CN107793215A - A kind of production method of the slow release fertilizer coating material of biodegradable high water absorbing capacity - Google Patents
A kind of production method of the slow release fertilizer coating material of biodegradable high water absorbing capacity Download PDFInfo
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- CN107793215A CN107793215A CN201710958917.6A CN201710958917A CN107793215A CN 107793215 A CN107793215 A CN 107793215A CN 201710958917 A CN201710958917 A CN 201710958917A CN 107793215 A CN107793215 A CN 107793215A
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- slow release
- polysuccinimide
- release fertilizer
- absorbing capacity
- coating material
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/04—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonamides, polyesteramides or polyimides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Biological Depolymerization Polymers (AREA)
- Fertilizers (AREA)
Abstract
A kind of slow release fertilizer coating material of biodegradable high water absorbing capacity, it is characterised in that polysuccinimide introduces ethoxy first, obtains ethoxy polysuccinimide；Secondly ethoxy polysuccinimide reacts with acryloyl chloride, then is hydrolyzed in sodium hydrate aqueous solution, obtains modified polyaspartic acid；Then bentonite is purified, obtains purifying bentonite；Finally to purify bentonite as nexus, acrylic acid, acrylamide and modified polyaspartic acid are polymerize by crosslinking and semi-intercrossing network technology, obtain a kind of slow release fertilizer coating material of biodegradable high water absorbing capacity.The slow release fertilizer coating material of the biodegradable high water absorbing capacity of the present invention, has higher water retention property, biodegradable, can be increased soil moisture content while improving slow release fertilizer sustained release performance.
Description
Technical field
The invention belongs to fertilizer field, and in particular to a kind of slow release fertilizer coating material of biodegradable high water absorbing capacity
Production method.
Background technology
In recent years, the loss due to fertilizer and poorly efficient utilization, have had resulted in the serious wasting of resources and huge economy
Loss, it is often more important that serious pollution is caused to human body, air, soil and grain.Therefore, the utilization of fertilizer how is improved
Rate, the application of fertilizer is organically combined with the Yield and quality of crops and environmental protection, have become fertilizer research
The focus paid special attention in field.
Since the fifties in last century, the developed country such as American-European and Japan is successively from rational distribution fertilizer nutrient and science
Fertilizer practice turn to the development of long-acting sustained-controll-release fertiliser, make every effort to change the characteristic of fertilizer in itself to improve the utilization of fertilizer
Rate.In terms of the development of domestic and international sustained-controll-release fertiliser and application present situation, coating coating class sustained-controll-release fertiliser represents sustained-controll-release fertiliser
Developing direction.Flexibility and the stability of its nutrients release are not only due to, and more importantly it can realize fertilizer
Nutrients release, soil nutrient are supplied and plant nutrient absorption three is mutually coordinated and matches.Thus it is to improving utilization rate of fertilizer,
The administration quantity and number of fertilizer are reduced, mitigates pollution of the unreasonable fertilising to environment and agricultural product, realizes agriculture and environment
Sustainable development, the amphitypy society for building " resources conservation " and " environment-friendly " have very great practical significance.
Popularization and application sustained-controll-release fertiliser is wanted under conditions of China's agricultural decentralized management, must just develop to be applied to
Field crop, slow controlled-release effect be good while price cheap kind again.And the key for solving problem be exploitation function admirable, into
This cheap and environment amenable slow-release material.
The content of the invention
It is an object of the invention to provide a kind of slow release fertilizer coating of environment-friendly biodegradable high water absorbing capacity
The production method of material.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of slow release fertilizer coating material of biodegradable high water absorbing capacity, it is characterised in that polysuccinimide draws first
Enter ethoxy, obtain ethoxy polysuccinimide；Secondly ethoxy polysuccinimide reacts with acryloyl chloride, then in hydrogen-oxygen
Change and hydrolyzed in sodium water solution, obtain modified polyaspartic acid；Then bentonite is purified, obtains purifying bentonite；Finally with pure
Change bentonite is nexus, and acrylic acid, acrylamide and modified polyaspartic acid are polymerize by crosslinking and semi-intercrossing network technology,
Obtain a kind of slow release fertilizer coating material of biodegradable high water absorbing capacity.
