CN108033863A - A kind of poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release nitrogenous fertilizer and preparation method thereof - Google Patents
A kind of poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release nitrogenous fertilizer and preparation method thereof Download PDFInfo
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- CN108033863A CN108033863A CN201711178856.8A CN201711178856A CN108033863A CN 108033863 A CN108033863 A CN 108033863A CN 201711178856 A CN201711178856 A CN 201711178856A CN 108033863 A CN108033863 A CN 108033863A
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- sodium alginate
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- isopropyl acrylamide
- fertilizer
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
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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
- C05G5/00—Fertilisers characterised by their form
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
- C05G5/37—Layered or coated, e.g. dust-preventing coatings layered or coated with a polymer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- General Health & Medical Sciences (AREA)
- Soil Sciences (AREA)
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- Engineering & Computer Science (AREA)
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- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a kind of poly- N N-isopropylacrylamides sodium alginate double-coating temperature sensitive sustained-release nitrogenous fertilizer, its preparation is first oxidant using sodium metaperiodate, sodium alginate oxidation processes are obtained into oxidized sodium alginate, using it as base material, urea is coated, sodium alginate cladding urea prills is obtained, then synthesizes the poly- N isopropyl acrylamide microgels of temperature sensing polymer, as Thermo-sensitive coated fertilizer, temperature sensitive sustained-release nitrogenous fertilizer is prepared through fluidized bed spray granulation.The present invention introduces temperature sensitive polymer on sodium alginate cladding urea prills surface, realize and the double-layer sustained release of nitrogenous fertilizer is coated, reach the effect of fertilizer conservation, reduce the loss and waste to fertilizer, and the sodium alginate through aldehyde radical need not be i.e. degradable under the specific conditions such as certain enzyme, avoids the problem that causing secondary pollution.
Description
Technical field
The present invention relates to a kind of slow-release fertilizer field, and in particular to a kind of poly-N-isopropyl acrylamide-sodium alginate is double-deck
Coat temperature sensitive sustained-release nitrogenous fertilizer and preparation method thereof.
Background technology
Coated control release fertilizer is Controlled Release Fertilizer kind main at present, and mainly using granular chemical fertilizer as core, top layer coats one layer
The inorganic substances or organic polymer of low aqueous solubility, change the stripping property of chemical fertilizer nutrient, extend or control fertilizer nutrient discharges.So
And existing coated control release fertilizer, there are of high cost, coated fertilizer difficult degradation, being manured into soil easily causes the shortcoming such as secondary pollution, because
This, find efficiently, cheap, environmental protection coated fertilizer is to develop coating controlled-release fertilizer be one of developing direction of current new-type fertilizer.
Coated fertilizer does not react usually with chemical fertilizer, by selecting different coated fertilizers, can obtain difference
Release performance, suitable for wider array of agricultural environment.But the sustained release of the degraded and fertilizer due to coated fertilizer, one season crop
Fertilizer may not released still after maturation, may result in the waste of fertilizer.So just have must for the development of temperature sensitive type coated fertilizer
It has been wanted that, different according to temperature in four seasons, fertilizer is normally discharged in high temperature season, is conducive to plant in growth period, maturity period to fertilizer
Absorption, it is and few in the winter time or reduce release, when the relatively-high temperature season of second year continues to be sustained, reach the effect of fertilizer conservation
Fruit, which reduces the loss and waste of fertilizer, decreases the cost of labor of multiple top dressing.
Sodium alginate (SA) has good biocompatibility, has nonpoisonous and tasteless characteristic, good biological degradability
With bio-compatible, stability, film forming, and certain toughness, intensity and bioadhesive.Sodium alginate can be with demagging, mercury
Ionic displacement reaction generation alginate hydrogel, but the drop of ionomer type SA gels occur for bivalent metal ion in addition
It is higher to solve product relative molecular mass, and bivalent positive ion is easily lost in, thus gel degradation is difficult to control, and its aldehyde radical
Product is then more degradable.
