CN109232099A - It is a kind of suitable for winter wheat or the phosphorus ammonium preparation method containing alginic acid synergistic carrier of spring maize base manure - Google Patents
It is a kind of suitable for winter wheat or the phosphorus ammonium preparation method containing alginic acid synergistic carrier of spring maize base manure Download PDFInfo
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- CN109232099A CN109232099A CN201811328684.2A CN201811328684A CN109232099A CN 109232099 A CN109232099 A CN 109232099A CN 201811328684 A CN201811328684 A CN 201811328684A CN 109232099 A CN109232099 A CN 109232099A
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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
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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Abstract
The present invention relates to the phosphorus ammonium preparation method for the synergistic carrier containing alginic acid for being suitable for winter wheat or spring maize base manure, which includes the preparation of seaweed acid extractant, the preparation of alginic acid extracting solution and the preparation of alginic acid synergistic carrier.Alginic acid synergistic carrier of the present invention is prepared in conjunction with ammonium phosphate production process is suitable for winter wheat/spring maize base manure alginic acid phosphorus ammonium.Compared with commercially available phosphorus ammonium, the soil pH in alginic acid phospho-ammonium fertilizer border 1cm reduces by 0.3~1.3 unit, and soil available phosphorus content is averagely higher than commercially available phosphorus ammonium processing 57.7% in fertile border 2cm, illustrates that the fixed speed of alginic acid phosphorus ammonium obviously slows down, soil Ca2- P and Ca8- P averagely improves 23.7% and 15.5% respectively；Wheat root weight and vigor improve 35% or more, and maize root system fresh weight and vigor averagely improve 20% or more respectively；Wheat yield averagely improves 12.6%, and utilization rate of nitrogen fertilizer improves 9.4 percentage points；Corn yield averagely improves 15.8%, and utilization rate of nitrogen fertilizer improves 10.6 percentage points.
Description
[technical field]
The invention belongs 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 preparation method containing alginic acid synergistic carrier of base manure.
[background technique]
The 5.5% of the world phosphor resource reserves Jin Zhan of 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 alginic acid, can be certain
Phosphorus is reduced in degree to fix, and improves phosphorus amount.CN102701866A disclose a kind of fermentation liquid seaweed extract material synergist and
Its production method and purposes, using natural seaweed as raw material, through microbial fermentation, then taken with alkali carries, the processes such as filters pressing produce seaweed
Extracting solution obtains fermentation alga liquid fertilizer synergist of the invention then to chelated microelements are added in liquid.
A kind of method that whole biologic enzymolysis method prepares seaweed plants growth regulator of CN107236766A, including prepare before production, is former
The pretreatment of material, level-one enzymatic hydrolysis, enzymolysis liquid removal of impurities, enzymolysis liquid homogeneous, secondary enzymolysis, post-processing, the isolating and purifying of somatotropin,
Fertilizer such as matches at nine steps eventually.It yet there are no and related contain alginic acid synergistic carrier suitable for winter wheat or spring maize base manure
The patent application of phosphorus ammonium and its related data.
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 containing alginic acid synergistic carrier of spring maize base manure
Ammonium 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 preparation side containing alginic acid synergistic carrier of spring maize base manure
Method.
The step of phosphorus ammonium preparation method, is as follows:
A, prepared by seaweed 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 seaweed acid extractant；
B, prepared by alginic acid extracting solution
100 parts by weight seawood meals are added to 800~1500 parts by weight in the seaweed acid extractant that step A is obtained, so
Its temperature is gradually increased to 70~90 DEG C under stiring afterwards, and keeps 6~12h at this temperature, is then cooled to room temperature, from
Heart separation, sediment discard, and obtain the alginic acid extracting solution；
C, chelating zinc solution preparation
100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine are added with 30 parts by weight of glycerin
In the water for being 50 DEG C to 1000 parts by weight temperature, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature
80 DEG C, stirring and dissolving obtains the chelating zinc solution；
D, prepared by alginic 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 alginic 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 alginic acid synergistic carrier；
E, the phosphorus ammonium preparation of the synergistic carrier containing alginic acid
During existing production of ammonium phosphate, the obtained alginic acid synergistic carrier of 10~100 parts by weight step D is added to
It in 1000 parts by weight of phosphoric acid cleaning solutions, is reacted in tubular reactor with liquefied ammonia, obtains the synergistic carrier containing alginic acid
Phosphorus ammonium.
