CN105801205A - Method for co-producing water-soluble microelement fertilizer by utilizing seaweed extract - Google Patents
Method for co-producing water-soluble microelement fertilizer by utilizing seaweed extract Download PDFInfo
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- CN105801205A CN105801205A CN201610105960.3A CN201610105960A CN105801205A CN 105801205 A CN105801205 A CN 105801205A CN 201610105960 A CN201610105960 A CN 201610105960A CN 105801205 A CN105801205 A CN 105801205A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
- C05D9/02—Other inorganic fertilisers containing trace elements
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention relates to a method for co-producing a water-soluble microelement fertilizer by utilizing a seaweed extract. The method comprises the following steps: washing fresh or dried seaweeds, adding the fresh or dried seaweeds to a reaction kettle containing a mixture of a certain mass of water and organic solvents according to a certain mass ratio, stirring the materials at a high speed for pulping (the dried seaweeds need to be soaked to swell and then are pulped), adding a certain mass of wetting and penetrating agents after pulping, soaking and extracting, recovering part of the organic solvents through low temperature and low pressure distillation after soaking at a certain temperature for a period of time, finally obtaining seaweed residues and the seaweed extract through filter pressing, mixing the seaweed extract with microelements, heating and stirring the materials until the microelements are completely dissolved and carrying out spray drying, thus obtaining the product. The method has the beneficial technical effects that combining the microelements with active ingredients of the seaweeds, the product has obvious effects on improvement of the stress resistance and disease resistance of crops; and besides, being fully water-soluble, the product can meet the requirements of modern agriculture.
Description
Technical field
The present invention relates to a kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile.
Background technology
It is still strong acid, highly basic high temperature and high pressure extraction that the Sargassum liquid main flow extracting method of alga fertilizer is prepared by China, and this extracting mode not only breaks up the effective ingredient in Sargassum, and produces low with safety in utilization.The method utilizing microorganism enzymolysis and extraction also achieves some progress, but owing to enzymolysis time is long, causes that extraction efficiency is too low, it is impossible to meet the market demand.Currently also have method strong acid, highly basic high temperature and high pressure extraction combined with enzymolysis, although saved extraction time, but in strong acid, highly basic high temperature and high pressure extraction process still can to a certain extent to Sargassum in effective ingredient damage.
Summary of the invention
The technical problem to be solved is to provide a kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile.Active component in Sargassum is combined by the method with trace element, can improve crop disease-resistant, resistance, improves crop yield.
In order to solve above-mentioned technical problem, the present invention by the following technical solutions:
A kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile, it is characterised in that carry out according to following steps:
1), fresh Sargassum is cleaned standby, or dry seaweed be dipped to fresh Sargassum moisture consistent state and clean standby, the alternate products that this step obtains is called A product;
2), water, organic solvent and product A are added separately in reactor, pull an oar in the lump;
3), beaten and added wetting and penetrating agent after slurry, soaked 12~72 hours at 20~45 DEG C;
4), low-temp low-pressure Distillation recovery part organic solvent: vapo(u)rizing temperature is 45~65 DEG C, and distillation pressure is-0.5~-1.2Mpa;
5), filter pressing obtain Sargassum slag and filtrate, described filtrate is seaweed extracted liquor;
6), being mixed with trace element by described seaweed extracted liquor, heated and stirred is dissolved completely, obtains trace element water-soluble fertilizer after spray drying;
Wherein the mass ratio of A product, water, organic solvent and wetting and penetrating agent is 5~30:10~85:10~85:0.01~0.1;, seaweed extracted liquor and trace element mass ratio be 55~75:25~45.
Described organic solvent is the two or more of a kind of or arbitrary proportion in ethanol, ether, methanol and ethyl acetate.
Described wetting and penetrating agent is dodecylbenzene sodium sulfonate, sodium lauryl sulphate, alkylphenol polyoxyethylene, sorbitan fatty acid ester-20, sorbitan fatty acid ester-30, sorbitan fatty acid ester-80, polyoxyethylene 20 sorbitan monolaurate-20, polyoxyethylene 20 sorbitan monolaurate-40, polyoxyethylene 20 sorbitan monolaurate-60, polyoxyethylene 20 sorbitan monolaurate-80, fatty alcohol-polyoxyethylene ether-3, fatty alcohol-polyoxyethylene ether-4, fatty alcohol-polyoxyethylene ether-5, fatty alcohol-polyoxyethylene ether-7, fatty alcohol-polyoxyethylene ether-9, fatty alcohol-polyoxyethylene ether-15, fatty alcohol-polyoxyethylene ether-20, a kind of or arbitrary proportion in fatty alcohol-polyoxyethylene ether-23 and dimethyl-silicon wet goods two or more.
