Preparation of nanocomposites and process application methods

CN122999135APending Publication Date: 2026-10-30JIANGXI RUNYU ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD +1
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Patent Information

Application Number
CN202511275808.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-08
Publication Date
2026-10-30

AI Technical Summary

Technical Problem

[0006]针对现有技术的不足,本发明提供了一种纳米复合材料的制备以及工艺应用方法,解决了制备过程中水洗不充分的问题

Benefits of technology

[0028]本发明提供了一种纳米复合材料的制备以及工艺应用方法。具备以下有益效果:

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Abstract

The application provides a preparation and process application method of nanocomposite, which comprises the following steps: S1, putting 2-8 parts of organic compound and 1-5 parts of acrylic compound into deionized water; S2, fully stirring in a water bath; S3, slowly adding 0.5-1.5 parts of polymerizable anionic surfactant; S4, heating; S5, removing unreacted substances by washing with 2-8 parts of ethanol for several times; S6, weighing 1-4 parts of the prepared polymer and dissolving in 50 mL of deionized water, and fully stirring and dissolving; S7, adding 0.05-0.2 parts of carbon nanotube and stirring uniformly, and then putting into a water bath; S8, fully washing 3-5 times with 5-8 parts of ethanol; S9, drying to obtain nanocomposite, and mixing 0.3-1% nanocomposite, ion conversion agent and lithium residue beryllium thallium together. The nanocomposite has high purity by fully stirring acrylamide, acrylic acid and deionized water first, then adding into the water bath to fully mix, and finally adding ethanol to repeatedly wash.
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Description

Technical Field

[0001] This invention relates to the field of leaching agents for water-washed lithium slag, specifically to the preparation and processing methods of a nanocomposite material. Background Technology

[0002] With the acceleration of industrialization, the mining and utilization of mineral resources has become an important pillar for the sustainable development of society and economy. However, the tailings generated in this process, especially those rich in heavy metals such as beryllium (Be) and thallium (Tl), pose a huge challenge to the ecological environment and public health. As highly toxic and environmentally persistent heavy metal elements, beryllium and thallium can accumulate in the environment for a long time and affect organisms through the food chain, causing irreversible health problems. Therefore, the effective treatment and disposal of heavy metals in tailings[4], especially beryllium and thallium, has become an urgent problem to be solved in the field of environmental science and engineering.

[0003] To address this challenge, researchers are constantly exploring and innovating heavy metal treatment technologies. Currently, methods such as chemical precipitation, ion exchange, membrane separation, plant absorption, biotechnology, and nanotechnology are widely used in heavy metal wastewater treatment. Nanotechnology, in particular, demonstrates great potential in this field due to its excellent adsorption performance, photocatalytic properties, and reduction capabilities. Through research and development, a magnetic Prussian blue (PB) nano-adsorbent (PB / Fe3O4 / SEP) supported on sepiolite has been successfully prepared. This novel material achieves deep treatment of TiO2 with its excellent adsorption capacity. Furthermore, through in-situ preparation of nanocomposites, combining ordered mesoporous Mobil No. 41 (MCM-41) with chitosan, a nanocomposite material with highly efficient Be adsorption capacity has been prepared. These studies not only demonstrate the enormous potential of nanotechnology in heavy metal treatment but also provide new ideas for the innovation and development of heavy metal treatment technologies for tailings.

[0004] Based on the adsorption advantages of nanocomposite materials, this study further explored the application effects of novel composite materials with carbon nanotubes as the matrix in the treatment of beryllium and thallium in tailings. It is hoped that this research will promote the innovation and development of heavy metal treatment technologies for tailings, contributing to the sustainable development of the mining industry, ecological environmental protection, and the protection of human health. Summary of the Invention

[0005] (a) Technical problems to be solved

[0006] To address the shortcomings of existing technologies, this invention provides a method for preparing and processing nanocomposite materials, which solves the problem of insufficient water washing during the preparation process.