Fan Lihong, Pan Xiaoran et al. are at it《The preparation of hydroxypropyl chitosan/oxidized sodium alginate hydrogel and characterization》One
Wen Zhong, oxidized sodium alginate is made by sodium alginate through sodium periodate oxidation, utilizes the ammonia on its aldehyde radical and hydroxypropyl chitosan
Hydrogel that can be in-situ cross-linked is prepared in base crosslinking.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of poly-N-isopropyl acrylamide-sodium alginate double-coating
Temperature sensitive sustained-release nitrogenous fertilizer and preparation method thereof.
A kind of poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release nitrogenous fertilizer, it is prepared first using height
Sodium iodate is oxidant, and sodium alginate oxidation processes are obtained oxidized sodium alginate, using it as base material, urea is coated,
Sodium alginate cladding urea prills are obtained, then synthesize temperature sensing polymer poly-N-isopropyl acrylamide microgel, as
Thermo-sensitive coated fertilizer, temperature sensitive sustained-release nitrogenous fertilizer is prepared through fluidized bed spray granulation.
Comprise the following steps that：
（1）The oxidation processes of sodium alginate：
40-60 parts by weight sodium alginates are dissolved in distilled water, 110-130 parts of ethanol is added and 100-110 parts of sodium metaperiodates is molten
Liquid, when 25-35 DEG C of lucifuge reaction 5-8 is small, product is washed repeatedly after suction filtration with the mixed solution of water and ethanol, is aoxidized
Sodium alginate；
（2）Above-mentioned oxidized sodium alginate is dissolved in the oxidized sodium alginate aqueous solution that distilled water is configured to 2%, by 45-65 parts of urea
It is added in sodium alginate aqueous solution, stirring is uniformly mixed it, and oxidized sodium alginate-urea mixed solution then is transferred to perseverance
To press in dropping funel, uniform speed slow is added dropwise in the calcium chloride water that concentration is 10%, and stirring cures 10-15 minutes, filtering,
25-35 DEG C of vacuum drying is placed in, obtains sodium alginate cladding urea prills；
（3）Poly-N-isopropyl acrylamide microgel synthesizes：
Weigh 60-80 parts of n-isopropyl acrylamide and 2-5 parts of N,N methylene bis acrylamides add equipped with mechanical agitation and
In the reaction bulb of condensation reflux unit, 1-4 parts of dodecyl sodium sulfates and 90-160 parts of distilled water are added, control bath temperature liter
Temperature treats that each component fully dissolves nitrogen charging gas bell 10-20 minutes in backward reaction solution, the dissolving in removing system to 35-45 DEG C
Oxygen, is warming up to 65-75 DEG C, adds 10-20 parts of ammonium persulfate aqueous solutions, when stirred under nitrogen atmosphere reaction 5-7 is small, natural cooling
To room temperature, be transferred in bag filter dialysis 48 it is small when, a deionized water is replaced when 8 is small, is configured to after the completion of dialysis
10% poly-N-isopropyl acrylamide microgel dispersion liquid is spare；
（4）The preparation of slow-release nitrogen fertilizer：
By step（2）Sodium alginate cladding urea prills add fluidized bed spray granulation machine in, adjustings fluidizing gas velocity be 1.5m/s,
Fluidized-bed layer temperature is 60 DEG C, atomization air pressure 0.3MPa, by step（3）Poly-N-isopropyl acrylamide microgel disperses
Urea surface is uniformly sprayed at after liquid mist, after fluidized drying is handled 25-35 minutes, obtains temperature sensitive sustained-release nitrogenous fertilizer.
Wherein, the step（1）The volume ratio of the mixed solution of middle water and ethanol is 1:1.
Wherein, the step（1）The concentration of meso-periodic acid sodium solution is 0.4mol/L.
Wherein, the step（3）Middle ammonium persulfate aqueous solution concentration is 8%, matching while using.
