WO2009070953A1 - Procédé de préparation d'un engrais minéral microporeux à partir de roche de silicates à l'aide d'une réaction chimique hydrothermale - Google Patents

Procédé de préparation d'un engrais minéral microporeux à partir de roche de silicates à l'aide d'une réaction chimique hydrothermale Download PDF

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WO2009070953A1
WO2009070953A1 PCT/CN2008/001185 CN2008001185W WO2009070953A1 WO 2009070953 A1 WO2009070953 A1 WO 2009070953A1 CN 2008001185 W CN2008001185 W CN 2008001185W WO 2009070953 A1 WO2009070953 A1 WO 2009070953A1
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potassium
rock
mineral fertilizer
reaction
water
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PCT/CN2008/001185
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Chinese (zh)
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Cheng Han
Jianming Liu
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Institute Of Geology And Geophysics Cas
Sino-Mineral Technology
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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D9/00—Other inorganic fertilisers

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  • the invention belongs to the field of mineral fertilizer production, and particularly relates to a method for preparing multi-element microporous mineral fertilizer from silicate rock by hydrothermal chemical reaction in a semi-wet state. Background technique
  • Plant growth requires not only NPK, but also medium elements such as silicon, calcium, magnesium, and sulfur, as well as trace elements such as iron, manganese, boron, and rare earth.
  • medium elements such as silicon, calcium, magnesium, and sulfur, as well as trace elements such as iron, manganese, boron, and rare earth.
  • trace elements such as iron, manganese, boron, and rare earth.
  • Each of the essential nutrients has its special function and cannot be Replaced by other elements.
  • the various fertility factors in the soil are not isolated, but interconnected and mutually constrained.
  • the yield of crops depends mainly on the supply of the least amount of nutrients in the soil (similar to the barrel theory, the storage capacity of the barrel depends on the twist of the shortest board), and the elements such as potassium, silicon, calcium and magnesium in the soil.
  • the shortage seriously restricts the absorption and utilization of nitrogen and phosphorus by crops.
  • maintaining a nutrient balance is a key factor for a sustainable agricultural farming system.
  • the existing hydrothermal chemical methods mainly include the following methods.
  • GB186199 discloses a method for extracting potassium from feldspar.
  • the potassium-containing rock is ground into a fine powder in a ball mill or a roller mill, and then the potassium-containing rock fine powder and the dilute hydrochloric acid solution are mixed and placed in an acid-resistant colloid mill. Grinding into a high-fine suspension, and transferring the obtained high-fineness suspension to the autoclave, heat treatment at about 225 ° C (25 atm), a large amount of potassium in the potassium-containing rock is dissolved into the solution, and filtered. , Evaporation and concentration, KC1 can be obtained.
  • the potassium-containing rock fine powder may also be mixed with an alkali solution, processed into a fine-grained suspension in a colloid mill, and then heat-treated in an autoclave, filtered, and concentrated by evaporation to obtain a KOH product.
  • Jumei Yamasaki conducted a high-pressure extraction of potassium from potassium feldspar with Ca(OH) 2 slurry at 100 ° C to 400 ° C.
  • the potassium leaching rate was 90% ( Jumei Yamasaki. J. Chem.Soc. Japan Ind Chem Sect.
  • Chemak found that at 150 °C ⁇ 200 °C, the KOH solution reacted with the shale in the Opalinus region of Switzerland to form calcium cross zeolite, which on the one hand activated potassium in the shale and on the other hand because the potassium ions were in the zeolite.
  • the cavity and channel are not filtered by water, and a long-acting potash can be prepared (JA Chermak.
  • Potassium feldspar powder is placed in a 300 ⁇ high pressure alkaline water system to dissociate the ore to obtain AI(OH) 3 and KOH solutions.
  • the inventors have also carried out research on extracting potassium from potassium-containing silicate rock (insoluble potassium ore) since 1996. Research, has won three invention patents (patent number ZLO 1100474.6, ZL01100475.4 and ZL02156824.3) 0 on the basis of learning from domestic and foreign experience in potassium, created a new hydrothermal chemical reaction method to extract potassium, KOH, K 2 C0 3 and K 2 S0 4 preparations were obtained.
  • the potassium-containing silicate rock used is mainly a special type of rock composed of authigenic silicate minerals. In this type of rock, the potassium-bearing minerals are mainly potassium feldspar, illite, glauconite, mica minerals, etc.
  • the chemical composition has a high K 2 0 content, generally more than 10%.
