CN110339670A - A kind of graphene composite material and preparation method thereof containing negative oxygen ion - Google Patents
A kind of graphene composite material and preparation method thereof containing negative oxygen ion Download PDFInfo
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Abstract
The invention discloses a kind of graphene composite material and preparation method thereof containing negative oxygen ion, material for air purification field, the graphene composite material containing negative oxygen ion includes component A and component B, in which: the mass percent of component A is 95%~99.67%；The mass percent of component B is 0.33%~5%；Wherein: component A by mass percent it is following at being grouped as: anthracite 82.6%~93.4%, binder 3.3%~8.7% and the negative ion powder 3.3%~8.7% of activation；Component B is that 66.7%~83.3% graphene and 16.7%~33.3% surfactant form by mass percent.The features such as component A and component B has synergistic effect, and being somebody's turn to do the graphene composite material containing negative oxygen ion has high mechanical strength, and pore structure is flourishing, and large specific surface area, adsorption rate is fast, and adsorption capacity is high, is easy to regenerate, durable.
Description
Technical field
The invention belongs to material for air purification fields, and in particular to a kind of graphene composite material containing negative oxygen ion and
Preparation method.
Background technique
In in recent years, air quality is always the problem that people are concerned about very much, with being done step-by-step for fairly comfortable life,
People also have higher requirement the quality of home environment, and finishing has become fashion at home.However people often ignore through
Cross influence of the living environment of finishing to health and safety.It is plastics that ceiling, wall veneer especially in house use, heat-insulated
Generally all contain formaldehyde in material and plastic furniture.Formaldehyde is a kind of colourless readily soluble irritative gas, when indoor content is 0.1
Just there are peculiar smell and sense of discomfort when milligram/cubic meter；0.5 milligram/cubic metre can stimulate eyes to cause to shed tears；0.6 milligram/cubic metre
Shi Yinqi throat discomfort or pain；Concentration is high again to cause Nausea and vomiting, cough, uncomfortable in chest, asthma even pulmonary emphysema；30 milligrams/
It can lead to death at once when cubic meter.Long Term Contact low dosage formaldehyde can also cause chronic respiratory disease, feminine menstrual disorder,
Pregnancy syndrome causes newborn's constitution to reduce, chromosome abnormality, or even causes nasopharyngeal carcinoma.Have there are also indoor general volatile
Machine object (abbreviation TVOC) is mainly from paint, aqueous coating, adhesive, cosmetics, detergent, wood-based plate, wallpaper, carpet etc..
TVOC is affected to human body, and the smell for directly stimulating human body and other organs are caused irritation mistake by its excessive concentration
Quick reaction, nerve effect etc..So air cleaning now becomes particularly important, especially the good of indoor air quality is closed with bad
It is human health degree.
Summary of the invention
In order to solve the above problems existing in the present technology, it is multiple that the present invention provides a kind of graphenes containing negative oxygen ion
Condensation material.
The technical scheme adopted by the invention is as follows a kind of graphene composite material containing negative oxygen ion, including component A and
Component B, in which: the mass percent of component A is 95%~99.67%；The mass percent of component B is 0.33%~5%；
Wherein: component A by mass percent it is following at being grouped as: the anthracite 82.6%~93.4% of activation, bonding
Agent 3.3%~8.7% and negative ion powder 3.3%~8.7%；
Component B is 66.7%~83.3% graphene and 16.7%~33.3% surfactant by mass percent
Composition.
The working principle of the invention has the beneficial effect that the graphene composite material for containing negative oxygen ion for indoor
The pernicious gases such as formaldehyde, TVOC and PM2.5 can be dispelled effectively, and because that can discharge a large amount of negative oxygen ion, be born
Oxonium ion can sterilize, dedusting, have certain effect to the disinfection and purification of air；It can also enhance human immunity, improve body
Detoxification ability makes the uneven normalization of hormone, avoids the generation of allergic reaction；Graphene has porous structure, has one
Fixed adsorption capacity, can enhance the adsorption capacity of component A, and component A and component B have synergistic effect.
The graphene composite material for containing negative oxygen ion has high mechanical strength, and pore structure is flourishing, large specific surface area,
The features such as adsorption rate is fast, and adsorption capacity is high, is easy to regenerate, durable.
It further limits, the anthracitic granularity is 100~400 mesh.
The working principle of the invention has the beneficial effect that so that anthracitic carbonization effect is more ideal, and is capable of increasing
More beneficial ingredients are generated so that reaction thoroughly carries out with the contact area of graphene powder.
