Mineral acid, it has extremely strong sequestering power to foreign metal ion, therefore, the pH of its not only adjustable system, but also can
To enhance the stability of Humic acid synergistic carrier by calcium, the magnesium plasma in chelating humic acid.
In Humic acid synergistic carrier preparation, the dosage of polyoxyethylene ether is 3~8 parts by weight, if polyoxyethylene ether
Dosage is lower than 3 parts by weight, then dispersion and permeance property are unobvious；If polyoxyethylene ether dosage is higher than 8 parts by weight, synergy is carried
Body viscosity is excessively high；Therefore, it is appropriate that polyoxyethylene ether dosage, which is 3~8 parts by weight,.
Similarly, O-phthalic alkanol amides dosage is 0.5~2.0 parts by weight, if O-phthalic alkanol amides
Dosage is lower than 0.5 parts by weight, then not significant to the osmotic effect for strengthening polyoxyethylene ether；If O-phthalic alkanol amides are used
Amount is higher than 2 parts by weight, then influences the dispersion performance of polyoxyethylene ether；Therefore, O-phthalic alkanol amides dosage be 0.5~
2.0 parts by weight are appropriate.
In this step, it is added after polyoxyethylene ether and O-phthalic alkanol amides and its solution is cooled to temperature 10
~40 DEG C.
According to the present invention, the concentration of the peroxophosphoric acid aqueous solution is 1~5mol/L.
The application method of Humic acid synergistic carrier of the present invention is as follows:
During existing production of ammonium phosphate, the obtained Humic acid synergistic carrier of 10~100 parts by weight step C is added to
It in 1000 parts by weight of phosphoric acid cleaning solutions, is reacted in tubular reactor with liquefied ammonia, obtains the carrier containing Humic acid synergistic
Phosphorus ammonium.
Existing production of ammonium phosphate process and its equipment used specifically may refer to " Modern Phosphating work technology and application ",
2013, Chemical Industry Press.
In this step, 1000 parts by weight of phosphoric acid cleaning solutions add 10~100 parts by weight Humic acid synergistic carriers.If
Humic acid synergistic carrier additive amount is lower than 10 parts by weight, then it is not significant to reduce the fixed effect of phosphorus；If Humic acid synergistic carrier
Additive amount is higher than 100 parts by weight, then causes phosphorus ammonium water content excessively high, increases drying process pressure.
[beneficial effect]
The beneficial effects of the present invention are:
1, Humic acid synergistic carrier of the present invention organic acidity functional group abundant can reduce particle phospho-ammonium fertilizer border pH 0.3~
1.4 units, the resiliency of enhanced fertilizer border soil；
2, Humic acid synergistic carrier of the present invention can reduce the fixation of phosphorus in the soil, soil in conjunction with the metal ions such as calcium, magnesium
23% and 16% is respectively increased in two phosphorus of earth calcium and eight phosphorus of calcium, and phosphorus and middle microelement in activating soil.
3, Humic acid synergistic carrier of the present invention stimulates root growth, improves root activity, promotes absorption of the crop to phosphorus element,
Further increase phosphate fertilizer utilization efficiency.Wheat root weight and vigor improve 35% or more, and maize root system fresh weight and vigor are distinguished
45.7% and 26.2% is averagely improved compared with control.Compared with commercially available phosphorus ammonium, the wheat yield of humic acid-ammonium phosphate of the present invention is averagely mentioned
High by 12.6%, phosphate fertilizer utilization efficiency improves 9.34 percentage points；Corn yield averagely improves 16.1%, and phosphate fertilizer utilization efficiency improves
10.7 percentage points.
[specific embodiment]
It will be better understood that the present invention by following embodiments.
