CN109647331B - Preparation method and application of composite adsorption material - Google Patents
Preparation method and application of composite adsorption material Download PDFInfo
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- CN109647331B CN109647331B CN201811444388.9A CN201811444388A CN109647331B CN 109647331 B CN109647331 B CN 109647331B CN 201811444388 A CN201811444388 A CN 201811444388A CN 109647331 B CN109647331 B CN 109647331B
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- 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
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- 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
- B01J20/10—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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Abstract
The invention provides a preparation method of a composite adsorption material, which comprises the following steps: mixing the adsorption particles with the 3D printing ink, and stirring to obtain composite ink; 3D printing is carried out on the composite ink to obtain a prefabricated body with a 3D structure; and aging, drying and thermally treating the prefabricated body to obtain the composite adsorbing material. Compared with the prior art, the method has the advantages that the 3D printing technology is utilized, the 3D printing structure is used for constructing the macropores on the hierarchical structure of the adsorption particles, the actual contact area of the adsorbed substance and the adsorption material is increased, the diffusion channel is increased, and the adsorption rate is greatly improved. The composite adsorption material prepared by the invention has a multi-scale hierarchical structure, can accelerate the adsorption rate while saving the adsorption material, can ensure that the composite adsorption material has certain strength and is not easy to fall off, avoids secondary pollution, has simple process, and has important significance in the aspects of design and production of composite materials, environment-friendly adsorption or slow release application of materials and the like.
Description
Technical Field
The invention relates to the technical field of adsorption materials, in particular to a preparation method and application of a composite adsorption material.
Background
Natural and synthetic high efficiency physical adsorption materials generally have a layered porous structure and a rich surface. The pores and the surface with the size equivalent to that of the adsorbate can effectively adsorb, and for general adsorbate materials, the suitable pores are generally between 0.1 and 5nm (micropores or small mesopores), and the size falls in the range of measuring the specific surface area through gas adsorption and desorption. Since the contribution of micropores to the specific surface area is very large, it is generally considered that the larger the specific surface area is, the better the adsorption performance is.
However, recent scientific research related to electrochemistry has found that the accessibility of effective adsorption pores greatly affects adsorption or surface reaction behavior. Liu et al constructed a microporous/macroporous (>50nm) composite structure sample, and found that the performance of the sample is several times better than that of a microporous/mesoporous (2-50nm) composite structure material with the same components; the specific surface area of the microporous/mesoporous material is about 3 times of that of the microporous/macroporous material, which shows that the method of constructing a channel with a large-scale structure to increase the accessibility of the micropores has great influence on final diffusion, adsorption or surface reaction.
In the field of environmental adsorption, whether gas phase or liquid phase, adsorption is generally performed by constructing adsorbent material particles coated with non-woven fabric. In the prior art, chinese patent document with application number 201710554249.0 reports an adsorbing material and a preparation method thereof, including: a fabric as a substrate; and an adsorbent adsorbed on the fabric, the adsorbent being a combination of a molecular sieve and a silica aerogel. The Chinese patent document with the application number of 201710678061.7 reports a high-efficiency adsorbing material for an air outlet of an air conditioner external fan, which comprises an activated carbon layer and non-woven fabric layers arranged on two sides of the activated carbon layer. However, the particles of the adsorbing material reported above are tightly packed together, which is not favorable for the diffusion of the adsorbate, and further affects the adsorption efficiency; some adsorbing materials also have the problem of fragility, and in addition, the particles are easy to contact and rub, and the surfaces of the particles are easy to fall off to form secondary pollution. How to increase the space interval of the adsorption particles and fix the adsorption particles becomes a difficult problem.
Disclosure of Invention
The invention aims to provide a preparation method and application of a composite adsorption material, which has a multi-scale hierarchical structure, good adsorption performance and simple process.
In view of this, the invention provides a preparation method of a composite adsorbing material, which comprises the following steps: mixing the adsorption particles with the 3D printing ink, and stirring to obtain composite ink; 3D printing is carried out on the composite ink to obtain a prefabricated body with a 3D structure; and aging, drying and thermally treating the prefabricated body to obtain the composite adsorbing material.
Preferably, the adsorption particles are one or more of silicon oxide particles, aluminum oxide particles and porous carbon particles.
