CN117567185A - Preparation method of refining product of phyllophyllum nodosum for water-soluble fertilizer - Google Patents
Preparation method of refining product of phyllophyllum nodosum for water-soluble fertilizer Download PDFInfo
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- CN117567185A CN117567185A CN202311536953.5A CN202311536953A CN117567185A CN 117567185 A CN117567185 A CN 117567185A CN 202311536953 A CN202311536953 A CN 202311536953A CN 117567185 A CN117567185 A CN 117567185A
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 45
- 238000007670 refining Methods 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 241000512259 Ascophyllum nodosum Species 0.000 claims abstract description 42
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000227 grinding Methods 0.000 claims abstract description 34
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- 238000000034 method Methods 0.000 claims abstract description 20
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 16
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 16
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- 238000004519 manufacturing process Methods 0.000 claims description 9
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- 229930187380 Inophyllum Natural products 0.000 claims description 6
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- 241000199919 Phaeophyceae Species 0.000 description 7
- 239000000648 calcium alginate Substances 0.000 description 7
- 235000010410 calcium alginate Nutrition 0.000 description 7
- 229960002681 calcium alginate Drugs 0.000 description 7
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 description 7
- 150000002482 oligosaccharides Chemical class 0.000 description 6
- -1 pectase Proteins 0.000 description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 5
- 241000195493 Cryptophyta Species 0.000 description 5
- 239000011575 calcium Substances 0.000 description 5
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- 239000005017 polysaccharide Substances 0.000 description 5
- 150000004804 polysaccharides Chemical class 0.000 description 5
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 4
- 229910001424 calcium ion Inorganic materials 0.000 description 4
- 210000002421 cell wall Anatomy 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 3
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- 238000010521 absorption reaction Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229940088598 enzyme Drugs 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
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- 230000002195 synergetic effect Effects 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000004902 Softening Agent Substances 0.000 description 2
- 241000209140 Triticum Species 0.000 description 2
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- 239000007787 solid Substances 0.000 description 2
- CJUUXVFWKYRHAR-UHFFFAOYSA-M 1-Naphthaleneacetic acid sodium salt Chemical compound [Na+].C1=CC=C2C(CC(=O)[O-])=CC=CC2=C1 CJUUXVFWKYRHAR-UHFFFAOYSA-M 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
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- UBXYXCRCOKCZIT-UHFFFAOYSA-N biphenyl-3-ol Chemical group OC1=CC=CC(C=2C=CC=CC=2)=C1 UBXYXCRCOKCZIT-UHFFFAOYSA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
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- 238000001914 filtration Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000003895 organic fertilizer Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 239000005648 plant growth regulator Substances 0.000 description 1
- 108010004131 poly(beta-D-mannuronate) lyase Proteins 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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- 239000002689 soil Substances 0.000 description 1
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- 239000011782 vitamin Substances 0.000 description 1
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Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F17/00—Preparation of fertilisers characterised by biological or biochemical treatment steps, e.g. composting or fermentation
- C05F17/20—Preparation of fertilisers characterised by biological or biochemical treatment steps, e.g. composting or fermentation using specific microorganisms or substances, e.g. enzymes, for activating or stimulating the treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Tropical Medicine & Parasitology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Molecular Biology (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a preparation method of a refining product of phyllophyllum nodosum for water-soluble fertilizer, and belongs to the technical field of phyllophyllum nodosum treatment. The method comprises the following steps: crushing the dry phyllophyllum nodosum to more than 200 meshes to obtain crushed phyllophyllum nodosum particles; taking water, ammonium bicarbonate and alginic acid lyase as softeners, adjusting the pH value of a softener system to 7-9, uniformly stirring crushed phyllophyllum nodosum particles and the softeners, and soaking and softening at normal temperature to obtain softened phyllophyllum nodosum; acetic acid is used as an acidulant, the pH value of the acidulant system is regulated to be 4-5, and softened Ascophyllum nodosum subjected to grinding step and the acidulant are mixed and acidified to obtain Ascophyllum nodosum refined product. The invention is applied to the aspect of water-soluble fertilizer, solves the problems of high separation difficulty of degradation products and limitation of the compounding property of the seaweed extract in the preparation of the seaweed extract for the existing fertilizer, realizes the degradation and utilization of the whole seaweed, and has the characteristics of normal-temperature extraction, high content of active ingredients, good compounding property and suitability for industrialization.