  • the potassium-containing silicate rock used in the prior art is mainly a special rock composed of autogenous silicate minerals having a relatively high content of ⁇ 2 ⁇ , and there is no method for producing mineral fertilizer by using ordinary silicate rock. . More importantly, to date, there has not been an effective nutrient that can simulate the geochemical weathering process, transform the various minerals in silicate rock into plant growth, and make it unique. Structural technology. Summary of the invention
  • the object of the present invention is to provide a hydrothermal chemical reaction method capable of converting a main element and a trace element in a silicate rock into a multi-element novel mineral fertilizer which can be absorbed by a plant.
  • reaction product is dried, pulverized and sieved to obtain a multi-element microporous mineral fertilizer.
  • the alkaline earth activators described therein include lime, light burned magnesia and dolomitic lime.
  • the second solution adopted by the present invention to solve the technical problem is: using a hydrothermal chemical reaction to prepare a multi-element microporous mineral fertilizer from a silicate rock, the characteristics of which include the following steps: (1) pulverizing and grinding the silicate rock, the alkaline earth activator and the activator into a powdery material;
  • reaction product is dried, pulverized and sieved to obtain a multi-element microporous mineral fertilizer.
  • the alkaline earth activator described therein includes lime, light burned magnesia and dolomitic lime, and the activator comprises gypsum and magnesium borate.
  • Multi-element microporous mineral fertilizer prepared from a potassium-containing silicate rock according to the method provided by the present invention, comprising
  • the invention transforms the main elements and trace elements in the silicate rock into a multi-mineral mineral fertilizer which can be absorbed by the plant, and reforms the concept of the traditional single element fertilizer or the simple element compound fertilizer.
  • the method for preparing a multi-element mineral fertilizer of the present invention can rapidly and cost-effectively convert various minerals in a silicate rock into an effective form that the plant can absorb, thereby possibly ending the human being at the root. It has historically relied on the natural weathering process to obtain the state of effective mineral nutrients in the soil.
  • Figure 1 is an X-ray powder crystal diffraction phase analysis diagram of a hydrothermal reaction product
  • Figure 2 is a scanning electron micrograph of a hydrothermal reaction product. detailed description
  • the silicate rock used for producing the mineral fertilizer is not particularly limited in the present invention, and complicated pre-treatment such as beneficiation, roasting, and the like is not required.
  • the alkaline earth activator used in the present invention may be either a relatively pure industrial lime or an industrial light burned magnesia, or a dolomitic lime obtained by calcination of dolomite, wherein CaO-MgO may be in any ratio.
  • the activator used in the present invention may be either gypsum or magnesium borate.
  • the presence of gypsum The activity of Ca(OH) 2 or/and Mg(OH) 2 is greatly stimulated, resulting in higher conversion.
  • Magnesium borate can promote the disintegration and destruction of the silicon oxytetrahedron and the aluminoxy tetrahedron structure in the silicate mineral, thereby achieving the purpose of increasing the conversion rate and increasing the content of the active ingredient in the product.
  • the particle size of the solid material is selected to be less than 200 mesh (i.e., 0.074 mm or less). Excessive particle size affects the rate of reaction, resulting in a decrease in the amount of active ingredient in the product. The particles should not be too fine, otherwise the power consumption in the grinding will increase, resulting in an increase in production costs.
  • the amount of water is extremely important. Too little water does not guarantee the dissolution of the various components, while too much water reduces the throughput of the material, thereby reducing productivity.
  • the amount of water used in the present invention is selected in accordance with the amount of the solid material so that the solid material is in a semi-wet state.
  • the ratio of the amount of water to the solid material i.e., the solid-liquid ratio, is 1:1 to 3, preferably 1:1.2 to 1.5.
  • the pressure in the reaction system is also important for the hydrothermal reaction.
  • steam can be introduced into the reaction system to keep the reaction pressure constant.
  • the greater the pressure the more favorable the hydrothermal reaction is.
  • the pressure of the introduced vapor is preferably 0.2 to 5 MPa, more preferably 0.5 to 2 MPa, and most preferably about 1.2 to 1.3 MPa.
  • the reaction temperature and time are important factors in determining the effect of the hydrothermal reaction.
  • the higher temperature facilitates the disintegration and destruction of the potassium-containing silicate in the hydrothermal chemical reaction, thereby achieving the purpose of increasing the conversion rate and increasing the content of the active ingredient in the product, and also shortening the reaction time and increasing the productivity.
