CN116589312A - Liquid silicon fertilizer prepared from fluorine-containing silica gel and preparation method thereof - Google Patents

Liquid silicon fertilizer prepared from fluorine-containing silica gel and preparation method thereof Download PDF

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Publication number
CN116589312A
CN116589312A CN202310300379.7A CN202310300379A CN116589312A CN 116589312 A CN116589312 A CN 116589312A CN 202310300379 A CN202310300379 A CN 202310300379A CN 116589312 A CN116589312 A CN 116589312A
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silica gel
fluorine
containing silica
liquid silicon
silicon fertilizer
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Inventor
谢德龙
邬斌威
刘翠侠
李莹莹
朱远蹠
马航
梅毅
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05B—PHOSPHATIC FERTILISERS
    • C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
    • 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
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
    • Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Soil Sciences (AREA)
  • Fertilizers (AREA)

Abstract

The invention relates to the technical field of soil improvement, and discloses a liquid silicon fertilizer prepared from fluorine-containing silica gel and a preparation method thereof, wherein the preparation method comprises the following steps: firstly, adding fluorine-containing silica gel into strong alkali for pretreatment, and reacting to generate water glass suspension; then adding a conditioner for filtering to obtain a water glass solution; and then adding a chelating agent and nitrogen, phosphorus and potassium fertilizers to carry out chelation reaction to generate the liquid silicon fertilizer. The purity of the silicon-containing raw material is improved through pretreatment of the fluorine-containing silica gel raw material, and the active ingredient Si in the silicon-containing raw material is easily absorbed and utilized by crops through the actions of the conditioner and the chelating agent, so that the lodging resistance and the disease and pest resistance of the crops are enhanced, and the yield and the quality of the crops are obviously improved on the basis of the same fertilizer application amount.

Description

Liquid silicon fertilizer prepared from fluorine-containing silica gel and preparation method thereof
Technical Field
The invention belongs to the technical field of soil improvement, and particularly relates to a liquid silicon fertilizer prepared from fluorine-containing silica gel and a preparation method thereof.
Background
With the diversification development of agricultural production in recent years, around the changes of production modes of facility agriculture, water and fertilizer integration and agricultural mechanization, researchers aim at improving the fertilizer utilization rate, and focus on developing a water-soluble efficient silicon fertilizer with functionalization and a silicon-containing series soil conditioner with acid soil improvement performance, wherein main products comprise organic complexing (chelating) silicon fertilizer, organic sugar alcohol silicon fertilizer, organic acid silicon fertilizer, acid (alkali) water-soluble silicon fertilizer, neutral water-soluble silicon fertilizer, nano silicon fertilizer, humic acid silicon fertilizer and the like.
The development of the silicon fertilizer technology can be divided into three stages. In 1978-2014, the first stage, the patent application with smaller published amount, and the research of acid soil conditioner using shell powder, gypsum, copolymer resin and other materials was started in developed countries such as japan, and only 1.5 patent applications with a structure of published result each year on average. In the second stage 2015-2020, after more than twenty years of precipitation, the silicon fertilizer for improving the acid soil becomes a scientific research hot spot, a large number of agricultural science and technology practitioners start to research the silicon fertilizer, and the publication amount of the finished patent application reaches the maximum value of 44 in 2017. In the third stage 2021, the patent disclosure amount of the silicon fertilizer achievement is rapidly reduced from 40 pieces in 2020 to 24 pieces in 2021, and one reason for this phenomenon is probably that the silicon fertilizer technology has tended to be mature after decades of development, and the technical innovation difficulty is high, so that the formed achievement is reduced.
Byproducts in the chemical industry, especially silica gel, have no suitable utilization way and can only be discharged to a slag yard for storage. The large amount of silica gel is piled up and placed, so that not only does not occupy a large piece of land, but also elements such as fluorine, phosphorus and the like can be slowly released when the silica gel is placed in the open air, thereby causing environmental pollution and being a resource waste.
The main component of the silica gel is silica, wherein the water content is 60-70%, the fluorine content is 4-6%, the aluminum content is 2-4%, the pH value is 2-3, and the activity is poor at normal temperature. Silica gel is often used to prepare water glass, but water glass is low in price and small in market.