Description
Technical Field
The invention belongs to the technical field of Ascophyllum nodosum treatment, and particularly relates to a preparation method of an Ascophyllum nodosum refined product for a water-soluble fertilizer.
Background
The leaf-soaking algae is rich in more than 40 mineral elements such as K, ca, mg, fe, zn, I, rich vitamins, algal polysaccharide, highly unsaturated fatty acid and various natural plant growth regulators, has high biological activity, can stimulate the generation of non-specific active factors in plants, regulates the balance of endogenous hormones, and has extremely strong growth promoting effect on crops.
The existing seaweed fertilizer extraction and preparation technology mainly comprises a chemical extraction method, a physical extraction method and a biological extraction method. Wherein, the chemical extraction method utilizes acid, alkali and organic solvent to treat seaweed cells to make the cells digested or endogenous substances solubilized, the method is simple and easy to operate, but the chemical reagent has great destructiveness on active substance components in seaweed cells; the physical method mainly comprises a homogenization filtration method, a osmotic shock method, an ultrasonic crushing method, a grinding method, a high-pressure homogenization method, a freeze crushing method and other methods for crushing seaweed cells, the seaweed extract obtained by the physical method is in a viscous slurry shape, has large molecular weight, mainly exists in the form of water insoluble matters, and has low utilization rate of seaweed active substances; the biological extraction method comprises enzyme hydrolysis extraction method and microorganism fermentation method, wherein the enzyme hydrolysis method comprises adding one or more of protease, pectase, cellulase, lyase, and oxidoreductase into seaweed slurry step by step or mixing, and degrading protein, polysaccharide, pectin, cellulose, etc. in seaweed cell wall into small molecule substances which are easy to be absorbed and utilized by plants, so as to release cell contents.
The main synergistic component for promoting plant growth in seaweed is degraded micromolecular alginic acid, the seaweed is soaked in water and then degraded by chemical, physical or biological methods, the finally separated clear liquid can be used as a synergistic fertilizer raw material for water-soluble fertilizer, and the separated water-insoluble seaweed residues have good water absorption and water retention properties and can be used for slow-release nutrition of organic fertilizer and soil improvement. However, problems with existing seaweed treatments include: 1. the difficulty of the existing seaweed extracts for fertilizers is the separation of degradation products, the separation of solid substances from viscous liquids, or the removal of gelatinous precipitates. The higher the concentration of the materials is, the harder the separation is, the seaweed is generally soaked by 10-30 times of water to realize solid-liquid separation, the alginic acid content of the liquid is generally 5-20g/L, the high-multiple water extraction leads to low content of active ingredients of the extracting solution, and the concentration cost is increased; 2. the chemical method has high temperature and high alkali, and the loss of active ingredients, such as 27-56% alginic acid, is converted into various carboxylic acid products under the condition of high temperature and high alkali, and the activity is low. Converting the mineral element alkaline condition into a precipitate; 3. the physical extraction method is that alginic acid in seaweed still exists mainly in the form of calcium alginate and has large molecular weight, so that the alginic acid cannot be effectively utilized by plants; 4. the existing enzymatic extraction is mainly suitable for processing kelp, has poor degradation effects on Ascophyllum nodosum, sargassum and the like, and has poor enzymolysis effect due to the fact that partial calcium alginate is embedded in the cell wall thickness and the enzyme cannot contact with a substrate. The water-soluble organic component content of the phyllophyllum nodosum is high, and the phyllophyllum nodosum is the best raw material for preparing the seaweed fertilizer currently accepted; 5. the existing seaweed extract has limitation on the compounding property, such as water insoluble flocculation formed by multivalent metal ions such as calcium or the like or acidic conditions.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to solve the technical problems that the existing seaweed extract for the fertilizer has high separation difficulty of degradation products and limitation of the compounding property of the seaweed extract, and provides the preparation method of the refining product of the water-soluble seaweed for the fertilizer, which realizes the degradation and utilization of the whole seaweed, has the characteristics of normal-temperature extraction, high active ingredient content, good compounding property and suitability for industrialization.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a preparation method of a refining product of phyllophyllum nodosum for water-soluble fertilizer, which comprises the following steps: a crushing step, a softening step, a grinding step and an acidification step; the crushing step comprises the following steps: crushing the dry phyllophyllum nodosum to more than 200 meshes to obtain crushed phyllophyllum nodosum particles; the softening step comprises the following steps: taking water, ammonium bicarbonate and alginic acid lyase as softeners, adjusting the pH value of a softener system to 7-9, uniformly stirring the crushed phyllophyllum nodosum particles and the softeners, and soaking and softening at normal temperature to obtain softened phyllophyllum nodosum; the acidification step comprises: acetic acid is used as an acidulant, the pH value of the acidulant system is regulated to be 4-5, and the softened Ascophyllum nodosum subjected to the grinding step and the acidulant are mixed and acidified to obtain the Ascophyllum nodosum refined product.