It further limits, described adhesive is coal tar, and moisture content is less than or equal to 5% in coal tar.
The working principle of the invention has the beneficial effect that phosphorus content is high in coal tar, is capable of a part of component A, plays
The effect of skeleton；Moisture content makes coal tar have good viscosity performance less than or equal to 5% in coal tar, does not influence nothing
The intensity of bituminous coal.
It further limits, the gas activation agent is vapor；The surfactant is polyethylene pyrrole network alkanone, 12
In alkyl pyrrolidone, dodecyl sodium sulfate, dimethylformamide, polyvinyl alcohol, polyethylene glycol or sodium lignin sulfonate
The mixture of one or more formation.
The present invention also provides a kind of preparation methods of graphene composite material containing negative oxygen ion, comprising the following steps:
S1: choosing and anthracite and crushed, by binder, negative ion powder and smashed anthracite mixing kneading,
Mixture A is obtained, mixture A is squeezed into carbon item and carbon item is cut into granular short carbon item；
S2: the short carbon item in step S1 is carbonized to obtain anhydrous short carbon item；
S3: anhydrous short carbon item is activated in gas activation agent, and cooling obtains component A；
S4: graphene, surfactant and solvent are mixed and stirred for uniformly, to obtain graphene dispersion solution；
S5: heating after component A is mixed with graphene dispersion solution, and heating time is 1~4 hour, and heating temperature 40~
80℃；Then it dries, drying temperature is 100~200 DEG C, and drying time is 5~15 hours, be can be obtained containing negative oxygen ion
Graphene composite material.
The working principle of the invention has the beneficial effect that the preparation method process flow is simple, and preparation cost is low, economy effect
Benefit is higher, is applicable to large-scale industrial production；By preparing component A and graphene dispersion solution, graphene dispersion respectively
Effective component in solution is component B, by heated after component A and graphene dispersion solution are mixed according to a certain percentage
Journey, the process enable graphene powder to be distributed in the surface component A and its hole well, and it is good to form stable and performance
The good graphene composite material containing negative oxygen ion.
It further limits, kneading temperature is 65~85 DEG C in step S1, and the kneading time is 15~30 minutes；It is squeezed in step S1
The pressure for pressing through journey is 190-230kgf/cm2。
It further limits, carburizing temperature is 480~520 DEG C in step S2, and heating rate is 15~20 DEG C/min, when carbonization
Between be 1~10 hour.
It further limits, activation temperature is 900~950 DEG C, activation time 2~10 hours in step S3.
It further limits, the concentration of graphene dispersion solution is 1mg/ml~10mg/ml in step S4.
It further limits, component A needs stirring 20~60 minutes in step S5 after mixing with graphene dispersion solution.
Detailed description of the invention
Fig. 1 is the process flow chart for preparing the graphene composite material containing negative oxygen ion.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention is further elaborated.
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc.
Term shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can be machine
Tool connection, is also possible to be electrically connected；It can be directly connected, two members can also be can be indirectly connected through an intermediary
Connection inside part.For the ordinary skill in the art, above-mentioned term can be understood in this hair as the case may be
Concrete meaning in bright.
In description of the invention, what some structures or device were not described specifically, it is interpreted as being able to achieve in the prior art
Structure or device.
Control group 1
A kind of preparation method of the material with adsorption capacity, comprising the following steps:
S1: it chooses feed coal and enters factory's crushing, feed coal is anthracite.Raw material anthracite is first crushed to the fineness of 200 mesh；
Then anthracite is weighed, coal tar is measured, phosphorus content is high in coal tar, can play the role of skeleton, the moisture in coal tar
≤ 5%, modest viscosity and the intensity that will not influence carbon item；
S2: and then by smashed anthracite and coal tar according to quality be respectively 96.2g and 3.84g mixing kneading；It rubs
Temperature control is at 65 DEG C, kneading 15 minutes during pinching；
S3: and then use hydraulic press the material extruding after kneading at the carbon item of high solidity, pressure is controlled in 190kgf/
cm2；
S4: the carbon item that step S3 is obtained is carbonized, specifically: carbonization then be need in the case where completely cutting off air into
Row, and the temperature needed is 480 DEG C, and heating rate will be controlled in 15 DEG C/min, and carbonization time is 1 hour；
S5: activation process, usually gas activation, the anhydrous short carbon item for first obtaining step S4 are put into activation furnace, so
Vapor is passed through in activation process afterwards, at 900 DEG C, activation time is 2 hours for the temperature control of activation；
S6: the short carbon item of activation that step S5 activation is completed is put into the cooling zone of machine, the temperature for activating short carbon item is cold
But to 60 DEG C, it is then sieved into cylindrical particle carbon and powder, obtains component G.
