CN116983953B - Preparation method of aerogel microspheres - Google Patents
Preparation method of aerogel microspheres Download PDFInfo
- Publication number
- CN116983953B CN116983953B CN202310829849.9A CN202310829849A CN116983953B CN 116983953 B CN116983953 B CN 116983953B CN 202310829849 A CN202310829849 A CN 202310829849A CN 116983953 B CN116983953 B CN 116983953B
- Authority
- CN
- China
- Prior art keywords
- ultrasonic treatment
- titanium dioxide
- time
- nano tube
- carbon nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000004964 aerogel Substances 0.000 title claims abstract description 27
- 239000004005 microsphere Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 35
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 35
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 22
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 11
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000008103 glucose Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002270 dispersing agent Substances 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000005416 organic matter Substances 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000306 component Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000021523 carboxylation Effects 0.000 description 2
- 238000006473 carboxylation reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000012217 deletion Methods 0.000 description 1
- 230000037430 deletion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- -1 nitrogenous organic compound Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
Abstract
The invention relates to a preparation method of aerogel microspheres, which comprises the following steps: s1, adding a carbon nano tube into a mixed solution of concentrated sulfuric acid and concentrated hydrochloric acid, performing ultrasonic treatment for the first time, washing and drying to obtain a carboxylated carbon nano tube, then adding the carboxylated carbon nano tube and graphene oxide into deionized water, adding a nitrogen-containing organic matter after ultrasonic treatment for the second time, and stirring to obtain a dispersion; s2, soaking titanium dioxide in alkali liquor, carrying out ultrasonic treatment, mixing with glucose, carrying out ball milling treatment, and purifying to obtain hydroxylated titanium dioxide; s3, adding the hydroxylated titanium dioxide and the dispersing agent into the dispersion liquid, heating and stirring, adding an oil phase, regulating the pH value after ultrasonic treatment, and obtaining a product through centrifugation, washing and drying. According to the invention, carboxylated carbon nanotubes, hydroxylated titanium dioxide and graphene oxide are compounded, and simultaneously nitrogen-containing organic matters are added, so that the compatibility among components is effectively improved, and the novel aerogel microsphere with good stability, adsorption capacity and catalytic performance is obtained.
Description
Technical Field
The invention belongs to the technical field of graphene aerogel, and particularly relates to a preparation method of aerogel microspheres.
Background
Graphene oxide has the characteristics of high specific surface area, rich surface functional groups, easiness in functionalization and high controllability, so that the graphene oxide is a novel carbon material with excellent performance. In the process of compounding with various materials such as metal, high polymer materials, metal oxides and the like, the graphene oxide can provide a larger specific surface area and prevent agglomeration of adhesion materials. Meanwhile, the graphene oxide material has excellent comprehensive property and excellent physicochemical property. The graphene oxide lamellar skeleton has a plurality of coexisting functional groups on the surface and the edge, so that the electrical properties of the graphene oxide lamellar skeleton can be modulated by regulating the number and the types of oxygen-containing functional groups, and the application range is very wide. The graphene is prepared into aerogel microspheres, so that the specific surface area of the material is fully utilized, a three-dimensional network can be formed inside, and the conductivity and mechanical capacity of the aerogel microspheres are improved.
The carbon nanotubes have ultra-high electrical conductivity, thermal conductivity and excellent mechanical properties. At present, a great deal of researches are carried out on the aspects of preparation technology, structural performance, application development and the like of the carbon nanotube aerogel at home and abroad. However, carbon nanotubes are difficult to disperse, it is very difficult to prepare a pure carbon nanotube aerogel with good dispersion, and other substances are generally required to be introduced to promote the dispersion, so that the excellent performance of the carbon nanotubes is difficult to fully develop, the conductivity of the aerogel is poor, the preparation process is complex, and the cost is high.
At present, the prior art combines graphene aerogel and carbon nano tubes with titanium dioxide with good photocatalytic activity, so as to fully utilize the advantages of the material structure and performance, and solve the defects and defects of the prior art in the aspects of mechanical performance, optical performance, electrical performance, stability and the like.
In view of the foregoing, it is necessary to develop a new technical solution to solve the problems existing in the prior art.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of aerogel microspheres, which is characterized in that carboxylated carbon nanotubes, hydroxylated titanium dioxide and graphene oxide are compounded, and simultaneously nitrogen-containing organic matters are added, so that the compatibility among components is effectively improved, and novel aerogel microspheres with good stability, adsorption capacity and catalytic performance are obtained.
