CN104525107A - Graphene-based haze-resisting mask filtering material and preparation method thereof - Google Patents
Graphene-based haze-resisting mask filtering material and preparation method thereof Download PDFInfo
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- CN104525107A CN104525107A CN201410722672.3A CN201410722672A CN104525107A CN 104525107 A CN104525107 A CN 104525107A CN 201410722672 A CN201410722672 A CN 201410722672A CN 104525107 A CN104525107 A CN 104525107A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/30—Particle separators, e.g. dust precipitators, using loose filtering material
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- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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Abstract
The invention relates to a graphene-based haze-resisting mask filtering material and a preparation method thereof. The material has a three-dimensional graphene sponge structure assembled from graphene oxide. The method and an application comprises the following points: (1) cross-linking agents such as ascorbic acid are added into a graphene oxide water solution; with a hydrothermal reaction, graphene slices are subjected to self assembly, such that porous spongy three-dimensional graphene is obtained; (2) the porous spongy graphene has good mechanical strength, and can be cut into different shapes; (3) the structure of the graphene sponge can be regulated through changing the size of graphene oxide and the addition amount of the cross-linking agents; (4) the porous spongy graphene has high specific surface area and relatively high quantity of surface functional groups; and the porous spongy graphene has high absorption effect and certain bacteria resistance. The preparation process of the graphene absorption material has simple process and low cost. With the method, graphene sponge pore size can be regulated. The graphene sponge can be used as a mask filtering sheet which can effectively filter air pollutants such as PM2.5 particles, and can be used in the fields such as dye and oil dirt absorption.
Description
Technical field
The present invention relates to sorbing material field, be specially a kind of Graphene sorbing material and its preparation method and application, can be used as mouth mask filter disc and effectively filter the air pollutants such as PM2.5, there is certain anti-microbial property simultaneously.
Background technology
In recent years, again and again produce haze weather in many big and medium-sized cities of China, the healthy and life of the serious threat people.The mechanism that haze weather produces is very complicated, and its chemical composition is also very complicated, may cause various diseases.Meanwhile, virus, germ etc. may be attached on the particle of air, spread disease.PM2.5 is particle maximum to harm in atmosphere pollution, and this particle diameter is equal to or less than 2.5 microns, medically becomes pellet.General mouth mask cannot filter PM2.5, and multiple haze mouth mask on the market also all effectively can not stop PM2.5 at present.And blocking effect is good, mouth mask as that in N95, cost is too high, and gas permeability is poor, can not Long-Time Service.Therefore need exploitation one to have excellent absorption property and anti-microbial property, gas permeability is better, effectively can stop the atmosphere pollutions such as PM2.5, and preparation technology is simple, filtering material with low cost.
Since Graphene was found from 2004, cause the great interest of scientific research circle immediately, become a large focus material of scientific research in recent years.Graphene is as a kind of emerging material, and its theoretical specific surface area can reach 2620m
2/ g is a kind of potential sorbing material.But because graphene film Rotating fields is easily reunited, form the two-dimensional structure material that porosity is very low, thus its properties and application scope is very restricted.
Utilize graphene oxide to be assembled into three-dimensional sponge shape structure graphite alkene, have large specific area, good absorption property, research simultaneously shows that graphene oxide has excellent anti-microbial property.The method preparing employing of three-dimensional grapheme can make hydro-thermal method and reducing agent reducing process etc., and current method all effectively can not control the size in its aperture, dyestuff, organic solvent etc. can only be used for and pollute absorption, can not effectively as air filtration sorbing material.
Summary of the invention
The object of the present invention is to provide a kind of mouth mask filter material that effectively can filter PM2.5, and there is certain anti-microbial property,
The scheme that the present invention solves the problems of the technologies described above is:
A kind of graphene-based haze mouth mask filter material, this material is the three-dimensional sponge shape structure of graphene oxide assembling, pore diameter range 100nm ~ 1.5 μm, specific area 100m
2/ g ~ 2000m
2/ g, Surface oxygen-containing groups ratio is 35% ~ 50%.
The preparation method of described graphene-based haze mouth mask filter material, comprises the steps:
(1) preparation of graphene oxide water solution: the graphite composite powder choosing different meshes is raw material, and prepare the graphene oxide of different size, ultrasonic disperse is in water.