S7: polyethylene pyrrole network alkanone 0.5g and water 500ml stirring, room temperature are ultrasonically treated 20 minutes, are configured to 1mg/ml
Aqueous dispersion A；
S8: by step S7 aqueous dispersion A and component G mix；
S9: mixture in step S8 is stirred 20 minutes, then reacts 1 hour at 40 DEG C, is warming up to again after the completion
100 DEG C dry 5 hours, and finally drying terminates that the materials A with adsorption capacity can be obtained, and measures its performance, as shown in table 1.
Control group 2
A kind of preparation method of the material with adsorption capacity, comprising the following steps:
S1: it chooses feed coal and enters factory's crushing, feed coal is anthracite.Raw material anthracite is first crushed to the fineness of 200 mesh；
Then anthracite is weighed, coal tar is measured, phosphorus content is high in coal tar, can play the role of skeleton, the moisture in coal tar
≤ 5%, modest viscosity and the intensity that will not influence carbon item；
S2: and then by smashed anthracite and coal tar according to quality 96.2g and 3.84g mixing kneading.Kneading process
Middle temperature control is at 65 DEG C, kneading 15 minutes；
S3: and then use hydraulic press the material extruding after kneading at the carbon item of high solidity, pressure is controlled in 190kgf/
cm2；
S4: the carbon item that step S3 is obtained is carbonized, specifically: carbonization then be need in the case where completely cutting off air into
Row, and the temperature needed is 480 DEG C, and heating rate will be controlled in 15 DEG C/min, and carbonization time is 1 hour；
S5: activation process, usually gas activation, the anhydrous short carbon item for first obtaining step S4 are put into activation furnace, so
Vapor is passed through in activation process afterwards, at 900 DEG C, activation time is 2 hours for the temperature control of activation；
S6: the short carbon item of activation that step S5 activation is completed is put into the cooling zone of machine, the temperature for activating short carbon item is cold
But to 60 DEG C, it is then sieved into cylindrical particle carbon and powder, obtains component G.
S7: quality is that 0.33g graphene powder, 0.17g polyethylene pyrrole network alkanone and 330ml are mixed, and room temperature is super
Sonication 20 minutes, it is configured to the graphene dispersion aqueous solution of 1mg/ml；
S8: by step S7 graphene dispersion aqueous solution and component G mix；
S9: mixture in step S8 is stirred 20 minutes, then reacts 1 hour at 40 DEG C, is warming up to again after the completion
100 DEG C dry 5 hours, and finally drying terminates that the material B with adsorption capacity can be obtained, and measures its performance, as shown in table 1.
Control group 3
A kind of preparation method of the material with adsorption capacity, comprising the following steps:
S1: it chooses feed coal and enters factory's crushing, feed coal is anthracite.Raw material anthracite is first crushed to the fineness of 200 mesh；
Then anthracite and negative ion powder are weighed in proportion, measures coal tar, phosphorus content is high in coal tar, can play the work of skeleton
With, moisture≤5% in coal tar, modest viscosity and the intensity that will not influence carbon item；
S2: and then by smashed anthracite 96.2g, negative ion powder 3.84g and coal tar 3.84g mixing kneading.Kneading
Temperature control is at 65 DEG C, kneading 15 minutes in the process；
S3: and then use hydraulic press the material extruding after kneading at the carbon item of high solidity, pressure is controlled in 190kgf/
cm2；
S4: the carbon item that step S3 is obtained is carbonized, specifically: carbonization then be need in the case where completely cutting off air into
Row, and the temperature needed is 480 DEG C, and heating rate will be controlled in 15 DEG C/min, and carbonization time is 1 hour；
S5: activation process, usually gas activation, the anhydrous short carbon item for first obtaining step S4 are put into activation furnace, so
Vapor is passed through in activation process afterwards, at 900 DEG C, activation time is 2 hours for the temperature control of activation；
S6: the short carbon item of activation that step S5 activation is completed is put into the cooling zone of machine, the temperature for activating short carbon item is cold
But to 60 DEG C, it is then sieved into cylindrical particle carbon and powder, obtains component C.
S7: polyethylene pyrrole network alkanone 0.5g and water 500ml stirring, room temperature are ultrasonically treated 20 minutes, are configured to 1mg/ml
Aqueous dispersion B；
S8: by step S7 aqueous dispersion B and component C mix；
S9: mixture in step S8 is stirred 20 minutes, then reacts 1 hour at 40 DEG C, is warming up to again after the completion
100 DEG C dry 5 hours, and finally drying terminates that the material C with adsorption capacity can be obtained, and measures its performance, as shown in table 1.
