CN110255568B - Internal and external double-layer amino modified SiO2Aerogel synthesis method and application thereof - Google Patents
Internal and external double-layer amino modified SiO2Aerogel synthesis method and application thereof Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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- C01B33/152—Preparation of hydrogels
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- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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- C01B33/1585—Dehydration into aerogels
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
Internal and external double-layer amino modified SiO2The synthesis method and the application of the aerogel comprise the following specific steps: taking 20ml of water glass, and removing sodium ions in the water glass by using a cation exchange resin column; adjusting the pH value of the obtained silicic acid solution to be 0.1-2.0 mol/L ammonia solution and 0.1-2.0 mol/L hydrochloric acid solution4.0 to 8.0; quickly carrying out ultrasonic treatment on a beaker containing silicic acid solution, and sequentially adding a mixture of silicic acid solution and water in a volume ratio of 1: 1: 1: and (3) slowly shaking the beaker by using a 16-epoxy chloropropane, APTES, ethylenediamine and n-hexane mixed modifier under an ultrasonic condition until the solution is gelatinized, then placing the gel for 5-24 h at the temperature of 30-65 ℃, adding 28ml of n-hexane into the gel, and continuously oscillating for 5-24 h at the temperature of 30-65 ℃. Finally, drying the wet gas gel for 10-48 h by using a vacuum freeze drying method to obtain the inner and outer double-layer amino modified SiO2An aerogel. The humic acid solution with the initial adsorption concentration of 1211mg/L of the aerogel can reach the adsorption balance within 90 minutes, and the adsorption quantity reaches 1194.4 mg/g.
Description
Technical Field
The invention relates to the technical field of adsorbent preparation, in particular to internal and external double-layer amino modified SiO2A synthesis method of aerogel and application thereof.
Background
The rapid development of global economy has led to serious environmental pollution, which has also become a serious challenge in the sustainable development process of society. In recent years, water pollution mainly caused by refractory organic matters is increasingly serious, and development of a low-cost and green treatment method is very critical. Among the difficult-to-degrade organic pollutants, high-concentration organic matters of humic acids are used as secondary pollutants generated in the garbage treatment process and are always difficult in the water treatment industry. When the high-concentration organic pollutants of humic acid pollute the water body, the phenomenon that the chroma and the turbidity of the water body are increased can be caused, and the biological toxicity of the humic acid complex can be increased[1]At the same time, humic acid can react with disinfectant containing chlorine to generate disinfection by-product with 'three-induced effect' (mutagenic, carcinogenic and teratogenic effect) in disinfection process[2]。
At present, the method for treating humic acid high concentration organic pollutants includes biochemical treatment method, advanced oxidation method, such as photocatalysis, ozone oxidation, ozone + photocatalysis oxidation, ozone catalysis oxidation, novel material adsorption method, membrane treatment technology and the like[3-7]. For humic acid contaminants in "aged" leachate, biological treatment is essentially ineffective due to the poor biodegradability of these contaminants. Wuwei et al studied TiO2Research results show that the humic acid is degraded from macromolecular acid to micromolecular acid, and the humic acid can be faded by photocatalysisAnd also greatly reduces the generation of disinfection by-products[8]. However, conventional photocatalytic materials such as these generally have two problems: 1. most of the photocatalysts can only utilize ultraviolet light for reaction, and cannot utilize the visible light part of sunlight; 2. the catalyst is prone to agglomeration due to its fine particle size, resulting in a reduction in the number of reactive sites between the catalyst and the contaminants. The adsorption method has the advantages of high removal efficiency, simple and convenient operation and no secondary pollution to water bodies caused by side reactions. Therefore, the development of a photocatalyst adsorbent capable of having excellent dispersibility and high specific surface area is urgent and important for the treatment of high concentration organic pollutants of humic acids.
