CN113816806A - Humic acid water-soluble fertilizer, preparation method and application - Google Patents
Humic acid water-soluble fertilizer, preparation method and application Download PDFInfo
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- CN113816806A CN113816806A CN202111142424.8A CN202111142424A CN113816806A CN 113816806 A CN113816806 A CN 113816806A CN 202111142424 A CN202111142424 A CN 202111142424A CN 113816806 A CN113816806 A CN 113816806A
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 106
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000004021 humic acid Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002351 wastewater Substances 0.000 claims abstract description 37
- 150000001875 compounds Chemical class 0.000 claims abstract description 30
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011591 potassium Substances 0.000 claims abstract description 21
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 21
- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 16
- 238000001704 evaporation Methods 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 13
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 239000002699 waste material Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000008346 aqueous phase Substances 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000003245 coal Substances 0.000 claims description 6
- 235000021049 nutrient content Nutrition 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 24
- 239000002689 soil Substances 0.000 abstract description 21
- 238000003860 storage Methods 0.000 abstract description 5
- 239000007789 gas Substances 0.000 abstract description 3
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 27
- 241000219109 Citrullus Species 0.000 description 23
- 235000012828 Citrullus lanatus var citroides Nutrition 0.000 description 23
- 238000011282 treatment Methods 0.000 description 13
- 238000005507 spraying Methods 0.000 description 8
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 235000013399 edible fruits Nutrition 0.000 description 5
- 235000015097 nutrients Nutrition 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000618 nitrogen fertilizer Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- FVBHYZVVSXFCOO-UHFFFAOYSA-N tert-butyl hydrogen sulfate Chemical compound CC(C)(C)OS(O)(=O)=O FVBHYZVVSXFCOO-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000008635 plant growth Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- WOFMVUZGDHWHLJ-UHFFFAOYSA-N 7,7-dimethyloctanoyl chloride Chemical compound CC(C)(C)CCCCCC(Cl)=O WOFMVUZGDHWHLJ-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000035558 fertility Effects 0.000 description 2
- 230000012010 growth Effects 0.000 description 2
- 238000003973 irrigation Methods 0.000 description 2
- 230000002262 irrigation Effects 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 244000144730 Amygdalus persica Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 240000008067 Cucumis sativus Species 0.000 description 1
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000219146 Gossypium Species 0.000 description 1
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 235000011430 Malus pumila Nutrition 0.000 description 1
- 235000015103 Malus silvestris Nutrition 0.000 description 1
- 239000005802 Mancozeb Substances 0.000 description 1
- 241000233679 Peronosporaceae Species 0.000 description 1
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- 240000003768 Solanum lycopersicum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 244000098338 Triticum aestivum Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
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- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 239000010871 livestock manure Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000021048 nutrient requirements Nutrition 0.000 description 1
- 239000003895 organic fertilizer Substances 0.000 description 1
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- 231100000719 pollutant Toxicity 0.000 description 1
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- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 description 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G22/00—Cultivation of specific crops or plants not otherwise provided for
-
- 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
- C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
Abstract
The invention discloses a humic acid water-soluble fertilizer, a preparation method and application thereof, wherein the humic acid water-soluble fertilizer contains 90-95% of compound fertilizer wastewater concentrated solution and 5-10% of potassium humate by mass, and the humic acid water-soluble fertilizer is prepared by utilizing wastewater generated in the existing compound fertilizer production process and tert-butyl peroxyneodecanoate wastewater. The humic acid water-soluble fertilizer prepared by the invention can enhance the water storage and retention capacity of soil, effectively improve the water, fertilizer, gas and heat conditions of the soil and enable the soil to become loose and fertile.
Description
Technical Field
The invention relates to the field of fertilizers, in particular to a humic acid-containing water-soluble fertilizer prepared from wastewater generated in compound fertilizer production, and a preparation method and application thereof.
Background
The humic acid water soluble fertilizer is an organic fertilizer, contains a large number of elements (nitrogen, phosphorus and potassium) required by plant growth and mineral source humic acid, and is mainly characterized by that it adopts water fertilizer and water fertilizer to apply simultaneously, and uses water to bring fertilizer, its effective absorption rate is more than one time higher than that of general chemical fertilizer, and its fertilizer efficiency is quick, and can meet the nutrient requirement of high-yield crops in quick growth period.
