CN116161989A - Silicon fertilizer prepared from rice hulls and preparation method thereof - Google Patents
Silicon fertilizer prepared from rice hulls and preparation method thereof Download PDFInfo
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- CN116161989A CN116161989A CN202310258037.3A CN202310258037A CN116161989A CN 116161989 A CN116161989 A CN 116161989A CN 202310258037 A CN202310258037 A CN 202310258037A CN 116161989 A CN116161989 A CN 116161989A
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- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 163
- 235000009566 rice Nutrition 0.000 title claims abstract description 163
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 131
- 239000010703 silicon Substances 0.000 title claims abstract description 131
- 239000003337 fertilizer Substances 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 240000007594 Oryza sativa Species 0.000 title abstract 2
- 241000209094 Oryza Species 0.000 claims description 161
- 239000000843 powder Substances 0.000 claims description 145
- 238000006243 chemical reaction Methods 0.000 claims description 50
- 239000000243 solution Substances 0.000 claims description 45
- 238000001035 drying Methods 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 29
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 26
- 238000001816 cooling Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 23
- 239000012286 potassium permanganate Substances 0.000 claims description 22
- 239000007790 solid phase Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 18
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 15
- 229920000515 polycarbonate Polymers 0.000 claims description 15
- 239000004417 polycarbonate Substances 0.000 claims description 15
- 238000000967 suction filtration Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 239000010903 husk Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- 229910021536 Zeolite Inorganic materials 0.000 claims description 10
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 10
- 229960000892 attapulgite Drugs 0.000 claims description 10
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 10
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 229910052625 palygorskite Inorganic materials 0.000 claims description 10
- WUUHFRRPHJEEKV-UHFFFAOYSA-N tripotassium borate Chemical compound [K+].[K+].[K+].[O-]B([O-])[O-] WUUHFRRPHJEEKV-UHFFFAOYSA-N 0.000 claims description 10
- 239000010457 zeolite Substances 0.000 claims description 10
- 239000004246 zinc acetate Substances 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 38
- 241000196324 Embryophyta Species 0.000 description 24
- 239000000047 product Substances 0.000 description 19
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 18
- 241000209082 Lolium Species 0.000 description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 12
- 229910052697 platinum Inorganic materials 0.000 description 9
- 239000002244 precipitate Substances 0.000 description 9
- 239000002689 soil Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000010306 acid treatment Methods 0.000 description 4
- 230000012010 growth Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- -1 cerium ions Chemical class 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 230000007773 growth pattern Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000008635 plant growth Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 240000004296 Lolium perenne Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910000551 Silumin Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000001339 epidermal cell Anatomy 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 235000015816 nutrient absorption Nutrition 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000003516 soil conditioner Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000009331 sowing Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a silicon fertilizer prepared from rice hulls and a preparation method thereof, belonging to the technical field of fertilizer preparation.
Description
Technical Field
The invention relates to the technical field of fertilizer production, in particular to a silicon fertilizer prepared from rice hulls and a preparation method thereof.
Background
The rice husk is agricultural solid waste generated in the course of processing rice. China is the largest paddy planting country in the world, and the paddy hulls have large yield, wide sources and low utilization rate. In the paddy rice producing area of China, the paddy rice hulls are generally regarded as waste materials to be discarded. However, since the surface of the rice husk is hard, the silicon content is high, the rice husk is not easily decomposed by bacteria, the stacking density is small, the volume is large, the stacking area is large, and the environment pollution is easy to cause, so that the efficient recycling of the rice husk has practical value.
Silicon fertilizer is considered as the fourth important crop fertilizer following nitrogen fertilizer, potassium fertilizer, phosphate fertilizer. Silicon is a fourth mineral element, an ideal soil conditioner, plays a very important role in plant growth, can enhance plant photosynthesis, thereby improving nutrient accumulation, simultaneously improving plant root activity, promoting root respiration and nutrient absorption, and if in plant epidermal cells, can enhance plant stalk strength and effectively reduce lodging phenomenon. However, although the silicon content in the soil is very high, the part of silicon which can be absorbed and utilized by crops, namely the effective silicon content, is low, most of silicon is in a very stable crystalline state and a non-crystalline state in the soil, the solubility is very low, and plants are difficult to absorb and utilize, so that the silicon nutrient required by the plants is often provided by applying a silicon fertilizer.