[0007] (II) Technical Solution

[0008] To achieve the above objectives, the present invention provides the following technical solution: Preparation of a nanocomposite material, comprising the following steps:

[0009] S1. Mix 2-8 parts of organic compound and 1-5 parts of acrylic compound into deionized water and stir until homogeneous to obtain mixture A;

[0010] S2. Mixture A is placed in a water bath at 80°C and stirred thoroughly for 1 hour to obtain mixture B;

[0011] S3. Slowly add 0.5-1.5 parts of polymerizable anionic surfactant to mixture B to obtain mixture C;

[0012] S4. Heat mixture C and add it into the stirring structure for a thorough stirring reaction for 6 hours;

[0013] S5. Wash several times with 2-8 parts of ethanol to remove unreacted substances, thus obtaining a pure polymer;

[0014] S6. Weigh 1-4 parts of the polymer prepared above and dissolve them in 50 mL of deionized water and stir thoroughly to dissolve.

[0015] S7. Slowly add 0.05-0.2 parts of carbon nanotubes, stir evenly, and then place in a water bath to react fully;

[0016] S8. After cooling to room temperature, wash thoroughly 3-5 times with 5-8 parts of ethanol.

[0017] S9. The obtained product is dried in a vacuum drying oven to finally obtain the nanocomposite material.

[0018] Preferably, the organic compound in step S1 is one of acrylamide, methacrylamide, and N,N-dimethylacrylamide; the acrylic compound in step S1 is one of acrylic acid and methacrylic acid; and the polymerizable anionic surfactant in step S3 is one of sodium p-styrene sulfonate, sodium allyl sulfonate, 2-acrylamido-2-methylpropane sulfonic acid, and potassium allyl sulfonate.

[0019] Preferably, the content of deionized water in step 1 is 100 mL.

[0020] Preferably, the temperature in step 4 is 80°C.

[0021] Preferably, the water bath temperature in step 7 is 80°C, and the reaction time in step 7 is 4 hours.

[0022] Preferably, the drying temperature and drying time of the vacuum drying oven in step 9 are 70°C and 12 hours.

[0023] A method for preparing and processing a nanocomposite material includes the following steps:

[0024] Preferably, in step S1, 0.3-1% of the nanocomposite material, 0.3-0.5% of the oxygen reducing agent, and lithium slag beryllium thallium are mixed together;

[0025] Preferably, in step S2, the mixture is stirred with a glass rod to allow for a full reaction and adsorption.

[0026] Preferably, the oxygen reducing agent in step S1 is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, and ferrous sulfate.

[0027] (III) Beneficial Effects

[0028] This invention provides a method for preparing and processing nanocomposite materials. It offers the following advantages:

[0029] First, acrylamide, acrylic acid, and deionized water are thoroughly stirred, then added to a water bath for further mixing. Next, p-styrene sulfonic acid is added, and finally, ethanol is added for repeated washing, ensuring thorough and complete water washing. This results in high purity for the preparation of nanocomposite materials. Attached Figure Description Figure 1 XPS testing of the nanocomposite material of the present invention; Figure 2 The image shows the FT-IR spectrum of AM, SSS, HPAA and nanocomposite materials of the present invention. Figure 3 Thermogravimetric analysis of the nanocomposite material of the present invention; Figure 4 The images show SEM images of the nanocomposite material of the present invention before and after adsorption: divided into four parts: before adsorption of Be ions, before adsorption of Tl ions, after adsorption of Be ions, and after adsorption of Tl ions (from left to right, from top to bottom). Figure 5 The adsorption performance of the nanocomposite material of the present invention at different initial concentrations is shown in Figure a: Be adsorption and Tl adsorption. Detailed Implementation

[0030] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0031] Example 1:

[0032] This invention provides a method for preparing a nanocomposite material, comprising the following steps:

[0033] S1. Mix 5 parts acrylamide and 1 part acrylic acid into deionized water and stir until homogeneous to obtain mixture A;

[0034] S2. Mixture A is placed in a water bath at 80°C and stirred thoroughly for 1 hour to obtain mixture B;

[0035] S3. Slowly add 0.5 parts of sodium p-styrene sulfonate to mixture B to obtain mixture C;

[0036] S4. Heat mixture C and add it into the stirring structure for a thorough stirring reaction for 6 hours;

[0037] S5. Wash several times with 2-8 parts of ethanol to remove unreacted substances, thus obtaining a pure polymer;

[0038] S6. Weigh one part of the polymer prepared above and dissolve it in 50 mL of deionized water and stir thoroughly to dissolve.

[0039] S7. Slowly add 0.05 parts of carbon nanotubes, stir evenly, and then place in a water bath to react fully;

[0040] S8. After cooling to room temperature, wash thoroughly three times with 5 parts ethanol.