Preferably, in the softening step, the weight of water in the softener is 3-5 times of the weight of the crushed Ascophyllum nodosum particles.
Preferably, in the softening step, the weight of ammonium bicarbonate in the softener is 5-10% of the weight of the crushed phyllophyllum nodosum particles.
Preferably, the grinding step adopts a grinder to grind the softened Ascophyllum nodosum until no obvious particles exist.
Preferably, the grinding step further includes: and taking a small amount of ground mixed liquid sample, adding water to dilute the mixed liquid sample to 200 times, observing the diluted mixed liquid state, and finishing grinding if no obvious insoluble matter exists, or else continuing grinding.
Preferably, the seaweed microparticle mixture with the particle size of 10um is obtained after the grinding step.
Preferably, the refining product of Ascophyllum nodosum obtained after the acidification step comprises water-soluble active ingredients and alginate fiber particles, and the water insoluble matter is less than 30g/L.
Preferably, the method further comprises a xanthan gum suspending step after the acidification step, and the xanthan gum suspending step comprises the following steps: and slowly adding xanthan gum into the refining product of the phyllophyllum inophyllum, fully stirring and grinding until the xanthan gum is completely dissolved, and obtaining brown to green uniform and stable refining product suspension of the phyllophyllum inophyllum for the water-soluble fertilizer.
Preferably, the amount of the xanthan gum used in the xanthan gum suspending step is 1-3 per mill of the weight of the refining product of Ascophyllum nodosum.
Preferably, the softening step is performed by soaking and softening for more than 8 hours at normal temperature.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of a refining product of Ascophyllum nodosum for water-soluble fertilizer, which comprises the steps of crushing Ascophyllum nodosum She Zaochao to more than 200 meshes to obtain micron-sized micronized Ascophyllum nodosum, adding water, ammonium bicarbonate and alginic acid lyase to obtain a mixed solution of Ascophyllum nodosum particles, grinding by a grinder to obtain a mixed solution of seaweed particles, adding acetic acid for acidizing after enzymolysis is finished, wherein the alginic acid content in the obtained refining product of Ascophyllum nodosum is more than or equal to 50g/L, so that the degradation and utilization of whole seaweed are realized, and the refining product has the characteristics of normal-temperature extraction, high active ingredient content, good complexing property and suitability for industrialization.
Drawings
Fig. 1 is a schematic process flow diagram of a preparation method of a refining product of phyllophyllum nodosum for water-soluble fertilizer.
Detailed Description
The following detailed description of the technical solutions in the specific embodiments of the present invention will be given with reference to the accompanying drawings. It is apparent that the described embodiments are only some specific implementations, but not all implementations, of the general technical solution of the present invention. All other embodiments, which are obtained by those skilled in the art based on the general inventive concept, fall within the scope of the present invention.
The invention provides a preparation method of a refining product of phyllophyllum nodosum for water-soluble fertilizer, which is shown in figure 1 and comprises the following steps: a crushing step, a softening step, a grinding step and an acidification step; the crushing step comprises the following steps: crushing the dry phyllophyllum nodosum to more than 200 meshes to obtain crushed phyllophyllum nodosum particles; the softening step comprises the following steps: taking water, ammonium bicarbonate and alginic acid lyase as softeners, adjusting the pH value of a softener system to 7-9, uniformly stirring the crushed phyllophyllum nodosum particles and the softeners, and soaking and softening at normal temperature to obtain softened phyllophyllum nodosum; the acidification step comprises: acetic acid is used as an acidulant, the pH value of the acidulant system is regulated to be 4-5, and the softened Ascophyllum nodosum subjected to the grinding step and the acidulant are mixed and acidified to obtain the Ascophyllum nodosum refined product. In a preferred embodiment, the softening step is performed by soaking at normal temperature for more than 8 hours. According to the preparation method of the refining product of the phyllophyllum nodosum for the water-soluble fertilizer, the phyllophyllum nodosum which is micronized by crushing the phyllophyllum nodosum She Zaochao to more than 200 meshes is obtained, water, ammonium bicarbonate and alginic acid lyase are added to obtain a mixed solution of phyllophyllum nodosum particles, the mixed solution of the phyllophyllum nodosum particles is obtained through grinding by a grinder, and acetic acid is added for acidizing treatment after enzymolysis is finished, so that the degradation and utilization of whole alga are realized, and the refining product has the characteristics of normal-temperature extraction, high active ingredient content, good compounding property and suitability for industrialization. In the step, the crushing step is to crush the dry leaf algae to above 200 meshes of granularity, and break up the seaweed fibers to realize micronization; the softening step is favorable for releasing alkali-soluble calcium alginate and performing oligosaccharide, and the main components of the obtained mixed solution are brown alginate oligosaccharides, fucoidin and other polysaccharides, alginate fibers, mannitol and the like; the grinding step realizes the liquefaction effect, is favorable for fully releasing alkali-soluble calcium alginate and performing oligosaccharide; the acidification step is favorable for releasing mineral elements such as calcium and the like and acid-soluble fucoidin, creating an acidic environment, realizing the alginate oligosaccharide hydrolysis, releasing more water-soluble components in the algae, and enabling the alginate oligosaccharide to coexist with the ionized mineral elements without flocculation.