At present, the varieties of artificially synthesized silicon fertilizer mainly comprise two major types of citrate-soluble silicon fertilizer and water-soluble silicon fertilizer, wherein the citrate-soluble silicon fertilizer is prepared from waste steel slag, fly ash and ore of a steel mill, the effective silicon of the citrate-soluble silicon fertilizer is part of silicon which is insoluble in water and soluble in acid and is absorbed and utilized by plants, the plants can only release organic acid through root systems to dissolve, the process is very slow, heavy metals can be contained in the fertilizer, heavy metal pollution can be caused in long-term field application, the cost of the ore is high, and the mineral reserve is limited, so that the actual requirement of agricultural production cannot be met; the effective silicon of the water-soluble silicon fertilizer is the part of silicon which is directly absorbed and utilized by plants after being dissolved in water, and the crop has higher absorption and utilization rate, but is usually synthesized by high-temperature chemistry, the production process is more complex, the cost is high, and the content of the effective silicon in the two silicon fertilizers is lower at present. The silicon content in the rice husk is about 10% -21%, which is a valuable resource, and the rice husk can be used for preparing the silicon fertilizer required by plant growth, but the effective silicon content in the prior art for preparing the silicon fertilizer by using the rice husk is low. Therefore, the invention provides the silicon fertilizer prepared from rice hulls and having low cost and high effective silicon content, and the problems of heavy metal pollution, environmental hazard, high cost and the like caused by applying the silicon fertilizer prepared by the traditional method are avoided.
Disclosure of Invention
In view of the above, the invention aims to provide a silicon fertilizer prepared from rice hulls and a preparation method thereof, which avoid heavy metal pollution, environmental hazard and high cost caused by applying the silicon fertilizer prepared by the traditional method, and solve the problems that the silicon fertilizer has low effective silicon content and is used for transforming and utilizing silicate which is difficult to be absorbed by plants in part of soil.
The invention solves the technical problems by the following technical means:
a silicon fertilizer prepared from rice hulls comprises the following raw materials: 60-80 parts by mass of modified rice hull powder, 7-9 parts by mass of calcium lignosulfonate, 10-18 parts by mass of zeolite, 12-20 parts by mass of potassium borate, 8-12 parts by mass of attapulgite powder and 2-5 parts by mass of zinc acetate.
Further, the preparation method of the silicon fertilizer comprises the following steps:
(1) Mixing the crushed zeolite and attapulgite powder, adding the mixture into water, uniformly stirring, adding calcium lignosulfonate, and uniformly stirring to obtain a mixed solution;
(2) Heating the mixed solution to 200-300 ℃, adding zinc acetate, stirring and reacting for 1-3h, cooling to normal temperature, adding potassium borate and modified rice hull powder, adjusting the pH of the reaction system to 6-7, heating the solution again to 400-500 ℃ for concentrating and drying, and finally crushing and filtering to obtain the silicon fertilizer.
Further, the modified rice hull powder comprises the following raw materials: 1-4 parts by mass of potassium permanganate, 14-20 parts by mass of rice hull powder, 0.5-2 parts by mass of polycarbonate powder, 2-5 parts by mass of cerium acetate, 1.5-4.8 parts by mass of silicate and 1-4 parts by mass of diethylenetriamine.
Further, the specific preparation steps of the modified rice hull powder are as follows:
(1) Preparing a potassium permanganate solution and a cerium acetate solution, mixing the potassium permanganate solution and the cerium acetate solution, adding rice hull powder, magnetically stirring for 2-4 hours, performing ultrasonic treatment for 0.5-1 hour, standing for 10-12 hours at room temperature, washing, filtering, drying, and drying to constant weight to obtain pretreated rice hull powder;
(2) Mixing the pretreated rice hull powder with water, adding silicate and polycarbonate powder for reaction for 8-12h, adding diethylenetriamine, heating to 50-70 ℃, keeping for 13-15 h, cooling, and sequentially carrying out suction filtration, washing, drying and cooling to obtain the modified rice hull powder.
Further, in the preparation step (1) of the modified rice hull powder, the concentration of the potassium permanganate solution is 0.2mol/L, and the concentration of the cerium acetate solution is 0.1mol/L.
The pyrogenic product silicon dioxide of the rice hull is taken as a framework, the pore structure of the rice hull powder is increased, potassium permanganate is added to oxidize the rice hull powder, oxygen-containing functional groups on the surface of the rice hull powder are enriched, cerium acetate is added into the pores of the rice hull powder, cerium ions replace impurity atoms such as sodium ions and potassium ions in the rice hull powder, cerium is a rare earth element, and the adsorption capacity of the rice hull powder to silicate can be enhanced. After the silicate improves the activity of the surface of the rice hull powder, the silicate is bonded with the active group of the rice hull powder, so that the silicate is easily grafted on the surface of the rice hull powder. The diethylenetriamine is covalently bonded with the surface groups of the rice hull powder, so that the rice hull powder carries polyamino compounds with strong hydrophilicity, carbonate is easy to hydrolyze in an acidic environment to generate carbonate ions, and the carbonate can react with silicate while adjusting pH, so that silicate which cannot be absorbed and utilized by plants is converted into silicate which can be absorbed by plants, the frequency of applying silicon fertilizer can be properly reduced, and silicon in the silicon fertilizer is prevented from being fixed into silicate to a certain extent
Further, the preparation method of the rice hull powder comprises the following steps:
(1) Crushing dry rice hulls serving as raw materials, adding the crushed dry rice hulls and water into a stainless steel high-temperature reaction kettle, uniformly mixing, sealing the reaction kettle, putting the reaction kettle into a constant-temperature oven for heating, setting the temperature to be 200-240 ℃, maintaining the temperature for 2-6 hours after the temperature is raised, and turning off a power supply to reduce the temperature to room temperature;
(2) And (3) carrying out suction filtration on a mixture generated by the reaction in the reaction kettle to obtain a solid-phase product, drying the collected solid-phase product in a baking oven at 40 ℃ for 24 hours to constant weight, and grinding and crushing the solid-phase product to obtain the rice hull powder.