The Chinese patent application publication No. CN111018611A discloses a method for preparing slow-release silicon fertilizer by using active silicon dioxide, which comprises the steps of reacting active silicon dioxide with sodium hydroxide or potassium hydroxide solution to generate liquid sodium silicate or potassium silicate, and spraying and adsorbing the liquid sodium silicate or potassium silicate and the dried silicon dioxide in an adsorption tower to form the slow-release silicon fertilizer. The method has the advantages that the treatment problem of activated silicon dioxide as a byproduct of preparing anhydrous hydrogen fluoride is solved, but the granular slow-release silicon fertilizer is available at present, and the method has no competitive strength in terms of economic benefit.
The Chinese patent application publication No. CN109305826A discloses a preparation method of a liquid silicon fertilizer rich in trace elements, which comprises the steps of mixing high-boron glass powder, quartz sand, potassium carbonate, calcium carbonate, ferric oxide, copper oxide and boron oxide to form a batch, adding the batch into a high-temperature crucible, mixing the cooled glass liquid with water, putting the mixture into a ball mill, ball milling the mixture through a 400-target standard sieve, and obtaining the liquid silicon fertilizer rich in trace elements. The product is still a molten silicate and is not entirely a water-soluble silicon fertilizer.
The Chinese patent application with publication number of CN113511924A discloses a liquid silicon-calcium fertilizer and a preparation method and application thereof. And (3) pulping the first solid to obtain water slurry, adding a mixed acid solution under stirring to react, and separating solid from liquid to obtain a second liquid. Finally, regulating the pH value to 5.5-10 by using a pH value regulator to obtain the liquid silicon-calcium fertilizer. The technical proposal has higher pH value and insufficient fertility.
The Chinese patent application with publication number of CN107746293A discloses a high-activity silicon fertilizer prepared from waste slag and a preparation method thereof, and the technical proposal is prepared by calcining coal gangue, sodium hydroxide, calcium oxide or weak base such as calcium hydroxide, sodium carbonate and the like. Although solving the problem of stacking a large amount of gangue, the patent needs three times of calcination and cooling, and the generated environmental pollution and the generated benefits are equivalent.
The Chinese patent application with publication number of CN107162670A discloses a silicon fertilizer or silicon compound fertilizer and a production method thereof. Compared with the traditional balanced compound fertilizer, the product has no obvious difference in nutrient release, sodium silicate is dissolved in less water environment to generate binding capacity, soil aggregate is easy to damage, and the product is contrary to the starting point of a soil conditioner.
The Chinese patent application with publication number of CN11021811A discloses a production method of agricultural liquid ion silicon fertilizer, which is prepared by fermenting and chelating nano silicon, perilla extract, chelating agent, urea, humic acid, monopotassium phosphate, potassium nitrate, carambola leaf extract and sugarcane, diluting by 100 times, and regulating pH to 5-6. The patent product has obvious effect, but the required process configuration is complicated, the actual production cost is high, the method cannot be applied to production on a large scale, only can be applied to cash crops, is difficult to popularize on other non-cash crops, and has no competitive power in terms of economic benefit.
The Chinese patent application publication No. CN105439718A discloses a liquid silicon fertilizer and a production process thereof, and the technical scheme is that a silicate compound and a compound such as alcohol fat are subjected to chelation reaction through ultrasonic chelation to obtain the chelation liquid silicon fertilizer. By this direct mixing type chelation, the silicate compound and the alcohol compound are not very chelated and the silicon nutrient is unstable and easily solidified when applied.
The Chinese patent application with publication number of CN111116241A discloses a method for preparing a full water-soluble silicon fertilizer from silicon ore, which is prepared by performing alkali fusion reaction on silicon ore (granite, amphibole, asbestos, feldspar, clay and mica), alkaline oxide (sodium hydroxide, potassium hydroxide, calcium oxide, magnesium oxide, sodium carbonate, potassium carbonate, sodium peroxide, calcium carbonate and magnesium carbonate) and other auxiliary materials. The effective SiO2 of the product obtained by the invention can reach more than 20%, but still is silicate component, pH is not adjusted, the direct application can cause root burning of crops, and the product is only suitable for partial crops planted in acid red soil, and has limited market potential.
The Chinese patent application with publication number of CN112645742A discloses a preparation method of a liquid nano silicon fertilizer, which adopts the technical scheme that sodium silicate or potassium silicate or a mixture thereof is prepared to obtain an aqueous solution, and active silicic acid is obtained through cation exchange resin, and the aqueous solution is prepared by matching aluminum salt and an alkaline pH regulator. The method has the advantages that the pH of the product is lower and is between 3 and 9, but the raw materials are purchased directly, the cost is high, and the market competitiveness is not achieved.