The refining product of the phyllophyllum comosum, which is obtained by the technical scheme, is a mixture containing the whole phyllophyllum comosum, contains water-soluble active ingredients and seaweed fiber particles, wherein the water-insoluble matters of the refining product are less than 30g/L, and meet the requirement of water-soluble fertilizer. According to the technical scheme, the phyllophyllum comosum is crushed in a micron order and subjected to combined enzymolysis to obtain the visual sensory water-soluble primary pulp, so that the sensory quality of the phyllophyllum comosum refined product after commercialization is improved. In the prior art, seaweed is extracted by soaking the seaweed with 10-30 times of water in the treatment process, and the seaweed fiber is crushed to greatly weaken the water absorption capacity, 3-5 times of water soaking extraction is realized under the link of removing solid-liquid separation, the water adding amount is greatly reduced, the concentration of active ingredients is improved, leaching of low-multiple water is realized in production, the links of solid-liquid separation and concentration links after extraction in the prior art are replaced, and full liquefaction and full utilization of the seaweed are realized. By utilizing the synergistic effect of alginic acid lyase and acetic acid, the dissolution of mineral elements such as calcium and acid-soluble components such as acid-soluble polysaccharide in the refining product of the Ascophyllum nodosum is realized, so that the acidic refining product of the Ascophyllum nodosum is obtained.
The enzymolysis process defining the softening step is performed under weak alkaline conditions, because the calcium alginate as an active ingredient in brown algae can be converted into water-soluble alginate under alkaline conditions. The technical scheme of the application specifically limits the use of water, ammonium bicarbonate and alginic acid lyase as softeners, because the pH value of the mixture of water, ammonium bicarbonate and brown algae is 7-8.5, the ammonium bicarbonate is weak base, damage to active ingredients of the brown algae is avoided, the activity of the alginic acid lyase is not affected, the ammonium bicarbonate is a fertilizer nutrient, water-soluble alginate and water-insoluble calcium alginate exist in brown algae, the water-soluble alginate is converted into brown alginate oligosaccharide under the action of the alginic acid lyase, the characteristic of forming water-insoluble gel with calcium is lost, under the existence of water-soluble micromolecular alginate (brown alginate oligosaccharide) and ammonium bicarbonate, calcium ions in the calcium alginate are subjected to ion exchange and are slowly dissolved, and the dissolved calcium ions can be degraded by the alginate lyase, so that the oligosaccharide degradation of alginic acid ingredients in the brown algae is finally realized. The technical scheme of the application also limits the use of acetic acid as an acidulant, because, on one hand, acetic acid is a fertilizer nutrient, on the other hand, acetic acid and free calcium ions cannot generate precipitate, and acetic acid is weak acid, so that the destruction to seaweed active ingredients is avoided, and in addition, acetic acid enables the brown seaweed oligosaccharide to have the characteristic of coexistence with high-concentration calcium ions and not flocculating and precipitating, so that the refining product of the phyllophyllum nodosum can be used for preparing a medium-element water-soluble fertilizer, and the calcium content concentration reaches more than 10%.