Described trace element is the two or more of a kind of or arbitrary proportion in ethylenediamine tetraacetic acid disodium zinc salt, disodiumedetate ferrous iron, disodiumedetate copper, disodiumedetate manganese, zinc sulphate heptahydrate, ferrous sulfate heptahydrate, copper sulphate pentahydrate, manganese sulfate monohydrate, ammonium molybdate, boric acid and Borax.
Described Sargassum refers to: a kind of or arbitrary proportion in Thallus Laminariae (Thallus Eckloniae), Thallus Porphyrae, Thallus Laminariae (Thallus Eckloniae), opotism and Entermorpha two or more.
In step 5), pressure filter selects filter cloth aperture to be 800~4500 orders.
In step 6), heated and stirred temperature controls at 40~65 DEG C.
The present invention has following Advantageous Effects:
1, in the present invention, Sargassum liquid adopts low temperature, Low Voltage Pure physics to extract, it is ensured that Sargassum effective ingredient is not destroyed.
2, seaweeds appearance has the protecting film of one layer of thickness; prevent external substance from invading; so simple water or organic solvent extract at normal temperatures and pressures can be very slow; the present invention adds wetting and penetrating agent can make the contact area of water and organic solvent and Sargassum increase; rapid solution breaks through described protecting film at normal temperatures and pressures; thus reaching the purpose of rapid extraction, therefore it is more convenient for the application of heavy industrialization.
3, the present invention adopts the extracting method that water and organic solvent combine, and reduces cost than simple organic solvent extraction.
4, the present invention adopts the extracting method that water and organic solvent combine, and adds the compatibility of product, meets the requirement of modern agriculture (water droplet filling).Because such as simple organic solvent extraction, it is possible to extract can not be dissolved completely in water, and product compatibility is poor, it is impossible to meets agricultural modernization (water droplet filling) requirement.
5, trace element effective ingredient in Sargassum is combined by the present invention, can significantly improve that crop is degeneration-resistant, disease resistance.
6, the present invention is entirely water-soluble meets modern agriculture demand.
Detailed description of the invention
The present invention is further illustrated below in conjunction with instantiation.
Embodiment 1
nullFresh Entermorpha after cleaning is joined in the reactor filling water and ethanol and pulls an oar,The sorbitan fatty acid ester-20 as wetting and penetrating agent and alkylphenol polyoxyethylene is added after making beating,Fresh Entermorpha、Water、Ethanol、Alkylphenol polyoxyethylene and sorbitan fatty acid ester-20 are 20:15:64.96:0.02:0.02 according to mass ratio,Soak 72 hours at 20 DEG C,In negative pressure 0.5Mpa,Distillation recovery part organic solvent under temperature 45 C,Pressure filter adopts 1000 order filter clothes to carry out filter pressing,Gained filtrate、Ethylenediamine tetraacetic acid disodium zinc salt、Disodiumedetate is ferrous、Disodiumedetate copper and boric acid mix according to mass ratio 65:15:10:9:1,Be heated to 40 DEG C of stirring and dissolving entirely complete after,Spray drying,Dried product is product of the present invention.
Embodiment 2
nullBy clean after dry Thallus Laminariae (Thallus Eckloniae) and dry Entermorpha be made into dry seaweed in proportion,It is dipped to and Fresh Laminaria Japonica moisture consistent state,Join and fill water、In the reactor of ethanol and ether,Pull an oar in the lump,The alkylphenol polyoxyethylene as wetting and penetrating agent and polyoxyethylene 20 sorbitan monolaurate-60 is added after making beating,The dry Thallus Laminariae (Thallus Eckloniae) soaked、Dry Entermorpha、Water、Ethanol、Ether、Mass ratio between alkylphenol polyoxyethylene and polyoxyethylene 20 sorbitan monolaurate-60 is 4:2:25:60.97:8:0.01:0.02,Soak 60 hours at 25 DEG C,In negative pressure 0.7Mpa,Distillation recovery part organic solvent under temperature 50 C,Pressure filter adopts 1200 order filter clothes to carry out filter pressing,Gained filtrate、Ethylenediamine tetraacetic acid disodium zinc salt、Zinc sulphate heptahydrate、Disodiumedetate manganese、Disodiumedetate copper and ammonium molybdate mix according to mass ratio 67.5:10:2:10:10:0.5,Be heated to 45 DEG C of stirring and dissolving entirely complete after,Spray drying,Dried product is product of the present invention.