An object of the present invention is to provide a method for preparing aerogel microspheres, comprising the steps of:
s1, adding a carbon nano tube into a mixed solution of concentrated sulfuric acid and concentrated hydrochloric acid, performing ultrasonic treatment for the first time, washing and drying to obtain a carboxylated carbon nano tube, then adding the carboxylated carbon nano tube and graphene oxide into deionized water, adding a nitrogen-containing organic matter after ultrasonic treatment for the second time, and stirring to obtain a dispersion;
s2, soaking titanium dioxide in alkali liquor, carrying out ultrasonic treatment, mixing with glucose, carrying out ball milling treatment, and purifying to obtain hydroxylated titanium dioxide;
s3, adding the hydroxylated titanium dioxide and the dispersing agent into the dispersion liquid, heating and stirring, adding an oil phase, regulating the pH value after ultrasonic treatment, and obtaining a product through centrifugation, washing and drying.
Further, in the step S1, the volume ratio of the concentrated sulfuric acid to the concentrated hydrochloric acid is (1-3): 1.
Further, in step S1, the time of the first ultrasonic treatment is 8-12h, the time of the second ultrasonic treatment is 1-2h, and the time of stirring is 30-60min.
Further, in step S1, the nitrogen-containing organic matter is selected from one or more of urea and thiourea.
Further, in the step S1, the mass ratio of the carboxylated carbon nano tube to the graphene oxide to the nitrogenous organic compound is (1-2): 1-8): 1-2.
Further, in step S2, the time of the ultrasound is 1-3 hours.
Further, in the step S2, the ball milling treatment time is 8-24 hours, and the ball-to-material ratio is (1-5): 1.
Further, in the step S2, the alkali liquor is 1-10mol/L sodium hydroxide solution.
Further, in step S3, the pH value ranges from 7 to 8.
Further, in step S3, the oil phase is n-hexane.
The invention has the following beneficial effects:
1. according to the preparation method, firstly, carboxylation modification is carried out on the carbon nano tube, and carboxyl is introduced into the surface of the carbon nano tube, so that the compatibility between the carbon nano tube and graphene oxide is improved, chemical bonding is easier to generate between the carbon nano tube and the graphene oxide, the stability is effectively enhanced, and the aerogel has a larger specific surface area; the invention also carries out hydroxylation treatment on the titanium dioxide, so that the hydroxylated titanium dioxide can generate stronger intermolecular acting force with oxygen-containing functional groups on the surfaces of the carboxylated carbon nano tube and the graphene oxide, and the composite strength among components is further improved, thereby forming a more stable adsorption structure; according to the invention, thiourea is adopted as a component, sulfur and nitrogen elements are introduced, the number of active sites is increased, the synergy is realized, the titanium dioxide loading capacity is increased, the stability of the aerogel microsphere is further enhanced, and the aerogel microsphere has good adsorption, photoelectricity and catalysis capabilities and wide application prospect.
2. The preparation method provided by the invention is simple, safe, convenient to operate, low in cost and beneficial to realizing large-scale industrial production.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are set forth. The starting materials, reactions and workup procedures used in the examples are those commonly practiced in the market and known to those skilled in the art unless otherwise indicated.
The words "preferred," "more preferred," and the like in the present disclosure refer to embodiments of the present disclosure that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
It should be understood that all numbers expressing, for example, amounts of ingredients used in the specification and claims, except in any operating example or otherwise indicated, are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.
The graphene oxide in the embodiment of the invention is purchased from Guangzhou Hongwu materials science and technology Co.
Carbon Nanotubes (MWCNTs) in the examples of the present invention were purchased from Shenzhen nanoport technologies Inc.
The dispersing agent in the embodiment of the invention is sodium hexametaphosphate.