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.
According to another preferred method of implementation of the present invention, in step, it will be stirred under conditions of 60~240rpm of revolving speed
It mixes the solution that dissolution obtains and is cooled to 30 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 seaweed is brown alga, bulk kelp or bubble leaf
Algae；The granularity of the seawood meal is less than 2mm.
According to another preferred method of implementation of the present invention, in stepb, under conditions of 1000~3000rpm of revolving speed
It is centrifugated 10~40min.
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 10~35 DEG C of temperature after base amide.
According to another preferred method of implementation of the present invention, in step E, alginic acid synergistic carrier and phosphoric acid washing liquid
Weight ratio is 25~80:1000.
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 preparation side containing alginic acid synergistic carrier of spring maize base manure
Method.
The step of phosphorus ammonium preparation method, is as follows:
A, prepared by seaweed 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 seaweed acid extractant；
Hydramine is a kind of using the nitrogen-atoms of ammonia as core, and the compound that the hydrogen atom of ammonia is replaced by alcohol, it can be with seaweed
Calcium, magnesium, iron plasma chelating in powder, improve the water solubility of this raw material, extract sea from seawood meal to help to improve
The recovery rate of alginic acid.
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. of Guoan of Zouping County with trade name N methyldiethanol amine
(MDEA) product sold.
Dimethylformamide is a kind of organic base, it is reacted with acidic-groups such as carboxyl, phenolic hydroxyl groups in alginic acid,
Alginic acid is set to become a kind of water-soluble alginic acid, so as to extract alginic acid from acid starting material containing seaweed, and it is also
It can increase methyl, methoxy functional mass contg in alginic 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).
Ethylene glycol can enhance due to the good intersolubility of water and low temperature resistance alginic 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 hydramine is lower than 20 parts by weight,
Alginic acid recovery rate can then be reduced；If the dosage of hydramine is higher than 50 parts by weight, alginic acid extractant liquid bubble will lead to
Excessively, tiny impurity is mixed in alginic acid liquid, the alginic acid purity liquid 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.
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 alginic acid recovery rate can be reduced；If the dosage of dimethylformamide is higher than 10 parts by weight, seaweed will lead to
Liquid bubble is excessive in sour extraction process, and tiny impurity is mixed in alginic acid liquid, the alginic acid purity decline of extraction；Cause
This, the dosage of dimethylformamide is that 5~10 parts by weight are suitable, preferably 6~9 parts by weight.
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 alginic acid liquid stability 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 alginic 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.
It, can be because of seaweed if the dosage of water is lower than 1000 parts by weight when other raw material dosages are in the range
Acid extractant excessive concentration, water consumption is low, and seaweed acid solubility is limited, then extracts the decline of alginic acid efficiency；If the use of water
, then can be too low because of alginic acid Extractant concentration when amount is higher than 2000 parts by weight, also result in the decline of alginic acid recovery rate；Therefore,
The dosage of water is that 1000~2000 parts by weight are suitable, preferably 1200~1800 parts by weight, more preferably 1400~
1600 parts by weight.
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 30
DEG C hereinafter, main purpose be guarantee seaweed acid extractant stability and quantifying it is standby.
B, prepared by alginic acid extracting solution
100 parts by weight seawood meals are added to 800~1500 parts by weight in the seaweed acid extractant that step A is obtained, so
Its temperature is gradually increased to 70~90 DEG C under stiring afterwards, and keeps 6~12h at this temperature, is then cooled to room temperature, from
Heart separation, sediment discard, and obtain the alginic acid extracting solution；
According to the present invention, the seaweed is brown alga, bulk kelp or yellow tang, and the seaweed that the present invention uses all is existing market
The product of upper sale, such as the brown alga that the present invention uses is the brown alga sold by the friendly company of Yantai Long Island three with trade name kelp；
The bulk kelp that the present invention uses is the bulk kelp sold by Shaanxi Si Nuote Bioisystech Co., Ltd with trade name bulk kelp original powder.
