CN109133942A - A kind of preparation method of the active nitride boron fibre of high-specific surface area - Google Patents
A kind of preparation method of the active nitride boron fibre of high-specific surface area Download PDFInfo
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Abstract
The present invention is a kind of preparation method of the active nitride boron fibre of high-specific surface area.This method is using melamine and boric acid as raw material, using hexamethylenetetramine as surfactant, is prepared for active nitride boron fibre with three-step approach.The active nitride boron fibre of preparation has of uniform size, has good draw ratio, and crystallization degree is low, surface defect is more, containing various active functional group, simultaneously, active nitride boron fibre has very high specific surface area and Kong Rong, provides higher adsorption capacity for its absorption property.This method is simple and easy, and raw material is cheap and easy to get, nontoxic, and product specific surface area is stablized, and shows excellent performance in terms of absorption organic dyestuff, metal ion and greenhouse gases.
Description
Technical field
The present invention relates to adsorbing domain, the method for the active porous boron nitride fiber of specially a kind of high-specific surface area.
Background technique
Boron nitride (BN) is a kind of important ceramic material, is referred to as because it has hexagonal structure identical with graphite
" white graphite ".The excellent properties of boron nitride material include extreme hardness, and dielectric constant is low, and high mechanical strength, low-density is big, are melted
Point is high, good corrosion resistance and inoxidizability, therefore boron nitride is in manufacture refractory material, lubricating oil, protection and optical coating, cutting
Tool, grinding-material, ceramic composite, electronic equipment and electric insulator etc. have huge potentiality.Boron nitride is received
Rice material mainly includes boron nitride nanometer ball, boron nitride nanosheet, boron nitride nano-tube and boron nitride fiber.
Nitride porous boron fibre is a kind of novel porous materials, internal by being mutually communicated or closed hole is constituted, and is had
High-specific surface area and cellular structure abundant, while stable chemical performance, thermal conductivity are high, insulation performance is good, and have hydrophobic
Characteristic.In addition, nitride porous boron material have special hydrogenation property and adsorption selectivity, hydrogen storage, gas absorption and
Separation field has very big application potential.Therefore the purity, specific surface area of nitride porous boron material, pore-size distribution, surface lack
It falls into and number of functional groups has important influence to the hydrogen storage of boron nitride material, absorption and separating property.Active boron nitride goes out
Further increase hydrogen storage, absorption and the separating property of porous boron nitride, the method for activating activities boron nitride is main at present
Have: in-situ chemical activation method, strong acid assistant chemical activation method and highly basic assistant chemical activation method；In-situ chemical activation method is mainly
Boron nitride fiber presoma is handled using activating agent, to improve the specific surface area of boron nitride fiber.It has been reported that at present
Method be to be added in two melamine solution of boric acid preparation active boron nitride presoma using P123 as surfactant, then
Active nitride boron fibre is formed in pyrolysis, but uses P123 expensive as activating agent, and the introducing of P123 is so that system
Standby active nitride boron fibre contains a large amount of impurities, and causes its chemical stability and high-temperature stability poor；Synthesis temperature is up to
1460 DEG C, energy consumption is larger.Therefore the method is not suitable for industrial mass production.The activation of strong acid and strong base assistant chemical
Method mainly activates nitride porous boron fibre using strong acid or highly basic as activator, to prepare stable chemical performance, inhales
Attached active sites active nitride boron fibre abundant；But the production for the active boron nitride for using strong acid or highly basic to obtain as activating agent
It measures very low.Therefore the method is not suitable for large scale preparation active boron nitride yet.
Summary of the invention
It is an object of the present invention to provide a kind of active nitrogen for preparing high-specific surface area for deficiency present in current techniques
Change the method for boron fibre.This method is firstly introduced hexamethylenetetramine and comes as surfactant processing porous boron nitride presoma
Active nitride boron fibre is prepared, synthesis method is simple, compared with introducing P123 as surfactant, hexamethylenetetramine price
It is cheap, and properties of product are stablized, and preparation repetitive rate is high, is suitble to industrial mass production, and the active nitride boron fibre is being inhaled
Excellent performance is shown in terms of attached organic dyestuff, metal ion and greenhouse gases.This method is simple and easy, and raw material is inexpensively easy
, nontoxic, product specific surface area is stablized.