(2) preparation of three-dimensional grapheme structure: add the crosslinking agents such as ascorbic acid (VC) in a certain amount of graphene aqueous solution, be assembled into three-dimensional sponge shape structure by the method for Hydrothermal Synthesis, obtain three-dimensional grapheme material after drying.
The preparation method of described graphene-based haze mouth mask filter material, the order number of graphite powder used is 5000 order ~ 15000 orders.The concentration of the graphene oxide solution after dispersion is 0.1mg/ml ~ 10mg/ml.
The preparation method of described graphene-based haze mouth mask filter material, prepare graphene oxide and adopt Hummer method to be oxidized graphite powder, graphene dispersion solvent is the aqueous solution, and ultrasonic splitting time is 30min ~ 5h.
The preparation method of described graphene-based haze mouth mask filter material, when Hydrothermal Synthesis prepares three-dimensional grapheme, graphene oxide solution concentration is 0.5mg/ml ~ 10mg/ml, and the temperature of hydro-thermal reaction is 60 DEG C ~ 180 DEG C, and the reaction time is 2h ~ 24h.Preferably, the concentration of graphene oxide solution is 1mg/ml ~ 5mg/ml, and the temperature of hydro-thermal reaction is 80 DEG C ~ 150 DEG C, and the reaction time is 4h ~ 24h.
The preparation method of described graphene-based haze mouth mask filter material, when preparing three-dimensional grapheme add that crosslinking agent can be among ascorbic acid, polyethylene glycol, dopamine, ethylenediamine one or more, add crosslinking agent and graphene oxide mass ratio be 1: 1 ~ 1: 100.Preferably, add crosslinking agent and select ascorbic acid (VC), the mass ratio of addition and graphene oxide is 1: 5 ~ 1: 50.
The preparation method of described graphene-based haze mouth mask filter material, when Hydrothermal Synthesis prepares three-dimensional grapheme, the drying mode of employing is vacuum freeze drying; Or put into alcohol immersion after freezing, take out and naturally dry in atmosphere after melting, three-dimensional material can not subside reunion.
The preparation method of described graphene-based haze mouth mask filter material, in three-dimensional grapheme structure preparation process, controls the size in three-dimensional structure aperture by the change size of graphene oxide and the addition of polymerizer.Preferably, the order number of graphite powder is selected to be 10000 order ~ 15000 orders when preparing graphene oxide.
The preparation method of described graphene-based haze mouth mask filter material, the size of prepared three-dimensional grapheme block materials and thickness, can be regulated and controled by the container pattern of hydro-thermal reaction device and size.The spongy graphene of gained porous has good mechanical strength, can be cut into difformity.
Beneficial effect of the present invention:
(1) utilize graphene oxide to be assembled into three-dimensional sponge shape structure graphite alkene, there is the specific area of superelevation, good absorption property.Use it for haze mouth mask filter disc, can effective filtered atmospheric pollutant.
(2) preparation of three-dimensional grapheme in the past can not control its pore size, and hole is larger.The present invention utilizes and regulates ascorbic acid (VC) addition successfully can control its aperture below micron order, effectively can stop PM2.5, simultaneously VC to human body without any harm, environmental protection.
(3) utilize Hydrothermal Synthesis three-dimensional sponge shape Graphene, not only there is superhigh specific surface area, and its surface also has a large amount of oxy radicals, strengthens its adsorption effect further.Research simultaneously shows that graphene oxide has antibacterial effect.
(4) drying means of the present invention is except traditional vacuum freeze drying, also proposed: after freezing for the material of hydro-thermal reaction, put into alcohol immersion, takes out and naturally dry in atmosphere after melting, and three-dimensional material can not subside reunion.Ethanolic solution can be recycled repeatedly, reduces the energy consumption that freeze drying brings, is more conducive to environmental protection.
(5) this Graphene sorbing material preparation process technique is simple, with low cost, the pore size of graphene sponge can be regulated and controled, there is good mechanical performance and processing characteristics, can be used as mouth mask filter disc and effectively filter the air pollutants such as PM2.5, also can be applicable to the fields such as dyestuff, greasy dirt absorption and air filter simultaneously.
Accompanying drawing explanation
Fig. 1,2,3 is SEM photos of gained three-dimensional grapheme material of the present invention.
