CN105110967A - Water-retention slow-release urea fertilizer and production method thereof - Google Patents
Water-retention slow-release urea fertilizer and production method thereof Download PDFInfo
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- CN105110967A CN105110967A CN201510587268.4A CN201510587268A CN105110967A CN 105110967 A CN105110967 A CN 105110967A CN 201510587268 A CN201510587268 A CN 201510587268A CN 105110967 A CN105110967 A CN 105110967A
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Abstract
The invention relates to water-retention slow-release urea fertilizer and a production method thereof. The production method comprises the steps of acrylic acid solution preparing, neutralization reaction performing, acrylamide adding, polymerization reaction performing, granulating and drying and the like. According to the water-retention slow-release urea fertilizer and the production method thereof, the water-retention slow-release urea fertilizer is safe, environmentally friendly, poisonless, odorless and free of any residual organic and inorganic harmful substances and does not pollute plants, soil, underground water and the like; soil moisture conservation and water saving are achieved, water evaporation can be effectively inhibited, water and soil loss is prevented, the water use efficiency can be increased by more than 20 percent, and the rainwater storage and retention capacity of the soil can be maximumly increased by more than 30 percent; the soil structure can be improved, and meanwhile the development of soil microorganisms can be facilitated.
Description
[technical field]
The invention belongs to fertilizer processing technique field.More specifically, the present invention relates to a kind of water-holding slow-release carbamide fertilizer; The invention still further relates to the production method of described water-holding slow-release carbamide fertilizer.
[background technology]
The agricultural water-holding slow-release carbamide fertilizer of environment-friendly highly efficient refers to and uses water conservation, water saving, the fertile material of joint in a large number for domain requirements such as agricultural, forestry, gardening, and a class Multifunction polymer composite of development, due to its uniqueness water suction, water conservation, fertilizer conservation and hold fertile performance, obtain in agricultural gardening, desertification control, farmland drought resisting production etc. and apply widely, such as CN101113119A discloses a kind of water-holding slow-release carbamide fertilizer and preparation method thereof.This preparation method is that Acrylic Acid Monomer potassium hydroxide neutralizes, and regulate pH with ammoniacal liquor, then add acrylamide, cation compound, linking agent, initiator, rapid reaction under nitrogen protection, obtains High hydrophilous resin, then mixes composite making with sequestrant.It is kernel fertilizer that CN1587211A discloses with granular urea, with vinylformic acid, potassium hydroxide, linking agent and initiator for polymer raw, chemical polymerization is utilized to manufacture cross linked polyacrylate potassium water-adsorbent polymer coated urea granulated fertilizer at urea granules surface direct formation of film at surface.
At present, at China's water-holding slow-release carbamide fertilizer research, application development rapidly, market demand is very large, but throughput is very little, and the product function of producing is few, performance is low, shows as field application expensive.Therefore need badly and create good product performance, there is multi-functional efficient agricultural water-holding slow-release carbamide fertilizer production technique.
The present inventor for many years in the research of high-performance water-retaining agent and the basis of production test, follow advanced technology, process, economical rationality, system optimal principle abundant research has been carried out to water-holding slow-release carbamide fertilizer technology, complete the present invention.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide a kind of water-holding slow-release carbamide fertilizer.
Another object of the present invention is to provide the production method of described water-holding slow-release carbamide fertilizer.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of production method of water-holding slow-release carbamide fertilizer.
The step of this production method is as follows:
A, preparation acrylic acid solution
Toward in and add vinylformic acid in still, be then that 1:1.0 ~ 1.2 add water, stirring and dissolving again according to the mass ratio of vinylformic acid and water, obtain a kind of acrylic acid aqueous solution;
B, neutralization reaction
In the acrylic acid aqueous solution that steps A obtains, add neutralizing agent, the vinylformic acid in described acrylic acid aqueous solution and the mass ratio of neutralizing agent are 1:0.5 ~ 1.2, stir and described neutralizing agent is dissolved, obtain a kind of acrylic acid brine solution;
C, interpolation acrylamide
In the acrylic acid brine solution that step B obtains, add acrylamide, the vinylformic acid in described acrylic acid brine solution and the mass ratio of acrylamide are 1:0.08 ~ 0.12, then stirring and dissolving, obtain a kind of acrylate and the blended aqueous solution of acrylamide;
D, polyreaction
Linking agent is added in the acrylate and the blended aqueous solution of acrylamide obtained in step C, the amount of described linking agent is 0.2 ~ 0.5% of vinylformic acid quality in acrylate and the blended aqueous solution of acrylamide, stirring and dissolving, then under the condition of temperature 80 ~ 130 DEG C, carry out thermopositive reaction 1.0 ~ 1.5h, obtain a kind of melting propylene hydrochlorate and acrylamide copolymer; Add in melting propylene hydrochlorate and acrylamide copolymer quality 10 ~ 50% urea fertilizer in described exothermal reaction process, utilize described thermopositive reaction to make it dissolve or use nano-dispersed equipment to make it disperse, evenly melt mixed with melting propylene hydrochlorate and acrylamide copolymer, after cooling, obtain a kind of urea and be dispersed in mixture in acrylate and acrylamide copolymer;
E, granulating and drying
The mixture that step D obtains is sent into pulverizer pulverize, the particle diameter obtained containing described urea fertilizer is divided to be acrylate and the acrylamide copolymer micelle of 4 ~ 6mm by sifted again, then described acrylate and acrylamide copolymer micelle are sent in microwave dryer, under the condition of temperature 105 ~ 130 DEG C, dry 15 ~ 25min, obtains described water-holding slow-release carbamide fertilizer.
According to another kind of preferred implementation of the present invention, in step, described vinylformic acid sodium acrylate, potassium acrylate, ammonium acrylate or vinylcarbinol replace.