Compared with prior art, the present invention has the following advantages：
（1）The present invention uses sodium periodate oxidation sodium alginate, obtains the oxidized sodium alginate with dialdehyde based structures, can replace
The crosslinking agents such as common formaldehyde, glutaraldehyde, it is nontoxic to soil environment, then made with the calcium cross-linked oxidized sodium alginate of chlorination
For shell, urea is tentatively coated, utilizes the amide groups in aldehyde groups, with poly-N-isopropyl acrylamide molecule afterwards
Group crosslinks reaction, and dehydration forms schiff bases, and temperature sensitive polymer, realization pair are introduced on sodium alginate cladding urea prills surface
The double-layer sustained release cladding of nitrogenous fertilizer, reaches the effect of fertilizer conservation, reduces the loss and waste to fertilizer, and the sodium alginate through aldehyde radical
Need not be i.e. degradable under the specific conditions such as certain enzyme, avoid the problem that causing secondary pollution.
（2）Existing hydrophilic radical in poly-N-isopropyl acrylamide molecule of the present invention（Amide group）There is hydrophobic grouping again
（Isopropyl group）, this special molecular structure cause poly-N-isopropyl acrylamide aqueous solution 31 DEG C -33 DEG C nearby deposit
In the transformation of hydrophilic/hydrophobic, so as to fulfill the long-acting release to nitrogenous fertilizer, in addition in the form of core/shell structure, by sodium alginate
It is crosslinked and combines with poly-N-isopropyl acrylamide microgel, under conditions of its original Thermo-sensitive is not changed, possesses more excellent
Biocompatibility and degradation capability.
Embodiment
A kind of poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release nitrogenous fertilizer, it is prepared first using height
Sodium iodate is oxidant, and sodium alginate oxidation processes are obtained oxidized sodium alginate, using it as base material, urea is coated,
Sodium alginate cladding urea prills are obtained, then synthesize temperature sensing polymer poly-N-isopropyl acrylamide microgel, as
Thermo-sensitive coated fertilizer, temperature sensitive sustained-release nitrogenous fertilizer is prepared through fluidized bed spray granulation.
Comprise the following steps that：
（1）The oxidation processes of sodium alginate：
50 parts by weight sodium alginates are dissolved in distilled water, 120 parts of ethanol and 100 parts of sodium periodate solutions is added, is kept away in 30 DEG C
When light reaction 6 is small, product is washed repeatedly after suction filtration with the mixed solution of water and ethanol, obtains oxidized sodium alginate；
（2）Above-mentioned oxidized sodium alginate is dissolved in the oxidized sodium alginate aqueous solution that distilled water is configured to 2%, 55 parts of urea are added
Enter into sodium alginate aqueous solution, stirring is uniformly mixed it, and oxidized sodium alginate-urea mixed solution then is transferred to constant pressure
In dropping funel, uniform speed slow is added dropwise in the calcium chloride water that concentration is 10%, and stirring cures 10 minutes, and filtering, is placed in 30
DEG C vacuum drying, obtain sodium alginate cladding urea prills；
（3）Poly-N-isopropyl acrylamide microgel synthesizes：
Weigh 70 parts of n-isopropyl acrylamide and 4 parts of N,N methylene bis acrylamides are added equipped with mechanical agitation and are condensed back to
In the reaction bulb for flowing device, 3 parts of dodecyl sodium sulfates and 120 parts of distilled water are added, control bath temperature is warming up to 40 DEG C, treats
Each component fully dissolves nitrogen charging gas bell 15 minutes in backward reaction solution, and the dissolved oxygen in removing system, is warming up to 70 DEG C, adds
15 parts of ammonium persulfate aqueous solutions, when stirred under nitrogen atmosphere reaction 6 is small, after cooled to room temperature, are transferred in bag filter thoroughly
Analyse 48 it is small when, a deionized water is replaced when 8 is small, be configured to after the completion of dialysis 10% poly-N-isopropyl acrylamide it is micro-
Gel dispersion liquid is spare；
（4）The preparation of slow-release nitrogen fertilizer：
By step（2）Sodium alginate cladding urea prills add fluidized bed spray granulation machine in, adjustings fluidizing gas velocity be 1.5m/s,
Fluidized-bed layer temperature is 60 DEG C, atomization air pressure 0.3MPa, by step（3）Poly-N-isopropyl acrylamide microgel disperses
Urea surface is uniformly sprayed at after liquid mist, after fluidized drying is handled 30 minutes, obtains temperature sensitive sustained-release nitrogenous fertilizer.
