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CN109399587A - Preparation method of mesoporous carbonitride and products thereof and application - Google Patents

Preparation method of mesoporous carbonitride and products thereof and application Download PDF

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Publication number
CN109399587A
CN109399587A CN201811553409.0A CN201811553409A CN109399587A CN 109399587 A CN109399587 A CN 109399587A CN 201811553409 A CN201811553409 A CN 201811553409A CN 109399587 A CN109399587 A CN 109399587A
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nano
zinc oxide
carbon nitride
mesoporous carbon
preparation
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Inventor
何丹农
徐少洪
王敬锋
林琳
陈超
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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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
    • C01B21/0605—Binary compounds of nitrogen with carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

本发明涉及一种介孔氮化碳的制备方法及其产品和应用，采用纳米氧化锌作为前驱体，先将纳米氧化锌采用研磨分散的方式制备成单分散性的纳米分散液，然后将氮化碳前驱体与氧化锌分散液充分混合之后进行焙烧，然后将焙烧产物在盐酸中充分搅拌，最终制备得到介孔氮化碳。采用本发明方法制备的介孔氮化碳，孔径小并且大小均一，具有操作简单，难度较低，且不会使用到危险性大的氢氟酸，且适合大规模推广。The invention relates to a preparation method, product and application of mesoporous carbon nitride. Nano-zinc oxide is used as a precursor, and nano-zinc oxide is first prepared into a monodisperse nano-dispersion by grinding and dispersing, and then nitrogen The carbonized precursor and the zinc oxide dispersion are fully mixed and then calcined, and then the calcined product is fully stirred in hydrochloric acid to finally prepare mesoporous carbon nitride. The mesoporous carbon nitride prepared by the method of the invention has small pore size and uniform size, has simple operation, low difficulty, does not use dangerous hydrofluoric acid, and is suitable for large-scale promotion.

