CN103159532A - Porous lignin particle composite fertilizer preparation method - Google Patents
Porous lignin particle composite fertilizer preparation method Download PDFInfo
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Abstract
The present invention provides a porous lignin particle composite fertilizer preparation method. The technical scheme comprises: carrying out a reaction of alkaline lignin and formaldehyde to prepare a lignin cross-linking body A; uniformly mixing the A, a pore-forming agent and a lignin particle setting agent; adjusting the pH value of the composite system, such that the pore-forming agent is coated by the A so as to settle; carrying out centrifugal separation to obtain a solid mixture B; adopting a specific process to remove the pore-forming agent in the B to obtain porous lignin C; adopting a fertilizer solution containing nitrogen, phosphorus, potassium and trace elements to soak the porous lignin C, and carrying out drying molding to prepare porous lignin composite fertilizer D; and uniformly mixing the porous lignin composite fertilizer D, an auxiliary material and an adhesive additive in a stirrer, and adopting a granulator to carry out extrusion granulation on the obtained mixture to prepare the porous lignin particle composite fertilizer. The porous lignin particle composite fertilizer has the following characteristics that: lignin biodegradation is slow, such that the porous lignin particle composite fertilizer can be adopted as a slow-release fertilizer in agriculture so as to solve problems of gradually reduced humus soil in soil due to inorganic fertilizer use and pollution on groundwater by nitrogen, phosphorus, potassium and trace elements in inorganic fertilizers; and the porous lignin particle composite fertilizer further has a porous structure so as to enhance a slow release effect of the composite fertilizer.
Description
Technical field
The present invention relates to the preparation method of a kind of crosslinked porous xylogen particle nitrogen/iron composite fertilizer, belong to the fertilizer preparation field.
Background technology
Xylogen and derivative thereof have several functions, can be used as dispersion agent, sorbent material/strippant, petroleum recovery auxiliary agent, asphalt emulsifier, development chemical modification lignin product, improve its added value and be area research person, the entrepreneurs such as domestic and international paper industry, vegetable chemistry, natural polymer chemistry, fine chemistry industry and environmental science and jointly pay close attention to for a long time, and actively be devoted to study major fields with technological development.Pulp and paper industry will be isolated the careless class xylogen of 3,000 ten thousand tons of left and right every year from plant, but the complicated reactive chemistry of its constituent functional group is few.The utilization of grass class xylogen is confined to the low value burning mostly, makes it be converted into chemical products with high added-value, will greatly promote the utility value of xylogen.Xylogen concentrates on the following aspects in the application of agriculture field at present:
1) fertilizer: alkali lignin is the aromatic series organic raw material of the high-polymerization degree that can obtain from the nature renewable resource, has characteristic nontoxic, inexpensive, that can be decomposed by microorganism.When with the element compounding application such as the needed nitrogen of plant-growth, phosphorus, potassium, along with the alkali lignin element that is degraded by microorganisms is released slowly, be the Crop utilization, fertilizer efficiency is long, contain various nutrient elements.
2) soil improvement agent: alkali lignin is as soil improvement agent, can be used to improve closely, saliferous and the soil that is corroded, make soil produce crumb structure, and then the water properties of change soil, can also promote the fertilizer efficiency of fertilizer, when especially using phosphate fertilizer, because alkali lignin has closing property of huge legendary turtle, can prevent effectively that phosphate fertilizer from anchoring on soil, improve significantly fertilizer efficiency.
3) liquid ground film: degradable xylogen mulch film developing low-cost, degradable, environmental friendliness, have higher physical strength.Be comprised of alkali lignin, collagen protein, tensio-active agent, whipping agent etc., be sprayed on the field by spray method, mulching soil surface filming, film have good wetting property, have the soil moisture conservation effect, effectively prevent the evaporation of moisture.Can be with the film bursting when plant seedlings grows, after for some time, mulch film degraded automatically, become humic acid fertilizer, can improve the crumb structure of soil.Also can add agricultural chemicals and fertilizer in this mulch film, become Multifunctional composite mulching film, its cost is lower.