Wherein, the step（1）The volume ratio of the mixed solution of middle water and ethanol is 1:1.
Wherein, the step（1）The concentration of meso-periodic acid sodium solution is 0.4mol/L.
Wherein, the step（3）Middle ammonium persulfate aqueous solution concentration is 8%, matching while using.
Claims (5)
1. a kind of poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release nitrogenous fertilizer, it is characterised in that it is prepared
The use of sodium metaperiodate is first oxidant, sodium alginate oxidation processes is obtained into oxidized sodium alginate, using it as base material, to urea into
Row cladding, obtains sodium alginate cladding urea prills, then synthesizes temperature sensing polymer poly-N-isopropyl acrylamide microgel,
As Thermo-sensitive coated fertilizer, temperature sensitive sustained-release nitrogenous fertilizer is prepared through fluidized bed spray granulation.
A kind of 2. poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release according to claims 1
The preparation method of nitrogenous fertilizer, it is characterised in that comprise the following steps that：
（1）The oxidation processes of sodium alginate：
40-60 parts by weight sodium alginates are dissolved in distilled water, 110-130 parts of ethanol is added and 100-110 parts of sodium metaperiodates is molten
Liquid, when 25-35 DEG C of lucifuge reaction 5-8 is small, product is washed repeatedly after suction filtration with the mixed solution of water and ethanol, is aoxidized
Sodium alginate；
（2）Above-mentioned oxidized sodium alginate is dissolved in the oxidized sodium alginate aqueous solution that distilled water is configured to 2%, by 45-65 parts of urea
It is added in sodium alginate aqueous solution, stirring is uniformly mixed it, and oxidized sodium alginate-urea mixed solution then is transferred to perseverance
To press in dropping funel, uniform speed slow is added dropwise in the calcium chloride water that concentration is 10%, and stirring cures 10-15 minutes, filtering,
25-35 DEG C of vacuum drying is placed in, obtains sodium alginate cladding urea prills；
（3）Poly-N-isopropyl acrylamide microgel synthesizes：
Weigh 60-80 parts of n-isopropyl acrylamide and 2-5 parts of N,N methylene bis acrylamides add equipped with mechanical agitation and
In the reaction bulb of condensation reflux unit, 1-4 parts of dodecyl sodium sulfates and 90-160 parts of distilled water are added, control bath temperature liter
Temperature treats that each component fully dissolves nitrogen charging gas bell 10-20 minutes in backward reaction solution, the dissolving in removing system to 35-45 DEG C
Oxygen, is warming up to 65-75 DEG C, adds 10-20 parts of ammonium persulfate aqueous solutions, when stirred under nitrogen atmosphere reaction 5-7 is small, natural cooling
To room temperature, be transferred in bag filter dialysis 48 it is small when, a deionized water is replaced when 8 is small, is configured to after the completion of dialysis
10% poly-N-isopropyl acrylamide microgel dispersion liquid is spare；
（4）The preparation of slow-release nitrogen fertilizer：
By step（2）Sodium alginate cladding urea prills add fluidized bed spray granulation machine in, adjustings fluidizing gas velocity be 1.5m/s,
Fluidized-bed layer temperature is 60 DEG C, atomization air pressure 0.3MPa, by step（3）Poly-N-isopropyl acrylamide microgel disperses
Urea surface is uniformly sprayed at after liquid mist, after fluidized drying is handled 25-35 minutes, obtains temperature sensitive sustained-release nitrogenous fertilizer.