Preferably, the 3D printing ink is one or more of dextrin-based ink, phenolic resin-based ink and polyimide-based ink.
Preferably, the mass ratio of the adsorption particles to the 3D printing ink is 1-5: 100.
preferably, the 3D structure is a wood heap structure.
Preferably, the 3D printing adopts a 3D bioprinter or a 3D direct writing forming device.
Preferably, the aging step is: soaking the preform in water or ethanol for 1-3 days.
Preferably, the drying is atmospheric drying, freeze drying or supercritical fluid drying.
Preferably, the heat treatment step is: heating to 500-.
The invention also provides application of the composite adsorbing material obtained by the preparation method in cell culture solution, and the adsorption effect is evaluated by adopting the residual concentration-time data of the adsorbed substance solution.
The invention provides a preparation method of a composite adsorption material, which comprises the following steps: mixing the adsorption particles with the 3D printing ink, and stirring to obtain composite ink; 3D printing is carried out on the composite ink to obtain a prefabricated body with a 3D structure; and aging, drying and thermally treating the prefabricated body to obtain the composite adsorbing material. The invention also provides application of the composite adsorbing material obtained by the preparation method in cell culture solution, and the adsorption effect is evaluated by adopting the residual concentration-time data of the adsorbed substance solution. Compared with the prior art, the method has the advantages that the 3D printing technology is utilized, the 3D printing structure is used for constructing the macropores on the hierarchical structure of the adsorption particles, the actual contact area of the adsorbed substance and the adsorption material is increased, the diffusion channel is increased, and the adsorption rate is greatly improved. The composite adsorption material prepared by the invention has a multi-scale hierarchical structure, can accelerate the adsorption rate while saving the adsorption material, can ensure that the composite adsorption material has certain strength and is not easy to fall off, avoids secondary pollution, has simple process, and has important significance in the aspects of design and production of composite materials, environment-friendly adsorption or slow release application of materials and the like.
Drawings
FIG. 1 is a schematic diagram of the preparation of a composite adsorbent material according to the present invention.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The embodiment of the invention discloses a preparation method of a composite adsorption material, which comprises the following steps: mixing the adsorption particles with the 3D printing ink, and stirring to obtain composite ink; 3D printing is carried out on the composite ink to obtain a prefabricated body with a 3D structure; and aging, drying and thermally treating the prefabricated body to obtain the composite adsorbing material.
The invention provides a design of a multi-scale hierarchical structure efficient adsorption material prepared based on a 3D printing technology, which is characterized in that the adsorption material or a composite material thereof is formed by 3D printing, the space interval of adsorption particles is increased by utilizing a 3D design pattern, the adsorption particles are fixed to form a whole adsorption material, and secondary pollution caused by particle falling is avoided while the adsorption efficiency is improved.
Preferably, the adsorbent particles have a high specific surface area, and more preferably are one or more of silica particles, alumina particles and porous carbon particles. The 3D printing ink is preferably one or more of dextrin-based ink, phenolic resin-based ink and polyimide-based ink. The invention controls the mass ratio of the adsorption particles to the 3D printing ink, and is beneficial to forming a micropore and small mesopore hierarchical structure after 3D printing. The mass ratio of the adsorbent particles to the 3D printing ink is preferably 1-5: 10, more preferably 3 to 5: 10, more preferably 5: 10.
preferably, the characteristics of the composite ink are tested by a rheometer so that the composite ink meets the condition of shear thinning, and the shear rate is preferably increased to 1000s-1And when the viscosity is reduced to the Pa.s magnitude, the composite ink is stably stored and waits for printing.
As a preferable aspect, the present invention is not particularly limited to the structure of the printed 3D structure, and the 3D structure is preferably a wood pile structure. The 3D printing preferably adopts a 3D bioprinter or a 3D direct-writing forming device, and the inner diameter of a needle head used by the printer is preferably 400 mu m. The invention designs the required 3D structure through a computer program, and then adopts a 3D bioprinter or a 3D direct-writing forming device to print.
Fig. 1 shows a schematic diagram of a principle of preparing a composite adsorbing material according to the present invention, wherein 1 is a 3D printing device, preferably a 3D bioprinter or a 3D direct writing molding device, 2 is a 3D printed composite adsorbing material, 3 is a cured 3D printing ink material, 4 is a layered structure of adsorbing particles, and 3 and 4 may be materials of different components or materials of the same component.
