CN110272314A - A method of preparing cladded type stalk fibre based water-holding slow-release fertilizer - Google Patents

A method of preparing cladded type stalk fibre based water-holding slow-release fertilizer Download PDF

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Publication number
CN110272314A
CN110272314A CN201910525676.5A CN201910525676A CN110272314A CN 110272314 A CN110272314 A CN 110272314A CN 201910525676 A CN201910525676 A CN 201910525676A CN 110272314 A CN110272314 A CN 110272314A
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fertilizer
cladded type
based water
stalk fibre
fibre based
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王惟帅
杨世琦
邢磊
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Institute of Environment and Sustainable Development in Agriculturem of CAAS
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Institute of Environment and Sustainable Development in Agriculturem of CAAS
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B7/00Fertilisers based essentially on alkali or ammonium orthophosphates
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C9/00Fertilisers containing urea or urea compounds
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/80Soil conditioners
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G5/00Fertilisers characterised by their form
    • C05G5/30Layered or coated, e.g. dust-preventing coatings
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F251/00Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
    • C08F251/02Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F261/00Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
    • C08F261/02Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
    • C08F261/04Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Soil Sciences (AREA)
  • Fertilizers (AREA)

Abstract

The invention discloses a kind of methods for preparing cladded type stalk fibre based water-holding slow-release fertilizer, this method is using stalk cellulose polysaccharide chain as skeleton, it is grafted to acrylic acid and its acrylamide substance generated with urea reaction in cellulosic backbone, three-dimensional net structure polymer is formed by cross-linking agents again, interpenetrating is carried out with polyvinyl alcohol simultaneously, form the super absorbent resin of half interpenetrating network structure, it is wrapped in outside fertiliser granulates again, and with polyvinyl alcohol, sodium alginate and carboxymethyl cellulose mixed liquid crosslinking film forming are coated on outermost layer, obtain cladded type stalk fibre based water-holding slow-release fertilizer.The present invention has good mechanical performance, water imbibition and the slow release effect excellent to fertilizer, reduces nutrient loss, improves the utilization rate of fertilizer, reduces the maintenance cost in later period farmland, improves the yield and quality of crops.The present invention has operating method simplicity, at low cost, improves the added value of stalk application, has also expanded the new approaches that stalk resource utilizes.

Description

A method of preparing cladded type stalk fibre based water-holding slow-release fertilizer
Technical field
The present invention relates to field of material engineering technology, prepare cladded type stalk fibre based water-holding slow-release in particular to a kind of The method of fertilizer.
Background technique
Agricultural crop straw is a kind of natural polymer resources along with the uninterrupted output of agricultural production of enormous amount.I State is a large agricultural country, and the stalk scale of construction is huge, and annual output is up to more than 900,000,000 tons, but stalk resource comprehensive utilization ratio is still relatively low, It how to be rationally the important content and Current resource of current environment green technology using the stalk cellulose resource of reproducibility One of the emphasis of exploitation and the work of ecological environmental protection area research.On the other hand, a large amount of to use in China's agricultural production process Nitrogenous fertilizer and phosphate fertilizer and utilization rate is too low, cause it to be largely lost to except farmland, and excessive ammonium salt and phosphatic discharge will cause Water body serious eutrophication destroys aquatic ecological balance, endangers human health.The holding capabilities for how enhancing nitrogen, phosphorus, improve it Farmland utilization rate is always the major issue of environment protection field.Cellulose is rich in agricultural crop straw, with environmental-friendly, easy The characteristics such as degradation, therefore have a good application prospect as slow-release fertilizer carrier material.
Carrier slow release fertilizer is fertilizer nutrient to be uniformly dispersed or is adsorbed in certain specific function material, fertilizer nutrient It is gradually released in the degradation process of functional material, can be improved utilization rate of fertilizer, keeps moisture, the abundant hair in soil Effect of the fertilizer to plant is waved, is of great immediate significance to China's agricultural sustainable development.