Detailed description of the invention
The present invention is further illustrated below in conjunction with accompanying drawing and following embodiment; should understand; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The temperature that following example is concrete, time etc. are also only examples in OK range, and namely, those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Below, in conjunction with specific embodiments the Synthesis and applications of the present invention's graphene-based haze mouth mask filter material is described in detail.
Embodiment 1
The embodiment of the present invention prepares the technological process of three-dimensional grapheme, comprises the steps:
The first step, prepares graphene oxide: in the present embodiment, graphite powder particle mean size is 10000 orders.Hummers method is utilized to synthesize graphene oxide (GO).By 2g graphite powder, 1g NaNO
3mix with the 230ml concentrated sulfuric acid in ice-water bath, slowly add 6g KMnO
4.Then be warming up at 35 DEG C, after stirring 30min, add 92ml deionized water, be warming up to 98 DEG C of reaction 15min.Afterwards, add the dilution of 280ml water wherein, and use 5ml 30%H
2o
2neutralize unnecessary KMnO
4.The color of mixed solution is brown color, filters while hot, and with deionized water cyclic washing to neutral, ultrasonic disperse obtains GO.
Second step, Hydrothermal Synthesis three-dimensional grapheme: getting 200ml mass fraction is that the graphene oxide solution of 5mg/ml pours diameter 25cm into, in the discoid reaction utensil of high 2cm, add ascorbic acid (VC) 0.5g stirring and make it fully mix, then that reaction utensil is airtight.Airtight reaction utensil is placed in 80 DEG C of hydro-thermal reaction 12h, the graphene oxide Spontaneous Contraction in reaction utensil is cross-linked into three-dimensional sponge structure.Then graphene sponge is carried out freeze drying, obtain flexible three-dimensional grapheme structure.
In sum, this three-dimensional sponge shape graphene-structured, pore diameter range 100nm ~ 1 μm, specific area is about 1500m
2/ g, Surface oxygen-containing groups ratio is about 40%.
By above-mentioned material cutting growth 15cm, the rectangle of wide 10cm, is filled in the intermediate layer of common cotton cloth respirator, becomes novel graphite alkene mouth mask.For checking its air filtration effect, the air box (Qingdao Haier Air Conditioner Co., Ltd, KZW-A01U1) detecting air quality is placed in closed container by us, seals opening with above-mentioned Graphene mouth mask.Test as a comparison, the common cotton cloth respirator of another group seals opening.Then container is placed in the environment being full of cigarette flue dust.We see that the tainer air box registration that Graphene mouth mask seals is 79 (excellent), and the tainer air box registration of common mouth mask sealing is 40 (serious pollutions).
As can be seen here, the present invention effectively can filter the air pollutants such as PM2.5 as mouth mask filter disc.
Embodiment 2
The embodiment of the present invention prepares the technological process of three-dimensional grapheme, comprises the steps:
The first step, prepares graphene oxide: in the present embodiment, graphite powder particle mean size is 15000 orders.Synthesis step is in the same manner as in Example 1.
Second step, Hydrothermal Synthesis three-dimensional grapheme: getting 200ml mass fraction is that the graphene oxide solution of 5mg/ml pours diameter 25cm into, in the discoid reaction utensil of high 2cm, add ascorbic acid (VC) 0.5g stirring and make it fully mix, then that reaction utensil is airtight.Airtight reaction utensil is placed in 160 DEG C of hydro-thermal reaction 6h, the graphene oxide Spontaneous Contraction in reaction utensil is cross-linked into three-dimensional sponge structure.Then graphene sponge is carried out freeze drying, obtain flexible three-dimensional grapheme structure.
In sum, this three-dimensional sponge shape graphene-structured, pore diameter range 100nm ~ 800nm, specific area is about 1000m
2/ g, Surface oxygen-containing groups ratio is about 40%.
This material effectively can filter the air pollutants such as PM2.5 as mouth mask filter disc equally.
Embodiment 3
The embodiment of the present invention prepares the technological process of three-dimensional grapheme, comprises the steps:
The first step, prepares graphene oxide: in the present embodiment, graphite powder particle mean size is 10000 orders.Synthesis step is in the same manner as in Example 1.