The application of the humic acid water-soluble fertilizer has a plurality of benefits on soil, on one hand, the fertilizer can increase the content of organic matters in the soil, effectively relieve soil hardening, improve the ecological environment of root systems, influence soil microorganisms, keep the activity of nutrient elements, simultaneously adjust the pH value of the soil, improve the cation exchange capacity and the soil moisture preservation capacity of the soil, keep the soil in good ventilation condition and warm condition, enhance the fertilizer preservation, fertilizer supply and buffer capacity of the soil, facilitate the release and preservation of nutrients, and facilitate cultivation and the growth and development of crop root systems; on the other hand, the fertilizer does not generate antagonism, can chelate calcium and magnesium ions in water soil, can completely avoid the generation of scale, and has the advantages of various formulas, less dosage, convenient application and low application cost compared with the traditional fertilizer.
Humic acid is formed by decomposing plant residues and is widely present in soil, river mud, and shallowly buried weathered coal, turf and lignite. Humic acid can produce adsorption action, reduce nitrogen leaching loss and phosphorus and potassium fixation, so that its fertilizer efficiency is raised. The humic acid is organically combined with the nitrogen fertilizer, so that nitrification can be inhibited, the loss of the nitrogen fertilizer and nitrogen pollution caused by the loss of the nitrogen fertilizer can be reduced, and the utilization rate of the nitrogen fertilizer can be improved. Humic acid contains various active groups with strong physiological activity, can stimulate the growth of plants, improve the activity of enzymes in crops, regulate metabolism, improve the activity of root systems and enhance the stress resistance. Meanwhile, after the humic acid is sprayed on the leaf surface, the pores of the leaf surface are reduced, the water transpiration is reduced, and the drought resistance of crops is improved.
The existing humic acid fertilizer is mostly produced by using waste water generated in fertilizer production as a raw material, but nutrient components in most kinds of waste water do not reach the standard, harmful substances exist, and the waste water is utilized and is not suitable for storage after being prepared, so that nutrient substances need to be supplemented in the preparation process, or the humic acid fertilizer is additionally applied to plants after being applied, the aim of completely utilizing the waste water cannot be achieved, in addition, the burden of the plants and the workload of operators are inevitably increased, particularly, the whole operation speed is slowed down and the plant growth is influenced during large-scale planting.
Disclosure of Invention
The invention aims to provide a humic acid water-soluble fertilizer, which can enhance the water storage and retention capacity of soil, effectively improve the water, fertilizer, gas and heat conditions of the soil and enable the soil to become loose and fertile.
The invention also aims to provide a preparation method of the humic acid water-soluble fertilizer, which can be used for preparing the humic acid water-soluble fertilizer by utilizing the waste water generated in the existing compound fertilizer production process and the tert-butyl peroxyneodecanoate waste water.
The invention further aims to provide application of the humic acid water-soluble fertilizer.
The invention discloses a humic acid water-soluble fertilizer, which contains 90-95% of compound fertilizer wastewater concentrated solution and 5-10% of potassium humate by mass fraction, wherein the compound fertilizer wastewater concentrated solution is obtained by evaporating and concentrating wastewater generated in compound fertilizer production, the potassium humate is obtained by mixing and heating tert-butyl peroxyneodecanoate waste liquid, weathered coal powder and a potassium hydroxide solution, and the tert-butyl peroxyneodecanoate waste liquid is obtained by recovering an aqueous phase solution in the process of synthesizing tert-butyl peroxyneodecanoate and then evaporating and concentrating.
Further, the compound fertilizer wastewater concentrated solution is waste containing a reaction tank cleaning solution, an ammonium nitrate evaporation cleaning solution and a calcium carbonate filter cake cleaning solutionWater, the waste water contains N, P2O5、K2O。
Specifically, N, P therein2O5、K2The total content of O is 18-22%.
The content of humic acid in the potassium humate is 40-60%, and the content of potassium oxide is 8-11%.