Further, the ratio of dry rice hulls to water is 1:10.
Further, the mixture generated by the reaction in the preparation step (2) of the rice hull powder is subjected to vacuum filtration by adopting a filter membrane with the diameter of 0.45 mu m.
The beneficial effects are that:
the silicon fertilizer prepared by the invention has the following advantages:
(1) According to the preparation method provided by the invention, rice hulls are used as raw materials and are converted into silicon fertilizer, so that the recycling of wastes is realized;
(2) In the process of preparing rice hull powder, the rice hull powder is treated for 4 hours at 220 ℃ and for 2 hours at 240 ℃ respectively, and the content of active silicon in the rice hull powder obtained by treating for 6 hours at 240 ℃ is 133.55mg/kg when the rice hull powder is prepared.
(3) The obtained silicon fertilizer has high silicon content and extremely low content of harmful impurities such as heavy metal ions, avoids the toxicity, environmental hazard and the like, and in addition, the hydrothermal carbon-based silicon fertilizer is easier to be absorbed by crops, so that the quality of the crops can be improved by application; the prepared silicon fertilizer can act with silicate in soil to convert ineffective silicon in the soil into effective silicon, and the silicon fertilizer is not needed to be added purely by human.
Drawings
Fig. 1: the rice hull powder after the reaction of examples 1-5 has an effective silicon content;
fig. 2: growth patterns of ryegrass after application of the silicon fertilizer prepared in example 6;
fig. 3: growth patterns of ryegrass after application of the silicon fertilizer prepared in example 5;
fig. 4: growth pattern of ryegrass after application of the silicon fertilizer prepared in comparative example 5.
Detailed Description
The invention will be described in detail below with reference to examples and figures:
the invention provides a silicon fertilizer prepared from rice hulls and a preparation method thereof, but rice hull powder is prepared in advance, and the specific preparation steps of the rice hull powder prepared by the invention are as follows:
example 1: preparation of Rice husk powder
The rice hull powder used in this example may be prepared by the steps of:
(1) Crushing 1kg of dry rice hulls serving as raw materials, and mixing the dry rice hulls with water according to a weight ratio of 1:10, adding the mixture into a stainless steel high-temperature reaction kettle, uniformly mixing, and sealing the reaction kettle; heating the reaction kettle in a constant temperature oven, setting the temperature to be 200 ℃, maintaining for 4 hours after the temperature is raised to 200 ℃, and turning off a power supply to reduce the temperature to room temperature;
(2) And (3) carrying out vacuum suction filtration on the mixture generated by the reaction in the reaction kettle by adopting a filter membrane with the diameter of 0.45 mu m to obtain a solid-phase product, and drying the collected solid-phase product in a baking oven with the temperature of 40 ℃ for 24 hours to constant weight to obtain the solid-phase product which is rice hull powder.
Example 2: preparation of rice husk powder
(1) Crushing 1kg of dry rice hulls serving as raw materials, and mixing the dry rice hulls with water according to a weight ratio of 1:10, adding the mixture into a stainless steel high-temperature reaction kettle, uniformly mixing, and sealing the reaction kettle; heating the reaction kettle in a constant temperature oven, setting the temperature to 220 ℃, maintaining for 4 hours after the temperature rises to 220 ℃, and turning off a power supply to reduce the temperature to room temperature;
(2) And (3) carrying out vacuum suction filtration on the mixture generated by the reaction in the reaction kettle by adopting a filter membrane with the diameter of 0.45 mu m to obtain a solid-phase product, and drying the collected solid-phase product in a baking oven with the temperature of 40 ℃ for 24 hours to constant weight to obtain the solid-phase product which is rice hull powder.
Example 3: preparation of Rice husk powder
(1) Crushing 1kg of dry rice hulls serving as raw materials, and mixing the dry rice hulls with water according to a weight ratio of 1:10, adding the mixture into a stainless steel high-temperature reaction kettle, uniformly mixing, and sealing the reaction kettle; heating the reaction kettle in a constant temperature oven, setting the temperature to 240 ℃, maintaining for 2 hours after the temperature rises to 240 ℃, and turning off a power supply to reduce the temperature to room temperature;
(2) And (3) carrying out vacuum suction filtration on the mixture generated by the reaction in the reaction kettle by adopting a filter membrane with the diameter of 0.45 mu m to obtain a solid-phase product, and drying the collected solid-phase product in a baking oven with the temperature of 40 ℃ for 24 hours to constant weight to obtain the solid-phase product which is rice hull powder.