The slow release fertilizer coating material of described biodegradable high water absorbing capacity, it is characterised in that it is by following steps
It is prepared：
（1）Polysuccinimide is added in DMF, at room temperature magnetic agitation 1.5-2h, it is fully dissolved, add ethanol
Amine, magnetic agitation 40-48h at room temperature, after reaction terminates, reaction mixture is dialysed 4-5d in deionized water, dialysis procedure
In, every 4-5h, a deionized water is changed, freeze-drying, obtains ethoxy polysuccinimide；
（2）By ethoxy polysuccinimide, triethylamine and DMF with 1：0.7-0.8：12-15 mass ratio, which is added to reaction, to be held
In device, 1.5-2h is stirred vigorously at room temperature so that ethoxy polysuccinimide is completely dissolved, and is transferred in ice-water bath, control
Temperature of reaction system is 0-4 DEG C, and the acryloyl chloride of 5-6 times of parts by weight is added dropwise, and after being added dropwise, continues magnetic agitation reaction
20-24h, filtering, filtrate are dialysed 3-4d in deionized water, in dialysis procedure, every 4-5h, change a deionized water, cold
It is lyophilized dry, obtain acryloyl-oxy ethylamino polysuccinimide；
（3）Acryloyl-oxy ethylamino polysuccinimide is added in the sodium hydrate aqueous solution of 15-18 times of parts by weight, room temperature
After lower magnetic agitation makes it fully dissolve, continue magnetic agitation hydrolysis 50-60min, reaction solution poured into absolute ethyl alcohol and precipitated,
Absolute ethyl alcohol washs 2-3 times, is dried in 50-60 DEG C of vacuum drying chamber, obtains modified polyaspartic acid；
（4）Bentonite is added in the deionized water of 18-20 times of parts by weight, fully stirred with 300-350r/min stir speed (S.S.)
80-100min is mixed, 50-60min is stood, takes upper strata suspension；Using hydrochloric acid solution regulation suspension pH to 5-6,60-65 DEG C
Temperature constant magnetic stirring 2-3h, 2-3h is stood, filtered, 80-90 DEG C of drying, obtain purifying bentonite；
（5）Acrylic acid is added in reaction vessel, under condition of ice bath, adds sodium hydrate aqueous solution to neutralization；In strength
Under stirring condition, acrylamide, purifying bentonite, ammonium persulfate and modified polyaspartic acid are sequentially added, is mixed evenly
Afterwards, lead to nitrogen, slowly raise temperature to 70-75 DEG C, temperature constant magnetic stirring 4-6h, discharge while hot, obtain polymer, by polymer
Shred, dried in 70-80 DEG C of thermostatic drying chamber, pulverize, obtain the slow release fertilizer coating of biodegradable high water absorbing capacity
Material.
The production method of the slow release fertilizer coating material of described biodegradable high water absorbing capacity, it is characterised in that step
Suddenly（1）Middle polysuccinimide, DMF, the mass ratio of monoethanolamine are 1：12-15：5-6.
The production method of the slow release fertilizer coating material of described biodegradable high water absorbing capacity, it is characterised in that institute
The DMF stated has to pass through drying process using preceding.
The production method of the slow release fertilizer coating material of described biodegradable high water absorbing capacity, it is characterised in that step
Suddenly（4）The concentration of middle hydrochloric acid solution is 0.1-0.15mol/L.
The production method of the slow release fertilizer coating material of described biodegradable high water absorbing capacity, it is characterised in that step
Suddenly（5）In the concentration of sodium hydrate aqueous solution be 0.01-0.02mol/L.
The production method of the slow release fertilizer coating material of described biodegradable high water absorbing capacity, it is characterised in that step
Suddenly（5）Middle acrylic acid, acrylamide, purifying bentonite, the mass ratio of ammonium persulfate and modified polyaspartic acid are 1：0.3-
0.32：0.25-0.28：0.005-0.006：0.06-0.08.
Beneficial effects of the present invention are：
Present invention polysuccinimide first introduces ethoxy, obtains ethoxy polysuccinimide；Secondly the poly- amber of ethoxy
Acid imide reacts with acryloyl chloride, then is hydrolyzed in sodium hydrate aqueous solution, obtains modified polyaspartic acid；Then by bentonite
Purifying, obtain purifying bentonite；Finally to purify bentonite as nexus, acrylic acid, acrylamide and modified polyaspartic acid
It is polymerize by crosslinking and semi-intercrossing network technology, obtains a kind of slow release fertilizer coating material of biodegradable high water absorbing capacity.
The coated fertilizer of the present invention has spacial framework, and this space net structure is made up of polyelectrolyte, and in high score
Very strong affinity between sub- electrolyte and water be present, simultaneously as high concentration inside coated fertilizer be present may move ion, because
This, produces osmotic pressure inside coated fertilizer, and under the affinity and the collective effect of osmotic pressure, substantial amounts of water can be inhaled
Receive inside coated fertilizer, therefore, coated fertilizer of the invention has good water absorption character；And prepared with this coated fertilizer
Slow release fertilizer, substantial amounts of moisture can be provided after fertilising for plant.Poly-aspartate and its derivative, urea can be suppressed
Nitrification and aminating reaction and reduce the loss of nitrogen, so as to improve the utilization rate of nutrient in slow release fertilizer；And there is class
The backbone of protein is similar to, thus there is good biological degradability and excellent biocompatibility, can be improved at present
The problem of slow release fertilizer coating material degradation poor performance.The slow release fertilizer coating material of the biodegradable high water absorbing capacity of the present invention
Material, has higher water retention property, biodegradable, and can improve soil moisture while improving slow release fertilizer sustained release performance contains
Amount.