One, embodiment is prepared
Embodiment 1: prepared by the phosphorus ammonium Humic acid synergistic carrier suitable for winter wheat base manure
The implementation steps of the embodiment are as follows:
A, prepared by humic acid extractant
30 parts by weight monoethanolamines, 8 parts by weight dimethylformamides and 8 parts by weight ethylene glycol are added to 2000 parts by weight
In the water that temperature is 60 DEG C, stirring and dissolving under conditions of revolving speed 60rpm, obtained solution is cooled to 40 DEG C of temperature hereinafter, obtaining
To the humic acid extractant；
B, prepared by humic acid extracting solution
The weathered coal humic acid raw mineral materials that 100 parts by weight granularities are 150 mesh is added to 1250 parts by weight to obtain in step A
To humic acid extractant in, its temperature is then gradually increased to 90 DEG C in the case where revolving speed is the stirring of 100rpm, and in this temperature
Degree is lower to keep 40min, is then cooled to room temperature, 5min is centrifugated under conditions of revolving speed 5000rpm, sediment discards, and obtains
To the humic acid extracting solution；
C, prepared by chelated zinc liquid
By 100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine and 30 parts by weight of glycerin
It is added in the water that 1000 parts by weight temperature are 50 DEG C, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature
80 DEG C of degree, stirring and dissolving obtain the chelated zinc liquid；
D, prepared by Humic acid synergistic carrier
16 parts by weight and 0.02 parts by weight polyethylene glycol are added to the humic acid that 100 parts by weight are obtained in step B
In extracting solution, it is then heated to temperature 50 C, 2.0 parts by weight cumyl peroxides is added, is then heated to temperature 100
DEG C, 60min is reacted at this temperature, adds 3 parts by weight of polyoxyethylene ethers and 1.5 parts by weight O-phthalic dialkylaminobenzoic acid acyls
Amine is cooled to 10 DEG C of temperature, its pH value is adjusted to 4.8 using the potassium pyrophosphate aqueous solution that concentration is 1mol/L, is then obtained
The phosphorus ammonium Humic acid synergistic carrier suitable for acid soil.
Embodiment 2: prepared by the phosphorus ammonium Humic acid synergistic carrier suitable for spring maize base manure
The implementation steps of the embodiment are as follows:
A, prepared by humic acid extractant
20 parts by weight diethanol amine, 5 parts by weight dimethylformamides and 5 parts by weight ethylene glycol are added to 1400 parts by weight
In the water that temperature is 64 DEG C, stirring and dissolving under conditions of revolving speed 120rpm, obtained solution is cooled to 40 DEG C of temperature hereinafter, obtaining
To the humic acid extractant；
B, prepared by humic acid extracting solution
The lignite humic acid raw mineral materials that 100 parts by weight granularities are 200 mesh is added to 800 parts by weight to obtain in step A
Humic acid extractant in, its temperature is then gradually increased to 90 DEG C in the case where revolving speed is the stirring of 130rpm, and in this temperature
Lower holding 48min, is then cooled to room temperature, is centrifugated 30min under conditions of 1000 rpm of revolving speed, and sediment discards, and obtains
To the humic acid extracting solution；
C, prepared by chelated zinc liquid
By 100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine and 30 parts by weight of glycerin
It is added in the water that 1000 parts by weight temperature are 50 DEG C, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature
80 DEG C of degree, stirring and dissolving obtain the chelated zinc liquid；
D, prepared by Humic acid synergistic carrier
20 parts by weight phenylacetic acids and 0.05 parts by weight polyethylene glycol are added to the humic acid that 100 parts by weight are obtained in step B
In extracting solution, it is then heated to temperature 50 C, 2.4 parts by weight cumyl peroxides is added, is then heated to temperature 100
DEG C, 80min is reacted at this temperature, adds 4 parts by weight of polyoxyethylene ethers and 0.5 parts by weight O-phthalic dialkylaminobenzoic acid acyl
Amine is cooled to 20 DEG C of temperature, its pH value is adjusted to 4.5 using the potassium pyrophosphate aqueous solution that concentration is 2mol/L, is then obtained
The phosphorus ammonium Humic acid synergistic carrier suitable for acid soil.