According to another kind of preferred implementation of the present invention, in stepb, described neutralizing agent is selected from sodium bicarbonate, sodium carbonate, saleratus, salt of wormwood, potassium hydroxide or ammoniacal liquor.
According to another kind of preferred implementation of the present invention, in step C, described acrylamide butylene acid amide replaces.
According to another kind of preferred implementation of the present invention, in step D, described linking agent is selected from TriMethylolPropane(TMP)-three (3-aziridinyl propionic ester), SAC-100 linking agent or Sulfothiorine.
According to another kind of preferred implementation of the present invention, in step D, in described exothermal reaction process, add the fertilizer containing middle amount nutritive element and micronutrient element.
According to another kind of preferred implementation of the present invention, in step D, described nano-dispersed equipment is selected from ultrafine powder equipment, super fine powder equipment, nano-pulverization equipment or fine grinding equipment.
The invention still further relates to the water-holding slow-release carbamide fertilizer adopting described production method to obtain.Described water-holding slow-release carbamide fertilizer is made up of urea and described acrylate and acrylamide copolymer, or described water-holding slow-release carbamide fertilizer is made up of urea and described acrylate and crotonamide multipolymer.
A preferred embodiment of the invention, the content of described urea is 10 ~ 50% of described acrylate and acrylamide copolymer or acrylate and crotonamide copolymer quality.
According to another kind of preferred implementation of the present invention, the described water-holding slow-release carbamide fertilizer water-holding slow-release carbamide fertilizer that to be a kind of urea nanoparticle in dispersed mode be distributed in described acrylate and acrylamide copolymer or acrylate and crotonamide multipolymer.
In more detail the present invention will be described below.
The present invention relates to a kind of production method of water-holding slow-release carbamide fertilizer.
The step of this production method is as follows:
A, preparation acrylic acid solution
Toward in and add vinylformic acid in still, be then that 1:1.0 ~ 1.2 add water, stirring and dissolving again according to the mass ratio of vinylformic acid and water, obtain a kind of acrylic acid aqueous solution.
Vinylformic acid is important organic synthesis raw material and synthetic resins monomer, is a kind of simple unsaturated carboxylic acid, is made up of a vinyl and a carboxyl.It has following chemical structure:
The present invention use vinylformic acid be generally use in the art, extensive product sold in current Chemical market.
In this step, the vinylformic acid that the present invention uses can use sodium acrylate, potassium acrylate, ammonium acrylate or vinylcarbinol to replace.Wherein potassium acrylate, ammonium acrylate all contain the nutritive element required for plant-growth.
The vinylformic acid that the present invention uses, sodium acrylate, potassium acrylate, ammonium acrylate or vinylcarbinol are all extensive product solds in the market.
In the present invention, when the mass ratio of vinylformic acid and water is for being greater than 1:1.0, then can acrylic acid aqueous solution excessive concentration, be unfavorable for follow-up polyreaction; When the mass ratio of vinylformic acid and water is less than 1:1.2, then acrylic acid aqueous solution concentration is too low, is also unfavorable for follow-up polyreaction; Therefore, the mass ratio of vinylformic acid and water is 1:1.0 ~ 1.2 is rational, and preferably, the mass ratio of vinylformic acid and water is 1:1.06 ~ 1.15.
B, neutralization reaction
In the acrylic acid aqueous solution that steps A obtains, add neutralizing agent, the vinylformic acid in described acrylic acid aqueous solution and the mass ratio of neutralizing agent are 1:0.5 ~ 1.2, stir and described neutralizing agent is dissolved, obtain a kind of acrylic acid brine solution.
In the present invention, described neutralizing agent should be appreciated that be all can with-the COOH in vinylformic acid or-OH base salify, polyacrylic acid and water-holding slow-release carbamide fertilizer are not produced to the mineral alkali of good impact, these mineral alkalis are all in protection scope of the present invention simultaneously.
Particularly, the neutralizing agent that the present invention uses is selected from sodium bicarbonate, sodium carbonate, saleratus, salt of wormwood, potassium hydroxide or ammoniacal liquor.
Preferably, described neutralizing agent is selected from sodium carbonate, saleratus, salt of wormwood, potassium hydroxide or ammoniacal liquor.
More preferably, described neutralizing agent is selected from sodium carbonate, salt of wormwood or ammoniacal liquor.
The neutralizing agent that the present invention uses is all product sold in the market.
In the present invention, when the mass ratio of vinylformic acid and neutralizing agent is for being greater than 1:0.5, then with incomplete in the vinylformic acid in acrylic acid aqueous solution; When the mass ratio of vinylformic acid and neutralizing agent is less than 1:1.2, then neutralizing agent is excessive, and a part of neutralizing agent does not participate in neutralization reaction, so all produces detrimentally affect to subsequent polymerisation reaction; Therefore, the mass ratio of vinylformic acid and neutralizing agent is 1:0.5 ~ 1.2 is rational, and preferably, the mass ratio of vinylformic acid and water is 1:0.8 ~ 1.0.
In the present invention, described neutralization reaction is carried out if used when sodium acrylate, potassium acrylate or ammonium acrylate raw material with regard to not needing.
In this neutralization procedure, usually need, by temperature Kong ≤35 DEG C of acrylic acid brine solution, acrylic acid loss can be reduced like this, cooling apparatus and cooling water can also be saved simultaneously, reduce production cost.
C, interpolation acrylamide
In the acrylic acid brine solution that step B obtains, add acrylamide, the vinylformic acid in described acrylic acid brine solution and the mass ratio of acrylamide are 1:0.08 ~ 0.12, then stirring and dissolving, obtain a kind of acrylate and the blended aqueous solution of acrylamide.
In this step, the object of adding acrylamide in acrylic acid brine solution is to allow acrylate fully mix with acrylamide, to allow them successfully can carry out copolyreaction.