The adsorption process is closely related to the surface property and material structure of the adsorption material, and the adsorption is generally divided into physical adsorption, chemical adsorption and ion exchange adsorption, and three or two of the adsorption processes may exist. Currently, activated carbon, zeolite molecular sieves and resin adsorbents are widely used adsorbents. However, activated carbon mainly has problems in that it is difficult to regenerate and to remove hydrophilic small molecular substances, which makes it difficult to implement large-scale industrial application. Currently, silica aerogels with high specific surface areas are the focus of current research. The silica aerogel is a high-dispersion light porous amorphous material with a continuous three-dimensional network structure formed by the mutual polymerization of nano-scale particles, and air media are filled in pores. In 1931, professor Kistler at Stanford university prepared silica aerogel by sol-gel method for the first time [1 ]. The aerogel is a solid substance with a micro-nano network structure, and has great application value in many fields due to the characteristics of large specific surface area, low density, low thermal conductivity and the like. With the intensive research on silicon source, modification, characterization and the like of the silicon dioxide aerogel prepared by researchers, the silicon dioxide aerogel gradually has wide application prospects in the fields of environmental management, catalysis, energy conservation, drug loading, aerospace and the like. However, how to carry out efficient amine modification on the silicon dioxide aerogel according to the characteristics of humic acid organic pollutant is a key scientific problem of the invention.
Disclosure of Invention
The invention aims to provide an internal and external double-layer amino modified SiO2Synthetic method and application of aerogel, ensuring internal and external double-layer amino modified SiO2The aerogel has high selectivity for adsorption of humic acid pollutants, keeps the structural characteristic of high specific surface area and excellent performance of the silicon dioxide aerogel, and solves the problem of low humic acid removal rate.
The technical scheme adopted by the invention is as follows: internal and external double-layer amino modified SiO2The synthesis method of the aerogel comprises the following steps:
(1) accurately weighing 5-60 g of rice hull ash and 5-28 g of sodium hydroxide by using an analytical balance, placing the rice hull ash and the sodium hydroxide into a round-bottom flask, heating to 50-150 ℃, and carrying out reflux stirring reaction for 1-10 hours;
(2) cooling the reacted product to room temperature, and then carrying out vacuum filtration to obtain water glass with the modulus of 1.5-4.2;
(3) taking 10-40 ml of water glass, and carrying out ion exchange through a strong-acid cation exchange resin 001 x 7(732 type) to remove sodium ions in the water glass to obtain a silicic acid solution;
(4) adjusting the obtained silicic acid solution to a pH value of 4.0-8.0 by using 0.1-2.0 mol/L ammonia solution and 0.1-2.0 mol/L hydrochloric acid solution, then rapidly carrying out ultrasound on a beaker containing the silicic acid solution, sequentially adding 0.1-2.5 ml of epoxy chloropropane, 0.1-2.5 ml of APTES, 0.1-2.5 ml of ethylenediamine and 5.0-30.0 ml of n-hexane into the silicic acid solution, slowly shaking the beaker under an ultrasonic condition until the solution is gelatinized, and then placing the gel for 5-24 hours at a temperature of 30-65 ℃; the epichlorohydrin: APTES: the volume ratio of the ethylenediamine is 1: 1: 1.
(5) adding 10-40 ml of n-hexane into the gel, and continuously oscillating for 5-24 hours at the temperature of 30-65 ℃;
(6) finally, drying the wet gas gel for 10-48 h by adopting a vacuum freeze drying method to obtain the inner and outer double-layer amino modified SiO2An aerogel.
The amino modifier is commercially available epichlorohydrin, 3-aminopropyltriethoxysilane and ethylenediamine.
The inner layer and the outer layer of amino modified SiO2The application of aerogel in purifying wastewater is to add the inner and outer double-layer amino modified SiO in humic acid wastewater to be purified2Aerogel, absorbing humic acid under the conditions of 25 ℃ and pH of 2.0-9.0, collecting the humic acid and the inner and outer double-layer amino modified SiO after absorbing for 0.1-1.5 h2The precipitate of aerogel can reach the adsorption treatment effect.
The inner layer and the outer layer of amino modified SiO2The application of the aerogel in wastewater purification is characterized in that the concentration of humic acid in a water body to be purified is 5-1200 mg/L.
The related chemical reaction equation of the invention is as follows:
the invention takes the agricultural waste rice hull ash as a silicon source and adopts the sol-gel technology to synthesize the inner and outer double-layer amino modified SiO2An aerogel.