[0041] S9. The obtained product is dried in a vacuum drying oven to finally obtain the nanocomposite material.

[0042] The organic compound in step S1 is one of acrylamide, methacrylamide, and N,N-dimethylacrylamide; the acrylic compound in step S1 is one of acrylic acid and methacrylic acid; and the polymerizable anionic surfactant in step S3 is one of sodium p-styrene sulfonate, sodium allyl sulfonate, 2-acrylamido-2-methylpropane sulfonic acid, and potassium allyl sulfonate.

[0043] The amount of deionized water in step 1 is 100 mL.

[0044] The temperature in step 4 is 80℃.

[0045] In step 7, the water bath temperature is 80℃, and the reaction time in step 7 is 4 hours.

[0046] In step 9, the drying temperature and drying time of the vacuum drying oven are 70℃ and 12h.

[0047] Example 2:

[0048] This invention provides a method for preparing a nanocomposite material, comprising the following steps:

[0049] S1. Mix 6 parts acrylamide and 3 parts acrylic acid into deionized water and stir until homogeneous to obtain mixture A;

[0050] S2. Mixture A is placed in a water bath at 80°C and stirred thoroughly for 1 hour to obtain mixture B;

[0051] S3. Slowly add 1 part of sodium p-styrene sulfonate into mixture B to obtain mixture C;

[0052] S4. Heat mixture C and add it into the stirring structure for a thorough stirring reaction for 6 hours;

[0053] S5. Wash several times with 2-8 parts of ethanol to remove unreacted substances, thus obtaining a pure polymer;

[0054] S6. Weigh out two portions of the polymer prepared above and dissolve them in 50 mL of deionized water. Stir thoroughly to dissolve.

[0055] S7. Slowly add 0.1 parts of carbon nanotubes, stir evenly, and then place in a water bath to react fully;

[0056] S8. After cooling to room temperature, wash thoroughly 4 times with 6 parts ethanol.

[0057] S9. The obtained product is dried in a vacuum drying oven to finally obtain the nanocomposite material.

[0058] Example 3:

[0059] This invention provides a method for preparing a nanocomposite material, comprising the following steps:

[0060] S1. Mix 7 parts acrylamide and 5 parts acrylic acid into deionized water and stir until homogeneous to obtain mixture A;

[0061] S2. Mixture A is placed in a water bath at 80°C and stirred thoroughly for 1 hour to obtain mixture B;

[0062] S3. Slowly add 1.5 parts of sodium p-styrene sulfonate to mixture B to obtain mixture C;

[0063] S4. Heat mixture C and add it into the stirring structure for a thorough stirring reaction for 6 hours;

[0064] S5. Wash several times with 2-8 parts of ethanol to remove unreacted substances, thus obtaining a pure polymer;

[0065] S6. Weigh out 3 portions of the polymer prepared above and dissolve them in 50 mL of deionized water. Stir thoroughly to dissolve.

[0066] S7. Slowly add 0.2 parts of carbon nanotubes, stir evenly, and then place in a water bath to react fully;

[0067] S8. After cooling to room temperature, wash thoroughly 5 times with 7 parts ethanol.

[0068] S9. The obtained product is dried in a vacuum drying oven to finally obtain the nanocomposite material.

[0069] Example 4:

[0070] A method for preparing and processing a nanocomposite material includes the following steps: S1, mixing 0.3% nanocomposite material, 0.5% oxygen reducing agent, and lithium slag beryllium thallium together;

[0071] S2. Stir the above mixture with a glass rod to allow for full reaction and adsorption.

[0072] In step S1, the oxygen reducing agent is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, or ferrous sulfate.

[0073] Example 5:

[0074] A method for preparing and processing a nanocomposite material includes the following steps: S1, mixing 0.5% nanocomposite material, 0.5% oxygen reducing agent, and lithium slag beryllium thallium together;

[0075] S2. Stir the above mixture with a glass rod to allow for full reaction and adsorption.

[0076] In step S1, the oxygen reducing agent is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, or ferrous sulfate.

[0077] Example 6:

[0078] A method for preparing and processing a nanocomposite material includes the following steps: S1, mixing 0.6% nanocomposite material, 0.5% oxygen reducing agent, and lithium slag beryllium thallium together;

[0079] S2. Stir the above mixture with a glass rod to allow for full reaction and adsorption.