Embodiment 3: prepared by the phosphorus ammonium Humic acid synergistic carrier suitable for spring maize base manure
The implementation steps of the embodiment are as follows:
A, prepared by humic acid extractant
40 parts by weight triethanolamines, 10 parts by weight dimethylformamides and 10 parts by weight ethylene glycol are added to 1000 parts by weight
In the water that temperature is 67 DEG C, stirring and dissolving under conditions of revolving speed 180rpm, obtained solution is cooled to 40 DEG C of temperature hereinafter, obtaining
To the humic acid extractant；
B, prepared by humic acid extracting solution
The weathered coal humic acid raw mineral materials that 100 parts by weight granularities are 250 mesh is added to 1500 parts by weight to obtain in step A
To humic acid extractant in, its temperature is then gradually increased to 90 DEG C in the case where revolving speed is the stirring of 180rpm, and in this temperature
Degree is lower to keep 60min, is then cooled to room temperature, 15min is centrifugated under conditions of revolving speed 2500rpm, and sediment discards,
Obtain the humic acid extracting solution；
C, prepared by chelated zinc liquid
By 100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine and 30 parts by weight of glycerin
It is added in the water that 1000 parts by weight temperature are 50 DEG C, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature
80 DEG C of degree, stirring and dissolving obtain the chelated zinc liquid；
D, prepared by Humic acid synergistic carrier
10 parts by weight salicylic acids and 0.10 parts by weight polyethylene glycol are added to the humic acid that 100 parts by weight are obtained in step B
In extracting solution, it is then heated to temperature 50 C, 3.0 parts by weight cumyl peroxides is added, is then heated to temperature 100
DEG C, 100min is reacted at this temperature, adds 8 parts by weight of polyoxyethylene ethers and 2.0 parts by weight O-phthalic dialkylaminobenzoic acid acyls
Amine is cooled to 30 DEG C of temperature, its pH value is adjusted to 5.5 using the potassium pyrophosphate aqueous solution that concentration is 4mol/L, is then obtained
The phosphorus ammonium Humic acid synergistic carrier suitable for acid soil.
Embodiment 4: prepared by the phosphorus ammonium Humic acid synergistic carrier suitable for winter wheat base manure
The implementation steps of the embodiment are as follows:
A, prepared by humic acid extractant
50 parts by weight N methyldiethanol amines, 6 parts by weight dimethylformamides and 6 parts by weight ethylene glycol are added to 1600 weights
Measuring part temperature is stirring and dissolving under conditions of revolving speed 240rpm in 70 DEG C of water, obtained solution be cooled to 40 DEG C of temperature with
Under, obtain the humic acid extractant；
B, prepared by humic acid extracting solution
The weathered coal humic acid raw mineral materials that 100 parts by weight granularities are 300 mesh is added to 1050 parts by weight to obtain in step A
To humic acid extractant in, its temperature is then gradually increased to 90 DEG C in the case where revolving speed is the stirring of 200rpm, and in this temperature
Degree is lower to keep 55min, is then cooled to room temperature, 22min is centrifugated under conditions of revolving speed 3600rpm, and sediment discards,
Obtain the humic acid extracting solution；
C, prepared by chelated zinc liquid
By 100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine and 30 parts by weight of glycerin
It is added in the water that 1000 parts by weight temperature are 50 DEG C, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature
80 DEG C of degree, stirring and dissolving obtain the chelated zinc liquid；
D, prepared by Humic acid synergistic carrier
13 parts by weight acetylsalicylic acid benzene carboxylic acids and 0.08 parts by weight polyethylene glycol are added to 100 parts by weight to obtain in step B
To humic acid extracting solution in, be then heated to temperature 50 C, add 2.8 parts by weight cumyl peroxides, then heat
To 100 DEG C of temperature, 120min is reacted at this temperature, adds 5 parts by weight of polyoxyethylene ethers and 1.0 parts by weight O-phthalics
Alkanol amides are cooled to 40 DEG C of temperature, its pH value is adjusted to 5.2 using the potassium pyrophosphate aqueous solution that concentration is 5mol/L,
Then the phosphorus ammonium Humic acid synergistic carrier suitable for acid soil is obtained.