In a preferred embodiment, in the softening step, the weight of water in the softener is 3 to 5 times the weight of the crushed Ascophyllum nodosum particles. According to the technical scheme, the seaweed fiber is crushed, so that the water absorption capacity of the seaweed fiber is greatly weakened, 3-5 times of water immersion extraction is realized under the link of removing solid-liquid separation, the water adding amount is greatly reduced, the concentration of effective components is improved, leaching of low-multiple water is realized in production, the link of solid-liquid separation after extraction and the concentrating link in the prior art process are replaced, and full liquefaction and full utilization of the oak are realized.
In a preferred embodiment, in the softening step, the weight of ammonium bicarbonate in the softener is 5-10% of the weight of the crushed phyllophyllum nodosum particles. It will be appreciated that the weight of ammonium bicarbonate in the softener may also be any point value within 6%, 7%, 8%, 9% and ranges thereof of the weight of the crushed phyllophyllum nodosum particles.
In a preferred embodiment, the grinding step uses a grinder to grind the softened Ascophyllum nodosum until no distinct particles are present. In order to determine the degree of grinding, the grinding step further includes: and taking a small amount of ground mixed liquid sample, adding water to dilute the mixed liquid sample to 200 times, observing the diluted mixed liquid state, and finishing grinding if no obvious insoluble matter exists, or else continuing grinding. And (3) obtaining the seaweed particle mixed solution with the particle size of 10um after the grinding step. The grinding step specifically comprises the following steps: setting parameters of a grinder, grinding the mixed solution until no obvious particles exist, so that alginic acid on the cell wall of the alga body is fully contacted with alginic acid lyase, and the reaction is complete; taking a small amount of ground mixed liquid sample, adding water to dilute the mixed liquid sample to 200 times, observing the state of the diluted mixed liquid, and showing a state without obvious insoluble substances, which indicates that alginic acid in cell walls of Ascophyllum nodosum is degraded for the second time, and completely reacting to generate water-soluble brown algae oligosaccharide, wherein algae is completely liquefied.
In a preferred embodiment, said refining of Ascophyllum nodosum obtained after said acidification step comprises water-soluble active principles and fine particles of alginate fibers, water insolubles < 30g/L. The refining product of the phyllophyllum nodosum meets the requirement of a water-soluble fertilizer, and when the fertilizer is applied, the water-soluble part of the refining product can be quickly absorbed by crops, and the seaweed fiber particles are slowly degraded and slowly absorbed. According to the technical scheme, the solid-liquid separation link is omitted through the improvement of the method, and the full utilization of seaweed is realized.
In a preferred embodiment, the method further comprises a xanthan gum suspending step after the acidifying step, the xanthan gum suspending step comprising: and slowly adding xanthan gum into the refining product of the phyllophyllum inophyllum, fully stirring and grinding until the xanthan gum is completely dissolved, and obtaining brown to green uniform and stable refining product suspension of the phyllophyllum inophyllum for the water-soluble fertilizer. In a preferred embodiment, the xanthan gum is used in the step of suspending the xanthan gum in an amount of 1 to 3% by weight of the refining product of Ascophyllum nodosum. The refining suspension of the phyllophyllum nodosum for the water-soluble fertilizer, which is obtained by the technical scheme, is rich in active ingredients such as water-soluble oligosaccharides, polysaccharides and the like, realizes the full utilization of the phyllophyllum nodosum, and can be used in the water-soluble fertilizer.
In order to more clearly and in detail describe the preparation method of the refining product of the phyllophyllum nodosum for the water-soluble fertilizer provided by the embodiment of the invention, the following description will be made with reference to specific embodiments.
Example 1
1. Crushing the dry leaf-soaking algae particles into 200 meshes, and weighing 500g.
2. Preparing a softening agent: 2500g of water, 25g of ammonium bicarbonate and 0.2g of alginic acid lyase. Adding Ascophyllum nodosum powder into softening agent, stirring thoroughly, and standing for 8 hr.
3. Repeatedly grinding the mixed solution by a grinder until no obvious particles exist. About 1g of the ground sample was taken and added to 200mL of water, resulting in no significant insoluble material. The standing was continued for 8 hours.
4. Detecting the pH of the material after standing, and adding acetic acid to adjust the pH to 4.0.
5. 5g of xanthan gum is taken and slowly added into the materials, and the materials are fully stirred and ground until the materials are completely dissolved. The green refining product of Ascophyllum nodosum is obtained, and the solid content is 23%.