Example 4: preparation of Rice hull powder
(1) Crushing 1kg of dry rice hulls serving as raw materials, and mixing the dry rice hulls with water according to a weight ratio of 1:10, adding the mixture into a stainless steel high-temperature reaction kettle, uniformly mixing, and sealing the reaction kettle; heating the reaction kettle in a constant temperature oven, setting the temperature to 240 ℃, maintaining for 4 hours after the temperature rises to 240 ℃, and turning off a power supply to reduce the temperature to room temperature;
(2) And (3) carrying out vacuum suction filtration on the mixture generated by the reaction in the reaction kettle by adopting a filter membrane with the diameter of 0.45 mu m to obtain a solid-phase product, and drying the collected solid-phase product in a baking oven with the temperature of 40 ℃ for 24 hours to constant weight to obtain the solid-phase product which is rice hull powder.
Example 5: preparation of Rice hull powder
(1) Crushing 1kg of dry rice hulls serving as raw materials, and mixing the dry rice hulls with water according to a weight ratio of 1:10, adding the mixture into a stainless steel high-temperature reaction kettle, uniformly mixing, and sealing the reaction kettle; heating the reaction kettle in a constant temperature oven, setting the temperature to 240 ℃, maintaining for 6 hours after the temperature rises to 240 ℃, and turning off a power supply to reduce the temperature to room temperature;
(2) And (3) carrying out vacuum suction filtration on the mixture generated by the reaction in the reaction kettle by adopting a filter membrane with the diameter of 0.45 mu m to obtain a solid-phase product, and drying the collected solid-phase product in a baking oven with the temperature of 40 ℃ for 24 hours to constant weight to obtain the solid-phase product which is rice hull powder.
After the rice hull powder prepared in examples 1 to 5 was subjected to the active silicon content test, it was found that the active silicon content of the rice hull powder prepared in example 5 was highest at 240℃for 6 hours, as shown in Table 1.
Table 1: EXAMPLES 1-5 effective silicon content of Rice husk powder after reaction
| Group of | Effective silicon content (mg/kg) |
| Example 1 | 99.55 |
| Example 2 | 107.38 |
| Example 3 | 102.24 |
| Example 4 | 122.73 |
| Example 5 | 133.55 |
Example 6: preparation of silicon fertilizer
In the embodiment, modified rice hull powder is required to be prepared before the silicon fertilizer is prepared, and the adopted modified rice hull powder is prepared by weighing the following raw materials according to the mass, wherein the rice hull powder is prepared by adopting the rice hull powder prepared in the embodiment 5:
preparing modified rice hull powder:
3kg of potassium permanganate, 17kg of rice hull powder, 1.5kg of polycarbonate powder, 3kg of cerium acetate, 3.2kg of silicate and 3kg of diethylenetriamine are weighed.
(1) Preparing 0.2mol/L potassium permanganate solution and 0.1mol/L cerium acetate solution, mixing the potassium permanganate solution and the cerium acetate solution, adding the rice hull powder prepared in the example 5, magnetically stirring for 3 hours, performing ultrasonic treatment for 1 hour, standing for 11 hours at room temperature, washing, filtering, drying at room temperature, and drying to constant weight to obtain pretreated rice hull powder;
(2) Mixing the pretreated rice hull powder with water, adding silicate and polycarbonate powder for reaction for 10 hours, adding diethylenetriamine, heating to 60 ℃, keeping for 14 hours, cooling, and sequentially carrying out suction filtration, washing, drying and cooling to obtain the modified rice hull powder.
And (3) preparing a silicon fertilizer:
70kg of modified rice hull powder, 8kg of calcium lignosulfonate, 14kg of zeolite, 16kg of potassium borate, 10kg of attapulgite powder and 3kg of zinc acetate are weighed.
(1) Mixing the crushed zeolite and attapulgite powder, adding the mixture into water, uniformly stirring the mixture at 198r/min, adding calcium lignosulfonate, and uniformly stirring the mixture to obtain a mixed solution;
(2) Heating the mixed solution to 250 ℃, adding zinc acetate, stirring and reacting for 2 hours, cooling to normal temperature, adding potassium borate and modified rice hull powder, adjusting the pH of the reaction system to 6.5, heating the solution again to 450 ℃ for concentrating and drying, and finally crushing and filtering to obtain the silicon fertilizer.
Example 7: preparation of silicon fertilizer
Preparing modified rice hull powder:
1kg of potassium permanganate, 14kg of rice hull powder, 0.5kg of polycarbonate powder, 2kg of cerium acetate, 1.5kg of silicate and 1kg of diethylenetriamine are weighed.