The preparation principle of the tert-butyl peroxyneodecanoate is as follows:
the preparation method of the tert-butyl peroxyneodecanoate comprises the following steps:
1) adding 70% sulfuric acid into tert-butyl alcohol, and keeping the integral temperature below 30 ℃ to generate tert-butyl hydrogen sulfate;
2) adding hydrogen peroxide and stirring, cooling to 10-20 ℃, adding tert-butyl hydrogen sulfate, stirring for 2 hours, standing for layering, filtering and reserving supernatant, neutralizing the supernatant with magnesium carbonate solution until the pH value is 6-7, and washing at low temperature to obtain tert-butyl hydroperoxide;
3) synthesizing tert-butyl peroxyneodecanoate by taking tert-butyl hydroperoxide and neodecanoyl chloride as raw materials;
4) and washing tert-butyl peroxyneodecanoate at low temperature, filtering, and recovering the aqueous phase solution for evaporation concentration and reuse.
The invention also discloses a preparation method of the humic acid water-soluble fertilizer, which is characterized by comprising the following steps:
1) collecting waste liquid generated in the production of compound fertilizer, evaporating and concentrating to N, P2O5、K2The total nutrient content of O reaches 18-22%;
2) separating and recovering the aqueous phase solution generated in the preparation process of tert-butyl peroxyneodecanoate, evaporating and concentrating until the concentration reaches 75-80%, mixing 150-200 parts of aqueous phase solution, 100-130 parts of weathered coal powder and 80-160 parts of potassium hydroxide solution according to parts by weight, heating at 70-90 ℃, and carrying out the following reactions:
when the pH value reaches 10-12, drying for 2-4h at the temperature of 95-130 ℃ to obtain potassium humate;
3) uniformly mixing 90-95% of compound fertilizer wastewater concentrated solution and 5-10% of potassium humate according to mass fraction, preserving heat in an environment of 90-100 ℃ and reacting for 55-60 h.
Preferably, the compound fertilizer waste liquid is evaporated and concentrated for 2-4h in the environment of 110-120 ℃.
Further, in order to prolong the preservation time of the fertilizer and ensure the purity of the product, the concentrated solution of the compound fertilizer wastewater is mixed with the potassium humate and reacts, and insoluble substances are filtered out after the reaction.
In order to accelerate the uniform mixing of the compound fertilizer wastewater concentrated solution and the potassium humate, stirring reaction is carried out after mixing.
The humic acid water-soluble fertilizer can be applied to planting of plants and crops.
The humic acid water-soluble fertilizer can effectively improve the water, fertilizer, gas and heat conditions of soil, so that the soil becomes loose and fertile. Meanwhile, the granular structure of the soil can be improved, and the drought resistance of crops can be improved under the drought condition. The invention utilizes the waste water generated in the preparation of two chemical products, on one hand, the influence of the waste water on the surrounding environment can be effectively reduced, the discharged pollutants are reduced, and on the other hand, the production cost of the humic acid water-soluble fertilizer can be reduced.
Drawings
FIG. 1 is a preparation flow chart of humic acid water-soluble fertilizer.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to examples and comparative examples. The following examples and comparative examples are only for more clearly illustrating the technical aspects of the present invention so that those skilled in the art can well understand and utilize the present invention, and do not limit the scope of the present invention.
The names and abbreviations of the experimental methods, production processes, instruments and equipment related to the examples and comparative examples of the present invention are all conventional names in the art, and are clearly and clearly understood in the related fields of use, and those skilled in the art can understand the conventional process steps and apply the corresponding equipment according to the names, and implement the process according to the conventional conditions or the conditions suggested by the manufacturers.
The various starting materials and reagents used in the examples and comparative examples of the present invention are not particularly limited in terms of their sources, and are all conventional products commercially available.
Wherein, the waste water produced in the production of the compound fertilizer comes from a cleaning solution of a neutralization tank, an ammonium nitrate evaporation cleaning solution and a calcium carbonate filter cake cleaning solution, and the three cleaning solutions are converged into a process waste water tank and evaporated and concentrated until the total nutrient content of N, P2O5 and K2O reaches 18-22%.
The humic acid-containing water-soluble fertilizer powder is from Shaanxi Dingtian Ji agricultural humic acid products Limited, the watermelon variety to be tested is Jingxin, and the two test raw materials are obtained by purchasing from manufacturers on the market.
Example 1 preparation of humic acid water soluble fertilizer.