Two, test example
Test example 1: influence of the Humic acid synergistic carrier of the present invention to phospho-ammonium fertilizer border soil pH and available phosphorus
Sample preparation: the method described according to this specification, the corruption prepared using embodiment 1, embodiment 2 and embodiment 3
Phytic acid synergistic carrier prepares the phosphorus ammonium containing the by weight 5% Humic acid synergistic carrier respectively.It is weighed described in 150g respectively
Phosphorus ammonium particle, be placed in length × width × height=5cm × 5cm × 5cm, aperture is to obtain in the stainless steel cloth mold of 0.5mm
Square humic acid-ammonium phosphate A (embodiment 1), square humic acid-ammonium phosphate B (embodiment 2), square humic acid-ammonium phosphate C (are implemented
Example 3).Commercially available phosphorus ammonium is handled according to the method described above obtains square phosphorus ammonium as control sample P.
Test procedure: it is by weight that square phosphorus ammonium P, square humic acid-ammonium phosphate A, B, C, which are placed in water content, respectively
In 18% Fluvo-Aquic Soils (Shandong Dezhou), compacting soil to bulk density 1.3 is cultivated 12 hours at 25 ± 2 DEG C of Yu Wendu.Culture
After, it is cut out respectively with blade apart from square phosphorus ammonium edge 1.5-2.0cm, 1.0-1.5cm, 0.5-1.0cm, 0-0.5cm
Soil.According to (Lu Rukun " soil agrochemistry analysis method " Beijing: Chinese agriculture Science Press, 2000.) standard
Analysis method tests pH, available phosphorus content in these humic acid-ammonium phosphate block manure border soil.Its testing result is listed in Table 1 below.
Table 1: the fertile border soil pH of humic acid-ammonium phosphate of the present invention and commercially available phosphorus ammonium, available phosphorus content testing result
Fertile border is the initial period of fertilizer conversion, decides the phosphorus fixed ammonium process in later period.These test results show this
The Humic acid synergistic carrier of invention preparation can significantly reduce the soil within phospho-ammonium fertilizer border soil pH, especially reduction fertilizer border 1cm
PH reduces by 0.3~1.4 pH unit of amplitude, i.e., the H in the fertile border soil liquid+Concentration improves 3~14 times；Soil in fertile border 2cm
Available phosphorus content is significantly higher than commercially available phosphorus ammonium processing, thus illustrates that the fixed speed of humic acid-ammonium phosphate of the present invention obviously slows down.
Test example 2: influence of the Humic acid synergistic carrier of the present invention to soil inorganic P form
Humic acid-ammonium phosphate and commercially available phosphorus ammonium prepared by test example 1 is by equivalent chemical fertilizer phosphorus (P2O50.30 g/kg is air-dried
Soil) the commitment principle design experiment, (Fluvo-Aquic Soils, mountain will be air-dried with the 100g for crossing 2mm sieve respectively for examination fertilizer (P, A, B, C)
East Germany state) it is uniformly mixed for examination soil, it is packed into plastic culture cup.It is repeated 4 times, is adjusted soil moisture content using moisturizing weight method
To 20%, culture cup is sealed, 25 DEG C of temperature of growth cabinet is placed in and keeps humidity culture, is taken in culture 3d, 42d, 97d
Sample, according to (Lu Rukun " soil agrochemistry analysis method " Beijing: Chinese agriculture Science Press, 2000.) standard method
Measure various forms content of inorganic phosphorus.These testing results are listed in Table 2 below.
Table 2: each form content of inorganic phosphorus in soil when the 3rd day, 42 days, 97 days of culture
In table:
Ca2- P represents available phosphorus, Ca8- P represents potential available phosphorus library, indicates soil P supply ability, Al-P represent with
Phosphorus, Ca of the phosphorus, Fe-P representative that aluminium combines in conjunction with iron10- P represents the phosphorus for being difficult to discharge from soil.
The result listed by table 2 is it is found that in culture the 3rd, 42 and 97 day, the soil Ca of humic acid-ammonium phosphate processing of the present invention2-
P averagely improves 19%, 29% and 22% than commercially available phosphorus ammonium respectively；Ca8- P averagely improves 8%, 24% and 14% respectively.Thus may be used
See, humic acid-ammonium phosphate of the present invention can not only reduce phosphorus and fix, and improve soil available phosphorus content, but also can supplement soil to have
Imitate phosphorus library.