(1) Preparing 0.2mol/L potassium permanganate solution and 0.1mol/L cerium acetate solution, mixing the potassium permanganate solution and the cerium acetate solution, adding the rice hull powder prepared in the example 5, magnetically stirring for 2 hours, ultrasonically stirring for 0.5 hours, standing for 10 hours at room temperature, washing, filtering, drying at room temperature, and drying to constant weight to obtain pretreated rice hull powder;
(2) Mixing the pretreated rice hull powder with water, adding silicate and polycarbonate powder for reaction for 8 hours, adding diethylenetriamine, heating to 50 ℃, keeping for 15 hours, cooling, and sequentially carrying out suction filtration, washing, drying and cooling to obtain the modified rice hull powder.
And (3) preparing a silicon fertilizer:
60kg of modified rice hull powder, 7kg of calcium lignosulfonate, 10kg of zeolite, 12kg of potassium borate, 8kg of attapulgite powder and 2kg of zinc acetate are weighed.
(1) Mixing the crushed zeolite and attapulgite powder, adding the mixture into water, uniformly stirring the mixture at 198r/min, adding calcium lignosulfonate, and uniformly stirring the mixture to obtain a mixed solution;
(2) Heating the mixed solution to 200 ℃, adding zinc acetate, stirring and reacting for 3 hours, cooling to normal temperature, adding potassium borate and modified rice hull powder, adjusting the pH value of the reaction system to 7, heating the solution again to 500 ℃ for concentrating and drying, and finally crushing and filtering to obtain the silicon fertilizer.
Example 8: preparation of silicon fertilizer
Preparing modified rice hull powder:
4kg of potassium permanganate, 20kg of rice hull powder, 2kg of polycarbonate powder, 5kg of cerium acetate, 4.8kg of silicate and 4kg of diethylenetriamine are weighed.
(1) Preparing 0.2mol/L potassium permanganate solution and 0.1mol/L cerium acetate solution, mixing the potassium permanganate solution and the cerium acetate solution, adding the rice hull powder prepared in the example 5, magnetically stirring for 4 hours, performing ultrasonic treatment for 1 hour, standing for 12 hours at room temperature, washing, filtering, drying at room temperature, and drying to constant weight to obtain pretreated rice hull powder;
(2) Mixing the pretreated rice hull powder with water, adding silicate and polycarbonate powder for reaction for 12 hours, adding diethylenetriamine, heating to 70 ℃, keeping for 13 hours, cooling, and sequentially carrying out suction filtration, washing, drying and cooling to obtain the modified rice hull powder.
And (3) preparing a silicon fertilizer:
80kg of modified rice hull powder, 9kg of calcium lignosulfonate, 18kg of zeolite, 20kg of potassium borate, 12kg of attapulgite powder and 5kg of zinc acetate are weighed.
(1) Mixing the crushed zeolite and attapulgite powder, adding the mixture into water, uniformly stirring the mixture at 198r/min, adding calcium lignosulfonate, and uniformly stirring the mixture to obtain a mixed solution;
(2) Heating the mixed solution to 300 ℃, adding zinc acetate, stirring and reacting for 1h, cooling to normal temperature, adding potassium borate and modified rice hull powder, adjusting the pH of the reaction system to 6, heating the solution again to 400 ℃ for concentrating and drying, and finally crushing and filtering to obtain the silicon fertilizer.
Comparative example 1: preparation of silicon fertilizer
The silicon fertilizer prepared in this comparative example is in contrast to the silicon fertilizer prepared in example 6, and is mainly different in that cerium acetate is not added to treat the rice hull powder in the preparation process of step (1) when preparing the modified rice hull powder, and the rest of raw material proportions and steps are the same as those of example 6, and the specific preparation steps are as follows:
preparing modified rice hull powder:
(1) Preparing 0.2mol/L potassium permanganate solution, adding the rice hull powder prepared in the example 5 into the potassium permanganate solution, magnetically stirring for 3 hours, performing ultrasonic treatment for 1 hour, standing for 11 hours at room temperature, washing, filtering, drying at room temperature, and drying to constant weight to obtain the pretreated rice hull powder.
And (3) preparing a silicon fertilizer:
the modified rice hull powder is prepared by the method, and the rest steps and raw materials are the same as those of the silicon fertilizer in the example 6.
Comparative example 2: preparation of silicon fertilizer
The silicon fertilizer prepared in this comparative example is in contrast to the silicon fertilizer prepared in example 6, and is mainly different in that polycarbonate powder is not added to treat rice hull powder in the preparation process of step (2) when preparing modified rice hull powder, and the rest of raw material proportions and steps are the same as those of example 6, and specific preparation steps are as follows:
preparing modified rice hull powder:
(2) Mixing the pretreated rice hull powder with water, adding silicate for reaction for 10 hours, adding diethylenetriamine, heating to 60 ℃, keeping for 14 hours, cooling, and sequentially carrying out suction filtration, washing, drying and cooling to obtain the modified rice hull powder.
