A method for preparing porous aluminosilicate glass using humus and the porous aluminosilicate glass.

Porous aluminosilicate glass was prepared by activating humus at high temperature and treating it with acids and alkalis. This solved the problem of impurities in humus, improved its mechanical properties and chemical stability, and enabled the efficient resource utilization of humus.

CN117326803BActive Publication Date: 2026-03-06SHENZHEN ENERGY ENVIRONMENT ENG CO LTD +1
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202311275042.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-09-28
Publication Date
2026-03-06
Estimated Expiration
2043-09-28

AI Technical Summary

Technical Problem

Humus contains impurities such as metal ions and organic matter, which leads to poor mechanical properties and chemical stability of porous glass, slow reaction rate, difficulty in effective resource utilization, and low silicon utilization efficiency.

Method used

High-temperature activated humus is mixed with sodium carbonate, calcined, ball-milled and sieved, and then purified by acid leaching. After purification, it is reacted with alkali to generate sodium silicate-sodium aluminate solution, which is then aged, washed and dried to prepare porous aluminosilicate glass.

Benefits of technology

The reaction rate was improved, the impurity removal effect was better, and the prepared porous aluminosilicate glass had good mechanical properties and chemical stability, realizing the high-value resource utilization of humus.

✦ Generated by Eureka AI based on patent content.
Patent Text Reader

Abstract

A method for preparing porous aluminosilicate glass using humus and the porous aluminosilicate glass. The method includes: (1) mixing humus with sodium carbonate, followed by calcination and ball milling to obtain activated humus with a particle size less than 100 mesh; (2) adding an acidic solution to the small-particle-size activated humus until the pH value is below 1 to react, allowing it to stand, and then performing solid-liquid separation to obtain a precipitate containing silicic acid, aluminosilicate minerals, and carbon, washing the precipitate until the pH value is 2-3; (3) adding an alkaline solution to the precipitate until the pH value is 11-14 to react, followed by solid-liquid separation to obtain a sodium silicate-sodium aluminate mixed solution; (4) adding an acidic solution to the sodium silicate-sodium aluminate mixed solution until the pH value is 9-10 to obtain a gel, which is then aged, washed, solvent-replaced, and dried to obtain porous aluminosilicate glass. This method effectively utilizes the resources of humus.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention belongs to the field of resource utilization of humus in landfills. Specifically, it relates to a method for preparing porous aluminosilicate glass using humus and the porous aluminosilicate glass. Background Technology

[0002] Heavy metals in nature are difficult to biodegrade, and they not only damage the ecological environment but also accumulate in the human body through the food chain, causing significant harm to human health. After being screened, humus is obtained from aged waste in landfills. Humus is a nutrient-rich soil formed from the decomposition and fermentation of plant leaves by microorganisms. The heavy metal content in humus is much higher than in uncontaminated soil. How to utilize humus from landfills while reducing the harm of heavy metals in it to the environment and human health is a challenging problem.

[0003] Porous materials are materials with a porous structure, possessing advantages such as low relative density, large specific surface area, and high porosity, and are widely used in catalysis, adsorbents, energy, and biomedicine. Humus soil has a high silica and aluminum content, making it a suitable source of silica and aluminum. A specific process can be used to first convert the humus soil into a gel, and then the gel can be prepared into porous aluminosilicate glass using the sol-gel method. Simultaneously, during the preparation of porous aluminosilicate glass from humus soil, acid leaching activates the humus, converting iron and aluminum in the soil into ionic states, and solid-liquid separation yields Fe. 3+ Al 3+ Ions can be used as water purification agents and have good application prospects, which makes full use of the main elements of humus.

[0004] However, humus contains many impurities, mainly metal ions and organic matter. The presence of metal ions hinders gel formation and affects the performance of the resulting porous material. Furthermore, the organic matter in humus undergoes high-temperature calcination, carbonizing into carbon. This carbon, present within the particles, cannot burn completely due to the oxygen-deficient environment and remains as carbon black. These larger carbon black particles affect the gel structure, resulting in poor strength of the final porous material. Additionally, inorganic particles in humus are encapsulated by organic colloids, and the humus contains a variety of silicates (aluminosilicates are silicates where a portion of the SiO4 tetrahedron is replaced by AlO4 tetrahedrons), some of which are highly resistant to acids and alkalis, resulting in a slow reaction rate with alkalis and low preparation efficiency.