Embodiment 3
nullFresh Laminaria Japonica after cleaning is joined and fills water、Ethanol、The reactor of ethyl acetate and ether is pulled an oar,The dodecylbenzene sodium sulfonate as wetting and penetrating agent is added after making beating、Alkylphenol polyoxyethylene、Sorbitan fatty acid ester-60 and dimethicone,Fresh Laminaria Japonica、Water、Ethanol、Ethyl acetate、Ether、Dodecylbenzene sodium sulfonate、Alkylphenol polyoxyethylene、Sorbitan fatty acid ester-60 and dimethicone are according to mass ratio 18:18:20:15:28.96:0.01:0.01:0.01:0.01,Soak 46 hours at 30 DEG C,In negative pressure 1.0Mpa,Distillation recovery part organic solvent at temperature 55 DEG C,Pressure filter adopts 1400 order filter clothes to carry out filter pressing,Gained filtrate mixes according to mass ratio 60:40 with zinc sulphate heptahydrate,Be heated to 50 DEG C of stirring and dissolving entirely complete after,Spray drying,Dried product is product of the present invention.
Embodiment 4
nullBy clean after dry Thallus Laminariae (Thallus Eckloniae)、Dry opotism and dry Entermorpha are made into dry seaweed in proportion,It is dipped to and Fresh Laminaria Japonica moisture consistent state,Join in the reactor filling water and ethanol and pull an oar,The sodium lauryl sulphate as wetting and penetrating agent and sorbitan fatty acid ester-60 is added after making beating,Dry Thallus Laminariae (Thallus Eckloniae) after immersion、Dry opotism、Dry Entermorpha、Water、Ether、Ethyl acetate、Sodium lauryl sulphate and sorbitan fatty acid ester-60 are according to mass ratio 3:3:1:25:25:42.96:0.02:0.02,Soak 24 hours at 35 DEG C,In negative pressure 1.2Mpa,Distillation recovery part organic solvent under temperature 50 C,Pressure filter adopts 2000 order filter clothes to carry out filter pressing,Gained filtrate、Ethylenediamine tetraacetic acid disodium zinc salt、Disodiumedetate is ferrous、Disodiumedetate manganese、Disodiumedetate copper、Boric acid and ammonium molybdate mix according to mass ratio 70:8:8:7.5:5:1:0.5,Be heated to 50 DEG C of stirring and dissolving entirely complete after,Spray drying,Dried product is product of the present invention.
Further illustrate below in conjunction with experimental data and the method have the benefit that
For the sample that Different Extraction Method on market is collected, carrying out the detection of Sargassum polysaccharides after oven drying at low temperature, testing result is table 1 such as.
Table 1
Highly basic extraction method | Highly basic adds enzymatic isolation method | Acidic hydrolysis | The inventive method | |
Sargassum polysaccharides (%) | 30.2 | 36.7 | 42.1 | 44.6 |
Adopt Sargassum polysaccharides content in this method extract the highest as can be seen from Table 1, Sargassum effective ingredient is destroyed minimum.
As follows with fertilizer efficiency experimental data under product equal conditions of the present invention for common trace element water-soluble fertile (except being not added with seaweed extracted liquor, other preparation condition is identical with product of the present invention):
1 materials and methods
1.1 experimental field overviews
Testing and carry out in self-operation experiment field, Fushan District, Yantai City, soil is brunisolic soil.Soil nutrient situation is: organic 78.3g/kg, alkali-hydrolyzable nitrogen 77.4mg/kg, available phosphorus 81.2mg/kg, available potassium 78.3mg/kg, pH6.00.
1.2 experiment materials to be tested
Fertile (except being not added with seaweed extracted liquor, other preparation condition is identical with the product of the present invention) sample of common trace element water-soluble and each 0.9kg of product of the present invention;1 mu of little Herba Spinaciae of same management.
1.3 experimental designs
Experiment is divided into 6 communities, and 2 communities are one group of totally 3 groups of experiment, repeats for 3 times, cross arrangement, divides 3 foliage-sprays according to plant growth situation, 0.1kg two kinds is tested fertilizer and is dissolved separately in 200kg water, and foliage-spray is in 2 communities respectively, repeats 3 times;Plot area 100m2,, surrounding sets protection row, north-south, line-spacing 25cm, spacing in the rows 12cm, every community 3333 strain.
1.4 experiments are implemented
Each process is except experiment fertilizer difference, and all consistent intensive shadow on lung of other agronomy control measures is sow August 27 in 2015, and JIUYUE 6 first time in 2015 processes, within 2015, JIUYUE 14 second time processes, within 2015, JIUYUE 22 third time processes, and October 4 in 2015 gathers in the crops, and adds up yield.