Second step, Hydrothermal Synthesis three-dimensional grapheme: getting 200ml mass fraction is that the graphene oxide solution of 5mg/ml pours diameter 25cm into, in the discoid reaction utensil of high 2cm, add dopamine (DA) 0.2g stirring and make it fully mix, then that reaction utensil is airtight.Airtight reaction utensil is placed in 120 DEG C of hydro-thermal reaction 12h, the graphene oxide Spontaneous Contraction in reaction utensil is cross-linked into three-dimensional sponge structure.Then put into ethanolic solution after graphene sponge is freezing to soak, naturally dry after removing solution, obtain flexible three-dimensional grapheme structure.
In sum, this three-dimensional sponge shape graphene-structured, pore diameter range 100nm ~ 1 μm, specific area is about 1300m
2/ g, Surface oxygen-containing groups ratio is about 40%.
This material effectively can filter the air pollutants such as PM2.5 as mouth mask filter disc equally.
Embodiment 4
The embodiment of the present invention prepares the technological process of three-dimensional grapheme, comprises the steps:
The first step, prepares graphene oxide: in the present embodiment, graphite powder particle mean size is 5000 orders.Synthesis step is in the same manner as in Example 1.
Second step, Hydrothermal Synthesis three-dimensional grapheme: getting 200ml mass fraction is that the graphene oxide solution of 5mg/ml pours diameter 25cm into, in the discoid reaction utensil of high 2cm, adds polyethylene glycol 1g and stirs and make it fully mix, then that reaction utensil is airtight.Airtight reaction utensil is placed in 120 DEG C of hydro-thermal reaction 10h, the graphene oxide Spontaneous Contraction in reaction utensil is cross-linked into three-dimensional sponge structure.Then graphene sponge is carried out freeze drying, obtain flexible three-dimensional grapheme structure.
In sum, this three-dimensional sponge shape graphene-structured, pore diameter range 300nm ~ 1.5 μm, specific area is about 500m
2/ g, Surface oxygen-containing groups ratio is about 40%.
This material effectively can filter the air pollutants such as PM2.5 as mouth mask filter disc equally.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a graphene-based haze mouth mask filter material, is characterized in that: this material is the three-dimensional sponge shape structure of graphene oxide assembling, pore diameter range 100nm ~ 1.5 μm, specific area 100m
2/ g ~ 2000m
2/ g.
2. the preparation method of material according to claim 1, is characterized in that, comprise the following steps:
(1) preparation of graphene oxide water solution: the graphite composite powder choosing different meshes is raw material, and prepare the graphene oxide of different size, ultrasonic disperse is in water.
(2) preparation of three-dimensional grapheme structure: add crosslinking agent in a certain amount of graphene aqueous solution, is assembled into three-dimensional sponge shape structure by the method for Hydrothermal Synthesis, obtains three-dimensional grapheme material after drying.
3. preparation method according to claim 2, is characterized in that, the order number of graphite powder used is 5000 order ~ 15000 orders, and the concentration of the graphene oxide solution after dispersion is 0.1mg/ml ~ 10mg/ml.
4. preparation method according to claim 2, is characterized in that, prepare graphene oxide and adopt Hummer method to be oxidized graphite powder, graphene dispersion solvent is the aqueous solution, and ultrasonic splitting time is 30min ~ 5h.
5. preparation method according to claim 2, is characterized in that, when Hydrothermal Synthesis prepares three-dimensional grapheme, graphene oxide solution concentration is 0.5mg/ml ~ 10mg/ml, and the temperature of hydro-thermal reaction is 60 DEG C ~ 180 DEG C, and the reaction time is 2h ~ 24h.
6. method according to claim 2, it is characterized in that, when preparing three-dimensional grapheme to add crosslinking agent be one or more among ascorbic acid, polyethylene glycol, dopamine, ethylenediamine, add crosslinking agent and graphene oxide mass ratio be 1: 1 ~ 1: 100.
7. preparation method according to claim 2, is characterized in that, when Hydrothermal Synthesis prepares three-dimensional grapheme, the drying mode of employing is vacuum freeze drying; Or put into alcohol immersion after freezing, take out after melting and naturally dry in atmosphere.
8. preparation method according to claim 2, is characterized in that, in three-dimensional grapheme structure preparation process, the size in aperture is controlled by the change size of graphene oxide and the addition of polymerizer.
9. preparation method according to claim 2, is characterized in that, the size of prepared three-dimensional grapheme block materials and thickness are regulated and controled by the container pattern of hydro-thermal reaction device and size, and the spongy graphene of gained porous can be cut into arbitrary shape.
