CN109553113A - A kind of preparation method of calcium hydroxide/boron nitride nm composite material - Google Patents
A kind of preparation method of calcium hydroxide/boron nitride nm composite material Download PDFInfo
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- CN109553113A CN109553113A CN201811538874.7A CN201811538874A CN109553113A CN 109553113 A CN109553113 A CN 109553113A CN 201811538874 A CN201811538874 A CN 201811538874A CN 109553113 A CN109553113 A CN 109553113A
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- boron nitride
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/14—Compounds containing boron and nitrogen, phosphorus, sulfur, selenium or tellurium
- C01B35/146—Compounds containing boron and nitrogen, e.g. borazoles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/02—Oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The present invention provides a kind of preparation method of calcium hydroxide/boron nitride nm composite material.It is put into ball milling in ball grinder after hexagonal boron nitride is mixed with ammonium hydrogen carbonate, two-dimentional boron nitride powder is obtained after high-temperature process, hydroxylating boron nitride is obtained after mixing hydro-thermal process with sodium hydrate aqueous solution；After mixing, sodium hydroxide solution reaction is added dropwise in hydroxylating boron nitride and calcium chloride, obtains calcium hydroxide/boron nitride nm composite material powder after taking out reactant heat treatment.The method disclosed in the present generates calcium hydroxide nano particle in boron nitride surface in situ, make even particle distribution, prevent the reunion of calcium hydroxide particle, and boron nitride improves the mechanical performance of historical relic, make historical relic that there is fire prevention, oxidation resistant function, reaction condition is mild, have prepare it is simple, at low cost, be easy to the characteristics of industrialized mass production.
Description
Technical field
The present invention relates to field of composite material preparation more particularly to a kind of calcium hydroxide/boron nitride nm composite materials
Preparation method.
Background technique
Calcium hydroxide is common construction material, also serves as fungicide and industrial chemicals etc., in medical treatment, metallurgy, glass, is made
Paper, process hides, calcium carbide and soil improvement, water process, gas purification etc. tool have been widely used.Nano calcium hydroxide is available
In mural painting reparation, depickling is carried out to paper relics, reinforces stone cultural artifact, the application in historical relic's protection gradually receives people
Concern.
The preparation method of nano calcium hydroxide has mechanical milling method, sol-gal process, the precipitation method, ion-exchange etc..But
It is that the nano calcium hydroxide particle of mechanical milling method preparation is inhomogenous, or even cannot reach Nano grade；Sol-gal process sinks
The nano calcium hydroxide of the synthesis such as shallow lake method, ion-exchange always exists the shortcomings that easy to reunite, difficult dispersion, thus limit its
Application in historical relic's protection.Li Xuan China is in patent of invention " nano calcium hydroxide/hexagonal nanometer boron nitride composite material preparation side
Method " nano calcium hydroxide/hexagonal nanometer boron nitride composite material is synthesized in aqueous solution in (application number CN201710491654),
Calcium hydroxide particle size is small, not easy to reunite, and hexagonal boron nitride has excellent lubricity and mechanical performance, thermally conductive good, insulation,
Thermal stability is high and not oxidizable, and radiation hardness improves the mechanical performance of historical relic, and historical relic is made to have fire prevention, oxidation resistant function.
However, boron nitride chemical property is stablized, surface lacks active group, thus dispersibility in a solvent is very poor, this is limited significantly
Improvement of the boron nitride to composite property.Two-dimentional boron nitride has similar structure with graphene, as hydroxide
The carrier of calcium nano and the component part of composite material, not only influence the performance of composite material, also participate directly in
The reaction generating process of inorganic particle influences the final size of inorganic nanoparticles.Develop the system of new composite material
Preparation Method, the shortcomings that can further improving nano calcium hydroxide easy to reunite, difficult dispersion.