The present invention solves technical solution used by the technical problem:
A kind of preparation method of the active nitride boron fibre of high-specific surface area, it is characterized in that the following steps are included:
(1) melamine and boric acid are put into the container for filling deionized water, are then put it into water-bath, water-bath
Temperature range is 70~90 DEG C, and stirring obtains clear transparent solutions；
Wherein, the concentration of melamine is 0.1~0.2mol/L, and boric acid concentration is 0.2~0.4mol/L；Molar ratio trimerization
Cyanamide: boric acid=1:2；
(2) hexamethylenetetramine is added in the solution that step (1) obtains, continues to stir, then react 20~40min,
Obtain clear solution；Wherein, molar ratio is melamine: hexamethylenetetramine=6:1~2；
(3) clear solution that step (2) obtains is naturally cooling to 40 DEG C, and keeps 9~13h, it is heavy to obtain white flock
It forms sediment；
(4) mixed solution obtained in step (3) is filtered, obtains white solid；
(5) white solid obtained in step (4) is dried at 40~80 DEG C 360~720min, obtains white fiber
Shape substance, as presoma；
(6) under a nitrogen by presoma obtained in step (5), 1100 DEG C of 4~6h of heat preservation, the active nitride of high specific area
Boron fibre.
Nitrogen flow maintains 60mL/min~100mL/min in the step (6).
Substantive distinguishing features of the invention are as follows:
The present invention is synthesized using three-step approach: the first step will mix according to a certain percentage containing boron source with the compound of nitrogen source
Form clear solution；Second step is added a certain amount of hexamethylenetetramine and is mixed to form clear solution, later in precursor solution
During crystallisation by cooling, hexamethylenetetramine enters in precursor fibre as surfactant doping, so that presoma is fine
The activity of dimension is enhanced, meanwhile, hexamethylenetetramine is also a kind of foaming agent, in high-temperature burning process, six methines four
Amine is generated gas by thermal decomposition, to increase the hole content of boron nitride fiber；Third step, by synthesized presoma in inertia
It is calcined under gas shield, finally obtains the active boron nitride fiber product of high-specific surface area.
The beneficial effects of the present invention are:
1. the length for the active nitride boron fibre that the method for the present invention obtains is 80~100 μm, diameter is 7~10 μm,
The fibre structure of even size and good draw ratio.
2. obtained active nitride boron fibre purity with higher of the invention and lower crystallization degree.Fiber table
The defect in face is more, adsorbs other substances for it and provides sufficient adsorption position, and active function groups are compared with horn of plenty, because
This, adsorption activity with higher.
3. the specific surface area for the active nitride boron fibre that the present invention obtains is up to 1448m2/ g, total pore volume are up to 0.761cm3/
G makes it have higher adsorption capacity.
4. the raw material that the present invention uses is boric acid, melamine and hexamethylenetetramine are cheap and easy to get, and synthetic method letter
Single, the cost performance for being used to prepare the active nitride boron fibre of high-specific surface area is very high, can be realized large-scale production.
5. the active nitride boron fibre that the present invention obtains shows in terms of absorption organic dyestuff, metal ion and greenhouse gases
Excellent performance out.Wherein to CO at 273K, normal pressure2Adsorbance be up to 62cm3/ g has very in gas absorption application aspect
Big development prospect.
Detailed description of the invention
The present invention is further described with specific implementation with reference to the accompanying drawing.
Fig. 1 is the XRD spectra of active nitride boron fibre in example 1.
Fig. 2 is the SEM picture of active boron nitride Precursors of Fibers in example 1.
Fig. 3 is the SEM picture of active nitride boron fibre in example 1.
Fig. 4 is the TEM picture of active nitride boron fibre in example 1.
Fig. 5 is nitrogen adsorption-desorption curve of the active nitride boron fibre in example 1.
Fig. 6 is the graph of pore diameter distribution of the active nitride boron fibre in example 1.
Fig. 7 is the FTIR curve of the active nitride boron fibre in example 1.
Fig. 8 is the CO of the active nitride boron fibre in example 12Adsorption curve.
Specific embodiment
Embodiment 1
(1) 0.06mol boric acid and 0.03mol melamine are put into the beaker for filling 200mL deionized water, then will
It is put into water-bath, and bath temperature is 85 DEG C, is stirred continuously, obtains clear transparent solutions；
(2) hexamethylenetetramine 0.005mol is added in the clear solution that step (1) obtains, continues to stir, reacts
30min；
(3) clear solution that step (2) obtains is naturally cooling to 40 DEG C, and keeps 11h, obtain white flock precipitate；
(4) mixed solution obtained in step (3) is filtered, obtains white pigmented samples；
(5) sample obtained in baking step (4), drying temperature section are 40 DEG C (time 360min), obtain white
Fibre-like sample, as presoma；
(6) sample obtained in step (5) is heat-treated in nitrogen stream, heat treatment temperature is 1100 DEG C of (nitrogen flows
Maintain 100mL/min), 4h is kept the temperature, white lightweight sample, as the active nitride boron fibre of high specific area are obtained.