Nitrogen, phosphorus, potassium and trace element are the indispensable fertilizer of growth of many farm crop.Little fertilizer is to provide the fertilizer of minimum plant element, and routine copper fertilizer, boron fertilizer, molydbenum fertilizer, manganese fertilizer, iron fertilizer and zinc fertilizer etc. all are called little fertilizer.But simply add in the soil mineral compound in conjunction with closely, saliferous and soil (for example, the saltings) poor effect that is corroded.Porous lignin particle compound fertilizer provided by the invention, more slowly can be used as slow release fertilizer on agricultural except having lignin biodegradation's speed, solved inorganic fertilizer and used and cause vegetable mould in soil to reduce gradually outside the advantage of being polluted by the nitrogen in mineral manure, phosphorus, potassium and trace element with underground water, also had because of it slow release effect that vesicular structure has strengthened composite fertilizer.
Summary of the invention
The invention provides a kind of preparation method of porous lignin particle compound fertilizer, technical scheme of the present invention is to prepare xylogen crosslinked A with alkali lignin and formaldehyde reaction, then A, pore-forming material and xylogen particle setting agent are evenly mixed.Adjust compound system pH value, make A coat the pore-forming material sedimentation, centrifugation gets solid mixture B.The pore-forming material that adopts special process to remove in B obtains porous xylogen C.With the solution soaking porous xylogen C of nitrogenous, phosphorus, potassium and trace element fertilizer, and drying and moulding prepares porous xylogen composite fertilizer D.With porous xylogen composite fertilizer D, auxiliary material, adhesive aid mixing in stirrer, adopt tablets press with the said mixture extruding pelletization, preparation porous lignin particle compound fertilizer.
The lignin particle compound fertilizer that the present invention relates to comprises preparation, coating sedimentation, pore-creating technique, composite fertilizer's immobilization and three steps of porous lignin particle compound fertilizer drying and moulding of crosslinked, it is characterized in that:
1) coat settling process: xylogen crosslinked 3.0g adds the NaOH solution dissolving of appropriate 5%-40%, add subsequently 0.3g pore-forming material solution to mix, it is acid regulating pH with 2%-10%HCl solution, and system has precipitation to generate, and centrifugation gets solid mixture B.
2) pore-creating process: centrifugation gets solid mixture B, adopts suitable physical method to remove pore-forming material and obtains porous xylogen C.
3) with the solution soaking porous xylogen C of nitrogenous, phosphorus, potassium and trace element fertilizer, and drying and moulding prepares porous xylogen composite fertilizer D.
4) with certain proportion respectively with porous lignin particle compound fertilizer D, auxiliary material, adhesive aid mixing in stirrer, adopt tablets press with the said mixture extruding pelletization, preparation porous lignin particle compound fertilizer.
Above-mentioned industrial lignin can be alkali lignin, sulfonated lignin or by separating the xylogen of preparation in stalk, wheat straw and not needing refining purifying.
Above-mentioned pore-forming material can be suitable macromolecular compound, comprises carboxymethyl cellulose, starch, polysaccharide, cyclodextrin, water-soluble linear macromolecular compound, the water-soluble three dimensional polymer that particle diameter is suitable etc.; Above-mentioned pore-forming material can be also mineral compound, comprises sodium-chlor, saltpetre, sodium sulfate, potassium aluminium sulfate, zinc nitrate, Sodium phosphate dibasic etc.
The above-mentioned special process of removing pore-forming material comprises heat pore-forming material evaporating method and solvent wash method etc.
Above-mentioned nitrogenous fertilizer can be bicarbonate of ammonia, SODIUMNITRATE, nitrocalcite, ammonium nitrate, calcium ammonium nitrate and urea etc.Above-mentioned phosphate fertilizer can be the compound fertilizers such as calcium phosphate, double superhosphate, ammonium phosphate etc. or fused(calcium magnesium)phosphate, thomas phosphate, ammoniated superphosphate, calcium metaphosphate.Above-mentioned potash fertilizer can be plant ash, salt of wormwood etc.Can also use the compound trace element fertilizers such as composite fertilizer such as saltpetre, primary ammonium phosphate, potassium primary phosphate.Above-mentioned copper fertilizer can be cupric nitrate, copper sulfate, cupric oxide, contain Copper Slag etc.Above-mentioned boron fertilizer can be borax, boric acid, boron mud.Above-mentioned molydbenum fertilizer can be nitric acid molybdenum, ammonium molybdate, Sodium orthomolybdate.Above-mentioned manganese fertilizer can be manganous sulfate, manganous carbonate, Manganous chloride tetrahydrate, manganese oxide etc.Above-mentioned iron fertilizer can be ferrous sulfate, ferrous ammonium sulphate, ferric oxide, iron protoxide, ferrous ammonium phosphate, ammonium sulfate iron etc.Above-mentioned zinc fertilizer can be zinc sulfate, basic zinc sulfate, zinc oxide, zinc chloride, zinc carbonate etc.Above-mentioned auxiliary material can be the additives such as the peat composed of rotten mosses, stalk, grass meal.