Summary of the invention
In order to overcome the shortcomings of that it is big that existing method prepares calcium hydroxide particle in composite material, a kind of hydroxide is proposed
Calcium/boron nitride nm composite material preparation method synthesizes calcium hydroxide nano particle in hydroxylating boron nitride surface in situ.Hydroxyl
Base can be connected to electrophilic boron atom surface by covalent bond, and hydroxylating boron nitride improves point of boron nitride in a solvent
Property is dissipated, is mixed with calcium hydroxide more uniformly, dispersion, carrying and buffer action, which effectively mention, prevents calcium hydroxide nano particle
Reunite；In calcium hydroxide synthesis process, calcium ion is adsorbed on hydroxyl, the calcium hydroxide nanoparticle size of fabricated in situ
It is small, meet the requirement in terms of historical relic reparation；In addition, the strong anti-oxidation of boron nitride, radiation hardness, thermal stability and good
Mechanical performance improves the mechanical performance of historical relic, and historical relic is made to have fire prevention, oxidation resistant function.
The present invention adopts the following technical scheme:
A kind of preparation method of calcium hydroxide/boron nitride nm composite material, includes the following steps:
(1) it is put into ball milling in ball grinder after mixing commercial hexagonal boron nitride with ammonium hydrogen carbonate, obtains two after high-temperature process
Boron nitride powder is tieed up, two-dimentional boron nitride powder is mixed with 5mmol/mL sodium hydrate aqueous solution to be added in water heating kettle, is heated to 120
DEG C, 12h is maintained, hydroxylating boron nitride is obtained；
(2) by hydroxylating boron nitride ultrasonic disperse into aqueous solution, calcium chloride is added, stirring at normal temperature is uniformly mixed subsequent
It is continuous to stir and be heated to 60-90 DEG C, sodium hydroxide solution is added dropwise into solution with the speed of 0.5-2mL/min, after being added dropwise
Continue to keep the temperature 30-60min, solution is naturally cooled into room temperature after completion of the reaction, is dried in vacuo after centrifugation washing, in protective atmosphere
400 DEG C of heat treatment 0.5-2h, obtain calcium hydroxide/boron nitride nm composite material powder.
The mass ratio of commercial hexagonal boron nitride and ammonium hydrogen carbonate in step (1) is 1: 1-1: 10, and ammonium hydrogen carbonate is in six sides
The intercalation of boron nitride edge assists ball milling stripping film layer.
Ball-milling Time in step (1) is 2-12h, revolving speed 100-400r/min.
High-temperature process temperature in step (1) is 400-700 DEG C, time 5-120min.
The concentration of two-dimentional boron nitride powder in aqueous solution in step (1) is 1-10mg/mL.
Hydroxylating boron nitride dispersion concentration in step (2) is 0.5-2mg/mL.
The concentration of calcium chloride is 3.5-18mg/mL in step (2), and the stirring at normal temperature time is 0.5-4h.
Concentration of sodium hydroxide solution is 0.4-2.3mmol/mL in step (2).
The present invention has the advantage that
(1) hydroxyl in boron nitride surface modification can greatly improve the dispersion performance of boron nitride in the solution, and be calcium
Ion provides adsorption site.
(2) calcium ion is because Electrostatic Absorption and chemisorption uniform adsorption are in the hydroxylating with dispersion and carrying effect
Boron surface is nitrogenized, is conducive to generate calcium hydroxide nano particle in boron nitride surface in situ after sodium hydroxide is added, makes particle point
Cloth is uniform, prevents the reunion of calcium hydroxide particle.
(3) strong anti-oxidation of boron nitride, radiation hardness, thermal stability and good mechanical performance, improve historical relic
Mechanical performance makes historical relic have fire prevention, oxidation resistant function.
(4) reaction condition is mild, have prepare it is simple, at low cost, be easy to the characteristics of industrialized mass production.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph that the method for the present invention prepares boron nitride material.