Description

Preparation method of mesoporous carbonitride and products thereof and application
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of preparation method of mesoporous carbonitride and products thereof and Using.
Background technique
Carbonitride is a kind of Huang by the way that carbon elements and nitrogen material abundant are carried out with certain roasting synthesis Color nanocrystal.Its crystal structure is similar to graphite-structure.Because nitridation carbon-based group only exists in a molecular layer, only Faint Van der Waals force can will connect between different molecular layer.It is widely known that light can produce in this material Raw electron-hole pair.Therefore, carbonitride has excellent photocatalysis performance.It can convert height for the solar energy of low-density The chemical energy of density or directly degradation and mineralising organic pollutant, have in terms of the problems such as solving energy shortage and environmental pollution Important application prospect.
Mesoporous carbonitride is since there are the apertures of a large amount of 2-50nm on carbonitride thin slice, so that it is with high ratio The features such as surface area, regular cellular structure, narrow pore-size distribution；For purer carbonitride, have excellent The absorption of macromolecular, separation characteristic, can play a greater role in catalysis reaction, higher photocatalysis efficiency is provided.And And this orderly duct is alternatively arranged as " microreactor ", improves catalytic performance.The preparation method of current mesoporous carbonitride is universal Template is used as using nano silicon oxide, mesoporous carbonitride is prepared by hard template method, Jie can be prepared in this way Hole carbonitride.But this method has some disadvantages, the method first is first to mix silica with carbon nitride precursor, is then roasted Burning obtains carbonitride, then mixes obtained powder with hydrofluoric acid, and dissolve silica can be obtained mesoporous nitrogen later Change carbon.It is well known that hydrofluoric acid has extremely strong corrosive acid as a kind of, it can consumingly corrode metal, glass and siliceous Object, such as sucking steam or contacting skin will cause burning of being difficult to cure, and be that a kind of height endangers poisonous substance；On the other hand, It is known that agglomeration easily occurs for nano material, by mixing silica with carbonitride since its surface can be excessive It is redissolved the mode fallen and prepares mesoporous carbonitride, since nano silicon oxide can reunite, this will result in final synthesising mesoporous The pore size of carbonitride is different, it could even be possible to having the aperture of several hundred nanosizeds；Therefore, using conventional method preparation Mesoporous carbonitride haves the shortcomings that aperture is different, and preparation process has the harm to people and environment, and preparation difficulty is higher, It is only applicable to laboratory preparation.
Summary of the invention
To prepare mesoporous carbonitride pore size inhomogenous for existing, prepares the higher disadvantage of difficulty, the object of the invention exists In providing a kind of preparation method of mesoporous carbonitride.
Another object of the present invention is: providing a kind of mesoporous nitridation carbon products of above method preparation.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention is realized by following proposal: one kind is by nano zinc oxide fluid dispersion as presoma, using salt Acid dissolution falls the mode of template to prepare the preparation method of mesoporous carbonitride, includes the following steps:
1) prepared by nano zinc oxide fluid dispersion: being in mass ratio 1:(0.05~0.6): (1~100) accurately weighs nano oxidized Dispersing agent is added in deionized water first, after stirring to dissolve, adds nano oxygen by zinc, dispersing agent and deionized water Change zinc, is uniformly mixed, then grinds, obtain the nano zinc oxide fluid dispersion that monodisperse is not reunited；
2) melamine, the matter of the nano zinc oxide fluid dispersion and melamine are added in above-mentioned nano zinc oxide fluid dispersion Amount is than being 1:(0.01~0.5), 3h is then stirred at 60~100 DEG C, obtains melamine after the evaporation of above-mentioned solution is done With nano zine oxide homogeneous mixture；It will be put into crucible after above-mentioned solid abrasive, with 2.5 DEG C/min of heating rate liter Temperature is roasted to 400~600 DEG C, is kept the temperature 1~5 hour, is obtained brownish black powder；
3) the brownish black powder for obtaining above-mentioned roasting takes out 0.5~1g, and 1~3mol/L of 100~300ml is added after grinding Hydrochloric acid in stir 2~6 hours, be then centrifuged for and cleaned using deionized water and ethyl alcohol, it is final it is dry after obtain Mesoporous carbonitride.
Nano zine oxide, as presoma, is first prepared by the present invention using nano zine oxide by the way of grinding distribution The nano dispersion fluid of monodispersity roasts, so after being then sufficiently mixed carbon nitride precursor with zinc oxide fluid dispersion Product of roasting is sufficiently stirred in hydrochloric acid afterwards, mesoporous carbonitride is finally prepared.
In step 1), milling time is 0.5~10 hour.
The dispersing agent is lauryl sodium sulfate, cetyl trimethylammonium bromide, lauryl sulfosuccinate list Ester disodium, fatty alcohol polyoxyethylene ether, sulfosuccinic acid monoesters disodium, Coconut Fatty Acid Monoethanolamide sulfosuccinic acid monoesters two Sodium, single Tryfac 5573, Monododecylphosphate potassium, laurel alcohol ether phosphate potassium, nonylphenol polyoxyethylene ether, polyethylene One of pyrrolidones or combinations thereof.
