CN109574018A - A kind of mesoporous nano material and preparation method thereof with humidity conditioning function - Google Patents
A kind of mesoporous nano material and preparation method thereof with humidity conditioning function Download PDFInfo
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- CN109574018A CN109574018A CN201811515795.4A CN201811515795A CN109574018A CN 109574018 A CN109574018 A CN 109574018A CN 201811515795 A CN201811515795 A CN 201811515795A CN 109574018 A CN109574018 A CN 109574018A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The preparation method of the invention discloses a kind of mesoporous nano material with humidity conditioning function comprising following processing step: 1) stock dispersion obtains clay slurry；2) hydro-thermal alkali activates: being in mass ratio 1:(0.45~2.6 by clay slurry, sodium hydroxide solution and deionized water): (0.01~1.2) is poured into hydrothermal reaction kettle after mixing, obtains alkali activation powder；3) hydro-thermal acid etching: it is 1:(1.3~5.2 that alkali is activated powder, hydrogen chloride solution and deionized water in mass ratio): (1.4~5.4) are poured into hydrothermal reaction kettle after mixing, obtain finished product.The present invention is using the natural nano layered silicate clay of China's rich reserves as raw material, without organic solvent, by hydro-thermal alkali activation and hydro-thermal acid etching carving technology prepare the mesoporous nano material with highly effective humidity conditioning performance, and preparation process is simple, preparation cost is cheap, it is easy to operate, be conducive to large-scale industrial production.
Description
Technical field
The present invention relates to field of inorganic materials, in particular to a kind of mesoporous material.
Background technique
Air humidity is closely bound up with human health, and the excessively high meeting of air humidity is so that the intracorporal thyroxine of people and adrenal gland
The concentration of element reduces, so that the metabolism of cell be caused to slow down, can make one listless, dispirited；Air humidity is too low
Human body water evaporation rate can be made to accelerate, dry skin and nasal membrane is caused to be stimulated, human body is induced and generate respiratory system
Illness.In addition, being all conducive to the breeding and propagation of some bacteriums and virus when air humidity is excessive or too small.Therefore, by air
Humid control is in the comfortable range of human body sensory (50~70%), it appears particularly necessary.And proved according to correlative study, aperture is
3.7~7.1nm's is mesoporous, by capillary condensation and desorption, has between 50~70% to maintenance indoor relative humidity
Effect the most significant.Aperture is the mesoporous material of 3.7~7.1nm, can discharge its absorption when ambient humidity is lower than 50%
Moisture content increases the humidity in air；The aqueous vapor in air can be absorbed, to reduce in air when ambient humidity is higher than 70%
Humidity.
Humidity adjusting material is that indoor humidity is adjusted using the porous material that aperture is 3.7~7.1nm.Natural mesoporous material
Blanking aperture distribution is wide in range, the aperture in only a small amount of hole in the range of 3.7~7.1nm, cause its quality hydroscopicity it is low, adjust
Wet effect is poor.Synthesising mesoporous material has duct orderly, and continuously adjustable and specific surface area are high in a certain range for pore size
Etc. features, be a kind of ideal humidity adjusting material.
Up to the present, the preparation patent in relation to mesoporous material has: " a kind of functionality mesoporous material and preparation method thereof "
CN106466593A, a kind of " mesoporous material " CN103043676A, " a kind of mesoporous material and its method of modifying and purposes "
CN105948071A, a kind of " synthetic method of total silicon mesoporous material " CN104418344A.These patents all use organic formwork
Legal system prepares mesoporous material, and not only time-consuming, at high cost, and needs largely to use organic solvent in preparation process, these are organic
The volatilization of solvent and burn off can have biggish potential hazard to environment.These disadvantages are unfavorable for the industrialization of mesoporous humidity adjusting material
Using production.
Summary of the invention
It is an object of the invention in view of the above shortcomings of the prior art, provide a kind of mesoporous nano with humidity conditioning function
The preparation method of material prepares hydroscopicity of the resulting mesoporous nano material with humidity conditioning function under high humidity environment and is up to
80%, have efficient humidity.