Preferably, the aging step is: soaking the preform in water or ethanol for 1-3 days. The drying is preferably carried out by atmospheric drying, freeze drying or supercritical fluid drying. The heat treatment step is preferably: heating to 500-; more preferably: heating to 600-.
Preferably, the composite adsorbent material is used for physical adsorption of a plurality of substances.
The invention also provides application of the composite adsorbing material obtained by the preparation method in cell culture solution, and the adsorption effect is evaluated by adopting the residual concentration-time data of the adsorbed substance solution.
According to the scheme, the preparation method of the composite adsorbing material has the advantages of simple process, simplicity and easiness, the prepared composite adsorbing material has a multi-scale hierarchical structure, high adsorption performance and good environmental safety, and has important significance on the aspects of design, industrial production, performance regulation and the like of the efficient adsorbing material. Has the following characteristics:
(1) the composite adsorbing material prepared by the invention has the characteristic of multi-scale hierarchical structure;
(2) the multi-scale hierarchical structure efficient adsorption material prepared by the 3D printing technology has the advantages of simple process, good adsorption performance, environmental protection, safety and the like;
(3) the invention can save the adsorbing material under the condition of the same volume and improve the performance, thereby having good economic benefit.
For further understanding of the present invention, the following embodiments are provided to illustrate the technical solutions of the present invention in detail, and the scope of the present invention is not limited by the following embodiments.
The raw materials adopted in the embodiment of the invention are all commercially available.
Example 1
And stirring and mixing the porous carbon-based physical adsorption material particles and the phenolic resin-based ink at normal temperature according to the mass ratio of 50:100 to form the composite ink. The ink was tested by rheometer to meet the conditions of shear thinning as the shear rate increased from near 0 to 1000s-1The viscosity decreases from approaching infinity to the order of 2 pa.s. And (5) stably storing the composite ink for printing.
Through the wooden heap structure of computer programming design, put into 3D bio-printer with compound ink, carry out the printing of 3D sample.
And (2) aging the printed sample for 3 days under the soaking of water, then performing supercritical fluid drying under the conditions of 40 ℃ and 10MPa, performing heat treatment at 1000 ℃ under the protection of nitrogen, wherein the heating rate is 10 ℃/min, and keeping for 2 hours after the highest temperature is reached to obtain the composite adsorbing material.
The prepared composite adsorbing material is used for adsorbing cell culture solution. The residual concentration of the effective components in the culture solution is calibrated and tested by an ultraviolet-visible-near infrared spectrophotometer, and the adsorption performance is evaluated.
The physical adsorption material in the embodiment is a carbon-based material, and a micropore and small mesopore hierarchical structure can be observed through detection of a nitrogen adsorption and desorption experiment, wherein the peak aperture is about 3 nm; the 3D structure is a wood pile structure; the inner diameter of the needle used for the printer is about 400 mu m; the concentration of the used cell culture solution is unknown, and the performance of the spectrophotometer is evaluated by adopting the relative concentration after linear calibration.
The results show that the composite adsorbing material prepared in the embodiment reduces the residual concentration to 50% in 50 minutes, and the residual relative concentration is only about 5% in 200 minutes; and the residual relative concentration of the original adsorption material, namely the porous carbon-based physical adsorption material with the same volume is slightly higher than 50 percent after the adsorption for 250 minutes. Under the same condition, the adsorption rate of the 3D printing adsorption material is 5 times higher than that of the original adsorption material (estimated when the residual relative concentration is 50%), which shows that the large-size structure formed by 3D printing can effectively improve a diffusion channel and enhance the contact property of micropores, thereby greatly improving the adsorption effect.
Example 2
Mixing alumina-based physical adsorption material particles and dextrin resin-based ink according to a mass ratio of 10: 100, and stirring and mixing at normal temperature to form the composite ink, wherein the prepared ink meets the shear thinning condition. And (5) stably storing the composite ink for printing. And designing a geometric structure through a computer program, and putting the composite ink into 3D direct-writing forming equipment to print a 3D sample.