Currently, research hotspot is had become about carrier slow release fertilizer, as Chinese invention patent CN201510796178.6 is public The preparation method for having opened a kind of environment-friendly type slow release fertilizer coated fertilizer, by modified starch be added to natural gum it is clear in and quickly mix It is even, it adds crosslinking agent and short-chain amylose activator is reacted to obtain the clear lotion of grafting modified of starch natural gum, as environment Friendly slow-release fertilizer coating materials;It is slow that Chinese invention patent CN201210090405.X discloses a kind of novel polysaccharide gel water conservation Fertilizer is released, constructs slow-releasing system in chemical fertilizer granule table with polymer three-dimensional gel networks that pure natural plant polyose is formed Face is wrapped to form coated water-retaining sustained-release layer;It is slow that Chinese invention patent CN201810755569.7 discloses a kind of carboxymethyl cellulose The preparation method for releasing fertile coated fertilizer, using carboxymethyl cellulose as raw material, borax is crosslinking agent, using ammonium chloride as reaction system Acid regulator be prepared for carboxymethyl cellulose slow-release fertilizer coating materials using glycerol as plasticizer, utilize borax be crosslinked carboxylic first Hydroxyl on base cellulose molecular chain while consuming part of hydroxyl, makes structural network become closely, also to mention its hydrophobicity It is high.Patent of invention CN201410656766.5 discloses a kind of preparation method of the fertilizer of water-soluble degradation material cladding, will It is scattered in chloroform after the mixing of poly- (α-malic acid), polyethylene glycol, heating stirring adds 1- ethyl-(3- dimethylamino Propyl) carbodiimide hydrochloride, reacts while stirring, obtains concentrate;Concentrate is added to petroleum ether, leaching sediment, It is rinsed with water sediment, then after being dried, obtains basis material;Urea, ammonium phosphate, ammonium sulfate are dispersed in water, then risen Starch is added in Wen Hou, and after mixing evenly, after cooling, the solids of precipitation is filtered out, obtains the fertilizer crystal of starch cladding;It will The fertilizer crystal that basis material, starch coat is mixed with water, then the aqueous solution being configured to by cyclodextrin is added dropwise while stirring, is added dropwise After, ultrasonic reaction is carried out, after reaction, stands the fertilizer coated to get degradation material.Although prepared by the above method Sustained-controll-release fertiliser have effective time long to a certain extent, utilization rate is high, and nutrient loss is few and advantages of environment protection, but Above method preparation cost is high, preparation-obtained slow-release fertilizer bad mechanical strength and easily generation fertilizer phenomenon of burst release, water retention property Practical agricultural production needs are not met by with slow release effect.
Summary of the invention
In view of the above shortcomings of the prior art, cladded type stalk fibre base is prepared the object of the present invention is to provide a kind of The method of the fertilizer of retaining water and releasing nutrients slowly, solve high existing carrier slow release fertilizer preparation cost, bad mechanical strength and easily occur fertilizer burst release, The problems such as water retention property and ineffective sustained release, while also solving the wasting of resources of straw refuse and asking for environmental pollution Topic.
In order to solve the above-mentioned technical problem, present invention employs the following technical solutions: a kind of to prepare cladded type stalk fibre The method of Wiki the fertilizer of retaining water and releasing nutrients slowly, comprising the following steps:
1) extraction of cellulose: stalk powder will be obtained after straw drying, removal of impurities, crushing, then to the straw Dilute acid soln is added in stalk powder, then heating stirring is sufficiently extracted, and is cooled to room temperature, then through suction filtration, drying and grinding, that is, mention Obtain cellulose powder;
2) preparation of cellulose base super absorbent resin: deionized water is added in the cellulose powder that step 1) is prepared In dispersion is sufficiently stirred, initiator is then added under nitrogen protection, sequentially adds acrylic acid, urea and crosslinking agent, sufficiently It after reaction, adds polyvinyl alcohol and continues to stir, after reaction, by obtained product through vacuum freeze drying, grinding, excessively 80 Mesh obtains the cellulose base super absorbent resin of half interpenetrating network structure;
3) preparation of fertilizer coating liquid: polyvinyl alcohol, sodium alginate and sodium carboxymethylcellulose are placed at 70~90 DEG C Sufficiently dissolution, the mixed liquor being cooled to room temperature is fertilizer coating liquid;
4) preparation of cladded type the fertilizer of retaining water and releasing nutrients slowly: by fertiliser granulates in granulating disc rotating circular disc, be then sprayed into step Rapid atomization fertilizer coating liquid 3) obtained, adds cellulose base super absorbent resin made from step 2), makes cellulose base height Water-absorbing resins are wrapped in outside fertiliser granulates, after package is uniform, continues to spray into the atomization fertilizer coating liquid, chlorination is then added Calcium and boric acid mixed-powder are crosslinked it in fertilizer surface, to get slow to the water conservation of cladded type stalk fibre base after dry tack free Release fertilizer.