Example 1
The preparation method of the aerogel microsphere comprises the following steps:
s1, adding 20g of carbon nanotubes into a mixed solution of 1L of concentrated sulfuric acid and 0.5L of concentrated hydrochloric acid, performing ultrasonic treatment at 50 ℃ for 10 hours, washing a product to be neutral by deionized water and ethanol, and drying overnight to obtain carboxylated carbon nanotubes;
adding 1g of the carboxylated carbon nanotube and 8g of graphene oxide into 200mL of deionized water, carrying out ultrasonic treatment for 1.5h, adding 1g of thiourea, and stirring for 60min to obtain a dispersion liquid;
s2, soaking 1g of titanium dioxide powder in 50mL of 5mol/L sodium hydroxide solution, performing ultrasonic treatment for 3 hours, washing to neutrality, mixing with glucose (titanium dioxide: glucose=1:5, m/m) after drying, performing ball milling treatment (ball-to-material ratio is 5:1) for 12 hours, and washing, centrifuging and drying to obtain hydroxylated titanium dioxide;
s3, adding 0.8g of the hydroxylated titanium dioxide and 0.1g of the dispersing agent into the dispersion liquid, stirring at 80 ℃ for 1h, adding 100mL of n-hexane, carrying out ultrasonic treatment for 5min, adjusting the pH value to 7, and centrifuging, washing and drying to obtain the product.
Example 2
The preparation method of the aerogel microsphere comprises the following steps:
s1, adding 20g of carbon nanotubes into a mixed solution of 1L of concentrated sulfuric acid and 0.5L of concentrated hydrochloric acid, performing ultrasonic treatment at 50 ℃ for 12 hours, washing a product to be neutral by deionized water and ethanol, and drying overnight to obtain carboxylated carbon nanotubes;
adding 1g of carboxylated carbon nanotubes and 8g of graphene oxide into 200mL of deionized water, carrying out ultrasonic treatment for 1h, adding 1g of urea, and stirring for 60min to obtain a dispersion liquid;
s2, soaking 1g of titanium dioxide powder in 50mL of 5mol/L sodium hydroxide solution, performing ultrasonic treatment for 3 hours, washing to neutrality, mixing with glucose (titanium dioxide: glucose=1:5, m/m) after drying, performing ball milling treatment (ball-to-material ratio is 5:1) for 12 hours, and washing, centrifuging and drying to obtain hydroxylated titanium dioxide;
s3, adding 0.8g of the hydroxylated titanium dioxide and 0.1g of the dispersing agent into the dispersion liquid, stirring at 80 ℃ for 1h, adding 100mL of n-hexane, carrying out ultrasonic treatment for 5min, adjusting the pH value to 7, and centrifuging, washing and drying to obtain the product.
Comparative example 1
This comparative example differs from example 1 in that thiourea was not added in step S1, and other components and preparation methods were the same as example 1.
Comparative example 2
This comparative example is different from example 1 in that in step S1, the carboxylation treatment is not performed on the carbon nanotubes (the carboxylated carbon nanotubes are replaced with ordinary carbon nanotubes of equal mass), and other components and preparation methods are the same as in example 1.
Comparative example 3
This comparative example differs from example 1 in that the hydroxylated titanium dioxide is replaced by an equal mass of ordinary titanium dioxide in step S3, the other ingredients and preparation method being the same as in example 1.
Test case
The aerogel microspheres prepared in examples 1-2 and comparative examples 1-3 were subjected to performance testing.
The testing method comprises the following steps:
adsorption performance: cd with concentration of 800mg/L 2+ Heavy metal solution, adding aerogel microspheres prepared in the example or the comparative example respectively in an amount of 1g/L, adsorbing for 24 hours at 25 ℃, and taking a water sample after adsorption to analyze the adsorption amount.
Photo-thermal performance: 1g of aerogel microspheres prepared in the examples or comparative examples were placed on the surface of a beaker containing 200mL of purified water, respectively, with a light intensity of 1kW/m 2 The evaporation rate was measured after 2 hours of irradiation with light.
The results obtained are shown in Table 1.