The technical solution used in the present invention is: a kind of preparation method of the mesoporous nano material with humidity conditioning function,
It comprises the technical steps that:
1) stock dispersion: by natural nano layered silicate clay and deionized water according to 7:(12~15) ratio be placed in
Ball milling in ball mill, sieving is handled after being milled to 300 mesh screen residues less than 0.3%, obtains clay slurry；
2) hydro-thermal alkali activate: by clay slurry, sodium hydroxide solution and deionized water be in mass ratio 1:(0.45~
2.6): (0.01~1.2) is poured into hydrothermal reaction kettle after mixing, 2~15h is reacted at a temperature of 95~145 DEG C, through vacuum
Filtering, deionized water are washed to neutral, drying, and alkali activation powder is obtained；
3) hydro-thermal acid etching: it is 1:(1.3~5.2 that alkali is activated powder, hydrogen chloride solution and deionized water in mass ratio):
(1.4~5.4) are poured into hydrothermal reaction kettle after mixing, and 2~15h is reacted at a temperature of 95~145 DEG C, be cooled to room temperature,
Washing obtains finished product through vacuum filter, drying, broken, sieving to neutrality.
Specifically, the present invention uses natural nano layered silicate clay mineral for primary raw material, is activated by hydro-thermal alkali,
The amorphous lagoriolite of in-situ preparation on sheet silicate structure, using hydro-thermal acid etching, by amorphous state lagoriolite
Middle Al-O, Na-O dissolution, so that a large amount of apertures of in-situ preparation are Jie of 3.7~7.1nm on remaining sheet silica skeleton
Hole duct has efficient humidity so that quality hydroscopicity of the mesoporous nano material under high humidity environment is up to 80%.
As a further improvement of the foregoing solution, natural nano layered silicate clay described in step 1) is selected to cover and take off
One of which in soil, kaolin and volcanic mud.
As a further improvement of the foregoing solution, the specific surface of natural nano layered silicate clay described in step 1)
Product is 20~50m2/g。
As a further improvement of the foregoing solution, the molar concentration of sodium hydroxide solution described in step 2) be 8~
16mol/L。
As a further improvement of the foregoing solution, the molar concentration of hydrogen chloride solution described in step 2) be 8~
12mol/L。
The object of the invention is also to provide a kind of mesoporous nano material with humidity conditioning function, by making as described above
Preparation Method is prepared.Specifically, mesoporous nano material main component of the invention is silica, and meso-hole structure is at 1000 DEG C
Still it is able to maintain that complete, high-temperature stability is good.
The beneficial effects of the present invention are: the present invention is original with the natural nano layered silicate clay of China's rich reserves
Material prepares receiving with highly effective humidity conditioning performance by the activation of hydro-thermal alkali and hydro-thermal acid etching carving technology without organic solvent
Rice mesoporous material will not generate toxic, the harmful organic exhaust gas for having biggish potential hazard to environment, and preparation process
Simply, preparation cost it is cheap, it is easy to operate, be conducive to large-scale industrial production.
Detailed description of the invention
Fig. 1 is the water adsorption curve graph that the detection in the embodiment of the present invention 4 obtains；
Fig. 2 is the moisture desorption curve graph that the detection in the embodiment of the present invention 4 obtains.
Specific embodiment
The present invention is specifically described below with reference to embodiment, in order to technical field personnel to of the invention
Understand.It is necessary to it is emphasized that embodiment is only intended to, the present invention will be further described herein, should not be understood as to this
The limitation of invention protection scope, fields person skilled in the art, the non-intrinsically safe that the present invention is made according to foregoing invention content
The modifications and adaptations of property, should still fall within protection scope of the present invention.Mentioned raw materials following simultaneously are unspecified, are
Commercial product；The processing step or preparation method not referred in detail be processing step known to a person skilled in the art or
Preparation method.