Fig. 2 is that the method for the present invention prepares calcium hydroxide/boron nitride nm composite material scanning electron microscope (SEM) photograph.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) ball milling 6h in ball grinder is put into after mixing the commercial hexagonal boron nitride that mass ratio is 1: 2 with ammonium hydrogen carbonate.
(2) product is put into 600 DEG C of environment, ammonium bicarbonate breaks down is gas.
(3) two-dimentional boron nitride powder is mixed with 5mmol/mL sodium hydrate aqueous solution is added in water heating kettle, heats 120 DEG C,
12h is maintained, hydroxylating boron nitride is obtained；
(4) by 100mg hydroxylating boron nitride ultrasonic disperse into 100mL aqueous solution, 666mg calcium chloride is added, room temperature stirs
2h is mixed, continues to stir and be heated to 90 DEG C after mixing.
(5) 10mmol/mL sodium hydroxide solution is added dropwise into solution with the speed of 1mL/min, subsequent continuation of insurance is added dropwise
Warm 30min.
(6) it is dried in vacuo after centrifugation washing, 400 DEG C of heat treatment 1h, obtain calcium hydroxide/graphene and receive in protective atmosphere
Nano composite material powder.
Fig. 1 includes the scanning electron microscope (SEM) photograph that the present embodiment prepares boron nitride material.
Fig. 2 includes that the present embodiment prepares calcium hydroxide/boron nitride nm composite material scanning electron microscope (SEM) photograph.
Embodiment 2
(1) ball milling 6h in ball grinder is put into after mixing the commercial hexagonal boron nitride that mass ratio is 1: 10 with ammonium hydrogen carbonate.
(2) product is put into 600 DEG C of environment, ammonium bicarbonate breaks down is gas.
(3) two-dimentional boron nitride powder is mixed with 5mmol/mL sodium hydrate aqueous solution is added in water heating kettle, heats 120 DEG C,
12h is maintained, hydroxylating boron nitride is obtained；
(4) by 100mg hydroxylating boron nitride ultrasonic disperse into 100mL aqueous solution, 666mg calcium chloride is added, room temperature stirs
2h is mixed, continues to stir and be heated to 90 DEG C after mixing.
(5) 10mmol/mL sodium hydroxide solution is added dropwise into solution with the speed of 1mL/min, subsequent continuation of insurance is added dropwise
Warm 30min.
(6) it is dried in vacuo after centrifugation washing, 400 DEG C of heat treatment 1h, obtain calcium hydroxide/graphene and receive in protective atmosphere
Nano composite material powder.
Embodiment 3
(1) ball milling 6h in ball grinder is put into after mixing the commercial hexagonal boron nitride that mass ratio is 1: 2 with ammonium hydrogen carbonate.
(2) product is put into 700 DEG C of environment, ammonium bicarbonate breaks down is gas.
(3) two-dimentional boron nitride powder is mixed with 5mmol/mL sodium hydrate aqueous solution is added in water heating kettle, heats 120 DEG C,
12h is maintained, hydroxylating boron nitride is obtained；
(4) by 100mg hydroxylating boron nitride ultrasonic disperse into 100mL aqueous solution, 666mg calcium chloride is added, room temperature stirs
2h is mixed, continues to stir and be heated to 90 DEG C after mixing.
(5) 10mmol/mL sodium hydroxide solution is added dropwise into solution with the speed of 1mL/min, subsequent continuation of insurance is added dropwise
Warm 30min.
(6) it is dried in vacuo after centrifugation washing, 400 DEG C of heat treatment 1h, obtain calcium hydroxide/graphene and receive in protective atmosphere
Nano composite material powder.
Embodiment 4
(1) ball milling 6h in ball grinder is put into after mixing the commercial hexagonal boron nitride that mass ratio is 1: 2 with ammonium hydrogen carbonate.
(2) product is put into 600 DEG C of environment, ammonium bicarbonate breaks down is gas.