TABLE 1 Performance test results
| Sample of | Adsorption quantity (mg/g) | Evaporation rate (kg.m) -2 ·h -1 ) |
| Example 1 | 221 | 1.63 |
| Example 2 | 208 | 1.55 |
| Comparative example 1 | 165 | 1.29 |
| Comparative example 2 | 172 | 1.37 |
| Comparative example 3 | 196 | 1.26 |
As can be seen from Table 1, the aerogel microspheres prepared in the examples 1-2 of the present invention have good adsorption performance and photo-thermal performance, especially the example 1 using thiourea as the component has more excellent performance, and the comparative examples 1-3 of the replacement and deletion components have reduced performance, which proves that the carboxylated carbon nanotubes, the hydroxylated titanium dioxide and the nitrogen-containing organic substances of the present invention have synergistic effect, and the performance of the aerogel microspheres is improved, so the present invention has good application prospects.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. The preparation method of the aerogel microsphere is characterized by comprising the following steps:
s1, adding a carbon nano tube into a mixed solution of concentrated sulfuric acid and concentrated hydrochloric acid, performing ultrasonic treatment for the first time, washing and drying to obtain a carboxylated carbon nano tube, then adding the carboxylated carbon nano tube and graphene oxide into deionized water, adding a nitrogen-containing organic matter after ultrasonic treatment for the second time, and stirring to obtain a dispersion;
s2, soaking titanium dioxide in alkali liquor, carrying out ultrasonic treatment, mixing with glucose, carrying out ball milling treatment, and purifying to obtain hydroxylated titanium dioxide;
s3, adding the hydroxylated titanium dioxide and the dispersing agent into the dispersion liquid, heating and stirring, adding an oil phase, regulating the pH value after ultrasonic treatment, and obtaining a product through centrifugation, washing and drying.
2. The method of claim 1, wherein in step S1, the volume ratio of concentrated sulfuric acid to concentrated hydrochloric acid is (1-3): 1.
3. The method of claim 1, wherein in step S1, the time of the first ultrasonic treatment is 8-12 hours, the time of the second ultrasonic treatment is 1-2 hours, and the time of stirring is 30-60 minutes.
4. The method of claim 1, wherein in step S1, the nitrogen-containing organic matter is one or more selected from urea and thiourea.
5. The method for preparing aerogel microspheres according to claim 1, wherein in step S1, the mass ratio of carboxylated carbon nanotubes, graphene oxide and nitrogen-containing organic substances is (1-2): 1-8): 1-2.
6. The method of claim 1, wherein in step S2, the time of the ultrasonic wave is 1-3 hours.
7. The method of claim 1, wherein in step S2, the ball milling is performed for 8-24 hours, and the ball-to-material ratio is (1-5): 1.
8. The method of claim 1, wherein in step S2, the alkali solution is 1-10mol/L sodium hydroxide solution.
9. The method of claim 1, wherein in step S3, the pH is in the range of 7-8.
10. The method of claim 1, wherein in step S3, the oil phase is n-hexane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310829849.9A CN116983953B (en) | 2023-07-07 | 2023-07-07 | Preparation method of aerogel microspheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310829849.9A CN116983953B (en) | 2023-07-07 | 2023-07-07 | Preparation method of aerogel microspheres |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116983953A CN116983953A (en) | 2023-11-03 |
| CN116983953B true CN116983953B (en) | 2024-02-02 |
Family
ID=88522322
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310829849.9A Active CN116983953B (en) | 2023-07-07 | 2023-07-07 | Preparation method of aerogel microspheres |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116983953B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109621902A (en) * | 2019-01-29 | 2019-04-16 | 辽宁大学 | Carbon nanotube and composite titania material and preparation method thereof and the application in recycling gallium |
| KR20200056759A (en) * | 2018-11-15 | 2020-05-25 | 한국과학기술연구원 | Photocatalyst material with titanium dioxide nanoparticles fixed to internal space of multi-walled carbon nanotube |
| CN113578212A (en) * | 2021-07-09 | 2021-11-02 | 西安理工大学 | Zinc oxide/graphene oxide/carbon nanotube aerogel and method |
| CN114368741A (en) * | 2021-12-31 | 2022-04-19 | 深圳市翔丰华科技股份有限公司 | Preparation method of graphene/carbon nanotube/silicon dioxide aerogel material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8222302B2 (en) * | 2005-11-29 | 2012-07-17 | The Hong Kong University Of Science And Technology | Titania-silica aerogel monolith with ordered mesoporosity and preparation thereof |