The modulus of the water glass prepared by the invention is 4.26, which is far higher than that of the commercial industrial water glass.
The equipment used in the invention is conventional laboratory equipment.
The invention has the outstanding advantages that:
1. by designing the inner and outer double-layer amino modification, the amino loading capacity is improved, the steric effect of a modified group is overcome, and the material has the performance of high speed and high adsorption capacity when used for adsorbing and treating high-concentration organic pollutants such as humic acids.
2. The adopted raw materials are agricultural solid wastes which are cheap and easily available, and belong to resource recycling, and the synthesis process is simple, convenient and practical.
Drawings
FIG. 1 shows the internal and external double-layer amino modified SiO of the present invention2A process flow diagram of a method for synthesizing an aerogel.
FIG. 2 shows the inner and outer double-layer amino modification of the present inventionSiO 22Field emission scanning electron microscopy of aerogel samples.
FIG. 3 shows the inner and outer double-layer amino modified SiO of the present invention2Aerogel sample Zeta potential.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the following examples.
Example 1
This example is the internal and external double-layer amino modified SiO of the invention2An example of a synthesis method of aerogel, using a sol-gel method for synthesis, consists of the following steps:
(1) accurately weighing 30g of rice hull ash and 8g of sodium hydroxide by using an analytical balance, placing the rice hull ash and the sodium hydroxide into a round-bottom flask, heating to 100 ℃, and carrying out reflux stirring reaction for 3.5 hours;
(2) cooling the product after reaction to room temperature, and then carrying out vacuum filtration to obtain water glass with the modulus of 4.26;
(3) taking 20ml of water glass with the modulus of 4.26 prepared from rice hull ash, carrying out ion exchange by using a strong acid cation exchange resin 001 x 7(732 type), and removing sodium ions in the water glass to obtain a silicic acid solution;
(4) the pH of the resulting silicic acid solution was adjusted to 4.5 with 1mol/L ammonia solution and 1mol/L hydrochloric acid solution. Then, the beaker containing the silicic acid solution was rapidly sonicated, and 0.93ml of epichlorohydrin, 0.93ml of APTES, 0.93ml of ethylenediamine and 16ml of n-hexane were sequentially added to the silicic acid solution. The beaker was slowly shaken under sonication until the solution gelled and the gel was allowed to stand at 45 ℃ for 12 h.
(5) Then 28ml of n-hexane was added to the gel, and the mixture was continuously shaken at 45 ℃ for 6 hours.
(6) Finally, drying the wet gas gel for 24 hours by adopting a vacuum freeze drying method to obtain the inner and outer double-layer amino modified SiO2An aerogel.
Example 2
This example shows the inner and outer double-layer amino modified SiO prepared by the present invention2Application example of aerogel in purifying wastewater, and double-layer amino modified SiO2As aerogelsThe adsorbent is used for purifying high-concentration humic acid solution, and the test conditions are as follows: the initial concentration of the humic acid solution is 1211mg/L, the adsorption time is 90 minutes, other conditions are the same as the example 1, a filter membrane with the thickness of 0.45 mu m is adopted for filtering, and the double-layer amino modified SiO is detected and calculated2The adsorption amount of the aerogel on humic acid is 1205.4mg/g, and the removal rate is 99.02%.
Therefore, the internal and external double-layer amino modified SiO prepared by the invention2The aerogel has a rapid and high-adsorption-capacity treatment effect on high-concentration humic acid solution.
Example 3
This example shows the inner and outer double-layer amino modified SiO prepared by the present invention2Application of aerogel in wastewater purification as another example, SiO is modified by double-layer amine group2Aerogel is used as an adsorbent, the pH of the solution is 3, the solution is filtered by a 0.45 mu m filter membrane under the same other conditions as in example 1, and the double-layer amino modified SiO is detected and calculated2The adsorption amount of the aerogel on humic acid is 48.75mg/g, and the removal rate is 85.28%.