[0005] In addition, after humus is processed through steps such as high temperature, acid dissolution, and solid-liquid separation, a solution containing sodium silicate can be obtained. However, sodium silicate is mostly present in solids, and the sodium silicate content in the solution is relatively low. Therefore, directly using the sodium silicate-containing solution after solid-liquid separation to prepare porous materials will result in low silicon utilization efficiency and will not be able to achieve good resource utilization of humus. Summary of the Invention

[0006] The purpose of this invention is to address the problems of poor mechanical properties and chemical stability of porous glass prepared from humus containing impurities such as metal ions and organic matter, slow reaction rates due to inorganic colloidal encapsulation, and consequently, ineffective resource utilization of humus and low silicon utilization efficiency. This invention fully activates the humus and reacts it with acid to remove soluble ions, obtaining a relatively pure precipitate. Then, under normal pressure, the precipitate reacts with an alkali to generate a sodium silicate-sodium aluminate solution. Finally, after impurity removal, aging, and drying, porous aluminosilicate glass is prepared. This method improves the reaction rate, achieves better impurity removal, and produces porous aluminosilicate glass with good mechanical properties and chemical stability, realizing high-value resource utilization of humus and suitable for large-scale humus processing. To achieve the above objectives, this invention provides a method for preparing porous aluminosilicate glass from humus and the porous aluminosilicate glass itself. The specific technical solution is as follows:

[0007] A first aspect of the present invention provides a method for preparing porous aluminosilicate glass using humus, comprising the following steps:

[0008] (1) Mix humus with sodium carbonate, and obtain activated humus with a particle size of less than 100 mesh by calcination, ball milling and sieving.

[0009] (2) Add acidic solution to small-particle-size activated humus soil until the pH value is below 1 to carry out the reaction. After standing, perform solid-liquid separation to obtain a precipitate containing silicic acid, aluminosilicate minerals and carbon. Wash the precipitate until the pH value is 2-3.

[0010] (3) Add an alkaline solution to the precipitate until the pH value reaches 11-14 to carry out the reaction, and then separate the solid and liquid to obtain a sodium silicate-sodium aluminate mixed solution;

[0011] (4) Add acidic solution to the sodium silicate-sodium aluminate mixed solution until the pH value is 9-10 to obtain a gel. Then, age, wash, replace solvent and dry to obtain porous aluminosilicate glass.

[0012] Specifically, the humus in step (1) is obtained by multi-stage screening of aged waste. The multi-stage screening is multi-stage drum screening. The first stage drum screen has a hole diameter of 10-15cm, the second stage drum screen has a hole diameter of 5-8cm, and the third stage drum screen has a hole diameter of 0.5-1cm.

[0013] Specifically, in step (1), the mass ratio of humus to sodium carbonate is 1:0.2-1, the calcination temperature is 750-1050℃, and the calcination time is 1-3h. Activation is achieved through calcination. At high temperature, humus reacts with substances such as sodium carbonate, which changes the crystal structure and composition of minerals in the soil and makes it more alkaline, thus allowing it to react with acids.

[0014] Specifically, in step (1), the sieving is performed using a mesh screen with an aperture of less than 100 mesh. The small particle size results in a large contact area with the acid, shortening the acid leaching time and allowing ions to diffuse more easily from the soil particles, leading to more complete ion precipitation. The separated ions are mainly Fe. 3+ And Al 3+ It can be used as a water purification agent and has good economic value.

[0015] Specifically, the acidic solution mentioned in step (2) is one of hydrochloric acid, sulfuric acid, or nitric acid solution, and the concentration of the acid is 1 to 5 mol / L;

[0016] Specifically, the settling time mentioned in step (2) is 3 to 12 hours;

[0017] Specifically, the reaction temperature in step (2) is 60–98°C and the time is 0.5–2 h.

[0018] Specifically, the washing reagent in step (2) is water. By washing the precipitate with water, residual soluble Al in the precipitate can be removed. 3+ Fe 3+ Ca 2+ H + Heavy metal ions, and Cl - SO4 2- NO3 - Using anions yields relatively pure silica gel, making subsequent reactions easier to control.

