CN106892434A - A kind of line borate monodimension nanometer material and preparation method thereof - Google Patents
A kind of line borate monodimension nanometer material and preparation method thereof Download PDFInfo
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- CN106892434A CN106892434A CN201710308791.8A CN201710308791A CN106892434A CN 106892434 A CN106892434 A CN 106892434A CN 201710308791 A CN201710308791 A CN 201710308791A CN 106892434 A CN106892434 A CN 106892434A
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- nanometer material
- monodimension nanometer
- line borate
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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
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/126—Borates of alkaline-earth metals, beryllium, aluminium or magnesium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of line borate monodimension nanometer material and preparation method thereof.Line borate monodimension nanometer material is 2 by atomic ratio：2：5 calcium, boron, oxygen composition, its width is 200 800 rans, and length is 10 20 microns.Be added dropwise to one of which in another solution under agitation for water-soluble Ca salt and borax first are each configured into solution by method.It is subsequently adding a certain amount of water-soluble alkali.Gained suspension is transferred in hydrothermal reaction kettle, and confined reaction at least 1 24h, obtains product at being placed in 120 280 DEG C, after carrying out separation of solid and liquid, washing and dry treatment successively to product, purpose product is obtained.
Description
Technical field
The present invention relates to nanofiber field, especially a kind of line borate monodimension nanometer material and preparation method thereof.
Background technology
Line borate is a kind of important industrial chemicals, is mainly widely used in optical material, ceramics, glass, lubricant, anti-
Rotten agent, anti-wear agent, fire retardant, etc. field.Binary biborate (CaOB can be divided into chemical constitution line borate2O3·
nH2O), binary tetraboric acid, the borate (2CaO3B of quaternary six2O3·nH2O), borate (CaO3B of binary six2O3·
nH2O), they exist generally in the form of the compound containing the crystallization water.In recent years, due to thing that one-dimensional boric acid calcium material is excellent
Physicochemical property, causes the interest of increasing researcher, and part researcher has carried out wet method and prepared line borate nanometer material
The research of material.As patent CN105821476A discloses the gentle of a kind of hydration of high length-diameter ratio and ABA calcium nano whisker
Hydro-thermal-thermal transition synthetic method, they are first by inorganic calcium compound and boron-containing compound in 40-70oMix under C, Ran Hou
50-90oInorganic base is added under conditions of C, (OH) containing Ca is obtained2Predecessor slurries.Products therefrom is placed in autoclave again
In carry out hydro-thermal reaction 2-18h, be washed out product and obtain final products.First step described in the method and second
What is obtained after step is both needed to carry out in a heated condition, and first step calcium compound mixes with boron compound is settled solution.
And it is Ca (OH) in its hydro-thermal forerunner's reaction solution2.For comparing, process is more complicated, and needs to add in material mixed process
Heat, is not suitable for the cost control in large-scale production.Therefore the boron of simple, the economic extensive homogeneous yardstick of method synthesis is developed
The technology of silicate nanometer material has very strong market value.
The content of the invention
The technical problem to be solved in the present invention is to overcome weak point of the prior art, there is provided a kind of structure is single, chi
Very little narrowly distributing, the line borate monodimension nanometer material of stable performance.
The invention solves the problems that another technical problem be that a kind of preparation side of above-mentioned line borate monodimension nanometer material is provided
Method.
A kind of line borate monodimension nanometer material, is made up of calcium, boron, oxygen, it is characterised in that：
The strontium, boron, the atomic ratio of oxygen are 2：2：5.
Described line borate monodimension nanometer material, it is characterised in that：
Its pattern is one dimension fibre shape.
Described line borate monodimension nanometer material, it is characterised in that：Its width is 200-800 nanometers, and length is that 10-20 is micro-
Rice.
The preparation method of the line borate monodimension nanometer material, it is characterised in that comprise the following steps：
Step 1, be in molar ratio according to the boric acid sodium water solution of 0.1-0.5mol/L and the calcium saline solution of 0.5-3mol/L first
1：The ratio of 1-5, boric acid sodium water solution or calcium saline solution are added dropwise in the other side's solution under stirring, obtain white suspension
Liquid；Wherein, the calcium salt in calcium saline solution is calcium chloride or calcium nitrate or calcium acetate；
Step 2, first by NaOH or potassium hydroxide or ammoniacal liquor or sodium carbonate with the mol ratio with boron be 4-10:1 ratio is thrown
Enter in suspension, then confined reaction at least 1-24h at mixed liquor is placed in into 120-280 DEG C, obtain reaction solution, to reaction solution according to
It is secondary carry out separation of solid and liquid, washing and dry treatment after, line borate monodimension nanometer material is obtained.
The preparation method of described line borate monodimension nanometer material, it is characterised in that the water for using is deionized water, or is steamed
Distilled water.