In this way, urea and acrylic acid reaction first generates acrylic amide grafted monomers, then acrylic amide grafting is single Body carries out graft copolymerization with cellulosic backbone and forms three-dimensional net structure under the action of crosslinking agent, is forming three-dimensional network knot Polyvinyl alcohol linear structure is added during structure, is wound each other interspersed, forms half interpenetrating network structure, enhances resin Mechanical strength and increase active site, wherein the addition of urea is conducive to the formation of polymer three-dimensional structure, and makes to synthesize Super absorbent resin can be sustained NH4+Ion assigns polymer fertilizer efficiency.
Preferably, the crop material source is at least one of corn, wheat, rape.The stalk powder Solid-to-liquid ratio with dilute acid soln is 1:30~70, and the dilute acid soln is 10% nitric acid.
Preferably, step 1) the heating stirring temperature is 85~110 DEG C, mixing time is 3~8h.
Preferably, the mass ratio of the cellulose powder and initiator is 1:0.25~0.5.
Preferably, the initiator is potassium peroxydisulfate and sodium sulfite, the matter of the potassium peroxydisulfate and sodium sulfite Amount is than being 1:1.
Preferably, cellulose powder described in step 2), acrylic acid, urea and crosslinking agent mass ratio be 1:1~ 3:0.2~1.2:0.05~0.08;The quality and cellulose mass ratio of the polyvinyl alcohol are 1:1.
Preferably, the crosslinking agent is N, N- methylene-bisacrylamide, N hydroxymethyl acrylamide or epoxy chlorine One of propane;The degree of neutralization of the acrylic acid is 70%~80%.
Preferably, the mass ratio of the step 3) polyvinyl alcohol, sodium alginate and sodium carboxymethylcellulose is 1: 0.25~0.5:0.05~0.08.
Preferably, the mass ratio of the cellulose base super absorbent resin and fertiliser granulates is 1:3~5;The fibre The mass ratio for tieing up plain base high water-absorption resin and calcium chloride and boric acid mixed-powder is 1:0.4~0.6.The calcium chloride and boric acid Mass ratio be 1:1.
Preferably, the fertiliser granulates are at least one of urea, Diammonium phosphate (DAP) and ammonium nitrate phosphorus.
The present invention also provides the cladded type stalk fibre based water-holding slow-release fertilizer obtained according to above-mentioned preparation method.
Compared with prior art, the invention has the following beneficial effects:
1, cladded type stalk fibre based water-holding slow-release fertilizer prepared by the present invention, will be fertile with stalk cellulose base high hydroscopic resin In material particle is wrapped in, and outermost layer is coated on polyvinyl alcohol, sodium alginate and carboxymethyl cellulose mixed liquid crosslinking film forming, Fertilizer efficiency Element release needs to increase by high hydroscopic resin layer and coating outer layer the diffusional resistance of fertilizer, improves fertilizer slow release Effect.The slow-release fertilizer of this method preparation not only has water conservation and fertilizer slow release double effects, also has stronger mechanical strength, more has Help keep soil moisture and improve utilization rate of fertilizer, meets agriculture Green Development requirement.
2, stalk cellulose base high hydroscopic resin prepared by the present invention is using stalk cellulose polysaccharide chain as skeleton, to draw It sends out agent and causes generation alkoxy free group, so that acrylic acid and urea and acrylic acid is reacted the acrylamide substance generated and be grafted to fibre It ties up on plain main chain, then forms three-dimensional net structure polymer by cross-linking agents, while carrying out interpenetrating with polyvinyl alcohol, formed The super absorbent resin of half interpenetrating network structure.The crosslinking interpenetrating of the polymer network makes the enhancing of its mechanical strength and active sites Point increases, and is more advantageous to load capacity and the fixing to fertilizer efficiency element and hydrone.