[0019] Specifically, in step (2), some metal ions are removed through acid dissolution and solid-liquid separation. Since some of the activated aluminum exists as a mineral with a Si-O-Al network structure, this part of the aluminum is relatively difficult to be precipitated by acid, so there will be aluminum residue. Aluminum can improve the chemical stability, mechanical strength, thermal stability, and tensile elastic modulus of glass, and reduce the tendency to crystallize, so that the glass has excellent mechanical, chemical and mechanical properties.

[0020] Specifically, the alkaline solution mentioned in step (3) is either sodium hydroxide or potassium hydroxide solution, and the concentration of the alkali is 6 to 10 mol / L.

[0021] Specifically, the reaction temperature in step (3) is 60–98°C and the reaction time is 6–24 h.

[0022] Specifically, the acidic solution mentioned in step (4) is one of hydrochloric acid, sulfuric acid, and nitric acid, with a concentration of 0.2 to 1 mol / L;

[0023] Specifically, the aging process described in step (4) involves standing for 24 to 48 hours;

[0024] Specifically, the washing reagent in step (4) is water, and the washing is performed 1 to 4 times;

[0025] Specifically, the solvent used in step (4) is a low surface tension organic solvent; the low surface tension organic solvent is selected from one or more of ethanol, isopropanol and n-hexane;

[0026] Specifically, the solvent replacement in step (4) is performed 1 to 4 times, the mass ratio of the solvent replacement gel to the added low surface tension organic solvent is 1:1 to 3 each time, and the solvent replacement time is 3 to 12 hours each time.

[0027] Specifically, the drying procedure in step (4) is as follows:

[0028] First stage: Dry at room temperature for 12–24 hours;

[0029] The second stage: raise the temperature from room temperature to 80-100℃ at a rate of 1-3℃ / min, and keep it at that temperature for 2-3 hours;

[0030] The third stage: the temperature is raised from 80-100℃ to 120-140℃ at a rate of 1-3℃ / min, and then held for 1-2 hours.

[0031] Fourth stage: Increase the temperature from 120-140℃ to 350-400℃ at a rate of 3-5℃ / min, and hold for 2-3 hours.

[0032] During the drying process described above, the internal particles of the gel network structure migrate after aging at high temperature, making the network structure more stable and improving the mechanical strength of the porous aluminosilicate glass.

[0033] In a second aspect, the present invention provides a porous aluminosilicate glass prepared according to any one of the preceding methods.

[0034] The method provided by this invention has the following reaction process:

[0035] By mixing soil and sodium carbonate and calcining them at high temperatures, the silicates in the soil react with the sodium carbonate, thereby reducing the soil's acid and alkali resistance and making it more susceptible to reactions with acids and alkalis, thus increasing soil activity. Simultaneously, high-temperature calcination removes most of the organic matter in the soil, disrupts its structure, and prevents inorganic matter from being encapsulated by organic colloids, reducing the difficulty of subsequent acid and alkali reactions and increasing the reaction rate.

[0036] High-temperature activated humus soil exhibits strong alkalinity. Adding hydrochloric acid while maintaining the pH below 1 triggers a vigorous acid-base neutralization reaction, at which point the Fe in the humus soil... 3+ Ca 2+ and some of the Al 3+ It is released from the soil in ionic form; after standing for a period of time, it forms a precipitate, which can be removed by solid-liquid separation. 3+ Ca 2+ Part of Al 3+ And heavy metal ions, to obtain precipitates, which are composed of silicic acid, aluminosilicate minerals and impurity carbon;

[0037] Then adjust the pH value of the precipitate to 11-14. The remaining metal ions in the solution will precipitate. At the same time, the silicic acid and aluminosilicate minerals in the solid react with the alkali to produce soluble sodium silicate and sodium aluminate, which will concentrate in the solution. Through solid-liquid separation, metal ions and carbon particles remaining after high-temperature burning can be removed to obtain a pure sodium silicate-sodium aluminate solution.