Embodiment 1
A kind of preparation method of the mesoporous nano material with humidity conditioning function comprising following processing step:
1) stock dispersion: being 35m by specific surface area2The kaolin and deionized water of/g is placed in ball milling according to the ratio of 7:13
Ball milling in machine crosses the processing of 300 meshes, obtains clay slurry after being milled to 300 mesh screen residues less than 0.3%；
2) hydro-thermal alkali activates: be in mass ratio 1 by clay slurry, the sodium hydroxide solution of 8mol/L and deionized water:
2.6:0.01 is poured into hydrothermal reaction kettle after mixing, reacts 2h at a temperature of 145 DEG C, is washed through vacuum filter, deionization
It washs to neutral, 150 DEG C of baking oven drying, obtains alkali activation powder；
3) hydro-thermal acid etching: it is 1 that alkali is activated powder, the hydrogen chloride solution of 8mol/L and deionized water in mass ratio:
1.3:1.4 is poured into hydrothermal reaction kettle after mixing, reacts 15h at a temperature of 95 DEG C, is cooled to room temperature, is washed to neutrality,
It is dried through vacuum filter, 115 DEG C of baking oven, is broken, crossing 200 meshes, obtaining 1 finished product of embodiment.
Embodiment 2
A kind of preparation method of the mesoporous nano material with humidity conditioning function comprising following processing step:
1) stock dispersion: being 20m by specific surface area2The kaolin and deionized water of/g is placed in ball milling according to the ratio of 7:12
Ball milling in machine crosses the processing of 300 meshes, obtains clay slurry after being milled to 300 mesh screen residues less than 0.3%；
2) hydro-thermal alkali activates: be in mass ratio 1 by clay slurry, the sodium hydroxide solution of 12mol/L and deionized water:
0.45:1.2 is poured into hydrothermal reaction kettle after mixing, reacts 15h at a temperature of 95 DEG C, is washed through vacuum filter, deionization
It washs to neutral, 115 DEG C of baking oven drying, obtains alkali activation powder；
3) hydro-thermal acid etching: it is 1 that alkali is activated powder, the hydrogen chloride solution of 10mol/L and deionized water in mass ratio:
5.2:5.4 is poured into hydrothermal reaction kettle after mixing, reacts 2h at a temperature of 145 DEG C, is cooled to room temperature, is washed to neutrality,
It is dried through vacuum filter, 150 DEG C of baking oven, is broken, crossing 200 meshes, obtaining 2 finished product of embodiment.
Embodiment 3
A kind of preparation method of the mesoporous nano material with humidity conditioning function comprising following processing step:
1) stock dispersion: being 50m by specific surface area2The kaolin and deionized water of/g is placed in ball milling according to the ratio of 7:15
Ball milling in machine crosses the processing of 300 meshes, obtains clay slurry after being milled to 300 mesh screen residues less than 0.3%；
2) hydro-thermal alkali activates: be in mass ratio 1 by clay slurry, the sodium hydroxide solution of 16mol/L and deionized water:
0.85:0.95 is poured into hydrothermal reaction kettle after mixing, reacts 6h at a temperature of 105 DEG C, is washed through vacuum filter, deionization
It washs to neutral, 120 DEG C of baking oven drying, obtains alkali activation powder；
3) hydro-thermal acid etching: it is 1 that alkali is activated powder, the hydrogen chloride solution of 12mol/L and deionized water in mass ratio:
2.6:4.1 is poured into hydrothermal reaction kettle after mixing, reacts 5h at a temperature of 120 DEG C, is cooled to room temperature, is washed to neutrality,
It is dried through vacuum filter, 135 DEG C of baking oven, is broken, crossing 200 meshes, obtaining 3 finished product of embodiment.