In described acrylic acid brine solution, when acrylic acid quality is 1, if when the quality of acrylamide is more than 0.08-0.12 scope, then acrylate and acrylamide can not fully react, cause acrylate or acrylamide not to participate in reaction completely, reduce its multipolymer productive rate; Therefore, the mass ratio of vinylformic acid and acrylamide is 1:0.08 ~ 0.12 is appropriate.
In this step, described acrylamide can replace with butylene acid amide, because the effect in the present invention of acrylamide and butylene acid amide and effect are all identical.
When using butylene acid amide, obtain a kind of acrylate and the blended aqueous solution of crotonamide.
The acrylamide that the present invention uses or crotonamide are all product solds in the market, the acrylamide product such as sold by Zhengzhou Rui Bo Chemical Co., Ltd., the crotonamide product sold by Chengdu Ai Keda chemical reagent company limited.
D, polyreaction
Linking agent is added in the acrylate and the blended aqueous solution of acrylamide obtained in step C, the amount of described linking agent is 0.2 ~ 0.5% of vinylformic acid quality in acrylate and the blended aqueous solution of acrylamide, stirring and dissolving, then under the condition of temperature 80 ~ 130 DEG C, carry out thermopositive reaction 1.0 ~ 1.5h, obtain a kind of melting propylene hydrochlorate and acrylamide copolymer; Add in melting propylene hydrochlorate and acrylamide copolymer quality 10 ~ 50% urea fertilizer in described exothermal reaction process, utilize described thermopositive reaction to make it dissolve or use nano-dispersed equipment to make it disperse, evenly melt mixed with melting propylene hydrochlorate and acrylamide copolymer, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and acrylamide copolymer.
In this step, reactor adopts the polypropylene reaction tray of band bar shaped lattice.Vinylformic acid and acrylamide carry out copolymerization under linking agent exists, concrete reaction can be entitled as " anti salt super absorbent resin is prepared in acrylate and acrylamide copolymerization " see people such as Yi Songhai, " Journal of Functional Polymers ", the polyreaction described in 16 (4), pp502-506 (2003).
In the present invention; linking agent should be appreciated that it is that one can at line style intermolecular bridging action; thus make the mutual bonding cross-linking of multiple thread-like molecule reticulate the material of structure; namely everyly can to promote or telomerized polymer molecule interchain covalent bonds is formed, simultaneously to water-holding slow-release carbamide fertilizer of the present invention without the material of any disadvantageous effect all in scope.
The linking agent that the present invention uses is selected from TriMethylolPropane(TMP)-three (3-aziridinyl propionic ester), SAC-100 linking agent or Sulfothiorine, they are all product solds in the market, TriMethylolPropane(TMP)-three (3-aziridinyl propionic ester) (CASNO.52234-82-9) product that such as Jiangsu Kangle New Materials Technology Co., Ltd. sells, the SAC-100 linking agent product that Shanghai You En Chemical Co., Ltd. sells.
In the present invention, if when the amount of described linking agent is more than 0.2-0.5% scope, linking agent required when then there will be acrylate and acrylamide is not enough, copolymerization carries out not thorough, correspondingly multipolymer productive rate reduces, or causes linking agent excessive, causes some other side reactions, cause copolymer products impure, affect its implementation result; Therefore, the amount of described linking agent is 0.2 ~ 0.5% is rational.
Urea fertilizer is added in the polymerization process of heat release, utilizing described thermopositive reaction to make it dissolve makes fertilizer be dispersed in polyacrylic acid with nanoparticle form by stirring, or use nano-dispersed device processes to make fertilizer be dispersed in polyacrylic acid with nanoparticle form, so not only significantly can reduce the loss that fertilizer causes in its production process, but also make fertilizer of the present invention have more excellent fertilizer conservation water retention property.
When adding urea fertilizer in described exothermal reaction process, also can need to add the fertilizer containing middle amount nutritive element and the fertilizer containing micronutrient element according to actual agriculture production.
The described fertilizer containing middle amount nutritive element is such as calcic fertilizer, as nitrocalcite, calcium carbonate, normal superphosphate, double superhosphate, precipitated phosphate, thomas phosphate, fused(calcium magnesium)phosphate etc.; Magnesium fertilizer, as magnesium sulfate, magnesium chloride, ammonium magnesium phosphate, fused(calcium magnesium)phosphate, rhombspar, magnesite etc.; Sulfur-containing fertilizer, image-stone cream, ammonium sulfate, potassium sulfate, magnesium sulfate etc.
The described fertilizer containing micronutrient element is such as boron fertilizer, as borax, boric magnesium fertilizer; Molydbenum fertilizer, as ammonium molybdate, Sodium orthomolybdate; Zinc fertilizer, as zinc sulfate, zinc oxide, zinc chloride; Copper is fertile, as copper sulfate; Manganese fertilizer, as manganous sulfate, manganese oxide; Iron fertilizer, as ferrous sulfate, ferrous ammonium sulphate etc.
Urea fertilizer addition, comprising the amount of the fertilizer containing middle amount nutritive element and micronutrient element, determines according to factors such as crop varieties, soil property, weather conditions, and this is easy to realize for those skilled in the art.
Described nano-dispersed equipment a kind ofly urea fertilizer granular powder can be made to be broken into nanoparticle and reach the equipment of dispersion.The nano-dispersed equipment that the present invention uses is selected from ultrafine powder equipment, super fine powder equipment, nano-pulverization equipment or fine grinding equipment, they are all product solds in the market, such as, described ultrafine powder equipment is with trade(brand)name 3216 type Suspension roller Raymond mill product sold by mining machinery company limited of Zhengzhou Tianrui; Described super fine powder equipment carries type pulverizing mill product sold by Shanghai Xi Zhi mine engineering Machinery Co., Ltd. with trade(brand)name Shanghai western sesame MTM series; Described nano-pulverization equipment is with trade(brand)name by company of Changzhou Ying Zhi Machinery Co., Ltd.
ceramic nano sand millproduct sold; Described fine grinding equipment is with trade(brand)name YQ300 Ultramicrofine crasher product sold by Zhengzhou Yu Qiang mechanical means company limited.