According to the present invention, brown alga, bulk kelp or yellow tang are crushed using existing conventional crushing plant, it is small collects granularity
Alginic acid extracting solution is prepared as raw material in the seawood meal of 2mm.
In the present invention, when seawood meal is 100 parts by weight, if the seaweed acid extractant dosage is lower than 800 parts by weight,
It then will lead to that liquid is thick to be difficult to carry out subsequent centrifugal treating；If the seaweed acid extractant dosage is higher than 1500 parts by weight,
The alginic acid extracting solution water content that then will lead to extraction is high, influences the application in urea.Therefore, the seaweed acid extractant is used
Amount is that 800~1500 parts by weight are appropriate.
In this step, in the case where revolving speed is the stirring of 100~200rpm by seawood meal and alginic acid extractant mixture
Temperature be gradually increased to 70~90 DEG C, and at this temperature keep 6~12h.Its extraction time is more than the range can not
It takes.If extraction time is shorter than 6h, alginic acid is extracted not exclusively, and alginic acid is caused to lose；If extraction time is more than
12h then causes the energy consumption for extracting alginic acid to increase, increased costs.Therefore, it is feasible that alginic acid extraction time, which is 6~12h,.
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 10~40min.The centrifuge that the present invention uses is current market sales of product, such as by Shanghai City centrifugal machine
Co., Ltd of research institute separates the product of sleeping spiral shell sedimentation centrifuge sale with trade name two-phase.
C, chelating zinc solution preparation
100 parts by weight of lemon acid potassium, 20 parts by weight D-sorbites, 50 parts by weight diethanol amine are added with 30 parts by weight of glycerin
In the water for being 50 DEG C to 1000 parts by weight temperature, then dissolution is added 200 parts by weight white vitriols, is then heated to temperature
80 DEG C, stirring and dissolving obtains the chelating zinc solution；
Potassium citrate, D-sorbite, diethanol amine, glycerol and the white vitriol that the present invention uses all are currently on the market
The product of sale.
D, prepared by alginic 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 alginic 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
Part step C is obtained to chelate zinc solution, obtains a kind of alginic acid synergistic carrier；
In the present invention, in the presence of with cumyl peroxide initiator and polyglycol surfactants, benzene carboxylic
The alginic acid in alginic acid extracting solution that acid is obtained with step B carries out graft reaction, then further increases the acidity of alginic 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.
It in the present invention,, can if benzene carboxylic acid dosage is lower than 10 parts by weight when other raw material dosages are in the range
Benzene carboxyl functional group incrementss are relatively low；If benzene carboxylic acid dosage is higher than 20 parts by weight, part alginic 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, poly- second
Glycol 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 60min, benzene carboxylic acid
It is inadequate with alginic 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.O-phthalic alkanol amides non-ionic surface active
Agent can enhance the osmotic effect of polyoxyethylene ether in the present invention and improve synergistic carrier stability.Peroxophosphoric acid is a kind of
Mineral acid containing phosphoric acid and several polyphosphoric acids, it has extremely strong sequestering power to foreign metal ion, and therefore, it both can be with
The pH of the system is adjusted, and the stabilization of alginic acid synergistic carrier can be enhanced by calcium, the magnesium plasma in chelating alginic acid
Property.
In alginic 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
~35 DEG C.
According to the present invention, the concentration of the peroxophosphoric acid aqueous solution is 1~5mol/L.
E, the phosphorus ammonium preparation of the synergistic carrier containing alginic acid
During existing production of ammonium phosphate, the obtained alginic acid synergistic carrier of 10~100 parts by weight step D is added to
It in 1000 parts by weight of phosphoric acid cleaning solutions, is reacted in tubular reactor with liquefied ammonia, obtains the synergistic carrier containing alginic acid
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 alginic acid synergistic carriers.If
Alginic 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 alginic 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: the present invention prepares seaweed acid extractant by raw material of serial organic base, further will
Carboxylic acid containing aromatic ring and alginic acid are grafted, and compatibility chelated zinc prepares alginic acid synergistic carrier, in conjunction with ammonium phosphate production process,
Preparation is suitable for winter wheat/spring maize base manure alginic acid phosphorus ammonium.