  • the excessively high reaction temperature requires higher and stricter heat resistance and pressure resistance performance of the reactor, resulting in an increase in equipment investment, which is not conducive to reducing production costs.
  • lower temperatures result in lower conversion rates, lower levels of active ingredients in the product, and excessive reaction times, increasing production costs.
  • the reaction temperature range of the present invention is preferably from 100 to 300 ° C, more preferably from 130 to 250 ° C, most preferably from 170 to 200 ° C, from the viewpoint of obtaining an ideal multi-element mineral fertilizer and reducing cost, and the reaction time is preferably It is 5 to 24 hours, more preferably 7 to 14 hours.
  • the hydrothermal reaction of the present invention is carried out under static conditions, which can greatly reduce energy consumption, make the technology simple, and is easy to implement in the process flow, and the worker is easy to operate and implement. Moreover, there is no discharge of waste water, waste gas and solid waste in the whole production process, which is a green environmental protection technology.
  • the results of the dissolution test on the hot water reaction product according to the procedures prescribed by the Ministry of Agriculture indicate that 65%-95% of the solid phase material composition can be dissolved in 0.5 mole hydrochloric acid solution, which is a water-soluble substance that can be absorbed by plants. Or hydrazine soluble components.
  • the water-soluble and hydrazine-soluble K 2 0 content is about 4%-6% (equivalent to the potassium and calcium fertilizer currently on the market), and is a chlorine-free potassium fertilizer.
  • this product is a good long-acting slow-release mineral fertilizer with potassium, silicon, calcium, magnesium, iron, manganese and boron.
  • the multi-element mineral fertilizer of the present invention is mainly composed of fine crystals of the following two synthetic minerals: Tobe mullite [Ca 5 Si 6 0 16 (OH) 2 .43 ⁇ 40] and hydrated calcium aluminosilicate [Ca 3 Al 2 (Si0 4 )(OH)
  • Figure 2 shows the results of scanning electron microscopy analysis of the multi-element mineral fertilizer of the present invention.
  • the particles of the new type of mineral fertilizer are very fine, and are nano-submicron; wherein the hydrated calcium aluminosilicate is micron-sized granules (particle size 1-5 microns).
  • the tobemorite stone is in the form of nano-scale flakes (the thickness of the flakes is tens to hundreds of nanometers).
  • the mineral fertilizer also shows a highly developed microporous structure under a scanning electron microscope, so the mineral fertilizer has a loose texture and a bulk density of only 0.70-0.80 g/cm 3 , so it is also called a microporous mineral fertilizer. Due to the unique fine particles and microporous structure of the mineral fertilizer, it has very high activity, which greatly improves its ability to be dissolved and absorbed by the plant root acid. Moreover, the unique microporous structure of this product also has the functions of retaining water and ensuring fertilizer, improving soil aggregate structure, and promoting ventilation and ventilation of plant roots.
  • the unique fine-grained and microporous structure of this mineral fertilizer is due to the use of a unique alkaline earth activator and a semi-wet process during its preparation, and the temperature, pressure and hydrothermal reaction are controlled just right. time.
  • the potassium silicon calcium fertilizer produced by the roasting process, the yellow phosphorus slag produced by the phosphating plant, and the silicon calcium fertilizer produced by the steel slag of the steel enterprise do not have such a microporous structure under the scanning electron microscope, and the X-ray powder crystal Diffraction phase analysis shows that it is amorphous or cryptocrystalline.
  • the multi-element microporous mineral fertilizer of the invention does not contain any harmful substances, and retains the natural material composition characteristics of the silicate rock itself. Like the soil formed by natural weathering, the farmland does not cause extratoxicity and pollution after application, and is suitable for Produce natural green food. Moreover, the multi-element microporous mineral fertilizer product of the invention can not cause agricultural non-point source pollution as a long-acting slow-release fertilizer.
  • Potassium-containing silicate rock from Nanshan, Miyun County, Beijing, its chemical composition (%) is as follows
  • X-ray powder crystal diffraction analysis indicates that the potassium-containing rock is mainly potassium feldspar, and the other is quartz.
  • Lime Contains 97% of CaO (chemically pure, China Pharmaceuticals Beijing Purchasing and Supply Station).
  • Potassium-containing silicate rock from Nanshan, Miyun County, Beijing, its chemical composition (%) is as follows
  • X-ray powder crystal diffraction analysis indicates that the potassium-containing rock is mainly potassium feldspar, and the other is quartz.