If when using crotonamide in step C, then this step is carried out in the following manner: linking agent is added in the acrylate and the blended aqueous solution of crotonamide obtained in step C, the amount of described linking agent is 0.2 ~ 0.5% of vinylformic acid quality in acrylate and the blended aqueous solution of crotonamide, stirring and dissolving, then under the condition of temperature 80 ~ 130 DEG C, carry out thermopositive reaction 1.0 ~ 1.5h, obtain a kind of melting propylene hydrochlorate and crotonamide multipolymer; Add with melting propylene hydrochlorate and crotonamide copolymer substance gauge 10 ~ 50% urea fertilizer in described exothermal reaction process, utilize described thermopositive reaction to make it dissolve or use nano-dispersed equipment to make it disperse, evenly melt mixed with melting propylene hydrochlorate and crotonamide multipolymer, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and crotonamide multipolymer.
E, granulating and drying
The mixture that step D obtains is sent into pulverizer pulverize, divided by sifted again and obtain acrylate that particle diameter is 4 ~ 6mm and acrylamide copolymer micelle, then described acrylate and acrylamide copolymer micelle are sent in microwave dryer, under the condition of temperature 105 ~ 130 DEG C, dry 15 ~ 25min, obtains described water-holding slow-release carbamide fertilizer.
The tablets press that the present invention uses, disintegrating apparatus, screening plant are all products that current agricultural materials market is sold, that generally adopt in fertilizer processing technique field.
The microwave dryer that the present invention uses is product sold on current agricultural materials market.
The method adopting GB15063-2009 composite fertilizer (compound manure) to specify measures, the water content of the water-holding slow-release carbamide fertilizer obtained is for described water-holding slow-release carbamide fertilizer total weight less than 5%, and the content of described urea fertilizer is 10 ~ 50% of described acrylate and acrylamide copolymer or acrylate and crotonamide copolymer quality.
The inventive method has following feature:
Direct solid alkali neutralizes, and does not need to join alkali still; Polyreaction is carried out at normal temperatures, reacting balance; Jel product adopts granulator granulation, and throughput is large; Aqueous gel fluidized is dry, and time of drying is short.
The present invention has that facility investment is few, stable operation, can while continuous seepage ammonium polyacrylate multipolymer and polyacrylic acid potassium water-holding agent, carry out the one-time formed agricultural water-holding slow-release carbamide fertilizer product of the composite synthesis of hot melt, the efficient agricultural water-holding slow-release carbamide fertilizer produced, excellent product performance, price are low, nutrient is adjustable, have arid, improve the soil, the multifunctionality such as fertilizer conservation.
[beneficial effect]
The invention has the beneficial effects as follows:
Water-holding slow-release carbamide fertilizer safety and environmental protection of the present invention, nonpoisonous and tasteless, not Pollution Plant, soil and groundwater etc., without any residual organic, inorganic hazardous material; Soil moisture conservation water-saving, can effectively suppress moisture to evaporate, prevent erosion, can improve efficiency of water application more than 20%, maximum increase soil rainwater retaining water retention capacity more than 30%, improves urea desorption column more than 15%; Can Soil structure be improved, make heavy soil, leak fertile sandy soil and secondary salt affected soil improved, promote that soil microorganisms grows simultaneously, improve the turnover utilising efficiency of soil organic matter; Absorption speed is fast, and general nature water is drawn to saturated maximum duration and is about 15-40 minute, the fastest 0.4 minute, and Water absorption is 150-300 times of own wt; Total nutrient is not less than 15%, not only can supply root system of plant moisture and nutrient in time, even and if at desert area and extreme dry climate, when annual rainfall reaches 200mm, also can plant grass and plant trees, improve plant nutrition level; Retaining non-rot root, the polyacrylic acid molecule suctioning water is expanded into hydrogel crystal, even if also can not rotten near root system of plant; Stable performance, even extreme arid, also can not suck-back plant moisture.
[embodiment]
The present invention can be understood better by following embodiment.
Embodiment 1: the preparation of water-holding slow-release carbamide fertilizer of the present invention
The implementation step of this embodiment is as follows:
A, preparation acrylic acid solution
Toward in and add vinylformic acid in still, be then that 1:1.10 adds water, stirring and dissolving again according to the mass ratio of vinylformic acid and water, obtain a kind of acrylic acid aqueous solution;
B, neutralization reaction
In the acrylic acid aqueous solution that steps A obtains, add sodium bicarbonate neutralizing agent, the vinylformic acid in described acrylic acid aqueous solution and the mass ratio of neutralizing agent are 1:0.7, stir and described neutralizing agent is dissolved, obtain a kind of acrylic acid brine solution;
C, interpolation acrylamide
In the acrylic acid brine solution that step B obtains, add acrylamide, the vinylformic acid in described acrylic acid brine solution and the mass ratio of acrylamide are 1:0.12, then stirring and dissolving, obtain a kind of acrylate and the blended aqueous solution of acrylamide;
D, polyreaction
TriMethylolPropane(TMP)-three (3-aziridinyl propionic ester) linking agent is added in the acrylate and the blended aqueous solution of acrylamide obtained in step C, the amount of described linking agent is 0.32% of vinylformic acid quality in acrylate and the blended aqueous solution of acrylamide, stirring and dissolving, then under the condition of temperature 102 DEG C, carry out thermopositive reaction 1.2h, obtain a kind of melting propylene hydrochlorate and acrylamide copolymer; Add in melting propylene hydrochlorate and acrylamide copolymer quality 42% urea fertilizer in described exothermal reaction process, stir, described thermopositive reaction is utilized to make it dissolve, evenly melt mixed with melting propylene hydrochlorate and acrylamide copolymer, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and acrylamide copolymer;
E, granulating and drying
The mixture that step D obtains is carried out pulverizing, sieving, the particle diameter obtained containing described urea fertilizer is acrylate and the acrylamide copolymer micelle of 4 ~ 6mm, then described acrylate and acrylamide copolymer micelle are sent in microwave dryer, dry 16min under the condition of temperature 112 DEG C, obtains described water-holding slow-release carbamide fertilizer.