Preparing a humic acid water-soluble fertilizer according to the steps shown in figure 1:
1) preparing compound fertilizer water waste liquid:
ammonium nitrate evaporation cleaning solution, compound fertilizer neutralization reaction tank cleaning solution and calcium carbonate filter cake cleaning solution generated in the compound fertilizer production process flow into the compound fertilizer process wastewater pool, 800L of wastewater in the compound fertilizer process wastewater pool of the factory is collected, and (N + P) in the wastewater is detected to obtain (N + P)2O5+K2O) the total nutrient content is 20.4 percent, the density is 1.14g/mL, the waste liquid is transferred to an evaporator, the waste liquid is evaporated and concentrated for about 3 hours at 110 ℃, the compound fertilizer waste water concentrated solution is obtained, and the total nutrient content is 25.3 percent and the density is 1.28 g/mL.
2) Generation and collection of aqueous phase solution in tert-butyl peroxyneodecanoate:
adding about 25L of tert-butyl alcohol into a reaction kettle, stirring and slowly adding about 9L of sulfuric acid with the concentration of 70% to generate tert-butyl hydrogen sulfate, and keeping the temperature below 30 ℃ in the whole adding process; adding 12L of hydrogen peroxide into another reaction kettle, cooling to 10-20 ℃ under the condition of stirring, adding 33L of prepared tert-butyl hydrogen sulfate into the reaction kettle at a high speed, stirring for 2 hours, and standing for layering; filtering and retaining supernatant, separating out a water layer, neutralizing the supernatant with a magnesium carbonate solution, detecting the pH of the supernatant to be 6.6, and washing at low temperature to obtain tert-butyl hydroperoxide; 20kg of 20% sodium hydroxide solution is dripped into the tert-butyl hydroperoxide within 20min, the temperature is kept lower than 20 ℃ in the whole process, the mixture is continuously stirred rapidly for 1h, and the neodecanoyl chloride is added into the mixture to synthesize the tert-butyl peroxyneodecanoate. After low-temperature washing, filtering, and recovering the washing liquid for evaporation concentration and reuse. Separating and collecting the water phase solution generated in the preparation process of tert-butyl peroxyneodecanoate, evaporating and concentrating for 4.5h at the temperature of 100 ℃, and detecting the concentration to be 77%.
3) Preparing potassium humate:
mixing 35kg of aqueous phase solution generated in the preparation process of tert-butyl peroxyneodecanoate, 24kg of weathered coal powder and 24kg of potassium hydroxide solution according to parts by weight, heating to react at 80 ℃, detecting the pH value to be 11, drying at 115 ℃ for 3.5h to obtain potassium humate, and detecting to obtain the potassium humate with the content of free humic acid of 52%;
4) mixing 940kg of compound fertilizer wastewater concentrated solution and 60kg of potassium humate uniformly, transferring into a reaction kettle, reacting at 97 ℃ for 58 hours, filtering out insoluble substances by rough filtration, transferring into a finished product storage tank, sampling, and detecting humic acid, (N + P) in the finished product storage tank2O5+K2O) total nutrient content to obtain total nutrient (N + P) with humic acid content more than or equal to 30g/L2O5+K2O) is more than or equal to 200g/L, and is subpackaged, sealed and packaged for warehousing by taking 5kg, 10kg and 20kg as units.
Example 2 fertilizer efficiency experiment of humic acid water soluble fertilizer.
According to the ' fertilizer registration management method ' of Ministry of agriculture ' and ' fertilizer effect test and evaluation general requirements ' (NY/T2544-2014), a formal fertilizer effect test was carried out in the watermelon field of Fenyang village in Zhao Kangzhen, Xi of Xiangfen county, and the basic conditions of the experimental sites are shown in Table 1.
The experiment is provided with three treatment methods, the three treatment methods are repeated for three times, the area of each cell is 5 mu, random arrangement is adopted, and the watermelon planting area of a control group is 1.5 mu. The treatment method comprises the following steps:
treatment 1: applying clear water;
and (3) treatment 2: applying 800 times of powder of water-soluble fertilizer containing humic acid from Dingtian company, wherein the humic acid is more than or equal to 4 percent and the (N + P) is2O5+K2O）≥20%；
And (3) treatment: applying the 800-time water aqua containing the humic acid water-soluble fertilizer.