| WO2014136073A1 (en) * | 2013-03-06 | 2014-09-12 | Ecole Polytechnique Federale De Lausanne (Epfl) | Titanium oxide aerogel composites |
-
2023
- 2023-07-07 CN CN202310829849.9A patent/CN116983953B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200056759A (en) * | 2018-11-15 | 2020-05-25 | 한국과학기술연구원 | Photocatalyst material with titanium dioxide nanoparticles fixed to internal space of multi-walled carbon nanotube |
| CN109621902A (en) * | 2019-01-29 | 2019-04-16 | 辽宁大学 | Carbon nanotube and composite titania material and preparation method thereof and the application in recycling gallium |
| CN113578212A (en) * | 2021-07-09 | 2021-11-02 | 西安理工大学 | Zinc oxide/graphene oxide/carbon nanotube aerogel and method |
| CN114368741A (en) * | 2021-12-31 | 2022-04-19 | 深圳市翔丰华科技股份有限公司 | Preparation method of graphene/carbon nanotube/silicon dioxide aerogel material |
Non-Patent Citations (6)
| Title |
|---|
| Design and Tailoring of a Three-Dimensional TiO2–Graphene–Carbon Nanotube Nanocomposite for Fast Lithium Storage;Shen，LF et al;《Journal of Physical Chenmistry Letters》;第2卷(第24期);第3096-3101页 * |
| Synthesis and characterization of mercapto-modified graphene/multi-walled carbon nanotube aerogels and their adsorption of Au(III) from environmental samples;Wang，SK et al;《Journal of Non-crystalline Solids》;第536卷;第120008页 * |
| TiO2-graphene sponge for the removal of tetracycline;Zhao，LQ et al;《Journal of Nanoparticle Research》;第17卷(第1期);第16页 * |
| 复合气凝胶的制备及对甲苯的吸附试验;王玮等;《消防科学与技术》(第10期);第100-103页 * |
| 石墨烯/SiO2复合气凝胶微球的制备及其吸附性能研究;吴鸣;《化工新型材料》;第47卷(第9期);第155-160+165页 * |
| 石墨烯/碳纳米管复合材料的制备及应用进展;赵冬梅等;《化学学报》;第72卷(第2期);第63-78页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116983953A (en) | 2023-11-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107754785B (en) | Graphene-manganese oxide composite catalyst for low-temperature catalytic oxidation of formaldehyde and preparation method thereof | |
| CN102698754B (en) | Nanometer iron oxide/carbon sphere compound catalyst and preparation method and application thereof | |
| CN108970608B (en) | Supported noble metal catalyst with coating structure, preparation method thereof and application thereof in Cu (II) liquid-phase catalytic reduction | |
| CN105289498B (en) | A kind of preparation method of biomass carbon carbon nanomaterial compound | |
| CN112264040B (en) | Carbon sphere-graphene oxide catalyst and preparation method and application thereof | |
| CN110586158A (en) | PdB/NH2-N-rGO catalyst and preparation method and application thereof | |
| Dai et al. | Hydrolysis of cellulose to glucose in aqueous phase with phosphate group modified hydroxy-rich carbon-based catalyst | |
| CN114505101A (en) | Organic dye degradation catalyst based on heterogeneous Fenton-like reaction, and preparation and application thereof | |
| CN110548483A (en) | preparation method and application of biochar/nano ferroferric oxide composite material | |
| CN113042086A (en) | In-situ preparation method and application of amino functionalized carbon nanotube loaded NiAuPd nano-catalyst | |
| CN104667973A (en) | Catalyst carrier material and preparation method thereof | |
| CN116983953B (en) | Preparation method of aerogel microspheres | |
| CN108199033A (en) | A kind of preparation method of lithium battery carbon/manganese dioxide composite material | |
| CN111185222A (en) | Zinc-based catalyst for catalyzing acetylene hydration reaction and preparation method thereof | |
| CN112156771B (en) | Preparation method and application of biological thallus supported catalyst | |
| CN112121834B (en) | MXene/CdS composite photocatalyst, preparation method thereof and application thereof in hydrogen production by water cracking | |
| WO2024011905A1 (en) | Metal-supported spinel nickel manganite nanosphere aerogel, preparation method therefor and use thereof | |
| CN115282965B (en) | Application of catalyst in treatment of styrene waste gas | |
| US11370659B2 (en) | Porous carbon-based metal catalyst as well as preparation method and application thereof | |
| CN113571720B (en) | Carbon-based catalyst containing metal platinum, preparation method and application thereof | |
| CN113398880A (en) | Preparation method of carbon-based composite microspheres with adsorption and catalytic degradation functions on dye molecules | |
| CN111408372B (en) | Copper-based CO with hollow nanosphere morphology 2 Preparation process of electro-reduction catalyst | |
| CN114180549A (en) | Preparation method and application of carbon material containing 3d metal single atom and nitrogen and oxygen co-doped | |
| CN103962142B (en) | Nucleocapsid perovskite type catalyst preparation method for methane methyl alcohol | |
| CN107555415B (en) | Method for preparing polyvinyl alcohol-based carbon microspheres by hydrothermal method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |