CN114132903A - Preparation method of hydrophilic nano boron nitride - Google Patents
Preparation method of hydrophilic nano boron nitride Download PDFInfo
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- CN114132903A CN114132903A CN202110024714.6A CN202110024714A CN114132903A CN 114132903 A CN114132903 A CN 114132903A CN 202110024714 A CN202110024714 A CN 202110024714A CN 114132903 A CN114132903 A CN 114132903A
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- boron nitride
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- hydrophilic nano
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
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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
Abstract
The invention discloses a hydrophilic nano boron nitride and a preparation method thereof, and the preparation method comprises the following steps: adding nano boron nitride into hydrogen peroxide, stirring uniformly, slowly adding a certain amount of concentrated sulfuric acid, stirring uniformly, continuing stirring for a period of time, after a material body is cooled, carrying out vacuum filtration, washing with deionized water until the pH value of filtrate is more than 6.0, putting a filter cake into an oven, drying until the water content is less than 1%, cooling and crushing to obtain the hydrophilic nano boron nitride. According to the invention, nano boron nitride is added into hydrogen peroxide, a certain amount of concentrated sulfuric acid is added, the stirring is uniform, the concentrated sulfuric acid absorbs water and releases heat, the decomposition of hydrogen peroxide is aggravated, and the function of an auxiliary oxidant is achieved, so that-OH hydroxyl groups are grafted on the surface of the nano boron nitride, then the nano boron nitride is cooled, filtered, washed by deionized water until the pH value of filtrate is greater than 6.0, dried by an oven until the water content is less than 1%, and then the nano boron nitride is crushed after cooling, so that the hydrophilic nano boron nitride is obtained.
Description
Technical Field
The invention relates to the technical field of nano boron chloride, in particular to a preparation method of hydrophilic nano boron nitride suitable for the field of cosmetics.
Background
Hexagonal boron nitride (h-BN) is an isomer of boron nitride, which has a structure similar to graphite, a hexagonal layered structure, a soft texture, a strong workability, and a white color, and is commonly called "white graphite".
The nanometer boron nitride has small grain size, large specific surface area, high surface activity, excellent dry lubrication capacity and extremely stable chemical property. The titanium dioxide particles containing nanostructured boron nitride are a perfect combination and added to sunscreen cream to protect human body from ultraviolet and infrared radiation of the sun. The nano boron nitride can also reduce the gloss of oily skin due to its high thermal conductivity.
Pure hexagonal boron nitride is mainly hydrophobic, and due to the interaction force existing among the nano particles, the surfactant cannot completely disperse the nano boron nitride in water, so that the use of the nano boron nitride is limited.
Disclosure of Invention
The invention aims to provide a preparation method of hydrophilic nano boron nitride, which can completely disperse the nano boron nitride in water.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of hydrophilic nano boron nitride comprises the following steps:
s1, adding the nano boron nitride into hydrogen peroxide, and stirring uniformly;
s2, adding concentrated sulfuric acid into the mixed solution obtained in the step S1 while stirring, and continuing stirring after uniformly stirring;
s3, cooling the mixed material to room temperature in the step S2, performing vacuum filtration, and washing with deionized water until the pH value of the filtrate is greater than 6.0;
and S4, taking the filter cake obtained in the step S3, putting the filter cake into an oven for drying, taking out the filter cake, cooling the filter cake to room temperature, and crushing the filter cake to obtain the hydrophilic nano boron nitride.
Preferably, the nano boron nitride is in a hexagonal crystal structure.
Preferably, the adding mass ratio of the nano boron nitride to the hydrogen peroxide in the step S1 is 1: 5-10.
Preferably, the mass ratio of the concentrated sulfuric acid to the S1 mixed solution in the step S2 is 1: 20-50
Preferably, in the step S2, concentrated sulfuric acid is added into the mixed solution while stirring, the mixed solution is uniformly stirred, and the stirring is continued for 1 to 3 hours;
preferably, the water content of the filter cake in the step S3 after the filter cake is dried in a drying oven is less than 1%.
Preferably, in the step S3, after the mixture body of the step S2 is cooled to room temperature, the mixture body is filtered by vacuum filtration and then washed by deionized water until the pH of the filtrate is more than 6.0.