Water-holding slow-release carbamide fertilizer prepared by this embodiment is a kind of urea fertilizer nanoparticle is distributed in acrylate and acrylamide copolymer water-holding slow-release carbamide fertilizer in dispersed mode.
Embodiment 2: the preparation of water-holding slow-release carbamide fertilizer of the present invention
The implementation step of this embodiment is as follows:
A, preparation sodium acrylate solution
Toward in and add sodium acrylate in still, be then that 1:1.00 adds water, stirring and dissolving again according to the mass ratio of sodium acrylate and water, obtain a kind of aqueous sodium acrylate solution;
C, interpolation acrylamide
In the aqueous sodium acrylate solution that steps A obtains, add butylene acid amide, the mass ratio of the vinylformic acid in described acrylic acid brine solution and butylene acid amide is 1:0.10, then stirring and dissolving, obtains a kind of acrylate and the blended aqueous solution of crotonamide;
D, polyreaction
SAC-100 linking agent is added in the acrylate and the blended aqueous solution of crotonamide obtained in step C, the amount of described linking agent is 0.20% of vinylformic acid quality in acrylate and the blended aqueous solution of crotonamide, stirring and dissolving, then under the condition of temperature 80 DEG C, carry out thermopositive reaction 1.5h, obtain a kind of melting propylene hydrochlorate and crotonamide multipolymer; Add in melting propylene hydrochlorate and acrylamide copolymer quality 10% urea fertilizer in described exothermal reaction process, re-using nano-dispersed equipment makes it disperse, evenly melt mixed with melting propylene hydrochlorate and crotonamide multipolymer, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and crotonamide multipolymer;
E, granulating and drying
The mixture that step D obtains is pulverized, screening, the particle diameter obtained containing described bicarbonate of ammonia urea fertilizer is acrylate and the acrylamide copolymer micelle of 4 ~ 6mm, then described acrylate and acrylamide copolymer micelle are sent in microwave dryer, dry 15min under the condition of temperature 130 DEG C, obtains described water-holding slow-release carbamide fertilizer.
Water-holding slow-release carbamide fertilizer prepared by this embodiment is that a kind of urea fertilizer nanoparticle is distributed in the water-holding slow-release carbamide fertilizer in acrylate and crotonamide multipolymer in dispersed mode.
Embodiment 3: the preparation of water-holding slow-release carbamide fertilizer of the present invention
The implementation step of this embodiment is as follows:
A, preparation potassium acrylate solution
Toward in and add vinylformic acid in still, be then that 1:1.05 adds water, stirring and dissolving again according to the mass ratio of vinylformic acid and water, obtain a kind of acrylic acid aqueous solution;
B, neutralization reaction
In the acrylic acid aqueous solution that steps A obtains, add saleratus neutralizing agent, the mass ratio of the vinylformic acid in described acrylic acid aqueous solution and saleratus neutralizing agent is 1:0.5, stirs and described neutralizing agent is dissolved, obtain a kind of acrylic acid brine solution;
C, interpolation acrylamide
In the acrylic acid brine solution that step B obtains, add acrylamide, the vinylformic acid in described acrylic acid brine solution and the mass ratio of acrylamide are 1:0.11, then stirring and dissolving, obtain a kind of acrylate and the blended aqueous solution of acrylamide;
D, polyreaction
Sulfothiorine linking agent is added in the acrylate and the blended aqueous solution of acrylamide obtained in step C, the amount of described linking agent is 0.38% of vinylformic acid quality in acrylate and the blended aqueous solution of acrylamide, stirring and dissolving, then under the condition of temperature 112 DEG C, carry out thermopositive reaction 1.3h, obtain a kind of melting propylene hydrochlorate and acrylamide copolymer; Add in melting propylene hydrochlorate and acrylamide copolymer quality 32% urea fertilizer in described exothermal reaction process, stir, re-using nano-dispersed equipment makes it disperse, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and acrylamide copolymer;
E, granulating and drying
The mixture that step D obtains is pulverized, screening, the particle diameter obtained containing described composite fertilizer (15-15-15) urea fertilizer is acrylate and the acrylamide copolymer micelle of 4 ~ 6mm, then described acrylate and acrylamide copolymer micelle are sent in microwave dryer, dry 10min under the condition of temperature 118 DEG C, obtains described water-holding slow-release carbamide fertilizer.
Water-holding slow-release carbamide fertilizer prepared by this embodiment is a kind of urea fertilizer nanoparticle is distributed in acrylate and acrylamide copolymer water-holding slow-release carbamide fertilizer in dispersed mode.