[0080] In step S1, the oxygen reducing agent is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, or ferrous sulfate.

[0081] Example 7:

[0082] A method for preparing and processing a nanocomposite material includes the following steps: S1, mixing 0.7% nanocomposite material, 0.5% oxygen reducing agent, and lithium slag beryllium thallium together;

[0083] S2. Stir the above mixture with a glass rod to allow for full reaction and adsorption.

[0084] In step S1, the oxygen reducing agent is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, or ferrous sulfate.

[0085] Example 8:

[0086] A method for preparing and processing a nanocomposite material includes the following steps: S1, mixing 0.8% nanocomposite material, 0.5% oxygen reducing agent, and lithium slag beryllium thallium together;

[0087] S2. Stir the above mixture with a glass rod to allow for full reaction and adsorption.

[0088] In step S1, the oxygen reducing agent is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, or ferrous sulfate.

[0089] Example 9:

[0090] A method for preparing and processing a nanocomposite material includes the following steps: S1, mixing 0.9% nanocomposite material, 0.5% oxygen reducing agent, and lithium slag beryllium thallium together;

[0091] S2. Stir the above mixture with a glass rod to allow for full reaction and adsorption.

[0092] In step S1, the oxygen reducing agent is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, or ferrous sulfate.

[0093] Example 10:

[0094] A method for preparing and processing a nanocomposite material includes the following steps: S1, mixing 1% nanocomposite material, 0.5% oxygen reducing agent, and lithium slag beryllium thallium together;

[0095] S2. Stir the above mixture with a glass rod to allow for full reaction and adsorption.

[0096] In step S1, the oxygen reducing agent is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, or ferrous sulfate.

[0108] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a nanocomposite material, characterized in that, Includes the following steps: S1. Mix 2-8 parts of organic compound and 1-5 parts of acrylic compound into deionized water and stir until homogeneous to obtain mixture A; S2. Mixture A is placed in a water bath at 80°C and stirred thoroughly for 1 hour to obtain mixture B; S3. Slowly add 0.5-1.5 parts of polymerizable anionic surfactant to mixture B to obtain mixture C; S4. Heat mixture C and add it into the stirring structure for a thorough stirring reaction for 6 hours; S5. Wash several times with 2-8 parts of ethanol to remove unreacted substances, thus obtaining a pure polymer; S6. Weigh 1-4 parts of the polymer prepared above and dissolve them in 50 mL of deionized water and stir thoroughly to dissolve. S7. Slowly add 0.05-0.2 parts of carbon nanotubes, stir evenly, and then place in a water bath to react fully; S8. After cooling to room temperature, wash thoroughly 3-5 times with 5-8 parts of ethanol. S9. The obtained product is dried in a vacuum drying oven to finally obtain the nanocomposite material.

2. The method for preparing a nanocomposite material according to claim 1, characterized in that: The organic compound in step S1 is one of acrylamide, methacrylamide, and N,N-dimethylacrylamide; the acrylic compound in step S1 is one of acrylic acid and methacrylic acid; and the polymerizable anionic surfactant in step S3 is one of sodium p-styrene sulfonate, sodium allyl sulfonate, 2-acrylamido-2-methylpropane sulfonic acid, and potassium allyl sulfonate.

3. The method for preparing a nanocomposite material according to claim 1, characterized in that: The amount of deionized water in step 1 is 100 mL.

4. The method for preparing a nanocomposite material according to claim 1, characterized in that: The temperature in step 4 is 80℃.

5. The method for preparing a nanocomposite material according to claim 1, characterized in that: The water bath temperature in step 7 is 80℃, and the reaction time in step 7 is 4 hours.

6. The method for preparing a nanocomposite material according to claim 1, characterized in that: In step 9, the drying temperature and drying time of the vacuum drying oven are 70℃ and 12h.

7. A method for preparing and processing a nanocomposite material, characterized in that: Includes the following steps: S1. Mix 0.3-1% nanocomposite material, 0.3-0.5% oxygen reducing agent and lithium slag beryllium thallium together; S2. Stir the above mixture with a glass rod to allow for full reaction and adsorption.

8. The preparation and processing method of a nanocomposite material according to claim 7, characterized in that: In step S1, the oxygen reducing agent is one of ozone, calcium hypochlorite, sodium hypochlorite, sodium peroxide, or ferrous sulfate.