According to the invention, nano boron nitride is added into hydrogen peroxide, a certain amount of concentrated sulfuric acid is added, the stirring is uniform, the concentrated sulfuric acid absorbs water and releases heat, the decomposition of hydrogen peroxide is aggravated, and the function of an auxiliary oxidant is achieved, so that-OH hydroxyl groups are grafted on the surface of the nano boron nitride, then the nano boron nitride is cooled, filtered, washed by deionized water until the pH value of filtrate is greater than 6.0, dried by an oven until the water content is less than 1%, and then the nano boron nitride is crushed after cooling, so that the hydrophilic nano boron nitride is obtained.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
The invention provides a preparation method of hydrophilic nano boron nitride, which comprises the following steps:
s1, adding nano boron nitride into hydrogen peroxide, wherein the adding mass ratio of the nano boron nitride to the hydrogen peroxide is 1: 5-10, and uniformly stirring;
s2, adding concentrated sulfuric acid into the mixed liquid obtained in the step S1 while stirring, wherein the mass ratio of the concentrated sulfuric acid to the mixed liquid obtained in the step S1 is 1: 20-50, and stirring for 1-3 hours after uniform stirring;
s3, cooling the mixed material to room temperature in the step S2, performing vacuum filtration, and washing with deionized water until the pH value of the filtrate is greater than 6.0;
and S4, taking the filter cake obtained in the step S3, putting the filter cake into an oven for drying, taking the filter cake out, cooling the filter cake to room temperature, and crushing the filter cake to obtain the hydrophilic nano boron nitride.
Furthermore, the nano boron nitride adopted by the invention is in a hexagonal crystal structure.
The invention is further detailed by the following experimental parameters:
example one
S1, adding 10g of nano boron nitride into 100g of hydrogen peroxide, and uniformly stirring;
s2, adding 5g of concentrated sulfuric acid into the mixed solution obtained in the step S1 while stirring, uniformly stirring, and continuously stirring for 1 hour;
s3, cooling the mixed material to room temperature in the step S2, performing vacuum filtration, and washing with deionized water until the pH of the filtrate is 6.7;
s4, taking the filter cake obtained in the step S3, putting the filter cake into a drying oven at 110 ℃ for drying for 3h, taking out the filter cake, cooling the filter cake to room temperature, and crushing the filter cake to obtain the hydrophilic nano boron nitride.
Example two
S1, adding 5g of nano boron nitride into 100g of hydrogen peroxide, and uniformly stirring;
s2, adding 3g of concentrated sulfuric acid into the mixed solution obtained in the step S1 while stirring, uniformly stirring, and continuously stirring for 2 hours;
s3, cooling the mixed material to room temperature in the step S2, performing vacuum filtration, and washing with deionized water until the pH of the filtrate is 7.0;
s4, taking the filter cake obtained in the step S3, putting the filter cake into a drying oven at 110 ℃ for drying for 3h, taking out the filter cake, cooling the filter cake to room temperature, and crushing the filter cake to obtain the hydrophilic nano boron nitride.
Example three
S1, adding 7g of nano boron nitride into 100g of hydrogen peroxide, and uniformly stirring;
s2, adding 3g of concentrated sulfuric acid into the mixed solution obtained in the step S1 while stirring, uniformly stirring, and continuously stirring for 3 hours;
s3, cooling the mixed material to room temperature in the step S2, performing vacuum filtration, and washing with deionized water until the pH of the filtrate is 7.3;
s4, taking the filter cake obtained in the step S3, putting the filter cake into a drying oven at 110 ℃ for drying for 3h, taking out the filter cake, cooling the filter cake to room temperature, and crushing the filter cake to obtain the hydrophilic nano boron nitride.
According to the invention, nano boron nitride is added into hydrogen peroxide, a certain amount of concentrated sulfuric acid is added, the stirring is uniform, the concentrated sulfuric acid absorbs water and releases heat, the decomposition of hydrogen peroxide is aggravated, and the function of an auxiliary oxidant is achieved, so that-OH hydroxyl groups are grafted on the surface of the nano boron nitride, then the nano boron nitride is cooled, filtered, washed by deionized water until the pH value of filtrate is greater than 6.0, dried by an oven until the water content is less than 1%, and then the nano boron nitride is crushed after cooling, so that the hydrophilic nano boron nitride is obtained.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A preparation method of hydrophilic nano boron nitride is characterized by comprising the following steps:
s1, adding the nano boron nitride into hydrogen peroxide, and stirring uniformly;
s2, adding concentrated sulfuric acid into the mixed solution obtained in the step S1 while stirring, and continuing stirring after uniformly stirring;
s3, cooling the mixed material to room temperature in the step S2, performing vacuum filtration, and washing with deionized water until the pH value of the filtrate is greater than 6.0;
and S4, taking the filter cake obtained in the step S3, putting the filter cake into an oven for drying, taking out the filter cake, cooling the filter cake to room temperature, and crushing the filter cake to obtain the hydrophilic nano boron nitride.