The Chinese patent application with publication number of CN107652066A discloses a sugar alcohol silicon fertilizer and a preparation method thereof, and the technical scheme is that the sugar alcohol silicon fertilizer is deoxidized and catalyzed by solution prepared from glucitol or fructosyl alcohol or xylitol and potassium hydroxide and industrial silicon. The method has the advantages of convenient raw material acquisition and simple operation process, but has the defects that dangerous gas hydrogen is generated when industrial silicon reacts with potassium hydroxide, and the actual production has great potential safety hazard.
In summary, in the prior art, there is no report of developing a silicon fertilizer by using silica gel as a byproduct of producing phosphate fertilizer, fluoride, and the like as a raw material.
Disclosure of Invention
The invention aims to provide a liquid silicon fertilizer prepared from fluorine-containing silica gel in view of the defects of the prior art, and aims to solve the problem of difficult utilization of byproduct resources of the prior silica gel, improve soil environment, enhance lodging resistance and disease and insect pest resistance of crops, and remarkably improve crop yield and quality on the basis of the same fertilizer application amount. The invention also aims to provide a preparation method of the liquid silicon fertilizer prepared by using the fluorine-containing silica gel.
The technical scheme adopted by the invention is as follows: a liquid silicon fertilizer prepared from fluorine-containing silica gel is prepared from the following components:
wherein the water glass solution C is prepared from fluorine-containing silica gel A and strong alkali B according to the weight part ratio of 1:1-3.8:1;
the nitrogen, phosphorus and potassium fertilizer G consists of 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride in fixed parts by weight.
Preferably, the liquid silicon fertilizer prepared from fluorine-containing silica gel is prepared from the following components:
wherein, the water glass solution C is prepared from fluorine-containing silica gel A and strong base B according to the proportion of 1:1 to 3.4:1 weight portion.
The fluorine-containing silica gel A comprises wet silica gel and dry silica gel, wherein the wet silica gel comprises the following active ingredients in percentage by mass: siO (SiO) 2 36-37% of Al 2 O 3 O to 1%, F to 4 to 5%, H 2 O is 50-51%; the dry silica gel comprises the following active ingredients in percentage by mass: siO (SiO) 2 74 to 75 percent of Al 2 O 3 O is 1-1%, F is 4-5%.
And the strong base B is one of analysis-grade sodium hydroxide or analysis-grade potassium hydroxide.
The conditioner D is glycerin, N-dimethyl diethanolamine or N, N-dimethyl diacetyl amide.
The chelating agent F is one or more of mannitol, D-sorbitol, xylitol, glycerol, ethanolamine, triethanolamine, yeast concentrated dry powder, humic acid essence, fulvic acid solid, amino acid, citric acid monohydrate and potassium humate.
The nitrogen, phosphorus and potassium fertilizer G is a mixture of nitrogen fertilizer urea, phosphorus fertilizer monoammonium phosphate and potassium fertilizer potassium chloride, and the weight proportion of the nitrogen, phosphorus and potassium fertilizer G is 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride.
A liquid silicon fertilizer prepared from fluorine-containing silica gel and a preparation method thereof are provided, wherein the method comprises the following steps:
s1, adding fluorine-containing silica gel A into an aqueous solution of strong base B, and reacting to generate sodium silicate solution C;
s2, adding a conditioning agent D into the water glass solution C, and then filtering to obtain a mixed solution E;
s3, adding a chelating agent F and a nitrogen, phosphorus and potassium fertilizer G into the mixed solution E to react to generate the liquid silicon fertilizer.
The water glass solution C is a mixture of silica gel and water glass solution.
The mixed solution E comprises the following active ingredients in percentage by mass: na (Na) 2 O is 3.02-8.02%, K 2 O is 5.68-12.26%, siO 2 4.48 to 21.98 percent, F is 0.42 to 2.12 percent, the pH value is 11.17 to 12.10, and the modulus M is 2.18 to 3.42.
In the step S1, the reaction temperature is 85-95 ℃ and the reaction time is 60-216 min.
The pH value of the liquid silicon fertilizer is 8-10.