Test example 3: influence of the Humic acid synergistic carrier of the present invention to growth of wheat roots and vigor
The Humic acid synergistic carrier prepared using embodiment 1, embodiment 2 and embodiment 4 studies rotten plant using sand culture test
Influence of the sour synergistic carrier to wheat and Maize Roots and vigor.These Humic acid synergistic carriers of the present invention are sought in Huo Gelan
Additive amount in nutrient solution is 0.2g/L, is denoted as A, B, C respectively, compares as 0g/L.The quartz sand of processing is attached to 500mL culture
In Portland (drainage hole is arranged at bottom), Ju Li Portland is along 2~3cm.The crop of processing is colonized in Pei Yang Portland, is repeated 6 times.Every 4 days
Pour 1 Huo Gelan nutrient solution, each 100mL, to keep certain humidity and nutrient density.21 days after crop emergence, root
According to " plant physiology experiment guidance " (publishing house, South China Science & Engineering University, 2015) standard method be measured by sampling root system fresh weight and
TTC vigor.The results are shown in Table 3 for its testing result.
Table 3: influence of the Humic acid synergistic carrier of the present invention to crop root growth and vigor
The absorbability of crop root is an important factor for determining utilization rate of fertilizer.The test result listed by table 3 it is found that
The wheat root fresh weight and vigor of Humic acid synergistic carrier A, B, C processing of the present invention averagely improve 46.5% and than control respectively
35.2%, 45.7% and 26.2% is respectively increased in maize root system fresh weight and vigor.
Test example 4: influence of the humic acid-ammonium phosphate of the present invention to wheat, corn yield and phosphate fertilizer utilization efficiency
For humic acid-ammonium phosphate (being denoted as A, B, C respectively) and the city that examination fertilizer is by the preparation of 1,2,4 humic acid carrier of embodiment
Sell phosphorus ammonium (P).Test uses earth pillar planting type, selects the pvc pipe of internal diameter 25cm and high 100cm, its pipe is buried in the earth,
2cm above ground level suitable for reading, prevents rainfall runoff from flowing into, and lower open-ended is directly contacted with natural soils, simulates field cultivation shape
State.Each earth pillar fills soil 55kg.Humic acid-ammonium phosphate of the present invention and commercially available phosphorus ammonium by etc. full phosphorus amount the commitment principle design difference apply phosphorus
Level, it is all uniformly mixed to impose in earth pillar 0~30cm soil layer；By sufficient supply principle design, nitrogenous fertilizer is urea for nitrogenous fertilizer, potash fertilizer,
Amount of application is N 0.2g/kg soil, and potash fertilizer is potassium sulfate, amount of application K2O 0.3g/kg soil.Nitrogenous fertilizer, potash fertilizer are used as base manure one
Secondary property is mixed to be applied in 0~30cm soil.
Supplied P level is P2O50.10g/kg, 8 repetitions.
Wheat test: the full uniform seed of selection, every column sow 30 wheat seeds, and seedling stage carries out thinning, and every basin is last
Stay 12 plants.
Corn trials: each earth pillar broadcasts 5 corn seeds, and seed level 3cm, 1 week laggard seedling in the ranks of emerging, finally every column stays
1 plant of corn.Phosphate fertilizer utilization efficiency is calculated according to following formula:
Phosphate fertilizer Apparent Availability=(apply phosphorus processing P uptake by plants-and do not apply phosphorus processing P uptake by plants)/phosphorus application amount × 100%,
These test results are listed in Table 4 below.
Table 4: influence of the humic acid-ammonium phosphate of the present invention to wheat, corn yield and phosphate fertilizer utilization efficiency
For the result listed by table 4 it is found that compared with commercially available phosphorus ammonium, the wheat yield of humic acid-ammonium phosphate A, B, C of the present invention are flat
12.6% is improved, phosphate fertilizer utilization efficiency improves 9.34 percentage points；Corn yield averagely improves 16.1%, and phosphate fertilizer utilization efficiency improves
10.7 percentage points.