2 results and analysis
The impact on little Herba Spinaciae character of 2.1 different disposal
The little Herba Spinaciae spraying product of the present invention relatively compares, and will be obvious that leaf dark green is plump.The blade that the JIUYUE 13 little Herba Spinaciae of part in 2015 is old has light green speckle to occur, think it is lack trace element, JIUYUE 14 sprays to be remedied, large area is concentrated to occur in that light green speckle after one week, what have is puce, most vacuum side of blades are with bloom, and some blades even occur in that rotten, are identified as downy mildew.A number of having an attack of one's old illness has been checked by JIUYUE on the 21st, spray common trace element water-soluble fertile (except being not added with seaweed extracted liquor, other preparation condition is identical with product of the present invention) 3 communities totally 1215 strain blades of sample will be obvious that light green speckle or puce speckle, 3 communities totally 699 strain blades spraying product of the present invention will be obvious that light green speckle or puce speckle, and the disease resistance improving crop is had obvious effect by product of the present invention as can be seen from the data.
The impact on little Herba Spinaciae yield of 2.2 different disposal
Table 2
As can be seen from Table 2, the little Herba Spinaciae yield spraying product of the present invention significantly improves.
Note: this experiment, based on experiment, is observed therefore width is wanted in row, the relatively common plantation of spacing in the rows in order to convenient, and the more common plantation of yield is much lower.
3 discuss
Test the product just for the different manufacturers Different Extraction Method can bought on market, and it has been Sargassum polysaccharides detection and contrast experiment, being not necessarily of being commercially available is best, and notebook data can only illustrate most like products that product of the present invention is better than on market to have bought;Containing abundant active substance in Sargassum, how being maximally utilized by these active substances is the R&D direction in our future.
Claims (7)
1. one kind utilizes the production method that seaweed extracted liquor coproduction trace element water-soluble is fertile, it is characterised in that carry out according to following steps:
1), fresh Sargassum is cleaned standby, or dry seaweed be dipped to fresh Sargassum moisture consistent state and clean standby, the alternate products that this step obtains is called A product;
2), water, organic solvent and product A are added separately in reactor, pull an oar in the lump;
3), beaten and added wetting and penetrating agent after slurry, soaked 12~72 hours at 20~45 DEG C;
4), low-temp low-pressure Distillation recovery part organic solvent: vapo(u)rizing temperature is 45~65 DEG C, and distillation pressure is-0.5~-1.2Mpa;
5), filter pressing obtain Sargassum slag and filtrate, described filtrate is seaweed extracted liquor;
6), being mixed with trace element by described seaweed extracted liquor, heated and stirred is dissolved completely, obtains trace element water-soluble fertilizer after spray drying;
Wherein the mass ratio of A product, water, organic solvent and wetting and penetrating agent is 5~30:10~85:10~85:0.01~0.1;, seaweed extracted liquor and trace element mass ratio be 55~75:25~45.
2. a kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile as claimed in claim 1, it is characterised in that: described organic solvent is the two or more of a kind of or arbitrary proportion in ethanol, ether, methanol and ethyl acetate.
null3. a kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile as claimed in claim 1,It is characterized in that: described wetting and penetrating agent is dodecylbenzene sodium sulfonate、Sodium lauryl sulphate、Alkylphenol polyoxyethylene、Sorbitan fatty acid ester-20、Sorbitan fatty acid ester-30、Sorbitan fatty acid ester-80、Polyoxyethylene 20 sorbitan monolaurate-20、Polyoxyethylene 20 sorbitan monolaurate-40、Polyoxyethylene 20 sorbitan monolaurate-60、Polyoxyethylene 20 sorbitan monolaurate-80、Fatty alcohol-polyoxyethylene ether-3、Fatty alcohol-polyoxyethylene ether-4、Fatty alcohol-polyoxyethylene ether-5、Fatty alcohol-polyoxyethylene ether-7、Fatty alcohol-polyoxyethylene ether-9、Fatty alcohol-polyoxyethylene ether-15、Fatty alcohol-polyoxyethylene ether-20、A kind of or arbitrary proportion in fatty alcohol-polyoxyethylene ether-23 and dimethyl-silicon wet goods two or more.
4. a kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile as claimed in claim 1, it is characterised in that: described trace element is the two or more of a kind of or arbitrary proportion in ethylenediamine tetraacetic acid disodium zinc salt, disodiumedetate ferrous iron, disodiumedetate copper, disodiumedetate manganese, zinc sulphate heptahydrate, ferrous sulfate heptahydrate, copper sulphate pentahydrate, manganese sulfate monohydrate, ammonium molybdate, boric acid and Borax.
5. a kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile as claimed in claim 1, it is characterised in that: described Sargassum refers to: a kind of or arbitrary proportion in Thallus Laminariae (Thallus Eckloniae), Thallus Porphyrae, Thallus Laminariae (Thallus Eckloniae), opotism and Entermorpha two or more.
6. a kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile as claimed in claim 1, it is characterised in that: in step 5), pressure filter selects filter cloth aperture to be 800~4500 orders.
7. a kind of production method utilizing seaweed extracted liquor coproduction trace element water-soluble fertile as claimed in claim 1, it is characterised in that: in step 6), heated and stirred temperature controls at 40~65 DEG C.
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