Compared with the prior art, the invention has the beneficial effects that: the problem of difficult utilization of the silica gel byproduct can be effectively solved, and the effective components in the silica gel byproduct are easily absorbed and utilized by crops under the action of the conditioner and the chelating agent; the silicon nutrient can enhance the lodging resistance and insect pest resistance of crops, and obviously improve the yield and quality of crops on the basis of the same fertilizer application amount; the preparation method is simple, and the synergistic effect of the components can be fully maintained and exerted
Drawings
FIG. 1 is a flow chart of a production process for preparing a liquid silicon fertilizer by using fluorine-containing silica gel.
Detailed Description
The invention is further described below with reference to the accompanying drawings. It should be noted that these embodiments are merely representative embodiments of the present invention, and the specific steps, parameters, etc. illustrated herein are not meant to limit the present invention or the corresponding embodiments.
Example 1
A preparation method of a liquid silicon fertilizer prepared from fluorine-containing silica gel comprises the following steps: adding 27 parts of water in a container, adding 5.54 parts of sodium hydroxide to prepare sodium hydroxide aqueous solution, controlling the temperature to 95 ℃, stirring at a rotating speed of 200r/min, adding 5.54 parts of dried silica gel for defluorinated silica gel reaction according to 5 times with uniform weight, and reacting 216After min, stirring was stopped at a pressure of 5.9X10 5 Standing for 24 hours under Pa pressure, and filtering to obtain a filter liquor as a water glass solution; wherein Na in the water glass filtrate 2 O content of 3.02%, siO 2 4.48%, F content 0.42%, pH 12.04, modulus M1.53;
100 parts of water glass solution and 17.3 parts of glycerin are added into a three-neck flask, the reaction temperature is controlled to be 80 ℃, after 120 minutes of reaction, the mixture is filtered, and the filtrate is transferred into a plastic bottle to test the pH value, wherein the pH value is 10.41;
adding the filtrate into a three-neck flask, adding 8.3 parts of mannitol, 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride, controlling the reaction temperature to 80 ℃, and performing chelation reaction under ultrasonic waves with the frequency of 20kHz for 120min to obtain the liquid silicon fertilizer prepared by the fluorine-containing silica gel, wherein the pH value is 10.00.
Example 2
A preparation method of a liquid silicon fertilizer prepared from fluorine-containing silica gel comprises the following steps: adding 200 parts of water in a container, adding 50.44 parts of sodium hydroxide to prepare sodium hydroxide aqueous solution, controlling the temperature to 95 ℃, stirring at a rotating speed of 200r/min, adding 172 parts of wet silica gel in 4 times according to uniform weight to perform defluorinated silica gel reaction, stopping stirring after the reaction time is 120min, and controlling the pressure to be 5.9x10 5 Standing for 24 hours under Pa pressure, and filtering to obtain a filter liquor as a water glass solution; wherein Na in the water glass solution 2 O content of 8.02%, siO 2 21.98%, F content 1.54%, pH 11.17, modulus M2.8;
100 parts of water glass solution and 17.3 parts of N-dimethyl diethanolamine are added into a three-neck flask, the reaction temperature is controlled to be 80 ℃, after 120 minutes of reaction, the solution is filtered, and the filtrate is transferred to a plastic bottle to test the pH value, wherein the pH value is 10.52;
adding the filtrate into a three-neck flask, adding 8.3 parts of D-sorbitol, 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride, controlling the reaction temperature to be 80 ℃, and performing chelation reaction under ultrasonic waves with the amplitude of 60 and the frequency of 20kHz for 180 minutes to obtain the liquid silicon fertilizer prepared by the fluorine-containing silica gel, wherein the pH value is 9.89.
Example 3
A preparation method of a liquid silicon fertilizer prepared from fluorine-containing silica gel comprises the following steps:
adding 147 parts of water in a container, adding 32.97 parts of potassium hydroxide to prepare potassium hydroxide aqueous solution, controlling the temperature to be 85 ℃, stirring at a rotating speed of 200r/min, adding 100 parts of wet silica gel for 1 time to perform defluorination silica gel reaction, stopping stirring after the reaction time is 120min, and controlling the pressure to be 5.9x10 5 Standing for 24h under Pa pressure, increasing the temperature to 90 ℃, stirring and reacting for 120min, and filtering to increase the reaction speed or reduce the reaction time, wherein the filtered solution is water glass solution; wherein, K in the water glass filtrate 2 O content of 5.68% and SiO 2 9.51%, F content 1.54%, pH 11.20, modulus M2.76;
100 parts of water glass solution and 17.3 parts of N-N dimethyl diacetyl amide are added into a three-neck flask, the reaction temperature is controlled to be 80 ℃, the reaction time is controlled to be 120min, after the reaction is finished, the filtration is carried out, the filtrate is transferred out into a plastic bottle to test the pH value, and the pH value is 13.98 at the moment;
adding the filtrate into a three-neck flask, adding 8.3 parts of xylitol, 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride, controlling the reaction temperature to be 80 ℃, and performing chelation reaction under ultrasonic waves with the frequency of 20kHz for 180 minutes to obtain the liquid silicon fertilizer prepared by the fluorine-containing silica gel, wherein the pH value is 9.96.