Example 4
This example shows the inner and outer double-layer amino modified SiO prepared by the present invention2Third example of aerogel application in wastewater purification, SiO modified with double-layer amine groups2Aerogel is used as an adsorbent, the pH of the solution is 5, the solution is filtered by a 0.45 mu m filter membrane under the same other conditions as in example 1, and the double-layer amino modified SiO is detected and calculated2The adsorption amount of the aerogel on humic acid is 47.84mg/g, and the removal rate is 94.85%.
Example 5
This example shows the inner and outer double-layer amino modified SiO prepared by the present invention2The fourth application example of the aerogel in purifying wastewater is to modify SiO by double-layer amine groups2Aerogel is used as an adsorbent, the pH of the solution is 9, the solution is filtered by a 0.45 mu m filter membrane under the same other conditions as in example 1, and the double-layer amino modified SiO is detected and calculated2The adsorption amount of the aerogel on humic acid was 47.17mg/g, and the removal rate was 93.84%.
Visible double-layer amino modified SiO2The aerogel can have the pH value of humic acid within the range of 3-9Fast and high-efficient adsorption treatment effect.
Claims (4)
1. Internal and external double-layer amino modified SiO2The synthesis method of the aerogel is characterized by comprising the following steps:
(1) accurately weighing 10-40 g of rice hull ash and 5-20 g of sodium hydroxide by using an analytical balance, placing the rice hull ash and the sodium hydroxide into a round-bottom flask, heating to 50-150 ℃, and carrying out reflux stirring reaction for 3-10 hours;
(2) cooling the product after reaction to room temperature, and then carrying out vacuum filtration to obtain water glass with the modulus of 4.26;
(3) taking 20ml of water glass, carrying out ion exchange by using a strong acid cation exchange resin 001 x 7(732 type), and removing sodium ions in the water glass to obtain a silicic acid solution;
(4) adjusting the pH value of the obtained silicic acid solution to 4.0-8.0 by using 0.1-2.0 mol/L ammonia solution and 0.1-2.0 mol/L hydrochloric acid solution, then rapidly carrying out ultrasound on a beaker containing the silicic acid solution, sequentially adding 0.2-5.0 ml of epoxy chloropropane, 0.2-5.0 ml of APTES and 0.2-5.0 ml of ethylenediamine serving as amino modifiers and 10-36 ml of n-hexane into the silicic acid solution, slowly shaking the beaker under the ultrasonic condition until the solution is gelatinized, and then placing the gel for 5-24 hours at the temperature of 30-65 ℃;
(5) adding 10-48 ml of n-hexane into the gel, and continuously oscillating for 5-24 hours at the temperature of 30-65 ℃;
(6) finally, drying the wet gas gel for 10-48 h by adopting a vacuum freeze drying method to obtain the inner and outer double-layer amino modified SiO2An aerogel.
2. The inner and outer double-layer amine-modified SiO of claim 12The synthesis method of the aerogel is characterized in that the amino modifier is commercially available epichlorohydrin, 3-aminopropyltriethoxysilane and ethylenediamine.
3. The internal and external double-layer amino modified SiO prepared by the method of claim 12The application of aerogel in purifying wastewater is characterized in that the aerogel is used in the wastewater to be purifiedIn the method, the inner layer and the outer layer of amino modified SiO are added2The aerogel adsorbs humic acid under the conditions of 25 ℃ and pH of 2.0-9.0, the humic acid and the inner and outer double-layer amino modified SiO are collected after 0.1-24 h of adsorption2The precipitation of the aerogel achieves the adsorption treatment effect.
4. The inner and outer double-layer amine-based modified SiO of claim 32The application of the aerogel in wastewater purification is characterized in that the concentration of humic acid in a water body to be purified is 5-1211 mg/L.
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| US11571681B2 (en) | 2020-02-05 | 2023-02-07 | King Fahd University Of Petroleum And Minerals | Aminated siliceous adsorbent from rice husk ash and a method of capturing carbon dioxide |
| CN112337436B (en) * | 2020-10-23 | 2022-10-21 | 广西大学 | Method for preparing sulfhydryl modified silicon dioxide aerogel as film diffusion gradient technology binding phase |
| CN115627013A (en) * | 2022-09-08 | 2023-01-20 | 苏州博大永旺新材股份有限公司 | Rice hull powder biomass-based fully-degradable material and preparation method thereof |
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