[0038] After adjusting the pH of a pure sodium silicate-sodium aluminate solution to 9-10, sodium silicate and sodium aluminate undergo a condensation reaction to form a sol. Following static aging, the sol particles slowly polymerize, forming a gel with a three-dimensional network structure. After drying and heat treatment, the network structure becomes more stable, thus preparing a porous aluminosilicate glass. The porous aluminosilicate glass prepared using this pure sodium silicate-sodium aluminate solution exhibits good chemical stability and mechanical strength.

[0039] The method of the present invention has the following beneficial effects:

[0040] (1) The present invention uses processes including high-temperature activation, acid leaching (a method of using acid to dissolve substances and thus separating the dissolved substances from other substances), and alkaline reaction to remove impurities from humus soil. The resulting sodium silicate-sodium aluminate solution has high purity, and the prepared porous aluminosilicate glass has good mechanical properties and chemical stability.

[0041] (2) This invention activates humus by high-temperature calcination with sodium carbonate in a certain proportion, altering the crystal structure and composition of minerals in the humus and making it more alkaline. Adding acid to it triggers a vigorous acid-base neutralization reaction, producing silicic acid and other substances, and neutralizing heavy metals and Fe. 3+ and some Al 3+ Extracted from the soil, and after solid-liquid separation, heavy metals and Fe can be obtained. 3+ Al 3+ Plasma, once recycled, has good economic value.

[0042] (3) The present invention uses humus to prepare porous aluminosilicate glass. On the one hand, the cost of humus is low, which reduces the preparation cost of porous aluminosilicate glass. On the other hand, it realizes the resource utilization of humus, which is difficult to process, and greatly increases the added value of humus. Detailed Implementation

[0043] The present invention will now be described in detail with reference to specific embodiments. These embodiments will help those skilled in the art to further understand the present invention, but do not limit the invention in any way. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention. These all fall within the scope of protection of the present invention.

[0044] Example 1

[0045] (1) Weigh 100 parts of humus and 20 parts of sodium carbonate, mix them thoroughly, put them into a high-temperature furnace at 1050℃, calcine for 3 hours, and after cooling, ball mill them and then pass them through a 100-mesh sieve to obtain small-particle activated humus.

[0046] (2) Add hydrochloric acid solution dropwise to 50 portions of the small-particle-size activated humus from step (1) to adjust the pH value to 1. Stir at 60°C for 2 hours to allow it to react fully. After standing for 2 hours, perform solid-liquid separation to obtain the precipitate. Use water to wash the precipitate at a solid-liquid mass ratio of 1:2 to adjust the pH value of the precipitate to 3;

[0047] (3) Add sodium hydroxide solution to the precipitate to adjust its pH value to 12, and react it at 60℃ for 24h. Then perform solid-liquid separation to obtain sodium silicate-sodium aluminosilicate precursor solution.

[0048] (4) Add hydrochloric acid solution to sodium silicate-sodium aluminate solution to adjust its pH value to 10, age at room temperature for 24 hours, wash the aged gel with water; use ethanol solution to replace the solvent in the washed gel, and dry the replaced gel according to the temperature program. The drying program is as follows: place at room temperature for 24 hours; raise from room temperature to 100℃ at a rate of 1℃ / min and keep at that temperature for 2 hours; raise from 100℃ to 140℃ at a rate of 3℃ / min and keep at that temperature for 1 hour; raise from 140℃ to 400℃ at a rate of 5℃ / min and keep at that temperature for 2 hours.

[0049] Example 2

[0050] (1) Weigh 50 parts of humus and 50 parts of sodium carbonate, mix them thoroughly, put them into a high-temperature furnace at 750℃, calcine for 3 hours, and after cooling, ball mill them and then pass them through a 200-mesh sieve to obtain small-particle-size activated humus.

[0051] (2) Add hydrochloric acid solution dropwise to 50 portions of the small-particle-size activated humus from step (1) to adjust the pH value to 1. Stir at 60°C for 1 hour to allow it to react fully. After standing for 2 hours, perform solid-liquid separation to obtain the precipitate. Wash the precipitate to a pH value of 3.

[0052] (3) Add sodium hydroxide solution to the precipitate to adjust its pH value to 12, and react it at 60℃ for 24h. Then perform solid-liquid separation to obtain sodium silicate-sodium aluminosilicate precursor solution.