(3) two-dimentional boron nitride powder is mixed with 5mmol/mL sodium hydrate aqueous solution is added in water heating kettle, heats 120 DEG C,
12h is maintained, hydroxylating boron nitride is obtained；
(4) by 100mg hydroxylating boron nitride ultrasonic disperse into 100mL aqueous solution, 666mg calcium chloride is added, room temperature stirs
1h is mixed, continues to stir and be heated to 90 DEG C after mixing.
(5) 10mmol/mL sodium hydroxide solution is added dropwise into solution with the speed of 1mL/min, subsequent continuation of insurance is added dropwise
Warm 30min.
(6) it is dried in vacuo after centrifugation washing, 400 DEG C of heat treatment 1h, obtain calcium hydroxide/graphene and receive in protective atmosphere
Nano composite material powder.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (8)
1. a kind of preparation method of calcium hydroxide/boron nitride nm composite material, includes the following steps:
(1) it is put into ball milling in ball grinder after mixing commercial hexagonal boron nitride with ammonium hydrogen carbonate, two-dimentional nitrogen is obtained after high-temperature process
Change boron powder, two-dimentional boron nitride powder is mixed with 5mmol/mL sodium hydrate aqueous solution to be added in water heating kettle, 120 DEG C are heated to,
12h is maintained, hydroxylating boron nitride is obtained；
(2) by hydroxylating boron nitride ultrasonic disperse into aqueous solution, calcium chloride is added, stirring at normal temperature continues to stir after mixing
It mixes and is heated to 60-90 DEG C, sodium hydroxide solution is added dropwise into solution with the speed of 0.5-2mL/min, is continued after being added dropwise
30-60min is kept the temperature, solution is naturally cooled into room temperature after completion of the reaction, is dried in vacuo after centrifugation washing, 400 in protective atmosphere
DEG C heat treatment 0.5-2h, obtain calcium hydroxide/boron nitride nm composite material powder.
2. preparation method according to claim 1, which is characterized in that commercial hexagonal boron nitride and carbonic acid in step (1)
The mass ratio of hydrogen ammonium is 1: 1-1: 10, and intercalation of the ammonium hydrogen carbonate in hexagonal boron nitride edge assists ball milling stripping film layer.
3. preparation method according to claim 1, which is characterized in that the Ball-milling Time in step (1) is 2-12h, revolving speed
For 100-400r/min.
4. preparation method according to claim 1, which is characterized in that the high-temperature process temperature in step (1) is 400-700
DEG C, time 5-120min.
5. preparation method according to claim 1, which is characterized in that the two-dimentional boron nitride powder in step (1) is water-soluble
Concentration in liquid is 1-10mg/mL.
6. preparation method according to claim 1, which is characterized in that the hydroxylating boron nitride dispersion in step (2) is dense
Degree is 0.5-2mg/mL.
7. preparation method according to claim 1, which is characterized in that the concentration of the calcium chloride in step (2) is 3.5-
18mg/mL, stirring at normal temperature time are 0.5-4h.
8. preparation method according to claim 1, which is characterized in that the concentration of sodium hydroxide solution in step (2) is
0.4-2.3mmol/mL。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919517A (en) * | 2021-03-04 | 2021-06-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Calcium oxide-doped boron nitride aerogel and preparation method and application thereof |
| CN113968688A (en) * | 2021-11-11 | 2022-01-25 | 青岛农业大学 | Modification method of recycled concrete aggregate, concrete composition and application thereof |
-
2018
- 2018-11-29 CN CN201811538874.7A patent/CN109553113A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919517A (en) * | 2021-03-04 | 2021-06-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Calcium oxide-doped boron nitride aerogel and preparation method and application thereof |
| CN113968688A (en) * | 2021-11-11 | 2022-01-25 | 青岛农业大学 | Modification method of recycled concrete aggregate, concrete composition and application thereof |
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Application publication date: 20190402 |