Example 4
A preparation method of a liquid silicon fertilizer prepared from fluorine-containing silica gel comprises the following steps:
adding 124.6 parts of water in a container, adding 32 parts of potassium hydroxide to prepare a potassium hydroxide aqueous solution, controlling the temperature to 95 ℃, stirring at a rotating speed of 200r/min, adding 77 parts of wet silica gel for defluorinated silica gel reaction for 5 times, stopping stirring after the reaction time is 180min, and filtering to obtain a filter liquor which is sodium silicate solution; wherein, K in the water glass filtrate 2 O content is 8.96%, siO 2 16.30%, F content 1.56%, pH 11.32, modulus M2.88;
100 parts of water glass solution and 17.3 parts of N-N dimethyl diacetyl amide are added into a three-neck flask, the reaction temperature is controlled to be 80 ℃, the reaction time is controlled to be 120min, the filtration is carried out, the filtrate is transferred out into a plastic bottle to test the pH value, and the pH value is 11.88;
adding the filtrate into a three-neck flask, adding 2 parts of glycerol, 3 parts of ethanolamine and 3.3 parts of triethanolamine, adding 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride, controlling the reaction temperature to 80 ℃, and performing chelation reaction under ultrasonic waves with the frequency of 20kHz for 120min to obtain the liquid silicon fertilizer prepared by the fluorine-containing silica gel, wherein the pH value is 9.99.
Example 5
A preparation method of a liquid silicon fertilizer prepared from fluorine-containing silica gel comprises the following steps: adding 119 parts of water in a container, adding 32 parts of potassium hydroxide to prepare a potassium hydroxide aqueous solution, controlling the temperature to 95 ℃, stirring at a rotating speed of 200r/min, adding 57 parts of wet silica gel for 1 time to perform defluorination silica gel reaction, stopping stirring after the reaction time is 120min, and filtering to obtain a filter liquor which is water glass solution; wherein, K in the water glass filtrate 2 The O content is 12.26 percent, siO 2 16.32%, F content 1.77%, pH 12.12, modulus M2.18;
100 parts of water glass solution and 17.3 parts of N-N dimethyl diacetyl amide are added into a three-neck flask, the reaction temperature is controlled to be 80 ℃, the reaction time is controlled to be 120min, the filtration is carried out, the filtrate is transferred out into a plastic bottle to test the pH value, and the pH value is 10.90;
adding filtrate into a three-neck flask, adding 5 parts of yeast concentrated dry powder, 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride, controlling the reaction temperature to 80 ℃, and performing chelation reaction under ultrasonic waves with the frequency of 20kHz for 120min to obtain the liquid silicon fertilizer prepared by the fluorine-containing silica gel, wherein the pH is 9.55.
Example 6
A preparation method of a liquid silicon fertilizer prepared from fluorine-containing silica gel comprises the following steps: adding 224 parts of water and 96 parts of potassium hydroxide into a container to prepare a potassium hydroxide aqueous solution, and controlling the temperatureStirring at 95deg.C and 200r/min, adding 250 parts of wet silica gel for defluorination silica gel reaction for 4 times, stopping stirring after 180min, and maintaining the pressure at 5.9x10 5 Standing for 24h under Pa pressure, filtering, and taking the filtered solution as water glass solution; wherein, K in the water glass filtrate 2 O content is 9.75%, siO 2 20.35%, F content 1.76%, pH 11.76, modulus M3.20;
100 parts of water glass solution and 17.3 parts of N-N dimethyl diacetyl amide are added into a three-neck flask, the reaction temperature is controlled to be 80 ℃, the reaction time is 120min, the filtration is carried out, the filtrate is transferred out into a plastic bottle to test the pH value, and the pH value is 10.80 at the moment;
adding the filtrate into a three-neck flask, adding 3 parts of humic acid essence and 4.5 parts of fulvic acid solid, 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride, controlling the reaction temperature to be 80 ℃, performing chelation reaction under ultrasonic waves with the frequency of 20kHz, and controlling the reaction time to be 120min to obtain the liquid silicon fertilizer prepared from fluorine-containing silica gel, wherein the pH value is 9.20.