And (3) preparing a silicon fertilizer:
the modified rice hull powder is prepared by the method, and the rest steps and raw materials are the same as those of the silicon fertilizer in the example 6.
Comparative example 3: preparation of silicon fertilizer
The silicon fertilizer prepared in this comparative example is in contrast to the silicon fertilizer prepared in example 6, and is mainly different in that diethylenetriamine is not added in the preparation process of step (2) in preparing the modified rice hull powder to treat the rice hull powder, and the rest of raw material proportions and steps are the same as those of example 6, and the specific preparation steps are as follows:
preparing modified rice hull powder:
(2) Mixing the pretreated rice hull powder with water, adding silicate and polycarbonate powder for reaction for 10 hours, cooling, and sequentially carrying out suction filtration, washing, drying and cooling to obtain the modified rice hull powder.
And (3) preparing a silicon fertilizer:
the modified rice hull powder is prepared by the method, and the rest steps and raw materials are the same as those of the silicon fertilizer in the example 6.
Comparative example 4: preparation of silicon fertilizer
The silicon fertilizer prepared in this comparative example is in contrast to the silicon fertilizer prepared in example 6, and the main difference is that step (1) is absent in preparing the modified rice hull powder, i.e. the rice hull powder is directly modified without a pretreatment step, and the proportions and steps of the rest raw materials are the same as those of example 6, and the specific preparation steps are as follows:
preparing modified rice hull powder:
(1) Mixing the rice hull powder prepared in the example 5 with water, adding silicate and polycarbonate powder for reaction for 10 hours, adding diethylenetriamine, heating to 60 ℃, keeping for 14 hours, cooling, and sequentially carrying out suction filtration, washing, drying and cooling to obtain the modified rice hull powder.
And (3) preparing a silicon fertilizer:
the modified rice hull powder is prepared by the method, and the rest steps and raw materials are the same as those of the silicon fertilizer in the example 6.
Comparative example 5: preparation of silicon fertilizer
The silicon fertilizer prepared in this comparative example is compared with the silicon fertilizer prepared in example 5, and the main difference is that in the preparation of the modified rice hull powder, the step (2) is absent, namely, the rice hull powder is directly prepared after pretreatment without secondary modification, and the proportion of the rest raw materials is the same as that of example 5, and the specific preparation steps are as follows:
preparing modified rice hull powder:
(1) Preparing 0.2mol/L potassium permanganate solution and 0.1mol/L cerium acetate solution, mixing the potassium permanganate solution and the cerium acetate solution, adding the rice hull powder prepared in the example 5, magnetically stirring for 3 hours, ultrasonically stirring for 1 hour, standing for 11 hours at room temperature, washing, filtering, drying at room temperature, and drying to constant weight to obtain pretreated rice hull powder;
and (3) preparing a silicon fertilizer:
the modified rice hull powder is prepared by the method, and the rest steps and raw materials are the same as those of the silicon fertilizer in the example 6.
Comparative example 6: preparation of silicon fertilizer
The silicon fertilizer prepared in this comparative example is in contrast to the silicon fertilizer prepared in example 6, and the main difference is that the modified rice hull powder is not used, only the rice hull powder prepared in example 5 is used, and the rest of the raw material ratios and steps are the same as those of example 6.
Comparative example 7: preparation of silicon fertilizer
The silicon fertilizer prepared in this comparative example is in contrast to the silicon fertilizer prepared in example 6, and is mainly different in that only activated carbon is used without using modified rice hull powder, and the rest of the raw material proportions and steps are the same as those of example 6.
Experiment one: effective silicon content test in silicon fertilizer
The silicon fertilizers prepared in example 6 and comparative examples 1 to 7 were selected, 5g of each sample was taken, the effective silicon content in each group of the prepared silicon fertilizers was tested with reference to the national standard NY/T797-2004, and a blank control group was additionally provided, and when the blank control group was measured, the conditions were the same except that no sample was added, and each was repeated three times.
The testing steps are as follows:
(1) Preparation of sample solution: weighing about 1g of each group of samples, placing the samples in a 250mL dry conical flask or volumetric flask with a plug, accurately adding 150mL of 0.5mol/L hydrochloric acid solution preheated to 28 ℃, plugging the plug, and oscillating; and (3) using a 30r/min up-down rotary oscillator to keep the temperature of the solution at 28-30 ℃ and oscillating for 1h. Immediately after the end of shaking, the filtrate was filtered through a dry funnel and a quick filter paper, and the first few ml of filtrate was discarded.