The present invention also provides a kind of mesoporous carbonitrides, are prepared according to any of the above-described the method.
Also, the present invention also provides a kind of mesoporous carbonitride in formaldehyde photocatalysis as the application of catalyst.
The method of the present invention preparation mesoporous carbonitride, aperture is small and size is uniform, have it is easy to operate, difficulty is lower, And it not will use the big hydrofluoric acid of risk, and be suitble to large-scale promotion.
Detailed description of the invention
The TEM photo of the mesoporous carbonitride of Fig. 1.
Specific embodiment
The present invention is further illustrated below by embodiment, is not intended to limit the scope of the invention.
Embodiment 1
A kind of preparation method of mesoporous carbonitride falls mould as presoma, using dissolving with hydrochloric acid using nano zinc oxide fluid dispersion The mode of plate prepares the preparation method of mesoporous carbonitride, as follows:
1) prepared by nano zinc oxide fluid dispersion: for 1:0.3:50 precise nano zine oxide, dispersing agent and going in mass ratio Ionized water, dispersing agent are lauryl sodium sulfate, and first dispersing agent is dissolved in deionized water, nano zine oxide is then added, is stirred Sand mill is added after mixing uniformly, (wherein milling time is 2 hours) is ground after adjusting technological parameter and obtains monodispersed receive Rice zinc oxide fluid dispersion.
It 2) is in mass ratio that 1:0.3 is mixed with appropriate melamine by nano zinc oxide fluid dispersion, then 80 DEG C of stirrings are steamed It is dry, obtained solid matter is put into crucible and is roasted, wherein heating rate is 2.5 DEG C/min, final calcination temperature For 500 DEG C and calcining time is 3 hours, obtains brownish black powder；
3) it finally, taking out 0.5g brownish black powder, is added in hydrochloric acid after grinding, wherein hydrochloric acid volume is 200ml, and concentration is 1mol/L is stirred 2 hours, be centrifuged and wash it is dry after finally obtain mesoporous carbonitride, as the TEM of the mesoporous carbonitride of Fig. 1 shines Shown in piece.
Embodiment 2
A kind of preparation method of mesoporous carbonitride, it is approximate with embodiment 1, as follows:
1) nano zinc oxide fluid dispersion prepare: mass ratio be 1:0.5:70 precise nano zine oxide, dispersing agent and go from Sub- water, dispersing agent are cetyl trimethylammonium bromide, and first dispersing agent is dissolved in deionized water, are then added nano oxidized Sand mill is added after stirring evenly in zinc, adjusts after technological parameter grinding 3 hours, obtains mono-dispersed nano zinc oxide point Dispersion liquid.
It 2) is in mass ratio that 1:0.2 is mixed with appropriate melamine by nano zinc oxide fluid dispersion, then 90 DEG C of high temperature stir It mixes and is evaporated, obtained solid matter is put into crucible and is roasted, wherein heating rate is 2.5 DEG C/min, final to roast Temperature is 550 DEG C, and calcining time is 4 hours, obtains brownish black powder；
3) 1g brownish black powder is taken out, it is 150ml that volume is added after grinding, and concentration is to stir 4 hours in 2mol/L hydrochloric acid, from The heart and wash it is dry after finally obtain mesoporous carbonitride.
Embodiment 3
A kind of preparation method of mesoporous carbonitride, it is approximate with embodiment 1, as follows:
1) prepared by nano zinc oxide fluid dispersion: for 1:0.2:80 precise nano zine oxide, dispersing agent and going in mass ratio Ionized water, dispersing agent are nonylphenol polyoxyethylene ether, and first dispersing agent is dissolved in deionized water, nano zine oxide is then added, Sand mill is added after stirring evenly, adjusts after technological parameter grinding 1 hour, obtains the dispersion of mono-dispersed nano zinc oxide Liquid.
It 2) is in mass ratio that 1:0.4 is mixed with appropriate melamine by nano zinc oxide fluid dispersion, then 85 DEG C of high temperature stir It mixes and is evaporated, obtained solid matter is put into crucible and is roasted, wherein heating rate is 2.5 DEG C/min, final to roast Temperature is 600 DEG C, and calcining time is 2 hours, obtains brownish black powder；
3) 0.5g brownish black powder is taken out, it is 300ml that volume is added after grinding, and concentration is that stirring 5 is small in the hydrochloric acid of 3mol/L When, be centrifuged and wash it is dry after finally obtain mesoporous carbonitride.
Embodiment 4
A kind of preparation method of mesoporous carbonitride, it is approximate with embodiment 1, as follows:
1) prepared by nano zinc oxide fluid dispersion: for 1:0.3:40 precise nano zine oxide, dispersing agent and going in mass ratio Ionized water, dispersing agent are the combination of lauryl sulfosuccinic acid monoester disodium and polyvinylpyrrolidone, are first dissolved in dispersing agent In deionized water, nano zine oxide is then added, sand mill is added after stirring evenly, grinding 3 is small after adjusting technological parameter When obtain mono-dispersed nano zinc oxide fluid dispersion.
It 2) is in mass ratio that 1:0.2 is mixed with appropriate melamine by nano zinc oxide fluid dispersion, then 100 DEG C of high temperature stir It mixes and is evaporated, obtained solid matter is put into crucible and is roasted, wherein heating rate is 2.5 DEG C/min, final to roast Temperature is 600 DEG C, and calcining time is 1 hour, obtains brownish black powder；
3) 1g brownish black powder is taken out, it is 150ml that volume is added after grinding, and concentration is to stir 2.5 hours in 3mol/L hydrochloric acid, It is centrifuged and washs drying and finally obtain mesoporous carbonitride later.