The preparation method of described line borate monodimension nanometer material, it is characterised in that to suspension and the solid-liquid of reaction solution
Separating treatment is centrifugation or is separated by filtration, and rotating speed during centrifugation is 2000-10000r/min, the time is 2-
30min。
The preparation method of described line borate monodimension nanometer material, it is characterised in that step（2）Described carrying out washing treatment refers to
Be to carry out the cleaning of 2-5 times to isolated solid using deionized water, it is centrifugation that solid is separated during cleaning
Or be separated by filtration.
The preparation method of described line borate monodimension nanometer material, it is characterised in that step（2）Described dried process is equal
It is that the solid after cleaning is placed at 20-85 DEG C to dry or dry.
Beneficial effect relative to prior art is：
First, obtained purpose product is characterized using X-ray diffractometer and ESEM respectively, from its result,
Purpose product is made up of calcium, boron, oxygen, and calcium, boron, the atomic ratio of oxygen are 2：2：5；The pattern of purpose product is threadiness, and width is
200-800 rans, length is 10-20 microns.This is 2 by atomic ratio：2：5 calcium, boron, the purpose product of oxygen composition,
Both larger advantage was provided with illumination field, and because its pattern is one dimension fibre shape, and it is extremely easy to as reinforcing material
Use.
Second, preparation method science, efficiently.Not only it has been obtained rational in infrastructure, it is adaptable to which the purpose of illumination field is produced
Thing --- line borate monodimension nanometer material, more there is that the reaction time is short.Particular, it is important that preparing purpose product
When, amorphous phase line borate particle is first obtained, then hydro-thermal method is used for, process is simple is suitable for mass production.
Brief description of the drawings
Fig. 1 is to use X-ray diffraction to obtained purpose product（XRD）The result that instrument is characterized, as shown in Figure 1, mesh
Product by Ca2B2O5·H2O is constituted；
Fig. 2 is the result characterized using ESEM to obtained purpose product, and as shown in Figure 2, purpose product is by a large amount of
Width is 200-800 rans in width, and length is constituted for 10-20 microns of fiber.
Specific embodiment
Preferred embodiment of the invention is described in further detail below in conjunction with the accompanying drawings.
Bought from market first or be voluntarily obtained：
Boric acid sodium water solution；
As the calcium chloride of calcium salt, calcium nitrate and calcium acetate；
As the deionized water and distilled water of water；
As the NaOH or potassium hydroxide or ammoniacal liquor or sodium carbonate of mineralizer.
Then,
Embodiment 1
What is prepared concretely comprises the following steps：
Step 1, is first in molar ratio 1 according to the boric acid sodium water solution of 0.1mol/L and the calcium chloride water of 0.5mol/L：2
Ratio, boric acid sodium water solution is added dropwise in the calcium chloride water under stirring, obtains white suspension；
Step 2, with the mol ratio with boron is 2 by NaOH:1 ratio is put into suspension, then mixed liquor is placed in into 150
Confined reaction at least 6h, obtains reaction solution at DEG C, after carrying out separation of solid and liquid, washing and dry treatment successively to reaction solution, system
Obtain line borate monodimension nanometer material.
Embodiment 2
What is prepared concretely comprises the following steps：
Step 1, is first in molar ratio 1 according to the boric acid sodium water solution of 0.2mol/L and the calcium nitrate aqueous solution of 1mol/L：3 ratio
Example, calcium nitrate is added dropwise in the lower boric acid sodium water solution of stirring, obtains white suspension；
Step 2, with the mol ratio with boron is first 6 by potassium hydroxide:1 ratio is put into suspension, then mixed liquor is placed in
Confined reaction at least 2h, obtains reaction solution at 180 DEG C, after carrying out separation of solid and liquid, washing and dry treatment successively to reaction solution,
Line borate monodimension nanometer material is obtained.
Embodiment 3
What is prepared concretely comprises the following steps：
Step 1, is first in molar ratio 1 according to the boric acid sodium water solution of 0.3mol/L and the calcium acetate aqueous solution of 1.5mol/L：4
Ratio, boric acid sodium water solution is added dropwise in the calcium acetate aqueous solution under stirring, obtains white suspension；
Step 2, with the mol ratio with boron is 8 by ammoniacal liquor:1 ratio is put into suspension, then mixed liquor is placed at 200 DEG C
Confined reaction at least 24h, obtains reaction solution, after carrying out separation of solid and liquid, washing and dry treatment successively to reaction solution, boron is obtained
Sour calcium monodimension nanometer material.
Embodiment 4
What is prepared concretely comprises the following steps：
Step 1, is first in molar ratio 1 according to the boric acid sodium water solution of 0.4mol/L and the calcium nitrate aqueous solution of 2mol/L：5 ratio
Example, calcium nitrate aqueous solution is added dropwise in the boric acid sodium water solution under stirring, obtains white suspension；
Step 2, with the mol ratio with boron is 10 by potassium hydroxide:1 ratio is put into suspension, then mixed liquor is placed in
Confined reaction at least 24h, obtains reaction solution at 240 DEG C, carries out separation of solid and liquid, washing and dry treatment successively to reaction solution
Afterwards, line borate monodimension nanometer material is obtained.