The planting and fertilizer application process comprises the following steps: sowing is started in 15 days of 4 months, seedlings emerge in 20 days of 4 months, thinning is carried out in 3 days of 5 months, tendrils are stretched in 20 days of 5 months, flowering is started in 20 days of 6 months, watermelons are expanded in 2 days of 7 months, and the watermelons are ripe in 25 days of 7 months. After beginning of spring, the machine ploughing is carried out once, the depth is 20 cm, 2500 kilograms of farmyard manure and 50 kilograms of special fertilizer for watermelon are applied to each mu. And (3) extending the watermelon vine in 20 days in 5 months, and applying 15 kg of urea per mu in combination with watering. And 6, 15 days after 6 months, watering once again when the watermelons begin to bloom and grow, and applying 20 kilograms of urea per mu.
Spraying humic acid-containing water-soluble fertilizer for three times continuously in the expansion period of the watermelon, wherein the specific time is 6 months for 20 days, 6 months for 27 days and 7 months for 3 days, and the spraying concentration is 800 times. The water is poured and sown once in 10 days in 4 months, the watering quantity is 30 squares/mu, the vine extending water is poured once in 20 days in 5 months, the watering quantity is 35 squares/mu, the expanding water is poured once in 20 days in 6 months, and the watering quantity is 40 squares/mu. Manually intertillage and weeding once in 5 months and 15 days in the watermelon seedling period, and spraying mancozeb once in 7 months and 1 day to prevent the downy mildew of watermelon.
After ripening, watermelon yields per plot and per acre were measured and the results are shown in table 2.
In the expanding period of the watermelon, 100 representative watermelon leaves were collected during the repetition of different treatments to measure the length and width of the leaves, and the results shown in table 3 were obtained, so that it can be seen that the humic acid water-soluble fertilizer prepared by the method shown in example 1 has the same treatment effect as the purchased fertilizer, and the average length and the average width of the leaves are increased compared with the control group without fertilizer, wherein the length of the leaves is increased by 0.7cm, and the width is increased by 0.6 cm.
In the mature period of the watermelons, 100 watermelons are picked randomly and weighed in the repeat of different treatments within 7 months and 20 days, the results are shown in table 4, the weight of fruits of plants treated by the humic acid water-soluble fertilizer prepared by the method and the commercial fertilizer is better than that of the fruits of plants treated by clear water, and the two levels are equivalent.
In the mature period of the watermelon, on the basis of measuring the weight of a single watermelon in 20 days in 7 months, the sugar content of the watermelon is also measured, and the result is shown in table 5, and the sweetness of the obtained fruit of the plant treated by the humic acid water-soluble fertilizer is equivalent to that of the commercially available fertilizer.
The results are shown in table 6, and it can be seen from table 6 that compared with the control group shown in treatment 1, the yield increase rate of 329 kg per mu is 10.5%, the yield increase rate is 494 yuan per mu, the income increase rate is 474 yuan per mu, and the yield-to-input ratio is 24.7: 1, extremely remarkable yield increase level is achieved after variance analysis.
Compared with a control group shown in treatment 1, the watermelon yield-increasing agent has the advantages that the length of leaves is increased by 0.7cm, the width is increased by 0.6cm, the weight of a single watermelon is increased by 1.6 kg, the sugar content is increased by 0.6%, 329 kg of watermelon is increased per mu, the yield-increasing rate reaches 10.5%, the yield-increasing value per mu is 494 yuan, the per mu purification income is 474 yuan, and the yield-input ratio is 24.7: 1, extremely remarkable yield increase level is achieved after variance analysis.
In the embodiment, the technical indexes of the 800-time aqueous solution (treatment 3) of the humic acid-containing water-soluble fertilizer applied by the invention are that the humic acid is more than or equal to 30g/L, (N + P2O5+ K2O) is more than or equal to 200g/L, the percentage content is that the humic acid is more than or equal to 2.5%, and the percentage content is (N + P2O5+ K2O) is more than or equal to 16.5%. In the purchased 800-time powder (treatment 2) of the humic acid-containing water-soluble fertilizer, the humic acid content is more than or equal to 4 percent, and the content of (N + P2O5+ K2O) is more than or equal to 20 percent; the fertility of (N + P2O5+ K2O) and humic acid with lower concentration in the step 3 is not influenced, the fertilizing effect can be achieved under the condition of adding less chemical components and additives, and the concentration of the existing water-soluble fertilizer is only required to be properly improved when higher fertility is required.