Claims (5)

1.一种介孔氮化碳的制备方法，其特征在于，采用纳米氧化锌分散液作为前驱体、采用盐酸溶解掉模板的方式来制备介孔氮化碳的制备方法，包括如下步骤：1. a preparation method of mesoporous carbon nitride, is characterized in that, adopts nano zinc oxide dispersion liquid as precursor, adopts the mode that hydrochloric acid dissolves away template to prepare the preparation method of mesoporous carbon nitride, comprises the steps: 1）纳米氧化锌分散液制备：按质量比为1:（0.05～0.6）：（1～100）精确称取纳米氧化锌、分散剂以及去离子水，首先将分散剂加入去离子水中，搅拌使其溶解后，再加入纳米氧化锌，搅拌混合均匀，然后研磨，得到单分散不团聚的纳米氧化锌分散液；1) Preparation of nano-zinc oxide dispersion: According to the mass ratio of 1: (0.05～0.6): (1～100), accurately weigh nano-zinc oxide, dispersant and deionized water, first add dispersant to deionized water, stir After dissolving it, adding nano-zinc oxide, stirring and mixing evenly, and then grinding to obtain a nano-zinc oxide dispersion liquid that is monodisperse and not agglomerated; 2）在上述纳米氧化锌分散液中加入三聚氰胺，所述纳米氧化锌分散液与三聚氰胺的质量比为1:（0.01～0.5），然后在60～100℃下搅拌3h，将上述溶液蒸发干之后得到三聚氰胺与纳米氧化锌均匀混合物；将上述固体研磨之后放入坩埚中，以2.5℃/分钟的升温速率升温到400～600℃焙烧，保温1～5小时，得到棕黑色粉体；2) Add melamine to the above nano-zinc oxide dispersion, the mass ratio of the nano-zinc oxide dispersion to melamine is 1: (0.01～0.5), then stir at 60～100 ℃ for 3h, and evaporate the above solution to dryness A uniform mixture of melamine and nano-zinc oxide is obtained; the above-mentioned solid is ground and put into a crucible, heated to 400-600° C. at a heating rate of 2.5° C./min for calcination, and kept for 1-5 hours to obtain a brown-black powder; 3）将上述焙烧得到的棕黑色粉体取出0.5～1g，研磨之后加入100～300ml的1～3mol/L的盐酸中搅拌2～6小时，然后离心并采用去离子水以及乙醇进行清洗，最终干燥之后得到介孔氮化碳。3) Take out 0.5-1 g of the brown-black powder obtained by the above roasting, add 100-300 ml of 1-3 mol/L hydrochloric acid after grinding, and stir for 2-6 hours, then centrifuge and wash with deionized water and ethanol. After drying, mesoporous carbon nitride is obtained. 2.根据权利要求1所述介孔氮化碳的制备方法，其特征在于步骤1）中，研磨时间为0.5～10小时。2 . The method for preparing mesoporous carbon nitride according to claim 1 , wherein in step 1), the grinding time is 0.5 to 10 hours. 3 . 3.根据权利要求1所述介孔氮化碳的制备方法，其特征在于分散剂为十二烷基硫酸钠、十六烷基三甲基溴化铵、月桂基磺化琥珀酸单酯二钠、脂肪醇聚氧乙烯醚、磺基琥珀酸单酯二钠、椰油酸单乙醇酰胺磺基琥珀酸单酯二钠、单月桂基磷酸酯、单十二烷基磷酸酯钾、月桂醇醚磷酸酯钾、壬基酚聚氧乙烯醚、聚乙烯吡咯烷酮中的一种或其组合。3. the preparation method of mesoporous carbon nitride according to claim 1 is characterized in that dispersant is sodium lauryl sulfate, cetyl trimethyl ammonium bromide, lauryl sulfosuccinic acid monoester two Sodium, fatty alcohol polyoxyethylene ether, disodium sulfosuccinate monoester, disodium cocoate monoethanolamide sulfosuccinate monoester, monolauryl phosphate, potassium monododecyl phosphate, lauryl alcohol One or a combination of potassium ether phosphate, nonylphenol polyoxyethylene ether, and polyvinylpyrrolidone. 4.一种介孔氮化碳，其特征在于根据权利要求1-3任一所述方法制备得到。4. A mesoporous carbon nitride, characterized in that it is prepared according to any one of claims 1-3. 5.一种根据权利要求4所述介孔氮化碳在甲醛光催化中作为催化剂的应用。5. An application of the mesoporous carbon nitride according to claim 4 as a catalyst in formaldehyde photocatalysis.
CN201811553409.0A 2018-12-18 2018-12-18 Preparation method of mesoporous carbonitride and products thereof and application Pending CN109399587A (en)

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CN112517047A (en) * 2020-12-29 2021-03-19 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of carbon nitride/titanium dioxide embedded heterojunction, product and application thereof

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