  • Lime Contains 97% of Ca0 (chemically pure, purchased from China Pharmaceuticals Beijing Supply Station).
  • Gypsum From the Xinjiang and Buxail County Xiazizi bentonite mining area, for the crystallized transparent gypsum, heated in a laboratory oven for 120 hours to obtain hemihydrate gypsum (CaS0 4 ⁇ 1/2H 2 0).
  • the obtained product was transferred to a filter, and the soluble potassium was extracted with water.
  • 100 ml of potassium-containing filter solution was obtained. After dilution, the concentration of potassium in the liquid sample was measured by a flame photometer. The measurement result was converted into a K 2 0 concentration of 5080 mg/L 5.000 g of potassium-containing rock ore powder containing K 2 0 639.5 mg.
  • the leachate is equivalent to a K 20 concentration of 5080 mg/l
  • 100 ml of the filtrate contains K 2 0 508.0 mg, and therefore, the dissolution rate of potassium in the potassium-containing mineral is 79.44%.
  • Example 3 Comparing Example 1 and Example 2, it can be seen that a certain amount of gypsum (herely hemihydrate gypsum) was added to the formulation, which stimulated the activity of lime, and the dissolution rate of potassium in the potassium-containing rock was increased by 8.45%.
  • gypsum hereinafter hemihydrate gypsum
  • Potassium-containing silicate rock taken from Nanshan, Miyun County, Beijing, its chemical composition (%) is as follows:
  • X-ray powder crystal diffraction analysis indicates that the silicate rock mineral composition is mainly potassium feldspar, and the others are quartz.
  • Lime Contains 97% of CaO (chemically pure, China Pharmaceuticals Beijing Purchasing and Supply Station).
  • silicate rock and lime are respectively ground to below 200 mesh to obtain silicate rock powder and lime powder; 15 ml of water is added to the plastic vessel, and then 5.700 g of silicate rock powder and 4.300 g of lime powder are added. Add to the vessel in turn, and stir to mix the materials evenly; (2) The plastic vessel containing the sample is placed in an autoclave and reacted at 191 ° C for 8 hours;
  • Potassium-containing silicate rock from Nanshan, Miyun County, Beijing, its chemical composition (%) is as follows;
  • X-ray powder crystal diffraction analysis indicated that the potassium-bearing rock mineral composition is mainly potassium feldspar, and the others are quartz.
  • Light burned boehmite ore The original ore sample was obtained from Liaoning Tiancheng Chemical Plant, and the raw ore coarse crushed sample was placed in a muffle furnace. At 70 (TC heating and constant temperature for 0.5 hour, it was taken out to obtain a light phase dominated by the glass phase. Burning magnesia ore.
  • Potassium-containing silicate rock taken from Nanshan, Miyun County, Beijing, its chemical composition (%) is as follows:
  • X-ray powder crystal diffraction analysis indicated that the potassium-bearing rock mineral composition is mainly potassium feldspar, and the others are quartz.
  • Potassium-containing silicate rock taken from Nanshan, Miyun County, Beijing, its chemical composition (%> is as follows:
  • X-ray powder crystal diffraction analysis indicated that the potassium-bearing rock mineral composition is mainly potassium feldspar, and the others are quartz.
  • Potassium-rich rock taken from Nanshan, Miyun County, Beijing, its chemical composition (%) is as follows:
  • X-ray powder diffraction analysis indicates that the potassium-rich rock mineral composition is mainly potassium feldspar, and the others are quartz.
  • Baiyun Lime Containing 53.23 % of CaO, 36.27% of MgO, and 8.07% loss on ignition, taken from the Babaoshan limestone mine in Huailai County, Hebei province.
  • Semi-hydrated gypsum purchased from the market.
  • the maximum conversion rate of the insoluble potassium in the raw material to soluble potassium can reach 95.91%.
  • Potassium-containing silicate rock ⁇ from Xuanhua, Zhangjiakou City, Hebei province, its chemical composition (%) is as follows:
  • X-ray powder diffraction analysis indicates that the mineral composition is mainly potassium feldspar and illite, and the others are quartz.
  • Lime Containing 84% CaO, containing Mg0 3%, produced by Xuanhua Iron and Steel Company Longyang Calcium Plant.
  • Gypsum Dihydrate gypsum, purchased from Xuanhua Building Materials Store.
  • Potassium-containing silicate rock ⁇ from Xuanhua, Zhangjiakou City, Hebei province, chemical composition (%) is as follows:
  • X-ray powder diffraction analysis indicates that the mineral composition is mainly potassium feldspar and illite, and the others are quartz.