Embodiment 4
A kind of preparation method of the mesoporous nano material with humidity conditioning function comprising following processing step:
1) stock dispersion: being 35m by specific surface area2The kaolin and deionized water of/g is placed in ball milling according to the ratio of 7:13
Ball milling in machine crosses the processing of 300 meshes, obtains clay slurry after being milled to 300 mesh screen residues less than 0.3%；
2) hydro-thermal alkali activates: be in mass ratio 1 by clay slurry, the sodium hydroxide solution of 16mol/L and deionized water:
1.3:0.7 is poured into hydrothermal reaction kettle after mixing, reacts 5h at a temperature of 120 DEG C, is washed through vacuum filter, deionized water
To neutral, 130 DEG C of baking oven drying, alkali activation powder is obtained；
3) hydro-thermal acid etching: it is 1 that alkali is activated powder, the hydrogen chloride solution of 12mol/L and deionized water in mass ratio:
3.9:2.7 is poured into hydrothermal reaction kettle after mixing, reacts 3h at a temperature of 130 DEG C, is cooled to room temperature, is washed to neutrality,
It is dried through vacuum filter, 125 DEG C of baking oven, is broken, crossing 200 meshes, obtaining 4 finished product of embodiment.
Embodiment 5
The natural nano phyllosilicate kaolin without soda acid etching is measured respectively according to standard JC/T 2082-2011
The water adsorption and desorption curve of finished product prepared by (control sample) and above-described embodiment 1~4, specific 1 He of testing result attached drawing
Shown in attached drawing 2, as can be seen that the preparation-obtained mesoporous nano material of the present invention has excellent tune from attached drawing 1 and attached drawing 2
Wet performance.
Above-described embodiment is the preferred embodiment of the present invention, all with similar technique of the invention and made equivalence changes,
It should belong to protection category of the invention.
Claims (6)
1. a kind of preparation method of the mesoporous nano material with humidity conditioning function, it is characterised in that comprise the technical steps that:
1) stock dispersion: by natural nano layered silicate clay and deionized water according to 7:(12~15) ratio be placed in ball milling
Ball milling in machine, sieving is handled after being milled to 300 mesh screen residues less than 0.3%, obtains clay slurry；
2) hydro-thermal alkali activates: being in mass ratio 1:(0.45~2.6 by clay slurry, sodium hydroxide solution and deionized water):
(0.01~1.2) is poured into hydrothermal reaction kettle after mixing, at a temperature of 95~145 DEG C react 2~15h, through vacuum filter,
Deionized water is washed to neutral, drying, and alkali activation powder is obtained；
3) hydro-thermal acid etching: it is 1:(1.3~5.2 that alkali is activated powder, hydrogen chloride solution and deionized water in mass ratio): (1.4
~5.4) it pours into hydrothermal reaction kettle after mixing, 2~15h is reacted at a temperature of 95~145 DEG C, is cooled to room temperature, washs
Finished product is obtained through vacuum filter, drying, broken, sieving to neutrality.
2. a kind of preparation method of mesoporous nano material with humidity conditioning function according to claim 1, it is characterised in that:
One of which of the natural nano layered silicate clay in montmorillonite, kaolin and volcanic mud described in step 1).
3. a kind of preparation method of mesoporous nano material with humidity conditioning function according to claim 1, it is characterised in that:
The specific surface area of natural nano layered silicate clay described in step 1) is 20~50m2/g。
4. a kind of preparation method of mesoporous nano material with humidity conditioning function according to claim 1, it is characterised in that:
The molar concentration of sodium hydroxide solution described in step 2) is 8~16mol/L.
5. a kind of preparation method of mesoporous nano material with humidity conditioning function according to claim 1, it is characterised in that:
The molar concentration of hydrogen chloride solution described in step 2) is 8~12mol/L.
6. a kind of mesoporous nano material with humidity conditioning function is prepared by the described in any item preparation methods of Claims 1 to 5
It forms.
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| CN110627078A (en) * | 2019-10-30 | 2019-12-31 | 武汉工程大学 | Method for preparing negative electrode material by modifying biotite through lithium ion exchange method |
| CN112573531A (en) * | 2019-09-27 | 2021-03-30 | 清华大学 | Method for preparing negative active material |
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| CN104557130A (en) * | 2015-01-20 | 2015-04-29 | 中国地质大学（武汉） | Preparation method of kaolin-based mesoporous silica material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112573531A (en) * | 2019-09-27 | 2021-03-30 | 清华大学 | Method for preparing negative active material |
| CN110627078A (en) * | 2019-10-30 | 2019-12-31 | 武汉工程大学 | Method for preparing negative electrode material by modifying biotite through lithium ion exchange method |
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