Fig. 1 is the XRD spectra of prepared active nitride boron fibre in embodiment 1, and the diffraction maximum of all indexings shows this
Product is hexagonal boron nitride, and diffraction maximum is weaker, illustrates that the crystallinity of active nitride boron fibre is lower, and without other miscellaneous phases
Diffraction maximum occur illustrate the product purity it is very high；Fig. 2 is the SEM picture of active boron nitride Precursors of Fibers in embodiment 1, should
Presoma is fibrous crystal body, and oriented crystalline is threadiness precipitating in aqueous solution.Fig. 3 is active boron nitride in embodiment 1
The SEM picture of fiber, the size of active nitride boron fibre is more uniform, and length is 80~100 μm, and diameter is 7~10 μm.Fig. 4
For the TEM picture of active nitride boron fibre in embodiment 1, wherein the rough surface of active nitride boron fibre, lacks containing a large amount of
Sunken and hole finds that the specific surface area of the active nitride boron fibre of the synthesis is up to 1448m by specific surface area analysis2/ g is (as schemed
Shown in nitrogen adsorption-desorption curve of active nitride boron fibre in 5 embodiments 1), characteristic aperture is mainly distributed on 1.15nm,
2.42nm and 3.97nm, total pore volume are up to 0.761cm3/ g (the pore-size distribution of the active nitride boron fibre in such as Fig. 6 embodiment 1
Figure).Fig. 7 show the FTIR curve of the active nitride boron fibre in example 1, and active nitride boron fibre has various active function
Organic dyestuff is adsorbed for it in group, and metal ion and greenhouse gases provide adsorption site abundant.Fig. 8 is shown in embodiment 1
Active nitride boron fibre CO2(test equipment is physical and chemical adsorption analyzer, model iQ-1900, test to adsorption curve
Condition is 273K, vacuum to normal pressure), active nitride boron fibre is under normal pressure to CO2Adsorbance be up to 62cm3/g。
Embodiment 2,3,4,5
The bath temperature of step (3) in embodiment 1 is changed to 70 DEG C, 75 DEG C, 80 DEG C and 90 DEG C respectively, other items
Operation is same as Example 1, obtains product with embodiment 1.
Embodiment 6,7,8,9
The soaking time of step (3) in embodiment 1 is changed to 9h, 10h, 12h and 13h, other operations respectively
It is same as Example 1, product is obtained with embodiment 1.
Embodiment 10,11,12,13
Drying temperature in embodiment 1 in step (5) is changed to 50 DEG C, 60 DEG C, 70 DEG C and 80 DEG C respectively, other items
Operation is same as Example 1, obtains product with embodiment 1.
Embodiment 14,15,16,17
By the nitrogen flow in embodiment 1 in step (6) be changed to respectively 60mL/min, 70mL/min, 80mL/min and
90mL/min, other operations are same as Example 1, obtain product with embodiment 1.
Embodiment 18,19
Soaking time in embodiment 1 in step (6) is changed to 5h and 6h respectively, other operations are and embodiment
1 is identical, obtains product with embodiment 1.
Unaccomplished matter of the present invention is well-known technique.
Claims (2)
1. a kind of preparation method of the active nitride boron fibre of high-specific surface area, it is characterized in that method includes the following steps:
(1) melamine and boric acid are put into the container for filling deionized water, are then put it into water-bath, bath temperature
Section is 70 ~ 90 DEG C, and stirring obtains clear transparent solutions；
Wherein, the concentration of melamine is 0.1 ~ 0.2 mol/L, and boric acid concentration is 0.2 ~ 0.4 mol/L；Molar ratio melamine
Amine: boric acid=1:2；
(2) hexamethylenetetramine is added in the solution that step (1) obtains, continues to stir, then react 20 ~ 40 min, obtain
Clear solution；Wherein, molar ratio is melamine: hexamethylenetetramine=6:1 ~ 2；
(3) clear solution that step (2) obtains is naturally cooling to 40 DEG C, and keeps 9 ~ 13 h, obtain white flock precipitate；
(4) mixed solution obtained in step (3) is filtered, obtains white solid；
(5) white solid obtained in step (4) is dried at 40 ~ 80 DEG C 360 ~ 720 min, obtains white fibrous object
Matter, as presoma；
(6) under a nitrogen by presoma obtained in step (5), 1100 DEG C of 4 ~ 6 h of heat preservation, the active boron nitride of high specific area
Fiber.