1, the organic acidity functional group of the rich choice of products can reduce by 0.3~1.3 unit of particle phospho-ammonium fertilizer border pH, enhancing
The resiliency of fertile border soil.
2, the fixation of phosphorus in the soil, two phosphorus of soil calcium and eight phosphorus of calcium difference can be reduced in conjunction with the metal ions such as calcium, magnesium
Improve 23.7% and 15.5%, and phosphorus and middle microelement in activating soil.
3, root growth is stimulated, root activity is improved, promotes absorption of the crop to phosphorus element.Wheat root weight and vigor are equal
35% or more is improved, relatively control averagely improves 20% or more respectively for maize root system fresh weight and vigor.
4, crop yield and phosphate fertilizer utilization efficiency are improved.Wheat yield averagely improves 12.6%, and utilization rate of nitrogen fertilizer improves 9.4
Percentage point；Corn yield averagely improves 15.8%, and utilization rate of nitrogen fertilizer improves 10.6 percentage points.
[specific embodiment]
It will be better understood that the present invention by following embodiments.
One, embodiment is prepared
Embodiment 1: suitable for winter wheat or the phosphorus ammonium preparation method containing alginic acid synergistic carrier of spring maize base manure
The implementation steps of the embodiment are as follows:
A, prepared by seaweed 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 temperature
Degree is in 60 DEG C of water, stirring and dissolving under conditions of revolving speed 60rpm, obtained solution is cooled to 30 DEG C of temperature hereinafter, obtaining
The seaweed acid extractant；
B, prepared by alginic acid extracting solution
Bulk kelp original powder by 100 parts by weight granularities less than 2mm is added to 800 parts by weight and mentions in the alginic acid that step A is obtained
It takes in agent, its temperature is then gradually increased to 70 DEG C under stiring, and keep 12h at this temperature, is then cooled to room temperature,
It is centrifugated 40min under conditions of revolving speed 1000rpm, sediment discards, and obtains the alginic 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 with 30 parts by weight of glycerin
In the water for being 50 DEG C to 1000 parts by weight temperature, 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 alginic acid synergistic carrier
16 parts by weight and 0.02 parts by weight polyethylene glycol are added to the alginic 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, adds 100
Parts by weight step C is obtained to chelate zinc solution, then obtains the alginic acid synergistic carrier.
E, the phosphorus ammonium preparation of the synergistic carrier containing alginic acid
During existing production of ammonium phosphate, the obtained alginic acid synergistic carrier of 10 parts by weight step D is added to 1000 weights
It measures in part phosphoric acid washing liquid, is reacted in tubular reactor with liquefied ammonia, obtain the phosphorus ammonium of the synergistic carrier containing alginic acid.
Embodiment 2: suitable for winter wheat or the phosphorus ammonium preparation method containing alginic acid synergistic carrier of spring maize base manure
The implementation steps of the embodiment are as follows:
A, prepared by seaweed 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 temperature
Degree is in 64 DEG C of water, stirring and dissolving under conditions of revolving speed 120rpm, obtained solution is cooled to 30 DEG C of temperature hereinafter, obtaining
The seaweed acid extractant；
B, prepared by alginic acid extracting solution
Kelp brown alga powder raw material by 100 parts by weight granularities less than 2mm is added to 1000 parts by weight in the sea that step A is obtained
In alginic acid extractant, its temperature is then gradually increased to 90 DEG C under stiring, and keep 6h at this temperature, be then cooled to
Room temperature is centrifugated 15min under conditions of revolving speed 2500rpm, and sediment discards, and obtains the alginic 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 with 30 parts by weight of glycerin
In the water for being 50 DEG C to 1000 parts by weight temperature, 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 alginic acid synergistic carrier
20 parts by weight phenylacetic acids and 0.05 parts by weight polyethylene glycol are added to the alginic 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, adds 100
Parts by weight step C is obtained to chelate zinc solution, then obtains the alginic acid synergistic carrier.