Embodiment 4: the preparation of water-holding slow-release carbamide fertilizer of the present invention
The implementation step of this embodiment is as follows:
A, preparation ammonium acrylate solution
Toward in and add ammonium acrylate in still, be then that 1:1.20 adds water, stirring and dissolving again according to the mass ratio of ammonium acrylate and water, obtain a kind of ammonium acrylate aqueous solution;
C, interpolation acrylamide
In the ammonium acrylate salt brine solution that step B obtains, add acrylamide, the vinylformic acid in described acrylic acid brine solution and the mass ratio of acrylamide are 1:0.08, then stirring and dissolving, obtain a kind of acrylate and the blended aqueous solution of acrylamide;
D, polyreaction
TriMethylolPropane(TMP)-three (3-aziridinyl propionic ester) linking agent is added in the acrylate and the blended aqueous solution of acrylamide obtained in step C, the amount of described linking agent is 0.26% of vinylformic acid quality in acrylate and the blended aqueous solution of acrylamide, stirring and dissolving, then under the condition of temperature 88 DEG C, carry out thermopositive reaction 1.0h, obtain a kind of melting propylene hydrochlorate and acrylamide copolymer; Add in melting propylene hydrochlorate and acrylamide copolymer quality 21% urea fertilizer in described exothermal reaction process, described thermopositive reaction is utilized to make it dissolve, evenly melt mixed with melting propylene hydrochlorate and acrylamide copolymer, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and acrylamide copolymer;
E, granulating and drying
The mixture that step D obtains is pulverized, screening, the particle diameter obtained containing described primary ammonium phosphate urea fertilizer is acrylate and the acrylamide copolymer micelle of 4 ~ 6mm, then described acrylate and acrylamide copolymer micelle are sent in microwave dryer, dry 25min under the condition of temperature 105 DEG C, obtains described water-holding slow-release carbamide fertilizer.
Water-holding slow-release carbamide fertilizer prepared by this embodiment is a kind of urea fertilizer nanoparticle is distributed in acrylate and acrylamide copolymer water-holding slow-release carbamide fertilizer in dispersed mode.
Embodiment 5: the preparation of water-holding slow-release carbamide fertilizer of the present invention
The implementation step of this embodiment is as follows:
A, preparation vinylcarbinol solution
Toward in and add potassium acrylate in still, be then that 1:1.10 adds water, stirring and dissolving again according to the mass ratio of potassium acrylate and water, obtain a kind of potassium acrylate aqueous solution;
C, interpolation acrylamide
In the potassium acrylate aqueous solution that step B obtains, add butylene acid amide, the vinylformic acid in the described potassium acrylate aqueous solution and the mass ratio of butylene acid amide are 1:0.09, then stirring and dissolving, obtain a kind of acrylate and the blended aqueous solution of crotonamide;
D, polyreaction
TriMethylolPropane(TMP)-three (3-aziridinyl propionic ester) linking agent is added in the acrylate and the blended aqueous solution of crotonamide obtained in step C, the amount of described linking agent is 0.44% of vinylformic acid quality in acrylate and the blended aqueous solution of crotonamide, stirring and dissolving, then under the condition of temperature 122 DEG C, carry out thermopositive reaction 1.4h, obtain a kind of melting propylene hydrochlorate and crotonamide multipolymer; Add with melting propylene hydrochlorate and crotonamide copolymer substance gauge 50% urea fertilizer in described exothermal reaction process, described thermopositive reaction is utilized to make it dissolve, evenly melt mixed with melting propylene hydrochlorate and crotonamide multipolymer, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and crotonamide multipolymer;
E, granulating and drying
The mixture that step D obtains is pulverized, screening, the particle diameter obtained containing described potassium sulfate urea fertilizer is acrylate and the crotonamide multipolymer micelle of 4 ~ 6mm, then described acrylate and crotonamide multipolymer micelle are sent in microwave dryer, dry 12min under the condition of temperature 124 DEG C, obtains described water-holding slow-release carbamide fertilizer.
Water-holding slow-release carbamide fertilizer prepared by this embodiment is that a kind of urea fertilizer nanoparticle is distributed in the water-holding slow-release carbamide fertilizer in acrylate and crotonamide multipolymer in dispersed mode.
Embodiment 6: the preparation of water-holding slow-release carbamide fertilizer of the present invention
The implementation step of this embodiment is as follows:
A, preparation acrylic acid solution
Toward in and add vinylformic acid in still, be then that 1:1.16 adds water, stirring and dissolving again according to the mass ratio of vinylformic acid and water, obtain a kind of acrylic acid aqueous solution;
B, neutralization reaction
In the acrylic acid aqueous solution that steps A obtains, add salt of wormwood neutralizing agent, the vinylformic acid in described acrylic acid aqueous solution and the mass ratio of neutralizing agent are 1:1.0, stir and described neutralizing agent is dissolved, obtain a kind of acrylic acid brine solution;
C, interpolation acrylamide
In the acrylic acid brine solution that step B obtains, add acrylamide, the vinylformic acid in described acrylic acid brine solution and the mass ratio of acrylamide are 1:0.10, then stirring and dissolving, obtain a kind of acrylate and the blended aqueous solution of acrylamide;
D, polyreaction
Sulfothiorine linking agent is added in the acrylate and the blended aqueous solution of acrylamide obtained in step C, the amount of described linking agent is 0.50% of vinylformic acid quality in acrylate and the blended aqueous solution of acrylamide, stirring and dissolving, then under the condition of temperature 130 DEG C, carry out thermopositive reaction 1.1h, obtain a kind of melting propylene hydrochlorate and acrylamide copolymer; Add in described exothermal reaction process in melting propylene hydrochlorate and acrylamide copolymer quality 18% urea fertilizer, it contains with the ferric sulfate of composite fertilizer's total weight 2.3%, magnesium sulfate, copper sulfate, borax, ammonium molybdate; Stir, re-use nano-dispersed equipment and make it disperse, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and acrylamide copolymer;
E, granulating and drying
The mixture that step D obtains is pulverized, screening, the particle diameter obtained containing described urea fertilizer is acrylate and the acrylamide copolymer micelle of 4 ~ 6mm, then described acrylate and acrylamide copolymer micelle are sent in microwave dryer, dry 20min under the condition of temperature 108 DEG C, obtains described water-holding slow-release carbamide fertilizer.
Water-holding slow-release carbamide fertilizer prepared by this embodiment is a kind of urea fertilizer nanoparticle is distributed in acrylate and acrylamide copolymer water-holding slow-release carbamide fertilizer in dispersed mode.