It can be seen that after Humic acid synergistic carrier prepared by the present invention is in conjunction with phosphorus ammonium, it can be significant by influencing fertilizer border pH
Slow down the fixation of phosphorus ammonium in alkaline soils, improves P availability, Available phosphate can also be supplemented.Humic acid of the present invention
Synergistic carrier can promote crop root growth, improve root activity, by enhancing Nutrient Absorption, improve phosphate fertilizer utilization efficiency.
Claims (10)
1. a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic support preparation method of spring maize base manure, it is characterised in that the system
The step of Preparation Method, is as follows:
A, prepared by humic acid extractant
20~50 parts by weight hydramine, 5~10 parts by weight dimethylformamides and 5~10 parts by weight ethylene glycol are added to 1000~
In the water that 2000 parts by weight temperature are 60~70 DEG C, stirring and dissolving is cooling, obtains the humic acid extractant；
B, prepared by humic acid extracting solution
100 parts by weight humic acid minerals raw materials are added to the humic acid extractant that 800~1500 parts by weight are obtained in step A
In, its temperature is then gradually increased to 90 DEG C under stiring, and keep 40~60min at this temperature, is then cooled to room
Temperature, centrifuge separation, sediment discard, and obtain the humic acid extracting solution；
C, prepared by chelated zinc liquid
100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine are added to 30 parts by weight of glycerin
In the water that 1000 parts by weight temperature are 50 DEG C, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature 80
DEG C, stirring and dissolving obtains the chelated zinc liquid；
D, prepared by Humic acid synergistic carrier
10~20 parts by weight benzene carboxylic acids and 0.02~0.10 parts by weight polyethylene glycol are added to 100 parts by weight to obtain in step B
Humic acid extracting solution in, be heated to temperature 50 C, add 2~3 parts by weight cumyl peroxides, be then heated to temperature
100 DEG C, 60~120min is reacted at this temperature, adds 3~8 parts by weight of polyoxyethylene ethers and 0.5~2.0 parts by weight are adjacent
Phthalic acid alkylamide, cooling, its pH value is adjusted to 4.5~5.5 by used phosphate aqueous solution, obtains a kind of winter wheat or summer
The phosphorus ammonium Humic acid synergistic carrier of corn base manure.
2. Humic acid synergistic support preparation method according to claim 1, it is characterised in that in step, the alcohol
Amine is one or more hydramine selected from monoethanolamine, diethanol amine, triethanolamine or N methyldiethanol amine.
3. Humic acid synergistic support preparation method according to claim 1, it is characterised in that in step, will be in revolving speed
The solution that stirring and dissolving obtains under conditions of 60~240rpm is cooled to 40 DEG C of temperature or less.
4. Humic acid synergistic support preparation method according to claim 1, it is characterised in that in step, hydramine, diformazan
The weight ratio of base formamide, ethylene glycol and water is 28~42:6~9:6~9:1200~1800.
5. Humic acid synergistic support preparation method according to claim 1, it is characterised in that in stepb, the corruption
Phytic acid raw mineral materials is weathered coal or lignite.
6. Humic acid synergistic support preparation method according to claim 1, it is characterised in that in stepb, the rotten plant
The granularity of sour raw mineral materials is 150~300 mesh.
7. Humic acid synergistic support preparation method according to claim 1, it is characterised in that in stepb, in revolving speed
5~30min is centrifugated under conditions of 1000~5000rpm.
8. the Humic acid synergistic support preparation method according to claim, it is characterised in that in step D, the benzene carboxylic
Acid is benzoic acid, phenylacetic acid, salicylic acid or acetylsalicylic acid.
9. Humic acid synergistic support preparation method according to claim 1, it is characterised in that in step D, described to cross phosphorus
The concentration of aqueous acid is 1~5mol/L.
10. Humic acid synergistic support preparation method according to claim 1, it is characterised in that in step D, polyoxy is added
Its solution is cooled to 10~40 DEG C of temperature after vinethene and O-phthalic alkanol amides.
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