E, the phosphorus ammonium preparation of the synergistic carrier containing alginic acid
During existing production of ammonium phosphate, the obtained alginic acid synergistic carrier of 30 parts by weight step D is added to 1000 weights
It measures in part phosphoric acid washing liquid, is reacted in tubular reactor with liquefied ammonia, obtain the phosphorus ammonium of the synergistic carrier containing alginic acid.
Embodiment 3: suitable for winter wheat or the phosphorus ammonium preparation method containing alginic acid synergistic carrier of spring maize base manure
The implementation steps of the embodiment are as follows:
A, prepared by seaweed 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 30 DEG C of temperature hereinafter, obtaining
To the seaweed acid extractant；
B, prepared by alginic acid extracting solution
Yellow tang powder raw material by 100 parts by weight granularities less than 2mm is added to the seaweed that 1500 parts by weight are obtained in step A
In acid extractant, its temperature is then gradually increased to 76 DEG C under stiring, and keep 10h at this temperature, be then cooled to
Room temperature is centrifugated 20min under conditions of revolving speed 2000rpm, and sediment discards, and obtains the alginic 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 with 30 parts by weight of glycerin
In the water for being 50 DEG C to 1000 parts by weight temperature, 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 alginic acid synergistic carrier
10 parts by weight salicylic acids and 0.10 parts by weight polyethylene glycol are added to the alginic 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, adds 100
Parts by weight step C is obtained to chelate zinc solution, then obtains the alginic acid synergistic carrier.
E, the phosphorus ammonium preparation of the synergistic carrier containing alginic acid
During existing production of ammonium phosphate, the obtained alginic acid synergistic carrier of 60 parts by weight step D is added to 1000 weights
It measures in part phosphoric acid washing liquid, is reacted in tubular reactor with liquefied ammonia, obtain the phosphorus ammonium of the synergistic carrier containing alginic acid.
Embodiment 4: suitable for winter wheat or the phosphorus ammonium preparation method containing alginic acid synergistic carrier of spring maize base manure
The implementation steps of the embodiment are as follows:
A, prepared by seaweed 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 30 DEG C of temperature with
Under, obtain the seaweed acid extractant；
B, prepared by alginic acid extracting solution
Wild kelp brown alga powder raw material by 100 parts by weight granularities less than 2mm is added to 1200 parts by weight and obtains in step A
Seaweed acid extractant in, its temperature is then gradually increased to 84 DEG C under stiring, and keep 8h at this temperature, it is then cold
But to room temperature, it is centrifugated 10min under conditions of revolving speed 3000rpm, sediment discards, and obtains the alginic acid and extracts
Liquid；
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 with 30 parts by weight of glycerin
In the water for being 50 DEG C to 1000 parts by weight temperature, 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 alginic 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 alginic 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 35 DEG C of temperature, its pH value is adjusted to 5.2 using the potassium pyrophosphate aqueous solution that concentration is 5mol/L,
100 parts by weight step C chelating zinc solution obtained is added, the alginic acid synergistic carrier is then obtained.
E, the phosphorus ammonium preparation of the synergistic carrier containing alginic acid
During existing production of ammonium phosphate, the obtained alginic acid synergistic carrier of 100 parts by weight step D is added to 1000 weights
It measures in part phosphoric acid washing liquid, is reacted in tubular reactor with liquefied ammonia, obtain the phosphorus ammonium of the synergistic carrier containing alginic acid.
Two, test example
Test example 1: alginic acid phospho-ammonium fertilizer of the present invention border soil pH and available phosphorus are compared with commercially available phosphorus ammonium
Sample preparation: the synergistic carrier containing alginic acid prepared by 150g embodiment 1, embodiment 2 and embodiment 3 is weighed respectively
They are placed in length × width × height=5cm × 5cm × 5cm by phosphorus ammonium (abbreviation alginic acid phosphorus ammonium) particle, aperture be 0.5mm not
It becomes rusty in steel wire mold, obtains square alginic acid phosphorus ammonium A, square alginic acid phosphorus ammonium B, square alginic acid phosphorus ammonium C.With city
Selling phosphorus ammonium is control sample P.