(2) Determination of the content: accurately sucking 50mL of filtrate in an evaporation dish, adding 40mL of hydrochloric acid saturated boric acid solution, uniformly mixing, evaporating to near dryness on a water bath, adding 40mL of hydrochloric acid and 20mL of 20g/L animal glue solution, and preserving the temperature in the water bath at 70-80 ℃ for 30min to dissolve and agglomerate silicon dioxide. The precipitate is filtered by a pouring method with quantitative filter paper, the evaporation dish and the precipitate are washed by warm hydrochloric acid solution for 4 times to 6 times, each time with the dosage of about 5mL to 10mL, then the evaporation dish and the precipitate are washed by hot water, each time with about 10mL of water, until no chloride ions exist, and the solution is inspected by using 10g/L of silver nitrate solution;
the precipitate was placed in a platinum crucible with filter paper, the platinum crucible was placed on an electric furnace with an asbestos gauze pad, carefully dried, and after ashing was completed, placed in a muffle furnace. Firing at 950 ℃ for 1h. Taking out, cooling for 30min, and weighing. Adding a plurality of drops of water to wet and precipitate, adding 2 drops of sulfuric acid solution, placing 3mL of hydrofluoric acid on an electric furnace with a asbestos net, slowly heating the platinum crucible until the sulfuric acid emits white smoke, and continuously heating and evaporating until the platinum crucible is nearly dry. Taking down the platinum crucible, cooling to room temperature, adding 5mL of hydrofluoric acid, continuously heating until the white smoke of sulfur trioxide is exhausted, transferring into a muffle furnace, and burning for 1h at 950 ℃. Taking out, cooling for 30min, and weighing.
Wherein the effective silicon content (SiO 2 ) In mass fraction W (SiO 2 ) The representation is:
W＝100×[(m 1 -m 2 )-(m 3 -m 4 )]/(m×50÷150)
m 1 (g) -mass of precipitate and platinum crucible before hydrofluoric acid treatment;
m 2 (g) -mass of precipitate and platinum crucible after hydrofluoric acid treatment;
m 3 (g) -blank testing the mass of the precipitate and platinum crucible before hydrofluoric acid treatment;
m 4 (g) -the mass of the precipitate and the platinum crucible after the hydrofluoric acid treatment was blank tested;
m-sample mass (g)
TABLE 1
| Group of | Effective silicon content/(%) |
| Example 6 | 83.60 |
| Comparative example 1 | 75.28 |
| Comparative example 2 | 71.15 |
| Comparative example 3 | 67.04 |
| Comparative example 4 | 74.57 |
| Comparative example 5 | 71.12 |
| Comparative example 6 | 67.41 |
| Comparative example 7 | 55.90 |
| Blank control | 34.95 |
Experiment II: growth status of ryegrass
And (3) selecting perennial ryegrass seeds with full particles, no insect damage and consistent size, sterilizing, and then performing a growth test, and accurately weighing 1.2kg of soil in the flowerpot. 100 seeds of each group are respectively mixed with the silicon fertilizer prepared in the example 6 and the comparative examples 1-7, evenly planted in a flowerpot, quantitatively watered after the seeds emerge, potted plants are placed in a greenhouse, the illumination is carried out for 16 hours, the temperature is (26+/-2) DEG C, the darkness is 8 hours, the temperature is (24+/-2) DEG C, and the relative humidity is 70%. Regulating the moisture by deionized water, and supplementing the soil moisture according to a weighing method at regular intervals so as to keep the soil moisture unchanged. Ryegrass was harvested at week 4 after sowing in 3 replicates and the results are shown in table 2.
TABLE 2
| Group of | Height of plant (cm) | Root length (cm) |
| Example 6 | 34.25 | 19.56 |
| Comparative example 1 | 30.60 | 18.87 |
| Comparative example 2 | 28.27 | 16.81 |
| Comparative example 3 | 29.23 | 18.04 |
| Comparative example 4 | 28.74 | 17.12 |
| Comparative example 5 | 27.98 | 16.03 |
| Comparative example 6 | 27.56 | 14.01 |
| Comparative example 7 | 26.03 | 13.45 |
| Blank control | 21.33 | 10.64 |
From tables 1 to 2, it is possible to:
1. the silicon fertilizer prepared in example 6 has 83.60% of effective silicon content, and ryegrass obtained by four weeks of cultivation by using the silicon fertilizer prepared in example 6 in experiment II has 34.25cm of plant height and 19.56cm of root length, which shows that the silicon fertilizer prepared according to the raw material proportion and the method disclosed by the invention has high content of active silicon, can be directly absorbed and utilized by plants, and has the best effect of promoting growth of ryegrass.
2. The effective silicon content of the comparative example 1 is reduced by 8.32% compared with that of the example 6, the plant height of ryegrass is 30.60cm, the root length is 18.87cm, no cerium acetate serving as a raw material is added in pretreatment, the adsorption capacity of rice hull powder to silicate is weakened, silicate cannot be adsorbed well, and the silicate is difficult to be converted in subsequent reaction. Comparative example 2 has an effective silicon content of 71.15%, ryegrass has a plant height of 28.27cm and a root length of 16.81cm, and the raw material polycarbonate is not added during pretreatment, so that the carbonic acid ions and silicate react to produce silicic acid required for plants, and the available effective silicon of the plants is provided by the silicon fertilizer only, so that the effect is poorer than that of example 6.