10. the application of material according to claim 1, is characterized in that, be filled in mouth mask intermediate layer, adsorb air pollutants such as PM2.5 as mouth mask filter disc, also can adsorb dyestuff, oils and organic solvent simultaneously.
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Cited By (17)
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| CN105111690A (en) * | 2015-09-25 | 2015-12-02 | 天津工业大学 | Method for improving mechanics properties of three-dimensional graphene structure body/polymer composite material |
| CN105251268A (en) * | 2015-11-03 | 2016-01-20 | 杜茂龙 | Graphene-based air filter material and preparation method thereof |
| CN105266238A (en) * | 2015-11-25 | 2016-01-27 | 常州纳美生物科技有限公司 | Anti-haze green mouth mask based on oxidized graphene and manufacturing method |
| CN106348601A (en) * | 2016-08-29 | 2017-01-25 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Radiation-proof healthcare ceramics and preparing method thereof |
| CN106348597A (en) * | 2016-08-29 | 2017-01-25 | 佛山市高明区诚睿基科技有限公司 | Method for photochromic low temperature antique glaze and preparing method thereof |
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| CN106348596A (en) * | 2016-08-29 | 2017-01-25 | 佛山市高明区诚睿基科技有限公司 | Method for antibacterial lead-free low temperature frit and preparing method thereof |
| CN106396387A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Antibacterial radiation-proof ceramic tile and preparation method thereof |
| CN106746652A (en) * | 2016-08-29 | 2017-05-31 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of antibacterial ceramic glaze and preparation method thereof |
| CN106746653A (en) * | 2016-08-29 | 2017-05-31 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of antibiotic radiation proof ceramic glaze and preparation method thereof |
| CN106744912A (en) * | 2017-03-10 | 2017-05-31 | 中国科学院新疆理化技术研究所 | A kind of preparation method of super-hydrophobic graphene aerogel |
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| CN105266238A (en) * | 2015-11-25 | 2016-01-27 | 常州纳美生物科技有限公司 | Anti-haze green mouth mask based on oxidized graphene and manufacturing method |
| CN106746652A (en) * | 2016-08-29 | 2017-05-31 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of antibacterial ceramic glaze and preparation method thereof |
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| CN106348596A (en) * | 2016-08-29 | 2017-01-25 | 佛山市高明区诚睿基科技有限公司 | Method for antibacterial lead-free low temperature frit and preparing method thereof |
| CN106396387A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Antibacterial radiation-proof ceramic tile and preparation method thereof |
| CN106348601A (en) * | 2016-08-29 | 2017-01-25 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Radiation-proof healthcare ceramics and preparing method thereof |
| CN106746653A (en) * | 2016-08-29 | 2017-05-31 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of antibiotic radiation proof ceramic glaze and preparation method thereof |
| CN106744912A (en) * | 2017-03-10 | 2017-05-31 | 中国科学院新疆理化技术研究所 | A kind of preparation method of super-hydrophobic graphene aerogel |
| CN107579231A (en) * | 2017-09-08 | 2018-01-12 | 安徽玄同工业设计有限公司 | The preparation method of three-dimensional graphite alkenyl ferric vandate |
| CN108620043A (en) * | 2018-05-28 | 2018-10-09 | 佛山市日日圣科技有限公司 | A kind of air purification graphene sponge material |
| CN108786729A (en) * | 2018-06-06 | 2018-11-13 | 张小伏 | The preparation method of mask graphene/active carbon in-situ plural gel adsorbent |
| CN108813755A (en) * | 2018-07-04 | 2018-11-16 | 万绵水 | A kind of mask |
| CN113493198A (en) * | 2020-03-19 | 2021-10-12 | 中国科学院上海硅酸盐研究所 | Ultra-light, super-elastic and high-conductivity three-dimensional porous graphene material and preparation method thereof |
| CN113493198B (en) * | 2020-03-19 | 2022-10-14 | 中国科学院上海硅酸盐研究所 | Ultra-light, super-elastic and high-conductivity three-dimensional porous graphene material and preparation method thereof |
| CN113405861A (en) * | 2021-07-28 | 2021-09-17 | 东南大学 | Novel sampling strip for detecting PM2.5 concentration in environment |
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