Test procedure: respectively by square phosphorus ammonium control sample P, square alginic acid phosphorus ammonium A, square alginic acid phosphorus ammonium
B, square alginic acid phosphorus ammonium C is placed in the Fluvo-Aquic Soils (Shandong Dezhou) of water content 18%, compacting soil to bulk density 1.3,
It is cultivated 12 hours at 25 ± 2 DEG C of temperature.After culture, cut out respectively with blade apart from phosphorus ammonium sample edge 1.5-2.0cm,
The soil of 1.0-1.5cm, 0.5-1.0cm, 0-0.5cm.According to (Shandong such as female " soil agrochemistry analysis method " Beijing: in
Agricultural science and technology publishing house of state, 2000.) pH in standard method test square phospho-ammonium fertilizer border soil, available phosphorus content.It is detected
The results are shown in Table 1.
Table 1: alginic acid phosphorus ammonium of the present invention is compared with the fertile border soil pH of commercially available phosphorus ammonium, available phosphorus content
Fertile border is the initial period of fertilizer conversion, decides the phosphorus fixed ammonium process in later period.These test results show this
The alginic acid phosphorus ammonium of invention preparation can significantly reduce the soil pH within fertile border soil pH, especially reduction fertilizer border 1cm, reduce width
Spend 0.3~1.3 pH unit, i.e., the H in the fertile border soil liquid+Concentration improves 3~13 times；Soil available phosphorus contains in fertile border 2cm
Amount is averagely higher than commercially available phosphorus ammonium processing 57.7%, illustrates that the fixed speed of alginic acid phosphorus ammonium obviously slows down.
(2) influence of the alginic acid phosphorus ammonium of the present invention to soil inorganic P form
Square alginic acid phosphorus ammonium and the commercially available phosphorus ammonium of square prepared by test example 1 is by equivalent chemical fertilizer phosphorus
(P2O50.30g/kg wind desiceted soil) the commitment principle design experiment, it will be for trying the 100g wind of fertilizer (P, A, B, C) respectively with 2mm sieve excessively
Dry (Fluvo-Aquic Soils, Shandong Dezhou) is uniformly mixed for examination soil, is packed into plastic culture cup.Each processing is repeated 4 times, and is used ...
Soil moisture content is adjusted to by weight 20% by gravimetric method, seals culture cup, is placed in 25 DEG C of growth cabinets of temperature and is kept wet
Degree culture, according to (for example female " soil agrochemistry analysis method " Beijing, Shandong: Chinese agriculture Science Press, 2000.) standard
Method measurement various forms content of inorganic phosphorus in culture 3d, 42d, 97d soil.Its testing result is listed in Table 2 below.
Table 2: various forms 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, that is, represents soil P supply ability.
The result listed by table 2 is it is found that in culture the 3rd, 42 and 97 day, the soil Ca of alginic acid phosphorus ammonium processing of the present invention2-
More commercially available phosphorus ammonium improves 18.7%, 30.5% and 22% to P respectively, averagely improves 23.7%；Ca8- P is respectively increased 8.5%,
23.8% and 14.6%, averagely improve 15.5%.It fixes, mentions it can be seen that alginic acid phosphorus ammonium of the present invention can not only reduce phosphorus
High soil available phosphorus content, can also supplement Available phosphate.