Example 7
A preparation method of a liquid silicon fertilizer prepared from fluorine-containing silica gel comprises the following steps: adding 224 parts of water in a container, adding 96 parts of potassium hydroxide to prepare a potassium hydroxide aqueous solution, controlling the temperature to 95 ℃, stirring at a rotating speed of 200r/min, sequentially adding 150, 50 and 50 parts of wet silica gel in batches for defluorinated silica gel reaction, stopping stirring after the reaction time is 180min, and filtering to obtain a filter liquor which is sodium silicate solution; wherein K in the water glass filtrate 2 The O content is 9.88 percent, siO 2 21.12%, F content 2.12%, pH 11.89, modulus M3.42;
100 parts of water glass solution and 17.3 parts of N-N dimethyl diacetyl amide are added into a three-neck flask, the reaction temperature is controlled to be 80 ℃, the reaction time is controlled to be 120min, the filtration is carried out, the filtrate is transferred out into a plastic bottle to test the pH value, and the pH value is 10.41;
adding the filtrate into a three-neck flask, adding 4 parts of amino acid and 1.5 parts of citric acid monohydrate, adding 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride, controlling the reaction temperature to 80 ℃, and performing chelation reaction under ultrasonic waves with the frequency of 20kHz for 150 minutes to obtain the liquid silicon fertilizer prepared from fluorine-containing silica gel, wherein the pH value is 8.86.
Example 8
A preparation method of a liquid silicon fertilizer prepared from fluorine-containing silica gel comprises the following steps:
adding 147 parts of water in a container, adding 20.6 parts of potassium hydroxide to prepare potassium hydroxide aqueous solution, controlling the temperature to 90 ℃, starting ultrasonic treatment with the frequency of 20kHz, adding 45 parts of wet silica gel at one time to perform defluorination silica gel reaction, filtering after the reaction time is 60 minutes, and taking a filter liquor as a water glass solution; wherein K in the water glass filtrate 2 The O content is 9.26 percent, siO 2 16.55%, F content 1.42%, pH 12.10, modulus M2.84;
100 parts of water glass solution and 17.3 parts of N-N dimethyl diacetyl amide are added into a three-neck flask, the reaction temperature is controlled to be 80 ℃, the reaction time is controlled to be 120min, the filtration is carried out, the filtrate is transferred out into a plastic bottle to test the pH, and the pH is 11.13 at the moment;
adding the filtrate into a three-neck flask, adding 4.5 parts of potassium humate, adding 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride, controlling the reaction temperature to 80 ℃, performing chelation reaction under ultrasonic waves with the frequency of 20kHz, and controlling the reaction time to 150 minutes to obtain the liquid silicon fertilizer prepared from fluorine-containing silica gel, wherein the pH value is 8.65.
Verification experiment
The field test was carried out in 2022 in Menghai county (99 deg. 56 '-100 deg. 41' east longitude, 21 deg. 28'-22 deg. 28' north latitude) of Xishuangbanna Dai nationality, yunnan province at Menghai code village test land, the climate type of which is tropical and subtropical monsoon climate. The average annual temperature is 18.7 ℃, the average annual sunshine hours are 2088 years, and the annual rainfall is 1341 mm. The soil type is sandy loam, and the weak acid soil with pH of 6.15. The application amount of the base fertilizer for investigation of rice growth in the middle of 8 months is 40 kg/mu, wherein the control group NPK comprises urea 26, diammonium phosphate 10 and potassium chloride 9 in parts by weight.
Table 1 comparison of rice yield and quality after application of different example samples with control fertilizer
As can be seen from Table 1, the samples of examples 1-3 significantly increased the tillering and effective spike count of rice compared to the NPK control treatment, while example 2 also increased the spike rate of rice, all superior to the common N PK fertilizer overall.