[0053] (4) Add hydrochloric acid solution to sodium silicate-sodium aluminate solution to adjust its pH value to 10, age at room temperature for 24 hours, wash the aged gel with water; use ethanol solution to replace the solvent in the washed gel, and dry the replaced gel according to the temperature program. The drying program is as follows: place at room temperature for 24 hours; raise from room temperature to 80℃ at a rate of 2℃ / min and keep at that temperature for 2 hours; raise from 80℃ to 140℃ at a rate of 3℃ / min and keep at that temperature for 1 hour; raise from 140℃ to 400℃ at a rate of 5℃ / min and keep at that temperature for 2 hours.

[0054] Example 3

[0055] (1) Weigh 100 parts of humus and 60 parts of sodium carbonate, mix them thoroughly, put them into a high-temperature furnace at 1050℃, calcine for 3 hours, and after cooling, ball mill them and then pass them through a 100-mesh sieve to obtain small-particle activated humus.

[0056] (2) Add hydrochloric acid solution dropwise to 50 portions of the small-particle-size activated humus from step (1) to adjust the pH value to 1. Stir at 98°C for 0.5 h to allow it to react fully. After standing for 2 h, perform solid-liquid separation to obtain the precipitate; wash the precipitate to a pH value of 3;

[0057] (3) Add sodium hydroxide solution to the precipitate to adjust its pH value to 12, and react it at 60℃ for 24h. Then perform solid-liquid separation to obtain sodium silicate-sodium aluminosilicate precursor solution.

[0058] (4) Add hydrochloric acid solution to sodium silicate-sodium aluminate solution to adjust its pH value to 10, age at room temperature for 24 hours, wash the aged gel with water; use ethanol solution to replace the solvent in the washed gel, and dry the replaced gel according to the temperature program. The drying program is as follows: place at room temperature for 24 hours; raise from room temperature to 100℃ at a rate of 3℃ / min and keep at that temperature for 6 hours; raise from 100℃ to 140℃ at a rate of 3℃ / min and keep at that temperature for 1 hour; raise from 140℃ to 400℃ at a rate of 5℃ / min and keep at that temperature for 2 hours.

[0059] Example 4

[0060] (1) Weigh 100 parts of humus and 20 parts of sodium carbonate, mix them thoroughly, put them into a high-temperature furnace at 950℃, calcine for 3 hours, and after cooling, ball mill them and then pass them through a 100-mesh sieve to obtain small-particle activated humus.

[0061] (2) Add hydrochloric acid solution dropwise to 50 portions of the small-particle-size activated humus from step (1) to adjust the pH value to 0. Stir at 75°C for 1 hour to allow it to react fully. After standing for 2 hours, perform solid-liquid separation to obtain the precipitate. Wash the precipitate to a pH value of 3.

[0062] (3) Add sodium hydroxide solution to the precipitate to adjust its pH value to 12, and react it at 60℃ for 24h. Then perform solid-liquid separation to obtain sodium silicate-sodium aluminosilicate precursor solution.

[0063] (4) Add hydrochloric acid solution to sodium silicate-sodium aluminate solution to adjust its pH value to 10, age at room temperature for 24 hours, wash the aged gel with water; use ethanol solution to replace the solvent in the washed gel, and dry the replaced gel according to the temperature program. The drying program is as follows: place at room temperature for 16 hours; raise from room temperature to 100℃ at a rate of 2℃ / min and keep at that temperature for 2 hours; raise from 100℃ to 120℃ at a rate of 1℃ / min and keep at that temperature for 2 hours; raise from 120℃ to 350℃ at a rate of 4℃ / min and keep at that temperature for 2 hours.

[0064] Example 5

[0065] (1) Weigh 100 parts of humus and 20 parts of sodium carbonate, mix them thoroughly, put them into a high-temperature furnace at 950℃, calcine for 3 hours, and after cooling, ball mill them and then pass them through a 100-mesh sieve to obtain small-particle activated humus.

[0066] (2) Add hydrochloric acid solution dropwise to 50 portions of the small-particle-size activated humus from step (1) to adjust the pH value to 1. Stir at 60°C for 2 hours to allow it to react fully. After standing for 2 hours, perform solid-liquid separation to obtain a precipitate. Wash the precipitate to a pH value of 3.