(3) influence of the alginic acid phosphorus ammonium of the present invention to wheat and Maize Roots and vigor
The alginic acid phosphorus ammonium prepared using embodiment 1, embodiment 2 and embodiment 4 studies alginic acid phosphorus using sand culture test
Influence of the ammonium to wheat and Maize Roots and vigor.Additive amount of the alginic acid phosphorus ammonium in Huo Gelan nutrient solution is 0.2g/
L is denoted as A, B, C respectively.The quartz sand handled well is attached in 500mL Pei Yang Portland (drainage hole is arranged at bottom), Ju Li Portland along 2~
3cm.The crop handled well is colonized in Pei Yang Portland, is repeated 6 times.Every 1 nutrient solution of pouring in 4 days, each 100mL, to protect
Hold certain humidity and nutrient density.21 days after crop emergence, according to " plant physiology experiment guidance " (South China Science & Engineering University
Publishing house, 2015) root system fresh weight and TTC vigor is measured by sampling in standard method.It the results are shown in Table 3.
Influence of the alginic acid phosphorus ammonium of the present invention of table 3 to crop root growth and vigor
The absorbability of crop root is an important factor for determining utilization rate of fertilizer.As shown in Table 3, alginic acid phosphorus ammonium A, B,
The relatively control averagely raising 37.1% and 35.2% respectively of the wheat root fresh weight and vigor of C processing, maize root system fresh weight and vigor
20.9% and 26.3% is respectively increased.
(4) influence of the alginic acid phosphorus ammonium of the present invention to wheat, corn yield and phosphate fertilizer utilization efficiency
For the alginic acid phosphorus ammonium and commercially available phosphorus ammonium of examination fertilizer Selection experiment (one) preparation, number identical as (one).Test is adopted
With earth pillar planting type, selection internal diameter is 25cm, and the pvc pipe of high 100cm is wholly embedded into soil, 2cm above ground level suitable for reading, is prevented
Only rainfall runoff flows into, and lower open-ended is directly contacted with natural soils, simulates field cultivation state.Each earth pillar fills soil 55kg.
Alginic acid phosphorus ammonium and commercially available phosphorus ammonium by etc. full phosphorus amount the commitment principle design different Supplied P levels, all uniformly it is mixed impose on earth pillar 0~
In 30cm soil layer；By sufficient supply principle design, nitrogenous fertilizer is urea for nitrogenous fertilizer, potash fertilizer, and amount of application is N0.2g/kg soil, and potash fertilizer is sulphur
Sour potassium, amount of application K2O 0.3g/kg soil.Nitrogenous fertilizer, potash fertilizer are used as base manure disposably to mix and apply 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.According to formula [phosphate fertilizer Apparent Availability=(apply phosphorus processing P uptake by plants-do not apply phosphorus processing P uptake by plants)/phosphorus application amount ×
100%] phosphate fertilizer utilization efficiency is calculated, the results are shown in Table 4.
Influence of the alginic acid phosphorus ammonium of the present invention of table 4 to wheat, corn yield and phosphate fertilizer utilization efficiency
As shown in Table 4, compared with commercially available phosphorus ammonium, the wheat yield of alginic acid phosphorus ammonium A, B, C averagely improve 12.6%, nitrogenous fertilizer
Utilization rate improves 9.4 percentage points；Corn yield averagely improves 15.8%, and utilization rate of nitrogen fertilizer improves 10.6 percentage points.
It can be seen that alginic acid phosphorus ammonium prepared by the present invention can significantly slow phosphorus ammonium in basic soil by influencing fertilizer border pH
In fixation, improve P availability, Available phosphate can also be supplemented.Promote crop root growth, improve root activity,
By enhancing Nutrient Absorption, phosphate fertilizer utilization efficiency is improved.
Claims (10)
1. a kind of suitable for winter wheat or the phosphorus ammonium preparation method containing alginic acid synergistic carrier of spring maize base manure, it is characterised in that
The step of preparation method, is as follows:
A, prepared by seaweed 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 seaweed acid extractant；
B, prepared by alginic acid extracting solution
100 parts by weight seawood meals are added to 800~1500 parts by weight in the seaweed acid extractant that step A is obtained, are then existed
Its temperature is gradually increased to 70~90 DEG C under stirring, and keeps 6~12h at this temperature, is then cooled to room temperature, centrifugation point
From sediment discards, and obtains the alginic acid extracting solution
C, chelating zinc solution preparation
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 chelating zinc solution；
D, prepared by alginic 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
Alginic 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, adds 100 parts by weight step
Rapid C is obtained to chelate zinc solution, obtains a kind of alginic acid synergistic carrier；
E, the phosphorus ammonium preparation of the synergistic carrier containing alginic acid
During existing production of ammonium phosphate, the obtained alginic acid synergistic carrier of 10~100 parts by weight step D is added to 1000 weights
It measures in part phosphoric acid washing liquid, is reacted in tubular reactor with liquefied ammonia, obtain the phosphorus ammonium of the synergistic carrier containing alginic acid.