And (3) aging the printed sample for 1 day under the soaking of water, drying the sample for 3 hours at 80 ℃ under normal pressure, performing heat treatment at 500 ℃ under the protection of nitrogen, wherein the heating rate is 10 ℃/min, and keeping the temperature for 2 hours after the highest temperature is reached to obtain the composite adsorbing material.
The adsorption performance of the composite adsorption material prepared by the embodiment and the alumina-based physical adsorption material adopted by the composite adsorption material is detected respectively, and the result shows that: under the same condition, the adsorption rate of the composite adsorption material prepared by the embodiment is better than that of the original adsorption material, which shows that the large-size structure formed by 3D printing can effectively improve a diffusion channel and enhance the accessibility of micropores, thereby greatly improving the adsorption effect.
Example 3
The silicon oxide-based physical adsorption material particles and the polyimide resin-based ink are stirred and mixed at normal temperature according to the mass ratio of 20:100 to form the composite ink, and the prepared ink meets the shear thinning condition. And (5) stably storing the composite ink for printing. Through computer programming frame construction, put into 3D bio-printer with compound ink, carry out the printing of 3D sample.
Aging a printed sample for 3 days under the soaking of ethanol, then drying the sample by supercritical fluid under the conditions of 40 ℃ and 10MPa, then carrying out heat treatment at 600 ℃ under the protection of nitrogen, wherein the heating rate is 10 ℃/min, and keeping for 2h after the highest temperature is reached to obtain the composite adsorbing material.
The adsorption performance of the composite adsorption material prepared by the embodiment and the silica-based physical adsorption material adopted by the composite adsorption material is detected respectively, and the result shows that: under the same condition, the adsorption rate of the composite adsorption material prepared by the embodiment is better than that of the original adsorption material, which shows that the large-size structure formed by 3D printing can effectively improve a diffusion channel and enhance the accessibility of micropores, thereby greatly improving the adsorption effect.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. The preparation method of the composite adsorption material is characterized by comprising the following steps of:
mixing the adsorption particles with the 3D printing ink, and stirring to obtain composite ink;
3D printing is carried out on the composite ink to obtain a prefabricated body with a 3D structure;
aging, drying and thermally treating the prefabricated body to obtain a composite adsorbing material;
the mass ratio of the adsorption particles to the 3D printing ink is 1-5: 100, respectively;
the aging step is as follows: soaking the prefabricated body in water or ethanol for 1-3 days;
the drying is normal pressure drying, freeze drying or supercritical fluid drying;
the heat treatment step is as follows: heating to 500-.
2. The preparation method according to claim 1, wherein the adsorption particles are one or more of silica particles, alumina particles and porous carbon particles.
3. The preparation method according to claim 1, wherein the 3D printing ink is one or more of dextrin-based ink, phenolic resin-based ink and polyimide-based ink.
4. The method of manufacturing of claim 1, wherein the 3D structure is a wood stack structure.
5. The method for preparing according to claim 1, wherein the 3D printing is performed by a 3D bioprinter or a 3D direct writing molding device.
6. Use of a composite adsorbent material obtained by the process according to any one of claims 1 to 5 in a cell culture medium, wherein the adsorption effect is evaluated using data on the residual concentration of the adsorbate solution versus time.
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| CN111672264B (en) * | 2020-06-09 | 2021-04-16 | 清华大学 | Adsorption thin layer for adsorbing gaseous pollutants and manufacturing method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104096535A (en) * | 2014-07-09 | 2014-10-15 | 西安交通大学 | High-adsorbability powdered material forming technology based on 3D printing technology |
| KR20180003074A (en) * | 2016-06-30 | 2018-01-09 | (주)아이투스 인터내셔날 | Nano-carbon structure filling type 3d printing material composition |
| CN107936685A (en) * | 2017-11-17 | 2018-04-20 | 同济大学 | A kind of preparation method of polyimides ink available for 3D printing |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104096535A (en) * | 2014-07-09 | 2014-10-15 | 西安交通大学 | High-adsorbability powdered material forming technology based on 3D printing technology |
| KR20180003074A (en) * | 2016-06-30 | 2018-01-09 | (주)아이투스 인터내셔날 | Nano-carbon structure filling type 3d printing material composition |
| CN107936685A (en) * | 2017-11-17 | 2018-04-20 | 同济大学 | A kind of preparation method of polyimides ink available for 3D printing |
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