3. The effective silicon content of the comparative example 3 is 16.56% less than that of the example 5, the plant height of ryegrass is 29.23cm, the root length is 18.04cm, and no raw material diethylenetriamine is added in the modification; the effective silicon content of comparative example 4 is 9.03% less than that of example 5, the plant height of ryegrass is 28.74cm, the root length is 17.12cm, rice hull powder is not pretreated, the oxygen-containing functional groups on the surface are less, the number of polycarbonate grafts on the surface of rice hull powder in the modification step is reduced, and cerium acetate modification is not introduced. The effective silicon content of comparative example 5 was 71.12%, the plant height of ryegrass was 27.98cm, the root length was 16.03cm, the rice hull powder was not modified, the surface activity was poor, and the original silumin in the soil could not be converted.
4. The effective silicon contents of comparative example 6 and comparative example 7 were 67.41% and 55.90%, respectively, the plant heights of ryegrass were 27.56cm and 26.03cm, respectively, and the root lengths were 14.01cm and 13.45cm, respectively, and compared with the blank control group, both groups had a certain influence on the growth of ryegrass, but the provided effective silicon was insufficient, and only the effect of a general fertilizer was achieved.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention. The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (8)
1. The silicon fertilizer prepared from rice hulls is characterized by comprising the following raw materials: 60-80 parts by mass of modified rice hull powder, 7-9 parts by mass of calcium lignosulfonate, 10-18 parts by mass of zeolite, 12-20 parts by mass of potassium borate, 8-12 parts by mass of attapulgite powder and 2-5 parts by mass of zinc acetate.
2. The preparation method of the silicon fertilizer prepared from rice hulls is characterized by comprising the following steps of:
(1) Mixing the crushed zeolite and attapulgite powder, adding the mixture into water, uniformly stirring, adding calcium lignosulfonate, and uniformly stirring to obtain a mixed solution;
(2) Heating the mixed solution to 200-300 ℃, adding zinc acetate, stirring and reacting for 1-3h, cooling to normal temperature, adding potassium borate and modified rice hull powder, adjusting the pH of the reaction system to 6-7, heating the solution again to 400-500 ℃ for concentrating and drying, and finally crushing and filtering to obtain the silicon fertilizer.
3. The method for preparing a silicon fertilizer by rice husk according to claim 2, wherein the modified rice husk powder comprises the following raw materials: 1-4 parts by mass of potassium permanganate, 14-20 parts by mass of rice hull powder, 0.5-2 parts by mass of polycarbonate powder, 2-5 parts by mass of cerium acetate, 1.5-4.8 parts by mass of silicate and 1-4 parts by mass of diethylenetriamine.
4. The method for preparing a silicon fertilizer by rice hulls according to claim 3, wherein the specific preparation steps of the modified rice hull powder are as follows:
(1) Preparing a potassium permanganate solution and a cerium acetate solution, mixing the potassium permanganate solution and the cerium acetate solution, adding rice hull powder, magnetically stirring for 2-4 hours, performing ultrasonic treatment for 0.5-1 hour, standing for 10-12 hours at room temperature, washing, filtering, drying, and drying to constant weight to obtain pretreated rice hull powder;
(2) Mixing the pretreated rice hull powder with water, adding silicate and polycarbonate powder for reaction for 8-12h, adding diethylenetriamine, heating to 50-70 ℃, keeping for 13-15 h, cooling, and sequentially carrying out suction filtration, washing, drying and cooling to obtain the modified rice hull powder.
5. The method of producing a silicon fertilizer according to claim 4, wherein the concentration of the potassium permanganate solution in the step (1) of producing the modified rice hull powder is 0.2mol/L and the concentration of the cerium acetate solution is 0.1mol/L.
6. The method for preparing a silicon fertilizer by rice hulls according to claim 4, wherein the rice hull powder is prepared by the following steps:
(1) Crushing dry rice hulls serving as raw materials, uniformly mixing the crushed dry rice hulls with water, heating the mixture, setting the temperature to be 200-240 ℃, maintaining the temperature for 2-6 hours after the temperature rises, and turning off a power supply to reduce the temperature to room temperature;
(2) And (3) carrying out suction filtration on a mixture generated by the reaction in the reaction kettle to obtain a solid-phase product, drying the collected solid-phase product in a baking oven at 40 ℃ for 24 hours to constant weight, and grinding and crushing the solid-phase product to obtain the rice hull powder.
7. The method of claim 6, wherein the mass ratio of dry rice hull to water is 1:10.
8. The method of claim 6, wherein the mixture produced by the reaction in step (2) is vacuum filtered through a 0.45 μm filter.
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