Above-mentioned adhesive aid can be that mud, discarded plant are the starch, Xylo-Mucine of raw material preparation etc.
Embodiment
Embodiment 1
Weighing industrial lignin 3.0g adds 20% NaOH solution 0.6mL, then regulate pH to 10 with distilled water, add subsequently 4.8mL formaldehyde, be transferred to after mixing in the 100mL there-necked flask, stir in 90 ℃ of waters bath with thermostatic control Cross-linked reaction 2h occurs, cooling, preparation xylogen crosslinked A, then A, appropriate bicarbonate of ammonia and xylogen particle setting agent are evenly mixed.Regulate pH to 5 with 10%HCl solution, add 2.03g urea, 0.4g iron nitrate.React 2h in 90 ℃ of water-baths; the xylogen cross-linking compounds is reacted fully with it; obtain the porous xylogen composite fertilizer D (relation of bicarbonate of ammonia add-on and porosity sees Table 1) of nitrogen content 23.96%, iron-holder 0.375%; with 50: 5: 42: 3 ratios were respectively with porous xylogen composite fertilizer D and the peat composed of rotten mosses, starch, water mixing in stirrer, adopted tablets press that the said mixture extruding pelletization is prepared porous particle xylogen composite fertilizer.Uncrosslinked xylogen raw material is control sample.To accurately take respectively above-mentioned porous particle xylogen composite fertilizer 1.0g and be placed in the dry Erlenmeyer flask of 250mL, add the 100mL distilled water immersion, the interval certain hour is got 3 groups of samples and is filtered, accurately get 0.05g sample Sulfuric-Acid Digestion after filter residue and drying, adopt Kjeldahl determination to measure the nitrogen content of residual residue in respective samples, get 3 groups of data mean values.As calculated, in 48 hours the porous lignin particle compound fertilizer (nitrogen content: 239.6mg/g) the slowly-releasing situation of nitrogen element sees Table 2, and slow release effect is obvious.
Relation (the unit: mg/g) of table 1 embodiment 1 bicarbonate of ammonia add-on and porosity
Slowly-releasing situation (the unit: mg/g) of table 2 embodiment 1 porous lignin particle compound fertilizer
Embodiment 2
The porous particle xylogen composite fertilizer 1.0g that accurately takes respectively in above-described embodiment 1 is placed in the dry Erlenmeyer flask of 250mL, add the 100mL distilled water immersion, the interval certain hour is got 3 groups of samples and is filtered, accurately get 0.05g sample Sulfuric-Acid Digestion after filter residue and drying, adopt Kjeldahl determination to measure the nitrogen content of residual residue in respective samples, get 3 groups of data mean values.As calculated, in 48 hours the porous lignin particle compound fertilizer (iron level: 3.75mg/g) the slowly-releasing situation of ferro element sees Table 3.
Slowly-releasing situation (the unit: mg/g) of table 3 embodiment 1 porous lignin particle compound fertilizer ferro element
Embodiment 3
Prepare xylogen crosslinked A according to the described step of embodiment 1, then A, appropriate saltpetre and 1% sodium alginate are evenly mixed.Adjusting compound system pH value is 5, makes A coat the saltpetre sedimentation, and centrifugation gets solid mixture B.Adopt water washing to remove B and obtain porous xylogen C.C is evenly mixed with the 0.4g iron nitrate, and dry preparation porous xylogen composite fertilizer D.Preparing porous particle xylogen composite fertilizer by the described granulation process of embodiment 1, the data of its porosity see Table 4.
The porous particle xylogen composite fertilizer 1.0g that accurately takes respectively in above-described embodiment 3 is placed in the dry Erlenmeyer flask of 250mL, add the 100mL distilled water immersion, the interval certain hour is got 3 groups of samples and is filtered, accurately get 0.05g sample Sulfuric-Acid Digestion after filter residue and drying, according to GBT14540-2003, adopt atomic absorption spectrophotometer to measure iron level in sustained-release liquid.Get 3 groups of data mean values.As calculated, in 48 hours the porous lignin particle compound fertilizer (iron level: 3.75mg/g) the slowly-releasing situation of ferro element sees Table 5.