Table 2 comparison of rice yield and quality after application of different example samples with control fertilizers:
from Table 2, it can be seen that examples 1-3 significantly increased the bending moment and flexural strength of rice, and the lodging resistance significantly better than that of the conventional NPK fertilizer, as compared to the NPK control treatment. Other embodiments of the invention have substantially the same effect.
In conclusion, the liquid silicon fertilizer prepared from the fluorine-containing silica gel and the preparation method can effectively solve the problem of phosphorus-based soil nutrient fixation, and the active ingredients in the liquid silicon fertilizer are easy to be absorbed and utilized by crops. Can solve the problem of difficult utilization of the existing byproduct resources, improve the phosphorus-based soil environment, strengthen the lodging resistance and the disease and pest resistance of crops, and obviously improve the yield and the quality of the crops on the basis of the same fertilizer application amount.
The foregoing is only illustrative of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims and their equivalents.

Claims (10)

1. The liquid silicon fertilizer prepared from the fluorine-containing silica gel is characterized by comprising the following components:
wherein the water glass solution is prepared from fluorine-containing silica gel and strong alkali according to the weight part ratio of 1:1-3.8:1;
the nitrogen-phosphorus-potassium fertilizer consists of 270 parts of urea, 150 parts of monoammonium phosphate and 350 parts of potassium chloride in fixed parts by weight.
2. The liquid silicon fertilizer prepared from fluorine-containing silica gel according to claim 1, which is prepared from the following components:
wherein the water glass solution is prepared from fluorine-containing silica gel and strong alkali according to the weight part ratio of 1:1-3.4:1.
3. The liquid silicon fertilizer prepared from fluorine-containing silica gel according to claim 1, wherein the fluorine-containing silica gel comprises wet silica gel and dry silica gel, wherein the wet silica gel comprises the following active ingredients in percentage by mass: siO (SiO) 2 36-37% of Al 2 O 3 0 to 1 percent, 4 to 5 percent of F and H 2 O is 50-51%; the dry silica gel comprises the following active ingredients in percentage by mass: siO (SiO) 2 74 to 75 percent of Al 2 O 3 0 to 1 percent and 4 to 5 percent of F.
4. The liquid silicon fertilizer prepared from fluorine-containing silica gel of claim 1, wherein the strong base is one of analytical grade sodium hydroxide or analytical grade potassium hydroxide.
5. A liquid silicon fertilizer prepared with fluorine-containing silica gel according to claim 1, wherein the conditioning agent is glycerol, N-dimethyldiethanolamine or N, N-dimethyldiacetamide.
6. The liquid silicon fertilizer prepared from fluorine-containing silica gel according to claim 1, wherein the chelating agent is one or a combination of more than two of mannitol, D-sorbitol, xylitol, glycerol, ethanolamine, triethanolamine, yeast concentrate dry powder, humic acid essence, fulvic acid solid, amino acid, citric acid monohydrate and potassium humate.
7. A method for preparing a liquid silicon fertilizer prepared from fluorine-containing silica gel according to any one of claims 1 to 6, comprising the steps of:
s1, adding fluorine-containing silica gel into an aqueous solution of strong alkali, and reacting to generate a water glass solution;
s2, adding a conditioner into the water glass solution, and then filtering to prepare a mixed solution;
s3, adding a chelating agent and nitrogen, phosphorus and potassium fertilizers into the mixed solution to react to generate the liquid silicon fertilizer.
8. The method for preparing the liquid silicon fertilizer by using the fluorine-containing silica gel as claimed in claim 7, wherein the mixed solution comprises the following active ingredients in percentage by mass: na (Na) 2 O is 3.02-8.02%, K 2 O is 5.68-12.26%, siO 2 4.48 to 21.98 percent, F is 0.42 to 2.12 percent, the pH value is 11.17 to 12.10, and the modulus M is 2.18 to 3.42.
9. The method for preparing a liquid silicon fertilizer by using fluorine-containing silica gel as claimed in claim 7, wherein in the step S1, the reaction temperature is 85-95 ℃ and the reaction time is 60-216 min.
10. The method for preparing a liquid silicon fertilizer by using fluorine-containing silica gel as claimed in claim 7, wherein the pH value of the liquid silicon fertilizer is 8-10.
CN202310300379.7A 2023-03-24 2023-03-24 Liquid silicon fertilizer prepared from fluorine-containing silica gel and preparation method thereof Pending CN116589312A (en)

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