A kind of 3. poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release according to claims 2
The preparation method of nitrogenous fertilizer, it is characterised in that the step（1）The volume ratio of the mixed solution of middle water and ethanol is 1:1.
A kind of 4. poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release according to claims 2
The preparation method of nitrogenous fertilizer, it is characterised in that the step（1）The concentration of meso-periodic acid sodium solution is 0.4mol/L.
A kind of 5. poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release according to claims 2
The preparation method of nitrogenous fertilizer, it is characterised in that the step（3）Middle ammonium persulfate aqueous solution concentration is 8%, matching while using.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711178856.8A CN108033863A (en) | 2017-11-23 | 2017-11-23 | A kind of poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release nitrogenous fertilizer and preparation method thereof |
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| CN201711178856.8A CN108033863A (en) | 2017-11-23 | 2017-11-23 | A kind of poly-N-isopropyl acrylamide-sodium alginate double-coating temperature sensitive sustained-release nitrogenous fertilizer and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108863629A (en) * | 2018-10-08 | 2018-11-23 | 浙江世佳科技有限公司 | A kind of preparation method of wheat bio-bacterial manure capsule and pill |
| CN109896895A (en) * | 2019-04-03 | 2019-06-18 | 合肥工业大学 | A kind of preparation method of temperature control sustained-release nitrogenous fertilizer |
| CN110200946A (en) * | 2019-06-26 | 2019-09-06 | 华南理工大学 | A kind of temperature sensitive and pH sensibility drug bearing microsphere and its preparation method and application |
| CN111187367A (en) * | 2020-01-07 | 2020-05-22 | 江苏省农业科学院 | Urea formaldehyde modified sodium alginate copolymer and application thereof |
| CN111410717A (en) * | 2020-04-20 | 2020-07-14 | 青岛农业大学 | Temperature-sensitive material, bactericide, preparation method and application thereof |
| CN113135793A (en) * | 2021-04-29 | 2021-07-20 | 中国热带农业科学院南亚热带作物研究所 | Temperature-responsive coated controlled-release fertilizer and preparation method thereof |
-
2017
- 2017-11-23 CN CN201711178856.8A patent/CN108033863A/en not_active Withdrawn
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108863629A (en) * | 2018-10-08 | 2018-11-23 | 浙江世佳科技有限公司 | A kind of preparation method of wheat bio-bacterial manure capsule and pill |
| CN108863629B (en) * | 2018-10-08 | 2021-07-20 | 浙江世佳科技股份有限公司 | Preparation method of biological bacterial manure capsules for wheat |
| CN109896895A (en) * | 2019-04-03 | 2019-06-18 | 合肥工业大学 | A kind of preparation method of temperature control sustained-release nitrogenous fertilizer |
| CN110200946A (en) * | 2019-06-26 | 2019-09-06 | 华南理工大学 | A kind of temperature sensitive and pH sensibility drug bearing microsphere and its preparation method and application |
| CN110200946B (en) * | 2019-06-26 | 2021-09-21 | 华南理工大学 | Temperature-sensitive and pH-sensitive drug-loaded microsphere as well as preparation method and application thereof |
| CN111187367A (en) * | 2020-01-07 | 2020-05-22 | 江苏省农业科学院 | Urea formaldehyde modified sodium alginate copolymer and application thereof |
| CN111187367B (en) * | 2020-01-07 | 2022-02-25 | 江苏省农业科学院 | Urea formaldehyde modified sodium alginate copolymer and application thereof |
| CN111410717A (en) * | 2020-04-20 | 2020-07-14 | 青岛农业大学 | Temperature-sensitive material, bactericide, preparation method and application thereof |
| CN111410717B (en) * | 2020-04-20 | 2022-05-10 | 青岛农业大学 | Temperature-sensitive material, bactericide, preparation method and application thereof |
| CN113135793A (en) * | 2021-04-29 | 2021-07-20 | 中国热带农业科学院南亚热带作物研究所 | Temperature-responsive coated controlled-release fertilizer and preparation method thereof |
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