2. phosphorus ammonium preparation method according to claim 1, it is characterised in that in step, the hydramine be it is a kind of or
A variety of hydramine selected from monoethanolamine, diethanol amine, triethanolamine or N methyldiethanol amine.
3. phosphorus ammonium preparation method according to claim 1, it is characterised in that in step, will be in 60~240rpm of revolving speed
Under conditions of the obtained solution of stirring and dissolving be cooled to 30 DEG C of temperature or less.
4. phosphorus ammonium preparation method according to claim 1, it is characterised in that in step, hydramine, dimethylformamide,
The weight ratio of ethylene glycol and water is 28~42:6~9:6~9:1200~1800.
5. phosphorus ammonium preparation method according to claim 1, it is characterised in that in stepb, the seaweed is brown alga, huge
Algae or yellow tang；The granularity of the seawood meal is less than 2mm.
6. phosphorus ammonium preparation method according to claim 1, it is characterised in that in step C, in 1000~3000rpm of revolving speed
Under conditions of be centrifugated 10~40min.
7. phosphorus ammonium preparation method according to claim 1, it is characterised in that in step D, the benzene carboxylic acid is benzene first
Acid, phenylacetic acid, salicylic acid or acetylsalicylic acid.
8. phosphorus ammonium preparation method according to claim 1, it is characterised in that in step D, the peroxophosphoric acid aqueous solution
Concentration is 1~5mol/L.
9. phosphorus ammonium preparation method according to claim 1, it is characterised in that in step D, polyoxyethylene ether and neighbour is added
Its solution is cooled to 10~35 DEG C of temperature after phthalic acid alkylamide.
10. phosphorus ammonium preparation method according to claim 1, it is characterised in that in step E, alginic acid synergistic carrier and phosphorus
The weight ratio of acid elution liquid is 25~80:1000.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274854A (en) * | 2013-06-17 | 2013-09-04 | 中国农业科学院农业资源与农业区划研究所 | Algae synergistic high-tower compound fertilizer and production method thereof |
| CN103274852A (en) * | 2013-06-17 | 2013-09-04 | 中国农业科学院农业资源与农业区划研究所 | Algae synergistic ammonium phosphate fertilizer and preparation method thereof |
| CN104478597A (en) * | 2014-12-16 | 2015-04-01 | 五洲丰农业科技有限公司 | Process for producing ureaformaldehyde slow release fertilizer with co-production of alginic acid liquid fertilizer |
| CN105085111A (en) * | 2015-08-12 | 2015-11-25 | 生之道生态农业科技股份有限公司 | Biological-organic fertilizer special for corn and preparation method thereof |
-
2018
- 2018-11-09 CN CN201811328684.2A patent/CN109232099A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274854A (en) * | 2013-06-17 | 2013-09-04 | 中国农业科学院农业资源与农业区划研究所 | Algae synergistic high-tower compound fertilizer and production method thereof |
| CN103274852A (en) * | 2013-06-17 | 2013-09-04 | 中国农业科学院农业资源与农业区划研究所 | Algae synergistic ammonium phosphate fertilizer and preparation method thereof |
| CN104478597A (en) * | 2014-12-16 | 2015-04-01 | 五洲丰农业科技有限公司 | Process for producing ureaformaldehyde slow release fertilizer with co-production of alginic acid liquid fertilizer |
| CN105085111A (en) * | 2015-08-12 | 2015-11-25 | 生之道生态农业科技股份有限公司 | Biological-organic fertilizer special for corn and preparation method thereof |
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