Relation (the unit: mg/g) of table 4 embodiment 1 saltpetre add-on and porosity
Slowly-releasing situation (the unit: mg/g) of table 5 embodiment 3 porous lignin particle compound fertilizer ferro elements
Claims (5)
1. the preparation method of a porous lignin particle compound fertilizer, the lignin particle compound fertilizer that the present invention relates to comprises preparation, coating sedimentation, pore-creating technique, composite fertilizer's immobilization and the porous lignin particle compound fertilizer drying and moulding five steps of crosslinked, it is characterized in that: 1) coat settling process: xylogen crosslinked 3.0g adds the NaOH solution dissolving of appropriate 5%-40%, add subsequently 0.3g pore-forming material solution to mix, it is acid regulating pH with 2%-10%HCl solution, system has precipitation to generate, and centrifugation gets solid mixture B.2) pore-creating process: centrifugation gets solid mixture B, adopts suitable physical method to remove pore-forming material and obtains porous xylogen C.3) with the solution soaking porous xylogen C of nitrogenous, phosphorus, potassium and trace element fertilizer, and drying and moulding prepares porous xylogen composite fertilizer D.4) with certain proportion respectively with porous lignin particle compound fertilizer D, auxiliary material, adhesive aid mixing in stirrer, adopt tablets press with the said mixture extruding pelletization, preparation porous lignin particle compound fertilizer.
2. lignin particle compound fertilizer according to claim 1 is characterized in that above-mentioned industrial lignin can be alkali lignin, sulfonated lignin or by separating the xylogen of preparation in stalk, wheat straw and not needing refining purifying.
3. lignin particle compound fertilizer according to claim 1, the above-mentioned nitrogenous fertilizer of its feature can be bicarbonate of ammonia, SODIUMNITRATE, nitrocalcite, ammonium nitrate, calcium ammonium nitrate and urea etc.Above-mentioned phosphate fertilizer can be the compound fertilizers such as calcium phosphate, double superhosphate, ammonium phosphate etc. or fused(calcium magnesium)phosphate, thomas phosphate, ammoniated superphosphate, calcium metaphosphate.Above-mentioned potash fertilizer can be plant ash, salt of wormwood etc.Can also use the compound trace element fertilizers such as composite fertilizer such as saltpetre, primary ammonium phosphate, potassium primary phosphate.Above-mentioned copper fertilizer can be cupric nitrate, copper sulfate, cupric oxide, contain Copper Slag etc.Above-mentioned boron fertilizer can be borax, boric acid, boron mud.Above-mentioned molydbenum fertilizer can be nitric acid molybdenum, ammonium molybdate, Sodium orthomolybdate.Above-mentioned manganese fertilizer can be manganous sulfate, manganous carbonate, Manganous chloride tetrahydrate, manganese oxide etc.Above-mentioned iron fertilizer can be ferrous sulfate, ferrous ammonium sulphate, ferric oxide, iron protoxide, ferrous ammonium phosphate, ammonium sulfate iron etc.Above-mentioned zinc fertilizer can be zinc sulfate, basic zinc sulfate, zinc oxide, zinc chloride, zinc carbonate etc.
4. above-mentioned pore-forming material can be suitable macromolecular compound, comprises carboxymethyl cellulose, starch, polysaccharide, cyclodextrin, water-soluble linear macromolecular compound, the water-soluble three dimensional polymer that particle diameter is suitable etc.; Above-mentioned pore-forming material can be also mineral compound, comprises sodium-chlor, saltpetre, sodium sulfate, potassium aluminium sulfate, zinc nitrate, Sodium phosphate dibasic etc.
5. lignin particle compound fertilizer according to claim 1, the above-mentioned auxiliary material of its feature can be the additives such as the peat composed of rotten mosses, stalk, grass meal.Above-mentioned adhesive aid can be that mud, discarded plant are the starch, Xylo-Mucine of raw material preparation etc.