3, cladded type stalk fibre based water-holding slow-release fertilizer prepared by the present invention is further using the method for outer layer crosslinking film forming Increase the mechanical strength of slow-release fertilizer, the method for the double-deck coating solves while promoting fertilizer slow release effect because mechanical strength is inadequate The problem of causing fertilizer to be released.The introducing of urea is conducive to the formation of cross-linked structure, while being grafted to fiber as the fertilizer efficiency factor On plain main chain, the fertilizer efficiency of stalk cellulose base high hydroscopic resin attached.
4, cladded type the fertilizer of retaining water and releasing nutrients slowly prepared by the present invention has good mechanical performance and water imbibition, imitates to fertilizer slow release Fruit, moreover it is possible to reduce nutrient loss, substantially increase the utilization rate of fertilizer, reduce the maintenance cost in later period farmland, make crops Yield and quality be improved.Using agricultural straw as raw material, the extraction and method of modifying for selecting preparation cost low, to stalk fibre Dimension element is modified, and prepares the super absorbent resin with half interpenetrating network structure, as the covering material of traditional fertilizer, Prepared fertilizer thin layer has biodegradable properties, and soil physical property, system can be improved with retain water and nutrients by being applied in soil Preparation Method is easy, improves the added value of stalk application, has also expanded the new approaches that stalk resource utilizes, and is cladded type The fertilizer of retaining water and releasing nutrients slowly has found a kind of cheap, environmental-friendly, reproducible raw material, reduces manufacturing cost, has to agriculture Green Development It is significant.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
One, a kind of method for preparing cladded type stalk fibre based water-holding slow-release fertilizer
Embodiment 1
1) extraction of cellulose: wheat stalk removes impurity removing after cleaning drying, crushed 20 mesh and obtains stalk powder, Then 10% nitric acid solution is added into the stalk powder, solid-to-liquid ratio 1:30 is subsequently placed in 85 DEG C of heating stirring 3h, mentions It after taking, is cooled to room temperature, then through suction filtration, drying and grinding, that is, extracts and obtain cellulose powder;
2) preparation of cellulose base super absorbent resin: deionized water is added in the cellulose powder that step 1) is prepared In, after dispersion 30min is sufficiently stirred in 75 DEG C of water-baths, potassium peroxydisulfate and sodium sulfite stirring are then added under nitrogen protection 15min, cellulose powder and potassium peroxydisulfate and sodium sulfite mixed-powder total mass ratio are 1:0.25, sequentially add degree of neutralization For 70% acrylic acid, urea and N, N- methylene-bisacrylamide, cellulose powder, acrylic acid, urea and N, N- methylene The mass ratio of bisacrylamide is 1:1:0.2:0.05, and after sufficiently 30~50min of reaction, cellulose powder equal quality is added Polyvinyl alcohol continues to stir 3h, after reaction, by obtained product through vacuum freeze drying, grinding, excessively 80 meshes, obtains half The stalk fibre base high water-absorption resin of inierpeneirating network structure;
3) preparation of fertilizer coating liquid: by polyvinyl alcohol, sodium alginate and sodium carboxymethylcellulose 1:0.25 in mass ratio: 0.05 mixing, then sufficiently dissolves at 70 DEG C, the mixed liquor being cooled to room temperature is fertilizer coating liquid;
4) preparation of cladded type the fertilizer of retaining water and releasing nutrients slowly: urea granules are placed in rotating circular disc in granulating disc, are then sprayed into Step 3) is obtained to be atomized fertilizer coating liquid, adds cellulose base super absorbent resin made from step 2), makes cellulose base The mass ratio of super absorbent resin and urea granules is 1:3, and cellulose base super absorbent resin is wrapped in outside fertiliser granulates, is wrapped After wrapping up in uniformly, continues to spray into the atomization fertilizer coating liquid, be evenly coated at the outer layer of cellulose base super absorbent resin, then The calcium chloride and boric acid mixed-powder that mass ratio is 1:1 is added, the additive amount of the mixed-powder is stalk fibre base high water absorption Property 0.4 times of resin quality, be crosslinked it in fertilizer surface, continue to rotate disk, taken out after 15min, dried at 40 DEG C to get To cladded type stalk fibre based water-holding slow-release fertilizer.