Embodiment
The slow release fertilizer coating material of the biodegradable high water absorbing capacity of the present embodiment, its by following steps prepare and
Into：
（1）Polysuccinimide is added in DMF, at room temperature magnetic agitation 2h, it is fully dissolved, add monoethanolamine, room
The lower magnetic agitation 48h of temperature, after reaction terminates, reaction mixture is dialysed in deionized water 5d, in dialysis procedure, every 5h,
A deionized water is changed, freeze-drying, obtains ethoxy polysuccinimide；
（2）By ethoxy polysuccinimide, triethylamine and DMF with 1：0.75：15 mass ratio is added in reaction vessel, room
2h is stirred vigorously under temperature so that ethoxy polysuccinimide is completely dissolved, and is transferred in ice-water bath, controls temperature of reaction system
For 0 DEG C, the acryloyl chloride of 6 times of parts by weight is added dropwise, after being added dropwise, continues magnetic agitation reaction 24h, filtering, filtrate exists
Dialyse 4d in deionized water, in dialysis procedure, every 5h, changes a deionized water, freeze-drying, obtains acryloyl-oxy second ammonia
Base polysuccinimide；
（3）Acryloyl-oxy ethylamino polysuccinimide is added in the sodium hydrate aqueous solution of 18 times of parts by weight, at room temperature
After magnetic agitation makes it fully dissolve, continue magnetic agitation hydrolysis 60min, reaction solution is poured into absolute ethyl alcohol and precipitated, it is anhydrous
Ethanol washs 3 times, is dried in 60 DEG C of vacuum drying chambers, obtains modified polyaspartic acid；
（4）Bentonite is added in the deionized water of 20 times of parts by weight, be sufficiently stirred with 300r/min stir speed (S.S.)
100min, 60min is stood, takes upper strata suspension；Using the pH to 5 of hydrochloric acid solution regulation suspension, 65 DEG C of temperature constant magnetic stirrings
2h, 3h is stood, filtered, 90 DEG C of drying, obtain purifying bentonite；
（5）Acrylic acid is added in reaction vessel, under condition of ice bath, adds sodium hydrate aqueous solution to neutralization；In strength
Under stirring condition, acrylamide, purifying bentonite, ammonium persulfate and modified polyaspartic acid are sequentially added, is mixed evenly
Afterwards, lead to nitrogen, slowly raise temperature to 75 DEG C, temperature constant magnetic stirring 6h, discharge while hot, obtain polymer, polymer is shredded,
Dried in 80 DEG C of thermostatic drying chambers, pulverize, obtain the slow release fertilizer coating material of biodegradable high water absorbing capacity.
The step of the present embodiment（1）Middle polysuccinimide, DMF, the mass ratio of monoethanolamine are 1：15：6.
The DMF of the present embodiment has to pass through drying process using preceding.
The step of the present embodiment（4）The concentration of middle hydrochloric acid solution is 0.1mol/L.
The step of the present embodiment（5）In the concentration of sodium hydrate aqueous solution be 0.01mol/L.
The step of the present embodiment（5）Middle acrylic acid, acrylamide, purifying bentonite, ammonium persulfate and modified poly- asparagus fern ammonia
The mass ratio of acid is 1：0.32：0.28：0.006：0.08.
Claims (7)
- A kind of 1. slow release fertilizer coating material of biodegradable high water absorbing capacity, it is characterised in that polysuccinimide first Ethoxy is introduced, obtains ethoxy polysuccinimide；Secondly ethoxy polysuccinimide reacts with acryloyl chloride, then in hydrogen Hydrolyzed in aqueous solution of sodium oxide, obtain modified polyaspartic acid；Then bentonite is purified, obtains purifying bentonite；Finally with Purifying bentonite is nexus, and acrylic acid, acrylamide and modified polyaspartic acid are gathered by crosslinking and semi-intercrossing network technology Close, obtain a kind of slow release fertilizer coating material of biodegradable high water absorbing capacity.