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Cited By (11)
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| CN104072210A (en) * | 2014-06-24 | 2014-10-01 | 深圳市芭田生态工程股份有限公司 | Multipurpose secondary/minor-element fertilizer, and preparation method and application thereof |
| CN105960988A (en) * | 2016-05-11 | 2016-09-28 | 丁广礼 | Deep pool lotus rhizome planting method |
| CN107721739A (en) * | 2017-10-31 | 2018-02-23 | 蚌埠标优美生态工程有限公司 | A kind of fermented stalk slow release fertilizer |
| CN108580529A (en) * | 2018-04-11 | 2018-09-28 | 毛强平 | A kind of restorative procedure of heavy-metal contaminated soil |
| CN108794711A (en) * | 2017-04-27 | 2018-11-13 | 东北林业大学 | Recovery technique of the polyphenol lignin low cross-linking polymer to organic agricultural chemicals soil pollution |
| CN108976031A (en) * | 2018-08-31 | 2018-12-11 | 怀化远东化肥有限公司 | A kind of chelate compound fertilizer and preparation method thereof of the long prevention and treatment sclerotiniose of fertilizer efficiency |
| CN109020701A (en) * | 2018-09-11 | 2018-12-18 | 浙江世佳科技有限公司 | A kind of high-performance bio bacterial manure |
| CN109134944A (en) * | 2018-08-28 | 2019-01-04 | 安徽聚欣新材料科技有限公司 | A kind of porous small ball and its application with different chemical functional groups |
| CN111253945A (en) * | 2020-03-23 | 2020-06-09 | 成都新柯力化工科技有限公司 | Acidified soil conditioner and preparation method thereof |
| CN111826165A (en) * | 2020-06-23 | 2020-10-27 | 成都新柯力化工科技有限公司 | Acidified soil cellulose-based modifier and preparation method thereof |
| CN112062641A (en) * | 2020-08-03 | 2020-12-11 | 华南农业大学 | Alkaline compound liquid fertilizer containing lignin-based long-acting nitrogen fertilizer and preparation method and application thereof |
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Cited By (15)
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| CN104072210B (en) * | 2014-06-24 | 2016-08-24 | 深圳市芭田生态工程股份有限公司 | Trace element fertilizer and its preparation method and application in a kind of multipurpose |
| CN104072210A (en) * | 2014-06-24 | 2014-10-01 | 深圳市芭田生态工程股份有限公司 | Multipurpose secondary/minor-element fertilizer, and preparation method and application thereof |
| CN105960988A (en) * | 2016-05-11 | 2016-09-28 | 丁广礼 | Deep pool lotus rhizome planting method |
| CN108794711A (en) * | 2017-04-27 | 2018-11-13 | 东北林业大学 | Recovery technique of the polyphenol lignin low cross-linking polymer to organic agricultural chemicals soil pollution |
| CN108794711B (en) * | 2017-04-27 | 2021-03-12 | 东北林业大学 | Technology for repairing organic pesticide soil pollution by polyphenol lignin low-crosslinking polymer |
| CN107721739A (en) * | 2017-10-31 | 2018-02-23 | 蚌埠标优美生态工程有限公司 | A kind of fermented stalk slow release fertilizer |
| CN108580529B (en) * | 2018-04-11 | 2020-07-03 | 江苏爱佳福如土壤修复有限公司 | Remediation method for heavy metal contaminated soil |
| CN108580529A (en) * | 2018-04-11 | 2018-09-28 | 毛强平 | A kind of restorative procedure of heavy-metal contaminated soil |
| CN109134944A (en) * | 2018-08-28 | 2019-01-04 | 安徽聚欣新材料科技有限公司 | A kind of porous small ball and its application with different chemical functional groups |
| CN108976031A (en) * | 2018-08-31 | 2018-12-11 | 怀化远东化肥有限公司 | A kind of chelate compound fertilizer and preparation method thereof of the long prevention and treatment sclerotiniose of fertilizer efficiency |
| CN109020701A (en) * | 2018-09-11 | 2018-12-18 | 浙江世佳科技有限公司 | A kind of high-performance bio bacterial manure |
| CN111253945A (en) * | 2020-03-23 | 2020-06-09 | 成都新柯力化工科技有限公司 | Acidified soil conditioner and preparation method thereof |
| CN111253945B (en) * | 2020-03-23 | 2021-06-18 | 江苏沃绿宝生物科技股份有限公司 | Acidified soil conditioner and preparation method thereof |
| CN111826165A (en) * | 2020-06-23 | 2020-10-27 | 成都新柯力化工科技有限公司 | Acidified soil cellulose-based modifier and preparation method thereof |
| CN112062641A (en) * | 2020-08-03 | 2020-12-11 | 华南农业大学 | Alkaline compound liquid fertilizer containing lignin-based long-acting nitrogen fertilizer and preparation method and application thereof |
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