Example 3 application method of humic acid water soluble fertilizer.
The humic acid water-soluble fertilizer obtained by the invention can be applied to solanaceous fruits such as watermelon, cucumber, tomato and the like; fruits such as apple, pear, peach and the like, and cash crops such as cotton, corn, wheat, flowers and the like.
When the humic acid water-soluble fertilizer prepared in the embodiment 1 is used, the dilution degree is selected according to the fertilization part, when the humic acid water-soluble fertilizer is sprayed on the leaf surface, the humic acid water-soluble fertilizer is diluted by 800 times, and is uniformly sprayed on the surface of the leaf of a crop, and the humic acid water-soluble fertilizer can be continuously used for 2 to 3 times at intervals of 10 to 15 days;
when the fertilizer is sprayed to roots, the fertilizer needs to be diluted by 200 times and 300 times, and the fertilizer is uniformly applied to soil at the roots of crops in the modes of flushing application, drip irrigation, sprinkling irrigation or sprinkling application and the like.
When in use, the blades are only fully covered with mist water droplets during spraying, and the mist can not be sprayed back and forth; the spraying is carried out on a fine day, the spraying is carried out before 10 am or 4 pm as much as possible, and the spraying is carried out again after 10 hours of the spraying.
Claims (9)
1. A humic acid water-soluble fertilizer comprises 90-95% of compound fertilizer wastewater concentrated solution and 5-10% of potassium humate by mass fraction, wherein the compound fertilizer wastewater concentrated solution is obtained by evaporating and concentrating wastewater generated in compound fertilizer production, the potassium humate is obtained by mixing and heating tert-butyl peroxyneodecanoate waste liquid, weathered coal powder and a potassium hydroxide solution, and the tert-butyl peroxyneodecanoate waste liquid is obtained by evaporating and concentrating an aqueous phase solution in a process of synthesizing tert-butyl peroxyneodecanoate after recovery.
2. The humic acid water-soluble fertilizer as claimed in claim 1, wherein the compound fertilizer wastewater concentrate is wastewater containing N, P, wherein the wastewater comprises reaction tank cleaning solution, ammonium nitrate evaporation cleaning solution and calcium carbonate filter cake cleaning solution2O5、K2O。
3. The humic acid water-soluble fertilizer as claimed in claim 2, wherein N, P2O5、K2The total content of O is 18-22%.
4. The humic acid water-soluble fertilizer as claimed in claim 1, wherein the humic acid potassium contains 40-60% of humic acid and 8-11% of potassium oxide.
5. The preparation method of the humic acid water-soluble fertilizer as claimed in claim 1, which is characterized by comprising the following steps:
collecting waste liquid generated in the production of compound fertilizer, evaporating and concentrating to N, P2O5、K2The total nutrient content of O reaches 18-22%;
separating and recovering the aqueous phase solution generated in the preparation process of tert-butyl peroxyneodecanoate, mixing 150-200 parts of aqueous phase solution, 100-130 parts of weathered coal powder and 80-160 parts of potassium hydroxide solution by weight after evaporation concentration until the concentration reaches 75-80%, heating at 70-90 ℃, and drying at 95-130 ℃ for 2-4h when the pH reaches 10-12 to obtain potassium humate;
uniformly mixing 90-95% of compound fertilizer wastewater concentrated solution and 5-10% of potassium humate according to mass fraction, and preserving heat for 55-60h at 90-100 ℃.
6. The preparation method as claimed in claim 5, wherein the compound fertilizer waste liquid is evaporated and concentrated for 2-4h at 110-120 ℃.
7. The preparation method as claimed in claim 5, wherein the mixed compound fertilizer waste water concentrated solution reacts with potassium humate, and then is subjected to rough filtration and insoluble matter is filtered off.
8. The preparation method as claimed in claim 5, wherein the concentrated solution of compound fertilizer wastewater and potassium humate are mixed and then stirred for reaction.
9. The application of the humic acid water-soluble fertilizer in the planting of plants and crops.
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