Embodiment 1
A kind of preparation method of the graphene composite material containing negative oxygen ion, comprising the following steps:
S1: it chooses feed coal and enters factory's crushing, feed coal is anthracite.Raw material anthracite is first crushed to the fineness of 200 mesh；
Then anthracite and negative ion powder are weighed in proportion, measures coal tar, phosphorus content is high in coal tar, can play the work of skeleton
With, moisture≤5% in coal tar, modest viscosity and the intensity that will not influence carbon item；
S2: and then by smashed anthracite 96.2g, negative ion powder 3.84g and coal tar 3.84g mixing kneading.Kneading
Temperature control is at 65 DEG C, kneading 15 minutes in the process；
S3: and then use hydraulic press the material extruding after kneading at the carbon item of high solidity, pressure is controlled in 190kgf/
cm2；
S4: the carbon item that step S3 is obtained is carbonized, specifically: carbonization then be need in the case where completely cutting off air into
Row, and the temperature needed is 480 DEG C, and heating rate will be controlled in 15 DEG C/min, and carbonization time is 1 hour；
S5: activation process, usually gas activation, the anhydrous short carbon item for first obtaining step S4 are put into activation furnace, so
Vapor is passed through in activation process afterwards, at 900 DEG C, activation time is 2 hours for the temperature control of activation；
S6: the short carbon item of activation that step S5 activation is completed is put into the cooling zone of machine, the temperature for activating short carbon item is cold
But to 60 DEG C, it is then sieved into cylindrical particle carbon and powder, obtains component C.
S7: quality is that 0.33g graphene powder, 0.17g polyethylene pyrrole network alkanone and 330ml are mixed, and room temperature is super
Sonication 20 minutes, it is configured to the graphene dispersion aqueous solution of 1mg/ml；
S8: by step S7 graphene dispersion aqueous solution and component C mix；
S9: mixture in step S8 is stirred 20 minutes, then reacts 1 hour at 40 DEG C, is warming up to again after the completion
100 DEG C dry 5 hours, and finally drying terminates that the graphene composite material of releasable negative oxygen ion can be obtained, and measure its performance,
As shown in table 1.
Embodiment 2
A kind of preparation method of the graphene composite material containing negative oxygen ion, comprising the following steps:
S1: it chooses feed coal and enters factory's crushing, feed coal is anthracite.Raw material anthracite is first crushed to the fineness of 100 mesh；
Then anthracite and negative ion powder are weighed in proportion, measures coal tar, phosphorus content is high in coal tar, can play the work of skeleton
With, moisture≤5% in coal tar, modest viscosity and the intensity that will not influence carbon item；
S2: and then by smashed anthracite 91.48g, negative ion powder 8.52g and coal tar 8.52g mixing kneading.Kneading
Temperature control is at 75 DEG C, kneading 26 minutes in the process；
S3: and then use hydraulic press the material extruding after kneading at the carbon item of high solidity, pressure is controlled in 209kgf/
cm2；
S4: the carbon item that step S3 is obtained is carbonized, specifically: carbonization then be need in the case where completely cutting off air into
Row, and the temperature needed is 500 DEG C, and heating rate will be controlled in 18 DEG C/min, and carbonization time is 8 hours；
S5: activation process, usually gas activation, the anhydrous short carbon item for first obtaining step S4 are put into activation furnace, so
Vapor is passed through in activation process afterwards, at 934 DEG C, activation time is 6 hours for the temperature control of activation；
S6: the short carbon item of activation that step S5 activation is completed is put into the cooling zone of machine, the temperature for activating short carbon item is cold
But to 46 DEG C hereinafter, be then sieved into cylindrical particle carbon and powder, component E is obtained.
S7:1.0g graphene powder, 0.08g dodecyl pyrrolidone, 0.08g dodecyl sodium sulfate, 0.08g diformazan
Base formamide, 0.08g polyvinyl alcohol and the stirring of 166.7ml water, room temperature are ultrasonically treated 64 minutes, are configured to the graphite of 6mg/ml
Alkene aqueous dispersion；
S8: by step S7 graphene dispersion aqueous solution and component E mix；
S9: mixture in step S8 is stirred 43 minutes, then reacts 3 hours at 72 DEG C, is warming up to again after the completion
156 DEG C dry 10 hours, and finally drying terminates that the graphene composite material of releasable negative oxygen ion can be obtained, and measure its property
Can, as shown in table 1.