  • Lime Contains 84% of Ca0, contains 3% of Mg0, and is produced by Xuanhua Iron and Steel Company Longyang Calcium Plant.
  • Light burned boehmite The ore sample was obtained from Liaoning Tiancheng Chemical Plant. The crude ore sample was placed in a muffle furnace, heated at 700 °C for 0.5 hour, and taken out to obtain a glass-based light burn. Boraxite ore.
  • test results are as follows:
  • Table 8 Main element content (wt%) of the multi-element microporous mineral fertilizer of Example 8.
  • Table 9 Trace element content (mg/k g , ie ppm) of the multi-element microporous mineral fertilizer of Example 8.
  • Component B Ba Cd Co Cr Cu Mo Ni Pb Sr V Zn Content 559.0 262.4 3.85 10.15 58.65 5.85 10.15 53.95 10.15 216.85 141.75 81.5
  • microporous mineral fertilizer Scanning electron microscopy (LE01450VP type, produced by Leo, Germany) was used to observe and analyze the microstructure of mineral fertilizers. It was found that the two main synthetic minerals of microporous mineral fertilizers are nano-submicron-sized fine particles. One is spherical (hydrated calcium aluminosilicate), the other mineral is flaky (tobe mullite), and a large number of micropores are distributed (see Figure 2), so it is called microporous mineral fertilizer.
  • the bulk specific gravity of the new microporous mineral fertilizer was determined by the conventional volumetric flask method and found to be 659 g/1 or 0.659 g/cm3. Obviously, its specific gravity is small, which is consistent with the large number of micropore distributions observed in SEM microscopic observations.
  • Example 8 Active ingredient of multi-element microporous mineral fertilizer (%) Table 11 Effective trace element content (mg/kg, ie ppm) of the multi-element microporous mineral fertilizer of Example 8.
  • Component B Ba Cd Co Cr Mo Ni Pb Sr V Zn Cu Contains a 458.70 78.70 0.20 2.90 23.10 2.90 30.30 2.90 211.89 94.30 18.20 0.00
  • the multi-element microporous mineral fertilizer prepared from silicate rock using the hydrothermal chemical reaction of the present invention contains about 4% to 6% of water-soluble and hydrazine-soluble K 2 0 (equivalent to a chlorine-free potassium fertilizer).
  • this product is a good multi-element sustained-release long-acting mineral fertilizer such as potassium, silicon, calcium, magnesium, iron, manganese and boron.

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  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

L'invention porte sur un procédé de préparation d'un engrais minéral microporeux à partir de roche de silicates à l'aide d'une réaction chimique hydrothermale, caractérisé par le mélange de poudre de roche de silicates, de poudre d'initiateur de type solonetz et de poudre d'activateur et par la conduite de la réaction hydrothermale dans une condition subhumide. Les substances minérales contenues dans la roche de silicates peuvent être converties en formes actives qui sont facilement absorbées par les plantes, avec des taux de transformation de 65 à 95 %. L'engrais à matière multiple obtenu par un tel procédé présente une structure microporeuse particulière.
PCT/CN2008/001185 2007-12-05 2008-06-18 Procédé de préparation d'un engrais minéral microporeux à partir de roche de silicates à l'aide d'une réaction chimique hydrothermale WO2009070953A1 (fr)

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US10196317B2 (en) 2013-05-06 2019-02-05 Massachusetts Institute Of Technology Alkali metal ion source with moderate rate of ion release and methods of forming
CN107855096A (zh) * 2017-11-20 2018-03-30 陕西师范大学 一种复盐相转化制备多级孔花球状纳米结构7MgO·2B2O3·7H2O的方法
CN107855096B (zh) * 2017-11-20 2020-07-28 陕西师范大学 一种复盐相转化制备多级孔花球状纳米结构7MgO·2B2O3·7H2O的方法
CN115124379A (zh) * 2021-03-24 2022-09-30 国家能源投资集团有限责任公司 粒状枸溶性硅肥及其制备方法
CN115215685A (zh) * 2022-07-24 2022-10-21 甘肃巨源达生物科技有限公司 一种具有盐碱地土壤调理功能的油页岩半焦基硅肥制备方法
CN115215685B (zh) * 2022-07-24 2024-05-14 白银丰宝农化科技有限公司 一种具有盐碱地土壤调理功能的油页岩半焦基硅肥制备方法

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