Embodiment 2
1) extraction of cellulose: corn stover removes impurity removing after cleaning drying, crushed 20 mesh and obtains stalk powder, Then 10% nitric acid solution is added into the stalk powder, solid-to-liquid ratio 1:50 is subsequently placed in 110 DEG C of heating stirring 5h, It after extraction, is cooled to room temperature, then through suction filtration, drying and grinding, that is, extracts and obtain cellulose powder;
2) preparation of cellulose base super absorbent resin: deionized water is added in the cellulose powder that step 1) is prepared In, after dispersion 50min is sufficiently stirred in 80 DEG C of water-baths, potassium peroxydisulfate and sodium sulfite stirring are then added under nitrogen protection 20min, cellulose powder and potassium peroxydisulfate and sodium sulfite (mass ratio of potassium peroxydisulfate and sodium sulfite is 1:1) mixed-powder Total mass ratio is 1:0.4, sequentially adds acrylic acid, urea and N that degree of neutralization is 70%, and N- methylene-bisacrylamide makes Cellulose powder, acrylic acid, urea and N, the mass ratio of N- methylene-bisacrylamide are 1:1:0.4:0.07, sufficiently react 30 After~50min, the polyvinyl alcohol that cellulose powder equal quality is added continues to stir 3h, after reaction, the product that will be obtained Through vacuum freeze drying, grinding, 80 meshes are crossed, obtains the stalk fibre base high water-absorption resin of half interpenetrating network structure;
3) preparation of fertilizer coating liquid: by polyvinyl alcohol, sodium alginate and sodium carboxymethylcellulose 1:0.4 in mass ratio: 0.05 mixing, then sufficiently dissolves at 80 DEG C, the mixed liquor being cooled to room temperature is fertilizer coating liquid;
4) preparation of cladded type the fertilizer of retaining water and releasing nutrients slowly: Diammonium phosphate (DAP) particle is placed in rotating circular disc in granulating disc, then Step 3) atomization fertilizer coating liquid obtained is sprayed into, cellulose base super absorbent resin made from step 2) is added, makes fiber The mass ratio of plain base high water-absorption resin and urea granules is 1:4, and cellulose base super absorbent resin is wrapped in fertiliser granulates Outside, after package is uniform, continue to spray into the atomization fertilizer coating liquid, be evenly coated at the outer of cellulose base super absorbent resin Layer, is then added calcium chloride and boric acid mixed-powder that mass ratio is 1:1, and the additive amount of the mixed-powder is stalk fibre base 0.5 times of super absorbent resin quality is crosslinked it in fertilizer surface, continues to rotate disk, take out after 20min, does at 50 DEG C It is dry fertile to get cladded type stalk fibre based water-holding slow-release is arrived.
Embodiment 3
1) extraction of cellulose: rape stalk removes impurity removing after cleaning drying, crushed 20 mesh and obtains stalk powder, Then 10% nitric acid solution is added into the stalk powder, solid-to-liquid ratio 1:50 is subsequently placed in 100 DEG C of heating stirring 4h, It after extraction, is cooled to room temperature, then through suction filtration, drying and grinding, that is, extracts and obtain cellulose powder;
2) preparation of cellulose base super absorbent resin: deionized water is added in the cellulose powder that step 1) is prepared In, after dispersion 30min is sufficiently stirred in 70 DEG C of water-baths, potassium peroxydisulfate and sodium sulfite stirring are then added under nitrogen protection 30min, cellulose powder and potassium peroxydisulfate and sodium sulfite (mass ratio of potassium peroxydisulfate and sodium sulfite is 1:1) mixed-powder Total mass ratio is 1:0.3, sequentially adds acrylic acid, urea and N that degree of neutralization is 80%, and N- methylene-bisacrylamide makes Cellulose powder, acrylic acid, urea and N, the mass ratio of N- methylene-bisacrylamide are 1:1:0.3:0.06, sufficiently react 30 After~50min, the polyvinyl alcohol that cellulose powder equal quality is added continues to stir 2h, after reaction, the product that will be obtained Through vacuum freeze drying, grinding, 80 meshes are crossed, obtains the stalk fibre base high water-absorption resin of half interpenetrating network structure;
3) preparation of fertilizer coating liquid: by polyvinyl alcohol, sodium alginate and sodium carboxymethylcellulose 1:0.3 in mass ratio: 0.05 mixing, then sufficiently dissolves at 80 DEG C, the mixed liquor being cooled to room temperature is fertilizer coating liquid;
4) preparation of cladded type the fertilizer of retaining water and releasing nutrients slowly: ammonium nitrate phosphorus particle is placed in rotating circular disc in granulating disc, then Step 3) atomization fertilizer coating liquid obtained is sprayed into, cellulose base super absorbent resin made from step 2) is added, makes fiber The mass ratio of plain base high water-absorption resin and urea granules is 1:4, and cellulose base super absorbent resin is wrapped in fertiliser granulates Outside, after package is uniform, continue to spray into the atomization fertilizer coating liquid, be evenly coated at the outer of cellulose base super absorbent resin Layer, is then added calcium chloride and boric acid mixed-powder that mass ratio is 1:1, and the additive amount of the mixed-powder is stalk fibre base 0.5 times of super absorbent resin quality is crosslinked it in fertilizer surface, continues to rotate disk, take out after 10min, does at 50 DEG C It is dry fertile to get cladded type stalk fibre based water-holding slow-release is arrived.