- 2. the slow release fertilizer coating material of the biodegradable high water absorbing capacity according to claims 1, it is characterised in that It is prepared by following steps：（1）Polysuccinimide is added in DMF, at room temperature magnetic agitation 1.5-2h, it is fully dissolved, add ethanol Amine, magnetic agitation 40-48h at room temperature, after reaction terminates, reaction mixture is dialysed 4-5d in deionized water, dialysis procedure In, every 4-5h, a deionized water is changed, freeze-drying, obtains ethoxy polysuccinimide；（2）By ethoxy polysuccinimide, triethylamine and DMF with 1：0.7-0.8：12-15 mass ratio, which is added to reaction, to be held In device, 1.5-2h is stirred vigorously at room temperature so that ethoxy polysuccinimide is completely dissolved, and is transferred in ice-water bath, control Temperature of reaction system is 0-4 DEG C, and the acryloyl chloride of 5-6 times of parts by weight is added dropwise, and after being added dropwise, continues magnetic agitation reaction 20-24h, filtering, filtrate are dialysed 3-4d in deionized water, in dialysis procedure, every 4-5h, change a deionized water, cold It is lyophilized dry, obtain acryloyl-oxy ethylamino polysuccinimide；（3）Acryloyl-oxy ethylamino polysuccinimide is added in the sodium hydrate aqueous solution of 15-18 times of parts by weight, room temperature After lower magnetic agitation makes it fully dissolve, continue magnetic agitation hydrolysis 50-60min, reaction solution poured into absolute ethyl alcohol and precipitated, Absolute ethyl alcohol washs 2-3 times, is dried in 50-60 DEG C of vacuum drying chamber, obtains modified polyaspartic acid；（4）Bentonite is added in the deionized water of 18-20 times of parts by weight, fully stirred with 300-350r/min stir speed (S.S.) 80-100min is mixed, 50-60min is stood, takes upper strata suspension；Using hydrochloric acid solution regulation suspension pH to 5-6,60-65 DEG C Temperature constant magnetic stirring 2-3h, 2-3h is stood, filtered, 80-90 DEG C of drying, obtain purifying bentonite；（5）Acrylic acid is added in reaction vessel, under condition of ice bath, adds sodium hydrate aqueous solution to neutralization；In strength Under stirring condition, acrylamide, purifying bentonite, ammonium persulfate and modified polyaspartic acid are sequentially added, is mixed evenly Afterwards, lead to nitrogen, slowly raise temperature to 70-75 DEG C, temperature constant magnetic stirring 4-6h, discharge while hot, obtain polymer, by polymer Shred, dried in 70-80 DEG C of thermostatic drying chamber, pulverize, obtain the slow release fertilizer coating of biodegradable high water absorbing capacity Material.
- 3. the production method of the slow release fertilizer coating material of the biodegradable high water absorbing capacity according to claims 2, Characterized in that, step（1）Middle polysuccinimide, DMF, the mass ratio of monoethanolamine are 1：12-15：5-6.
- 4. the production method of the slow release fertilizer coating material of the biodegradable high water absorbing capacity according to claims 2, Characterized in that, described DMF has to pass through drying process using preceding.
- 5. the production method of the slow release fertilizer coating material of the biodegradable high water absorbing capacity according to claims 2, Characterized in that, step（4）The concentration of middle hydrochloric acid solution is 0.1-0.15mol/L.
- 6. the production method of the slow release fertilizer coating material of the biodegradable high water absorbing capacity according to claims 2, Characterized in that, step（5）In the concentration of sodium hydrate aqueous solution be 0.01-0.02mol/L.
- 7. the production method of the slow release fertilizer coating material of the biodegradable high water absorbing capacity according to claims 2, Characterized in that, step（5）Middle acrylic acid, acrylamide, the quality for purifying bentonite, ammonium persulfate and modified polyaspartic acid Than for 1：0.3-0.32：0.25-0.28：0.005-0.006：0.06-0.08.
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Cited By (2)
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|---|---|---|---|---|
| CN114538995A (en) * | 2022-01-27 | 2022-05-27 | 青岛农业大学 | Nitrogen fertilizer synergist, preparation method and application |
| CN114713618A (en) * | 2022-06-08 | 2022-07-08 | 河北协同化学有限公司 | Phytoremediation promoter for treating heavy metal pollution based on phytoremediation technology |
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| CN114538995A (en) * | 2022-01-27 | 2022-05-27 | 青岛农业大学 | Nitrogen fertilizer synergist, preparation method and application |
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| CN114713618A (en) * | 2022-06-08 | 2022-07-08 | 河北协同化学有限公司 | Phytoremediation promoter for treating heavy metal pollution based on phytoremediation technology |
| CN114713618B (en) * | 2022-06-08 | 2022-08-23 | 河北协同化学有限公司 | Phytoremediation promoter for treating heavy metal pollution based on phytoremediation technology |
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Application publication date: 20180313 |