The detection is carried out according to the requirements of organic water-soluble fertilizers, and the appearance and technical index requirements of alginic acid (liquid) as a fertilizer synergist are shown in table 1:
the water-insoluble substances are detected according to the determination of the water-insoluble substance content and the pH of NY/T1973-2021 water-soluble fertilizer: 5g/L meets the requirement that the water insoluble matters in HG/T5932-2021 fertilizer synergist alginic acid are less than or equal to 30 g/L;
detecting according to m-hydroxybiphenyl spectrophotometry, and the content of alginic acid: 60g/L meets the requirement that the high-content alginic acid synergist in HG/T5932-2021 fertilizer synergist alginic acid is more than or equal to 50 g/L.
TABLE 1 Fertilizer synergist alginic acid (liquid) appearance and technical index requirements
Example 2
The test method comprises the following steps: treating wheat seeds with 5% hydrogen peroxide for 10 min for sterilization, and then washing with clear water for 3 times; the refining products of Ascophyllum nodosum obtained in example 1 were immersed in 0.5ppm, 1ppm and 5ppm sodium naphthalene acetate solutions for 6 hours at 5ppm, 10ppm, 50ppm and 100ppm, then cultured on wet filter paper, and shoot length and root length were measured on day 10.
The results are shown in Table 2: the refining product of the phyllophyllum nodosum has a promoting effect on the growth of wheat buds and root systems at a set concentration, and has obvious difference from a control ratio.
Table 2 control results
Claims (10)
1. The preparation method of the refining product of the phyllophyllum nodosum for the water-soluble fertilizer is characterized by comprising the following steps of: a crushing step, a softening step, a grinding step and an acidification step;
the crushing step comprises the following steps: crushing the dry phyllophyllum nodosum to more than 200 meshes to obtain crushed phyllophyllum nodosum particles;
the softening step comprises the following steps: taking water, ammonium bicarbonate and alginic acid lyase as softeners, adjusting the pH value of a softener system to 7-9, uniformly stirring the crushed phyllophyllum nodosum particles and the softeners, and soaking and softening at normal temperature to obtain softened phyllophyllum nodosum;
the acidification step comprises: acetic acid is used as an acidulant, the pH value of the acidulant system is regulated to be 4-5, and the softened Ascophyllum nodosum subjected to the grinding step and the acidulant are mixed and acidified to obtain the Ascophyllum nodosum refined product.
2. The method for producing a refining product of Ascophyllum nodosum for a water-soluble fertilizer according to claim 1, wherein in the softening step, the weight of water in the softener is 3 to 5 times the weight of the pulverized Ascophyllum nodosum particles.
3. The method for producing a refining product of Ascophyllum nodosum for a water-soluble fertilizer according to claim 1, wherein in the softening step, the weight of ammonium bicarbonate in the softener is 5-10% of the weight of the crushed Ascophyllum nodosum particles.
4. The method for producing a refining product of Ascophyllum nodosum for a water-soluble fertilizer according to claim 1, wherein the grinding step is carried out by grinding the softened Ascophyllum nodosum with a grinder until no distinct particles are present.
5. The method for producing a refining product of Ascophyllum nodosum for a water-soluble fertilizer according to claim 4, wherein the grinding step further comprises: and taking a small amount of ground mixed liquid sample, adding water to dilute the mixed liquid sample to 200 times, observing the diluted mixed liquid state, and finishing grinding if no obvious insoluble matter exists, or else continuing grinding.
6. The method for producing a refining product of Ascophyllum nodosum for a water-soluble fertilizer according to claim 5, wherein the grinding step is followed by obtaining a mixed solution of fine particles of seaweed having a particle size of 10 μm.
7. The method for producing a refining product of Ascophyllum nodosum for water-soluble fertilizer according to claim 1, wherein the refining product of Ascophyllum nodosum obtained after the acidification step contains water-soluble active ingredients and alginate fiber particles, and the water-insoluble matter is less than 30g/L.
8. The method for preparing a refining product of a water-soluble fertilizer by using a phyllophyllum nodosum according to claim 1, further comprising a xanthan gum suspending step after the acidification step, wherein the xanthan gum suspending step comprises: and slowly adding xanthan gum into the refining product of the phyllophyllum inophyllum, fully stirring and grinding until the xanthan gum is completely dissolved, and obtaining brown to green uniform and stable refining product suspension of the phyllophyllum inophyllum for the water-soluble fertilizer.
9. The method of claim 8, wherein the xanthan gum is used in an amount of 1-3% by weight of the refining product.
10. The method for producing a refining product of Ascophyllum nodosum for a water-soluble fertilizer according to claim 1, wherein the softening step is performed by soaking at room temperature for 8 hours or more.
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