Comparative example 1
Operating procedure is removed in step 2) with embodiment 1 and is not added with polyvinyl alcohol.
Comparative example 2
Operating procedure is removed in step 4) with example 1 and is not added with calcium chloride and boric acid.
Two, performance test
Cladded type stalk fibre based water-holding slow-release fertilizer prepared by Examples 1 to 3 and comparative example 1~2, (1) mechanical strength Coefficient uses constant temperature oscillation method, with intact fertiliser granulates accounting (%) for foundation;(2) fertilizer water imbibition uses method of nylon bag, Calculate the ratio (g/g) of water suction saturation front and back mass change amount;(3) water-retaining property uses earth pillar method in soil, measures identical infiltrate Distance, influence of the fertilizer to infiltration capacity, infiltration capacity is with Markov bottle water level decreasing height (cm) for foundation;(4) fertilizer slow release characteristic Using bag filter Cumulative release amount method, the release characteristics of fertilizer in water are measured, with each fertilizer efficiency element Cumulative release amount after 30 days The ratio (%) of total amount and embedding fertilizer efficiency element total amount is foundation;(5) biological degradability uses soil burying, and measurement is not With the residual mass for burying resin after the time, its mass loss rate (%) after 30 days is calculated;(6) coating is investigated using adsorption experiment Resin is to the fixing adsorption capacity of fertilizer efficiency element, with the object ion (NH of 100mg/L4 +、NO3 -、PO4 3-), a certain amount of preparation tree Rouge is adsorbent material, and shaken cultivation to adsorption equilibrium measures adsorbance percentage.The results are shown in Table 1 for it.
Table 1
As it can be seen from table 1 the mechanical strength of cladded type the fertilizer of retaining water and releasing nutrients slowly prepared by the present invention improves compared with comparative example 16% or more, avoid because mechanical strength not enough due to caused by fertilizer be released;Slow-release fertilizer of the invention is significantly increased to fertilizer efficiency The load capacity and fixing of element and hydrone have good slow release effect to fertilizer, greatly reduce nutrient loss, improve fertilizer Utilization rate, while decreasing the maintenance cost in later period farmland, be improved the yield of crops and quality.In addition, system Standby obtained fertilizer has the characteristics such as at low cost, degradable, environmental-friendly.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not limitation with the present invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (10)

1. a kind of method for preparing cladded type stalk fibre based water-holding slow-release fertilizer, which comprises the following steps:
1) extraction of cellulose: stalk powder will be obtained after straw drying, removal of impurities, crushing, then to the straw powder Dilute acid soln is added in end, then heating stirring is sufficiently extracted, and is cooled to room temperature, then through suction filtration, drying and grinding, that is, extract To cellulose powder;
2) preparation of cellulose base super absorbent resin: the cellulose powder that step 1) is prepared is added in deionized water and is filled Divide and be dispersed with stirring, initiator is then added under nitrogen protection, sequentially adds acrylic acid, urea and crosslinking agent, sufficiently reacts Afterwards, it adds polyvinyl alcohol to continue to stir, after reaction, by obtained product through vacuum freeze drying, grinding, excessively 80 mesh Sieve, obtains the cellulose base super absorbent resin of half interpenetrating network structure;
3) preparation of fertilizer coating liquid: polyvinyl alcohol, sodium alginate and sodium carboxymethylcellulose are placed at 70~90 DEG C sufficiently Dissolution, the mixed liquor being cooled to room temperature is fertilizer coating liquid;
4) preparation of cladded type the fertilizer of retaining water and releasing nutrients slowly: by fertiliser granulates in granulating disc rotating circular disc, be then sprayed into step 3) Atomization fertilizer coating liquid obtained, adds cellulose base super absorbent resin made from step 2), makes cellulose base high water absorption Property resin be wrapped in outside fertiliser granulates, package uniformly after, continue to spray into the atomization fertilizer coating liquid, then be added calcium chloride and Boric acid mixed-powder is crosslinked it in fertilizer surface, arrives cladded type stalk fibre based water-holding slow-release after dry tack free Fertilizer.
2. preparing the method for cladded type stalk fibre based water-holding slow-release fertilizer according to claim 1, which is characterized in that step 1) The heating stirring temperature is 85~110 DEG C, and mixing time is 3~8h.
3. preparing the method for cladded type stalk fibre based water-holding slow-release fertilizer according to claim 1, which is characterized in that the fibre The mass ratio for tieing up plain powder and initiator is 1:0.25~0.5.
4. preparing the method for cladded type stalk fibre based water-holding slow-release fertilizer according to claim 1, which is characterized in that described to draw Agent is sent out as potassium peroxydisulfate and sodium sulfite, the mass ratio of the potassium peroxydisulfate and sodium sulfite is 1:1.
5. preparing the method for cladded type stalk fibre based water-holding slow-release fertilizer according to claim 1, which is characterized in that step 2) Described in cellulose powder, acrylic acid, urea and crosslinking agent mass ratio be 1:1~3:0.2~1.2:0.05~0.08, it is described The quality and cellulose powder mass ratio of polyvinyl alcohol are 1:1.
6. preparing the method for cladded type stalk fibre based water-holding slow-release fertilizer according to claim 1, which is characterized in that the friendship Connection agent is any one in N,N methylene bis acrylamide, N hydroxymethyl acrylamide and epoxychloropropane;The propylene The degree of neutralization of acid is 70%~80%.
7. preparing the method for cladded type stalk fibre based water-holding slow-release fertilizer according to claim 1, which is characterized in that step 3) The mass ratio of the polyvinyl alcohol, sodium alginate and sodium carboxymethylcellulose is 1:0.25~0.5:0.05~0.08.
8. preparing the method for cladded type stalk fibre based water-holding slow-release fertilizer according to claim 1, which is characterized in that the fibre The mass ratio for tieing up plain base high water-absorption resin and fertiliser granulates is 1:3~5;The cellulose base super absorbent resin and calcium chloride Mass ratio with boric acid mixed-powder is 1:0.4~0.6.
9. preparing the method for cladded type stalk fibre based water-holding slow-release fertilizer according to claim 1, which is characterized in that the fertilizer Material particle is at least one of urea, Diammonium phosphate (DAP) and ammonium nitrate phosphorus.
10. the cladded type stalk fibre based water-holding slow-release fertilizer obtained by the preparation method described in claim 1~9.