[0067] (3) Add sodium hydroxide solution to the precipitate to adjust its pH value to 13, and react it at 60℃ for 24h. Then perform solid-liquid separation to obtain sodium silicate-sodium aluminosilicate precursor solution.

[0068] (4) Add hydrochloric acid solution dropwise to the sodium silicate-sodium aluminate solution to adjust its pH value to 10, age it at room temperature for 24 hours, and wash the aged gel with water; use ethanol solution to replace the solvent in the washed gel, and dry the replaced gel according to the temperature program. The drying program is as follows: place at room temperature for 12 hours; raise the temperature from room temperature to 100℃ at a rate of 1℃ / min and keep it at that temperature for 2 hours; raise the temperature from 100℃ to 140℃ at a rate of 2℃ / min and keep it at that temperature for 1 hour; raise the temperature from 140℃ to 400℃ at a rate of 4℃ / min and keep it at that temperature for 2 hours.

[0069] Comparative Example 1

[0070] (1) The humus was treated with a thermal desorption device for 4 hours and the desorption temperature was set at 100℃ to remove moisture, organic matter and some metal volatilization from the humus. After the pretreated humus was passed through a 100-mesh screen, NaOH additive was added and mixed according to the mass ratio of humus: sodium carbonate = 1:2. The mixture was ball-milled for 2 hours and fully melted at 1000℃ for 90 minutes. The mixture was then poured into water and cooled to obtain glass slag.

[0071] (2) Remove the glass slag from the water cooler, add 1.5 mol / L hydrochloric acid to the glass slag and stir to dissolve the glass slag. Finally, perform solid-liquid phase separation to separate the liquid phase, and then filter to obtain a water glass solution.

[0072] (3) Add hydrochloric acid solution to the water glass solution to adjust its pH value to 10, age it at room temperature for 24 hours, and wash the aged gel with water; use ethanol solution to replace the solvent in the washed gel, and dry the replaced gel according to the temperature program. The drying program is as follows: place at room temperature for 24 hours; raise the temperature from room temperature to 100℃ at a rate of 1℃ / min and keep it at that temperature for 2 hours; raise the temperature from 100℃ to 140℃ at a rate of 3℃ / min and keep it at that temperature for 1 hour; raise the temperature from 140℃ to 400℃ at a rate of 5℃ / min and keep it at that temperature for 2 hours.

[0073] Comparative Example 2

[0074] In step (2) of this comparative example, the pH value of acid leaching was adjusted to 2; otherwise, it was the same as in Example 1.

[0075] Comparative Example 3

[0076] In this comparative example, no alkaline solution is added in step (3); otherwise, it is the same as in Example 1.

[0077] The aluminosilicate glasses prepared in the examples and comparative examples were subjected to performance tests, and the test results are shown in Table 1. The chemical stability of the aluminosilicate glasses was characterized by the weight change after acid immersion. The weight change experiment after acid immersion in this invention was conducted by immersing 100g of the prepared porous aluminosilicate glass in 500ml of 5mol / L hydrochloric acid for 4 weeks, followed by drying the porous aluminosilicate glass, and comparing the weight change before and after acid immersion to characterize the chemical stability of the porous aluminosilicate.

[0078] Test Results

[0079] Table 1. Performance tests of porous aluminosilicate glasses prepared in the examples and comparative examples.

[0080] Test Items Alumina content Porosity Specific surface area aperture Compressive strength (thickness 1cm) Weight change after acid leaching Silica utilization rate Example 1 7.5% 30% <![CDATA[280m 2 / g]]> 4nm 25MPa Less than 0.1% 90% Example 2 6.8% 35% <![CDATA[300m 2 / g]]> 7nm 23Mpa Less than 0.1% 98% Example 3 6.6% 39% <![CDATA[330m 2 / g]]> 3nm 19Mpa Less than 0.1% 94% Example 4 7.1% 30% <![CDATA[285m 2 / g]]> 4nm 24MPa Less than 0.1% 96% Example 5 7.2% 34% <![CDATA[310m 2 / g]]> 4nm 24MPa Less than 0.1% 96% Comparative Example 1 19% 10% <![CDATA[121m 2 / g]]> 10nm 15MPa Reduce by 30% 20% Comparative Example 2 9.3% 20% <![CDATA[203m 2 / g]]> 8nm 10MPa Reduce by 2% 90% Comparative Example 3 7.6% 16% <![CDATA[152m 2 / g]]> 2nm 12MPa Reduce by 1% 80%

[0081] The test results above show that Comparative Example 1, due to the presence of many impurities and low sodium silicate content in the obtained water glass solution, exhibited poor gelation effect. Furthermore, the excessively high aluminum content made the aluminosilicate glass prone to breakage during drying, resulting in a product with fewer pores, poor mechanical properties, poor chemical stability, and low silicon utilization efficiency, hindering the effective resource utilization of humic soil. Comparative Examples 2 and 3, due to relatively poor impurity removal, still contained impurities in the obtained water glass solution or sodium silicate-sodium aluminate solution, resulting in relatively poor gelation effect, fewer pores, and relatively poor mechanical and chemical stability in the obtained products. The method provided by this invention demonstrates better impurity removal. The porous aluminosilicate glass prepared in the examples exhibits a rich pore structure and good mechanical properties. Furthermore, tests such as compressive strength and chemical stability confirm that the prepared porous aluminosilicate glass meets the performance requirements of glass products and has good application prospects. In addition, the porous aluminosilicate glass prepared in the examples shows a relatively high silica utilization rate, indicating that the method of this invention has a high utilization rate of humic soil, achieving better resource utilization and significantly increasing the added value of humic soil.

Claims

1. A method for producing porous aluminosilicate glass using humic soil, characterized by, The method comprises the following steps: (1) mixing humus with sodium carbonate, the mass ratio of humus to sodium carbonate being 1:0.2-1, obtaining activated humus with a particle size less than 100 mesh by calcination, ball milling and sieving, the calcination temperature being 750-1050℃, and the calcination time being 1-3h; (2) adding an acid solution dropwise to the activated humus with a small particle size until the pH value is below 1, and then carrying out reaction, and after standing, carrying out solid-liquid separation, obtaining precipitated material containing silicic acid, aluminosilicate minerals and carbon, and washing the precipitated material until the pH value is 2-3; (3) adding an alkaline solution dropwise to the precipitated material until the pH value is 11-14, and then carrying out reaction at a temperature of 60-98℃ for 6-24h, and then carrying out solid-liquid separation, obtaining a sodium silicate-sodium aluminate mixed solution; (4) adding an acid solution dropwise to the sodium silicate-sodium aluminate mixed solution until the pH value is 9-10, obtaining a gel, and then carrying out aging, washing, solvent replacement and drying, obtaining porous aluminosilicate glass; the drying procedure is as follows: first stage: drying at room temperature for 12-24h; second stage: increasing the temperature from room temperature to 80-100℃ at a rate of 1-3℃ / min, and keeping the temperature for 2-3h; third stage: increasing the temperature from 80-100℃ to 120-140℃ at a rate of 1-3℃ / min, and keeping the temperature for 1-2h; fourth stage: increasing the temperature from 120-140℃ to 350-400℃ at a rate of 3-5℃ / min, and keeping the temperature for 2-3h.

2. The method for preparing porous aluminosilicate glass using humic soil according to claim 1, characterized by, The acid solution in step (2) is one of hydrochloric acid, sulfuric acid and nitric acid.

3. The method for preparing porous aluminosilicate glass using humic soil according to claim 1, characterized by, The reaction temperature in step (2) is 60-98℃, and the reaction time is 0.5-2h.

4. The method for preparing porous aluminosilicate glass using humic soil according to claim 1, characterized by, The acid solution in step (4) is one of hydrochloric acid, sulfuric acid and nitric acid.

5. The method for making porous aluminosilicate glasses using humic clay of claim 1, wherein, The solvent for solvent replacement in step (4) is a low-surface-tension organic solvent, and the low-surface-tension organic solvent is one or more selected from the group consisting of ethanol, isopropanol and n-hexane.

6. Porous aluminosilicate glass, which is prepared by the method according to any one of claims 1-5.

Citation Information

Patent Citations

  • Treatment method of silicon-aluminum-based waste residue containing heavy metal, silicon-aluminum gel and application of silicon-aluminum gel

    CN114634183A

  • Method for preparing aerogel felt and aerogel insulation board by taking humus as raw material

    CN116283211A