2. the preparation method of the active nitride boron fibre of high-specific surface area as described in claim 1, it is characterized in that the step
Suddenly nitrogen flow maintains the mL/min of 60 mL/min ~ 100 in (6).
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109894103A (en) * | 2019-03-01 | 2019-06-18 | 河北工业大学 | The method adsorbed carbon dioxide using conjugated polymer and boron nitride composite and monitor its slow release |
| CN110255516A (en) * | 2019-07-30 | 2019-09-20 | 河北工业大学 | A kind of synthetic method of active boron nitride nanotube |
| CN110496588A (en) * | 2019-06-20 | 2019-11-26 | 中国科学院长春应用化学研究所 | A kind of adsorption method of radioiodine |
| CN110629323A (en) * | 2019-10-14 | 2019-12-31 | 河北工业大学 | Method for synthesizing porous boron nitride fiber with high length-diameter ratio under assistance of organic solvent |
| CN111073742A (en) * | 2019-12-23 | 2020-04-28 | 潍坊春丰新材料科技有限公司 | Boron nitride powder with high lubrication and large specific surface area and preparation method thereof |
| CN112271406A (en) * | 2020-10-30 | 2021-01-26 | 湖北第二师范学院 | Boron nitride fiber coated diaphragm for lithium ion battery and preparation method thereof |
| CN112877810A (en) * | 2021-02-01 | 2021-06-01 | 山东大学 | Preparation method of porous boron nitride fiber with high specific surface area |
| WO2022039234A1 (en) * | 2020-08-20 | 2022-02-24 | デンカ株式会社 | Boron nitride particles, method for producing boron nitride particles, resin composition, and method for producing resin composition |
| CN114195106A (en) * | 2022-01-10 | 2022-03-18 | 南京大学 | Preparation method of boron nitride porous material with high specific surface area |
| CN114751388A (en) * | 2019-06-14 | 2022-07-15 | 河北科技大学 | Porous boron nitride and preparation method thereof, nano gold boron nitride composite photocatalyst and preparation method and application thereof |
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| US20170008766A1 (en) * | 2015-07-07 | 2017-01-12 | Korea Institute Of Energy Research | Synthesis of boron nitride and coating method of the same |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109894103B (en) * | 2019-03-01 | 2021-12-14 | 河北工业大学 | Method for adsorbing carbon dioxide and monitoring slow release thereof by using conjugated polymer and boron nitride composite material |
| CN109894103A (en) * | 2019-03-01 | 2019-06-18 | 河北工业大学 | The method adsorbed carbon dioxide using conjugated polymer and boron nitride composite and monitor its slow release |
| CN114751388A (en) * | 2019-06-14 | 2022-07-15 | 河北科技大学 | Porous boron nitride and preparation method thereof, nano gold boron nitride composite photocatalyst and preparation method and application thereof |
| CN110496588A (en) * | 2019-06-20 | 2019-11-26 | 中国科学院长春应用化学研究所 | A kind of adsorption method of radioiodine |
| CN110255516A (en) * | 2019-07-30 | 2019-09-20 | 河北工业大学 | A kind of synthetic method of active boron nitride nanotube |
| CN110255516B (en) * | 2019-07-30 | 2020-10-09 | 河北工业大学 | Synthesis method of active boron nitride nanotube |
| CN110629323A (en) * | 2019-10-14 | 2019-12-31 | 河北工业大学 | Method for synthesizing porous boron nitride fiber with high length-diameter ratio under assistance of organic solvent |
| CN110629323B (en) * | 2019-10-14 | 2021-11-16 | 河北工业大学 | Method for synthesizing porous boron nitride fiber with high length-diameter ratio under assistance of organic solvent |
| CN111073742A (en) * | 2019-12-23 | 2020-04-28 | 潍坊春丰新材料科技有限公司 | Boron nitride powder with high lubrication and large specific surface area and preparation method thereof |
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| CN114195106A (en) * | 2022-01-10 | 2022-03-18 | 南京大学 | Preparation method of boron nitride porous material with high specific surface area |
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