Test example 1: water-holding slow-release carbamide fertilizer application effect of the present invention
Test site: western market town, Tongzhou, Beijing;
Test materials: cucumber seeds
Test method:
A, test group: water-holding slow-release carbamide fertilizer prepared by embodiment 3;
If two process: process I is 2g/ basin, is converted to 100kg/ mu; Process II is 3g/ basin, is converted to 150kg/ mu; Each process repetition 3 times.
B, control group: the acrylic acid-acrylamide that Chemicals company limited of Zhengzhou Pfizer produces and the water-holding slow-release carbamide fertilizer that the urea that embodiment 3 uses obtains according to weight ratio 75:25 Homogeneous phase mixing, 2g/ basin, is converted to 100kg/ mu.
C, blank group: the urea fertilizer that embodiment 3 uses, its amount with process 1 identical, 0.5g/ basin, is converted to 25kg/ mu.
Testing sequence: prior to seeding these fertilizer are fully mixed with soil, then place three days.20 cucumber seeds sowed by every basin, and after planting water 300 milliliters/basin immediately.
Seed soaking on May 6, sowing on May 9, May 14 emerged, May 18 emerged completely, do not water emerging in 20 days.Seedling rate (cucumber seed is emerged and counted the ratio with cucumber seed sum) and upgrowth situation thereof are listed in table 1.
Table 1: use water-holding slow-release carbamide fertilizer of the present invention and cucumber is emerged and the impact in seedling stage
Can be known by the result of table 1 and find out, compare with blank group with control group, the water-holding slow-release carbamide fertilizer using the embodiment of the present invention 3 can significantly improve cucumber seed seedling rate.Cucumber seedling growth situation comparing result has absolutely proved that water-holding slow-release carbamide fertilizer of the present invention has good water retention capacity, significantly can improve the growth of cucumber seedling.
Test example 2: water-holding slow-release carbamide fertilizer application effect of the present invention
Test site: the Chinese Academy of Agricultural Sciences;
Test method: column simulation method
A, test group: water-holding slow-release carbamide fertilizer prepared by embodiment 3;
If two process: process I is 2g/ basin, is converted to 100kg/ mu; Process II is 3g/ basin, is converted to 150kg/ mu; Each process repetition 3 times.
B, control group: the acrylic acid-acrylamide that Chemicals company limited of Zhengzhou Pfizer produces and the water-holding slow-release carbamide fertilizer that the urea that embodiment 3 uses obtains according to weight ratio 75:25 Homogeneous phase mixing, 2g/ basin, is converted to 100kg/ mu.
C, blank group: the urea fertilizer that embodiment 3 uses, its amount with in process 1 urea-containing amount identical, 0.5g/ basin, is converted to 25kg/ mu.
Testing sequence: prior to seeding these fertilizer are fully mixed with soil, then soil is loaded in earth pillar.Add water saturated field capacity in earth pillar, leave standstill 1 angel's liquid manure fully with and, then add same water gaging leaching.When soil moisture content is down to field capacity about 40%, then carries out second time and to water and leaching process.Carry out the 3rd leaching process in the same fashion.
Before adopting the method that describes in this specification sheets to measure shower, first time shower, second time shower, third time shower soil nitrogen concentrations, its measurement result is listed in table 2:
Table 2: soil nitrogen concentrations measurement result
The result listed as can be seen from table 2, after 3 showers, the Soil Nitrogen nutrient content of blank group is reduced to 0.058% by 0.125%, i.e. nitrogen nutrients loss 53.6%, the Soil Nitrogen nutrient content of control group is reduced to 0.067% by 0.132%, i.e. nitrogen nutrients loss 49.2%, the fertilizer conservation performance of control group is obviously better than blank group.The Soil Nitrogen nutrient content of process 1 is reduced to 0.092% by 0.130%, i.e. nitrogen nutrients loss 29.2%, and the Soil Nitrogen nutrient content of process 2 is reduced to 0.132% by 0.178%, i.e. nitrogen nutrients loss 25.8%, and their fertilizer conservation performance is obviously better than control group.These result explanations, use acrylic acid-acrylamide water-keeping material can improve the sustained release performance of urea fertilizer, the water-holding slow-release carbamide fertilizer adopting scorification of the present invention to prepare has pole significant difference than the water keeping fertilizer be mixed to get by water-keeping material and fertilizer at fertilizer slow release aspect of performance, and namely the sustained release performance of water-holding slow-release carbamide fertilizer of the present invention is far superior to the fertilizer slow release performance of other group.
Test example 3: water keeping fertilizer application effect of the present invention
Test site: western market town, Tongzhou, Beijing;
Test materials: Semen Brassicae campestris
Test method:
A, test group: water-retention fertilizer prepared by embodiment 3;
If three process: process I is 2g/ basin, is converted to 100kg/ mu; Process II is 3g/ basin, is converted to 150kg/ mu; Each process repetition 3 times.
B, control group: the acrylic acid-acrylamide that Chemicals company limited of Zhengzhou Pfizer produces and the water keeping fertilizer that the urea fertilizer that embodiment 3 uses obtains according to weight ratio 75:25 Homogeneous phase mixing, 2g/ basin, is converted to 100kg/ mu.
C, blank group: embodiment 3 use urea fertilizer with process 1 nitrogen total amount identical, 0.5g/ basin, is converted to 25kg/ mu.
Testing sequence: fully mixed with soil by these fertilizer prior to seeding, waters 500ml water/basin, places one day.45 rapeseed seeds sowed by every basin, earthing.Later stage does not rewater.