CN201910525676.5A 2019-06-18 2019-06-18 A method of preparing cladded type stalk fibre based water-holding slow-release fertilizer Pending CN110272314A (en)

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CN111233581A (en) * 2020-03-17 2020-06-05 云南省烟草公司红河州公司 Tobacco special fertilizer for improving water retention performance of tobacco planting soil
CN111264317A (en) * 2019-12-06 2020-06-12 庆元县枫陌生态农业开发有限公司 Chenopodium quinoa willd planting method in east China
CN112499872A (en) * 2020-12-10 2021-03-16 浙江鸿盛化工有限公司 Conditioner and treatment method of 2, 4-dinitrochlorobenzene waste acid
CN112759066A (en) * 2021-01-15 2021-05-07 华设设计集团环境科技有限公司 Straw filler for sewage treatment and preparation method thereof
CN113371884A (en) * 2021-07-07 2021-09-10 广州华景建设有限公司 Rainwater recycling process suitable for garden landscape
CN113443941A (en) * 2021-08-13 2021-09-28 承德石油高等专科学校 Composite water-retention slow-release fertilizer and preparation method thereof
CN113480693A (en) * 2021-06-25 2021-10-08 广西大学 Preparation method of cassava residue/polyvinyl alcohol semi-through network super-absorbent microspheres
CN113943433A (en) * 2021-11-23 2022-01-18 万华化学集团股份有限公司 High-performance acrylic acid water-absorbent resin and preparation method thereof
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CN114890841A (en) * 2022-03-24 2022-08-12 武汉绿农瑞益生物科技有限公司 Long-acting microbial compound fertilizer and preparation method thereof
CN114890838A (en) * 2022-06-09 2022-08-12 兰州城市学院 Slow-release fertilizer with slope stability and preparation method and application thereof
CN114933509A (en) * 2022-05-09 2022-08-23 武汉绿农瑞益生物科技有限公司 Slow-release compound fertilizer and preparation method thereof
CN115286456A (en) * 2022-08-24 2022-11-04 广东海洋大学 Preparation method and application of water-retention slow-release compound fertilizer

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Cited By (18)

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Publication number Priority date Publication date Assignee Title
CN110746235A (en) * 2019-12-04 2020-02-04 河西学院 Preparation method of nitrogen-phosphorus-potassium compound slow-release fertilizer based on corn straws
CN111264317A (en) * 2019-12-06 2020-06-12 庆元县枫陌生态农业开发有限公司 Chenopodium quinoa willd planting method in east China
CN111233581A (en) * 2020-03-17 2020-06-05 云南省烟草公司红河州公司 Tobacco special fertilizer for improving water retention performance of tobacco planting soil
CN112499872B (en) * 2020-12-10 2022-11-11 浙江鸿盛化工有限公司 Conditioner and treatment method of 2, 4-dinitrochlorobenzene waste acid
CN112499872A (en) * 2020-12-10 2021-03-16 浙江鸿盛化工有限公司 Conditioner and treatment method of 2, 4-dinitrochlorobenzene waste acid
CN112759066A (en) * 2021-01-15 2021-05-07 华设设计集团环境科技有限公司 Straw filler for sewage treatment and preparation method thereof
CN112759066B (en) * 2021-01-15 2023-11-03 华设设计集团环境科技有限公司 Straw filler for sewage treatment and preparation method thereof
CN113480693A (en) * 2021-06-25 2021-10-08 广西大学 Preparation method of cassava residue/polyvinyl alcohol semi-through network super-absorbent microspheres
CN113371884A (en) * 2021-07-07 2021-09-10 广州华景建设有限公司 Rainwater recycling process suitable for garden landscape
CN113443941A (en) * 2021-08-13 2021-09-28 承德石油高等专科学校 Composite water-retention slow-release fertilizer and preparation method thereof
CN113943433A (en) * 2021-11-23 2022-01-18 万华化学集团股份有限公司 High-performance acrylic acid water-absorbent resin and preparation method thereof
CN113943433B (en) * 2021-11-23 2023-05-30 万华化学集团股份有限公司 High-performance acrylic acid water-absorbent resin and preparation method thereof
CN114195586A (en) * 2021-12-31 2022-03-18 广州市中景园林环保工程有限公司 Fertilizer with long fertilizer efficiency for landscaping and preparation method thereof
CN114890841A (en) * 2022-03-24 2022-08-12 武汉绿农瑞益生物科技有限公司 Long-acting microbial compound fertilizer and preparation method thereof
CN114933509A (en) * 2022-05-09 2022-08-23 武汉绿农瑞益生物科技有限公司 Slow-release compound fertilizer and preparation method thereof
CN114890838A (en) * 2022-06-09 2022-08-12 兰州城市学院 Slow-release fertilizer with slope stability and preparation method and application thereof
CN115286456A (en) * 2022-08-24 2022-11-04 广东海洋大学 Preparation method and application of water-retention slow-release compound fertilizer
CN115286456B (en) * 2022-08-24 2024-04-09 广东海洋大学 Preparation method and application of water-retention slow-release compound fertilizer

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