2. The hydrophilic nano boron nitride and the preparation method thereof according to claim 1, wherein the hydrophilic nano boron nitride is prepared by the following steps: the nanometer boron nitride is in a hexagonal crystal structure.
3. The hydrophilic nano boron nitride and the preparation method thereof according to claim 1, wherein the hydrophilic nano boron nitride is prepared by the following steps: in the step S1, the adding mass ratio of the nano boron nitride to the hydrogen peroxide is 1: 5-10.
4. The hydrophilic nano boron nitride and the preparation method thereof according to claim 1, wherein the hydrophilic nano boron nitride is prepared by the following steps: the mass ratio of the concentrated sulfuric acid to the S1 mixed solution in the step S2 is 1: 20-50.
5. The hydrophilic nano boron nitride and the preparation method thereof according to any one of claims 1 or 4, wherein: and S2, adding concentrated sulfuric acid into the mixed solution while stirring, uniformly stirring, and continuously stirring for 1-3 h.
6. The hydrophilic nano boron nitride and the preparation method thereof according to claim 1, wherein the hydrophilic nano boron nitride is prepared by the following steps: and in the step S3, the water content of the filter cake after being dried in the drying oven is less than 1%.
7. The hydrophilic nano boron nitride and the preparation method thereof according to any one of claims 1 or 6, wherein: and in the step S3, after the mixed material in the step S2 is cooled to room temperature, carrying out vacuum filtration, and then washing with deionized water until the pH of the filtrate is more than 6.0.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115887248A (en) * | 2022-12-26 | 2023-04-04 | 广州联锴粉体科技有限公司 | Sunscreen product containing modified hexagonal boron nitride and preparation method thereof |
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| JP2011102203A (en) * | 2009-11-10 | 2011-05-26 | Teijin Ltd | Boron nitride nanotube derivative, its dispersion, and method for producing the boron nitride nanotube derivative |
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| CN106395768A (en) * | 2016-11-01 | 2017-02-15 | 吉林大学 | Ultrathin boron nitride nanosheet synthesis method |
| CN107151002A (en) * | 2017-07-18 | 2017-09-12 | 深圳市泽纬科技有限公司 | A kind of method that individual layer or few layer boron nitride nanosheet are prepared by intercalator of the concentrated sulfuric acid |
| CN109338762A (en) * | 2018-08-28 | 2019-02-15 | 苏州印丝特纺织数码科技有限公司 | A kind of preparation method of the digit printing ink modified based on boron nitride nanosheet |
| CN109455682A (en) * | 2018-12-17 | 2019-03-12 | 盐城师范学院 | A kind of preparation method of boron nitride-graphene film |
| CN111170289A (en) * | 2020-03-13 | 2020-05-19 | 泉州师范学院 | Method for large-scale preparation of hydrophobic hexagonal boron nitride nanosheets |
-
2021
- 2021-01-08 CN CN202110024714.6A patent/CN114132903A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030039604A1 (en) * | 2001-05-18 | 2003-02-27 | Chunming Niu | Modification of nanotubes oxidation with peroxygen compounds |
| CN101715611A (en) * | 2007-05-28 | 2010-05-26 | 塞拉姆氢技术公司 | Method of activating boron nitride |
| JP2011102203A (en) * | 2009-11-10 | 2011-05-26 | Teijin Ltd | Boron nitride nanotube derivative, its dispersion, and method for producing the boron nitride nanotube derivative |
| CN105982823A (en) * | 2016-04-20 | 2016-10-05 | 江西联锴新材料有限公司 | Aqueous-dispersible boron nitride powder for cosmetics and preparation method thereof |
| CN106395768A (en) * | 2016-11-01 | 2017-02-15 | 吉林大学 | Ultrathin boron nitride nanosheet synthesis method |
| CN107151002A (en) * | 2017-07-18 | 2017-09-12 | 深圳市泽纬科技有限公司 | A kind of method that individual layer or few layer boron nitride nanosheet are prepared by intercalator of the concentrated sulfuric acid |
| CN109338762A (en) * | 2018-08-28 | 2019-02-15 | 苏州印丝特纺织数码科技有限公司 | A kind of preparation method of the digit printing ink modified based on boron nitride nanosheet |
| CN109455682A (en) * | 2018-12-17 | 2019-03-12 | 盐城师范学院 | A kind of preparation method of boron nitride-graphene film |
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| CN115887248A (en) * | 2022-12-26 | 2023-04-04 | 广州联锴粉体科技有限公司 | Sunscreen product containing modified hexagonal boron nitride and preparation method thereof |
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