Embodiment 5
What is prepared concretely comprises the following steps：
Step 1, is first in molar ratio 1 according to the boric acid sodium water solution of 0.5mol/L and the calcium chloride water of 2.5mol/L：4
Ratio, boric acid sodium water solution is added dropwise in the calcium chloride water under stirring, obtains white suspension；
Step 2, with the mol ratio with boron is 6 by sodium carbonate:1 ratio is put into suspension, then mixed liquor is placed in into 280 DEG C
Lower confined reaction at least 12h, obtains reaction solution, after carrying out separation of solid and liquid, washing and dry treatment successively to reaction solution, is obtained
Line borate monodimension nanometer material.
Obviously, those skilled in the art can be carried out to line borate 1-dimention nano fiber of the invention and preparation method thereof
Various changes and modification are without departing from the spirit and scope of the present invention.So, if to these modifications of the invention and modification category
Within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to comprising these changes and modification.
Claims (8)
1. a kind of line borate monodimension nanometer material, is made up of calcium, boron, oxygen, it is characterised in that：
The strontium, boron, the atomic ratio of oxygen are 2：2：5.
2. line borate monodimension nanometer material according to claim 1, it is characterised in that：
Its pattern is one dimension fibre shape.
3. line borate monodimension nanometer material according to claim 2, it is characterised in that：Its width is 200-800 nanometers, long
Spend is 10-20 microns.
4. a kind of preparation method of line borate monodimension nanometer material as claimed in claim 1, it is characterised in that including following step
Suddenly：
Step 1, be in molar ratio according to the boric acid sodium water solution of 0.1-0.5mol/L and the calcium saline solution of 0.5-3mol/L first
1：The ratio of 1-5, boric acid sodium water solution or calcium saline solution are added dropwise in the other side's solution under stirring, obtain white suspension
Liquid；Wherein, the calcium salt in calcium saline solution is calcium chloride or calcium nitrate or calcium acetate；
Step 2, first by NaOH or potassium hydroxide or ammoniacal liquor or sodium carbonate with the mol ratio with boron be 4-10:1 ratio is thrown
Enter in suspension, then confined reaction at least 1-24h at mixed liquor is placed in into 120-280 DEG C, obtain reaction solution, to reaction solution according to
It is secondary carry out separation of solid and liquid, washing and dry treatment after, line borate monodimension nanometer material is obtained.
5. the preparation method of line borate monodimension nanometer material according to claim 4, it is characterised in that the water for using is to go
Ionized water, or distilled water.
6. the preparation method of line borate monodimension nanometer material according to claim 4, it is characterised in that to suspension and anti-
Answer liquid separation of solid and liquid process be centrifugation or be separated by filtration, rotating speed during centrifugation be 2000-10000r/min, when
Between be 2-30min.
7. the preparation method of line borate monodimension nanometer material according to claim 4, it is characterised in that step（2）It is described
Carrying out washing treatment refer to carrying out isolated solid using deionized water the cleaning of 2-5 times, solid-state is separated during cleaning
Thing is centrifugation or is separated by filtration.
8. the preparation method of line borate monodimension nanometer material according to claim 4, it is characterised in that step（2）It is described
Dried process be to be placed in the solid after cleaning at 20-85 DEG C and dry or dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710308791.8A CN106892434A (en) | 2017-05-04 | 2017-05-04 | A kind of line borate monodimension nanometer material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710308791.8A CN106892434A (en) | 2017-05-04 | 2017-05-04 | A kind of line borate monodimension nanometer material and preparation method thereof |
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| CN106892434A true CN106892434A (en) | 2017-06-27 |
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| CN201710308791.8A Pending CN106892434A (en) | 2017-05-04 | 2017-05-04 | A kind of line borate monodimension nanometer material and preparation method thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105821476A (en) * | 2016-05-09 | 2016-08-03 | 曲阜师范大学 | Mild hydrothermal-thermal transition synthetic method for high-draw-ratio hydrated and anhydrous calcium borate nanowhisker |
-
2017
- 2017-05-04 CN CN201710308791.8A patent/CN106892434A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105821476A (en) * | 2016-05-09 | 2016-08-03 | 曲阜师范大学 | Mild hydrothermal-thermal transition synthetic method for high-draw-ratio hydrated and anhydrous calcium borate nanowhisker |
Non-Patent Citations (1)
| Title |
|---|
| LI YANG ETAL: "Hydrothermal synthesis, characterization, and luminescence of Ca2B2O5:RE (RE = Eu3+, Tb3+, Dy3+) nanofibers", 《JOURNAL OF NANOPARTICLE RESEARCH》 * |
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Application publication date: 20170627 |
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