Adopt the method described in this specification sheets to determine after planting the 0th day, soil moisture content when the 5th day, the 10th day, the 15th day, the 20th day, the measurement result of its soil moisture content is listed in table 3:
Table 3: the measurement result of soil moisture content
The result listed as can be seen from table 3, at after planting the 20th day, the soil moisture content of blank group was 3.10%, and the soil moisture content of control group is 7.16%, and the water retention property of control group is obviously better than blank group.At after planting the 20th day, the soil moisture content of process 1 was 11.48%, and the soil moisture content of process 2 is 12.56%, and their water retention property is obviously better than control group.These results absolutely prove, use acrylic acid-acrylamide water-keeping material can improve fertilizer water retention property, the water-holding slow-release carbamide fertilizer adopting scorification of the present invention to prepare has pole significant difference than the water keeping fertilizer be mixed to get by water-keeping material and fertilizer in water retention property, and namely the water retention property of water-holding slow-release carbamide fertilizer of the present invention is far superior to the water retention property of other group.Good with the water retention property of process 2 owing to processing 1, cole crop can make full use of these nutrition, therefore its well-grown, improves its Oil-seed yield.
Claims (10)
1. adopt hot melt process to produce a method for water-holding slow-release carbamide fertilizer, it is characterized in that the step of this production method is as follows:
A, preparation acrylic acid solution
Toward in and add vinylformic acid in still, be then that 1:1.0 ~ 1.2 add water, stirring and dissolving again according to the mass ratio of vinylformic acid and water, obtain a kind of acrylic acid aqueous solution;
B, neutralization reaction
In the acrylic acid aqueous solution that steps A obtains, add neutralizing agent, the vinylformic acid in described acrylic acid aqueous solution and the mass ratio of neutralizing agent are 1:0.5 ~ 1.2, stir and described neutralizing agent is dissolved, obtain a kind of acrylic acid brine solution;
C, interpolation acrylamide
In the acrylic acid brine solution that step B obtains, add acrylamide, the vinylformic acid in described acrylic acid brine solution and the mass ratio of acrylamide are 1:0.08 ~ 0.12, then stirring and dissolving, obtain a kind of acrylate and the blended aqueous solution of acrylamide;
D, polyreaction
Linking agent is added in the acrylate and the blended aqueous solution of acrylamide obtained in step C, the amount of described linking agent is 0.2 ~ 0.5% of vinylformic acid quality in acrylate and the blended aqueous solution of acrylamide, stirring and dissolving, then under the condition of temperature 80 ~ 130 DEG C, carry out thermopositive reaction 1.0 ~ 1.5h, obtain a kind of melting propylene hydrochlorate and acrylamide copolymer; Add in melting propylene hydrochlorate and acrylamide copolymer quality 10 ~ 50% urea fertilizer in described exothermal reaction process, utilize described thermopositive reaction to make it dissolve or use nano-dispersed equipment to make it disperse, evenly melt mixed with melting propylene hydrochlorate and acrylamide copolymer, after cooling, obtain a kind of urea fertilizer and be dispersed in mixture in acrylate and acrylamide copolymer;
E, granulating and drying
The mixture that step D obtains is sent into pulverizer pulverize, the particle diameter obtained containing described urea fertilizer is divided to be acrylate and the acrylamide copolymer micelle of 4 ~ 6mm by sifted again, then described acrylate and acrylamide copolymer micelle are sent in microwave dryer, under the condition of temperature 105 ~ 130 DEG C, dry 15 ~ 25min, obtains described water-holding slow-release carbamide fertilizer.
2. production method according to claim 1, is characterized in that in step, and described vinylformic acid sodium acrylate, potassium acrylate, ammonium acrylate or vinylcarbinol replace.
3. production method according to claim 1, is characterized in that in stepb, and described neutralizing agent is selected from sodium bicarbonate, sodium carbonate, saleratus, salt of wormwood, potassium hydroxide or ammoniacal liquor.
4. production method according to claim 1, is characterized in that in step C, and described acrylamide crotonamide replaces.
5. production method according to claim 1, is characterized in that in step D, and described linking agent is selected from TriMethylolPropane(TMP)-three (3-aziridinyl propionic ester), SAC-100 linking agent or Sulfothiorine.
6. production method according to claim 1, is characterized in that in step D, adds the fertilizer containing middle amount nutritive element and micronutrient element in described exothermal reaction process.
7. production method according to claim 1, is characterized in that in step D, and described nano-dispersed equipment is selected from ultrafine powder equipment, super fine powder equipment, nano-pulverization equipment or fine grinding equipment.
8. the water-holding slow-release carbamide fertilizer that described in claim, production method obtains any one of claim 1-7, it is characterized in that described water-holding slow-release carbamide fertilizer is made up of urea and described acrylate and acrylamide copolymer, or described water-holding slow-release carbamide fertilizer is made up of urea and described acrylate and crotonamide multipolymer.
9. water-holding slow-release carbamide fertilizer according to claim 8, is characterized in that the content of described urea is 10 ~ 50% of described acrylate and acrylamide copolymer or acrylate and crotonamide copolymer quality.
10. production method according to claim 8, the water-holding slow-release carbamide fertilizer that it is characterized in that it to be a kind of urea nanoparticle in dispersed mode be distributed in described acrylate and acrylamide copolymer or acrylate and crotonamide multipolymer.
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| ES2711655A1 (en) * | 2017-10-25 | 2019-05-06 | Jean Claude Garrigue | RETAINING GEL OF HUMIDITY AND SOIL CONDITIONING SUBSTANCES AND PLANTS, AND THE PROCESS OF OBTAINING THEM (Machine-translation by Google Translate, not legally binding) |
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| CN113307696A (en) * | 2021-05-18 | 2021-08-27 | 济南大学 | Method for preparing nitrogen-based fertilizer from furfuryl alcohol, formic acid and urea |
| CN113480374A (en) * | 2021-08-16 | 2021-10-08 | 青岛农业大学 | Water-retention slow-release compound fertilizer and preparation method thereof |
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