Embodiment 3
A kind of preparation method of the graphene composite material containing negative oxygen ion, comprising the following steps:
S1: it chooses feed coal and enters factory's crushing, feed coal is anthracite.Raw material anthracite is first crushed to the fineness of 400 mesh；
Then anthracite and negative ion powder are weighed in proportion, measures coal tar, phosphorus content is high in coal tar, can play the work of skeleton
With, moisture≤5% in coal tar, modest viscosity and the intensity that will not influence carbon item；
S2: and then by smashed anthracite 91.48g, negative ion powder 8.52g and coal tar 8.52g mixing kneading.Kneading
Temperature control is at 85 DEG C, kneading 30 minutes in the process；
S3: and then use hydraulic press the material extruding after kneading at the carbon item of high solidity, pressure is controlled in 230kgf/
cm2；
S4: the carbon item that step S3 is obtained is carbonized, specifically: carbonization then be need in the case where completely cutting off air into
Row, and the temperature needed is 520 DEG C, and heating rate will be controlled in 20 DEG C/min, and carbonization time is 10 hours；
S5: activation process, usually gas activation, the anhydrous short carbon item for first obtaining step S4 are put into activation furnace, so
Vapor is passed through in activation process afterwards, at 950 DEG C, activation time is 10 hours for the temperature control of activation；
S6: the short carbon item of activation that step S5 activation is completed is put into the cooling zone of machine, the temperature for activating short carbon item is cold
But to 30 DEG C hereinafter, be then sieved into cylindrical particle carbon and powder, component F is obtained.
S7: graphene powder 4.562g, 0.229g dimethylformamide, 0.229g polyvinyl alcohol, 0.229g polyethylene glycol,
0.229g sodium lignin sulfonate and the stirring of 456.2ml water, room temperature are ultrasonically treated 80 minutes, are configured to the graphene of 10mg/ml
Aqueous dispersion；
S8: by step S7 graphene dispersion aqueous solution and component F mix；
S9: mixture in step S8 is stirred 60 minutes, then reacts 4 hours at 80 DEG C, is warming up to again after the completion
200 DEG C dry 15 hours, and finally drying terminates that the graphene composite material of releasable negative oxygen ion can be obtained, and measure its property
Can, as shown in table 1.
Each substance performance table of table 1
As known from compared to Example 1 by control group 1, it is added to the releasable negative oxygen ion of negative ion powder and graphene powder
Graphene composite material, iodine sorption value, negative oxygen ion burst size, wear rate and compression strength all have good performance；
As known from compared to Example 1 by control group 2, when negative ion powder is added, negative oxygen ion burst size is obviously increased, and is conducive to human body
Health；As known from compared to Example 1 by control group 3, when graphene powder is added, iodine sorption value, wear rate and compression strength
Apparent increase is all had, is conducive to the absorption of small molecular weight impurity, such as formaldehyde, TVOC and PM2.5 pernicious gas, and can
Extend using the time and is readily transported.
The present invention is not limited to above-mentioned optional embodiment, anyone can show that other are various under the inspiration of the present invention
The product of form, however, make any variation in its shape or structure, it is all to fall into the claims in the present invention confining spectrum
Technical solution, be within the scope of the present invention.
Claims (10)
1. a kind of graphene composite material containing negative oxygen ion, which is characterized in that including component A and component B, in which: component A
Mass percent be 95%~99.67%；The mass percent of component B is 0.33%~5%；
Wherein: component A by mass percent it is following at being grouped as: anthracite 82.6%~93.4%, the binder of activation
3.3%~8.7% and negative ion powder 3.3%~8.7%；
Component B is 66.7%~83.3% graphene and 16.7%~33.3% surfactant group by mass percent
At.
2. graphene composite material according to claim 1, which is characterized in that the anthracitic granularity is 100~400
Mesh.
3. graphene composite material according to claim 1, which is characterized in that described adhesive is coal tar, coal tar
Middle moisture content is less than or equal to 5%.
4. graphene composite material according to claim 1-3, which is characterized in that the gas activation agent is water
Steam；The surfactant is polyethylene pyrrole network alkanone, dodecyl pyrrolidone, dodecyl sodium sulfate, dimethyl methyl
One of amide, polyvinyl alcohol, polyethylene glycol or sodium lignin sulfonate or the mixture of a variety of formation.
5. a kind of preparation method of the graphene composite material according to any one of claims 1-4 containing negative oxygen ion,
It is characterized in that, comprising the following steps:
S1: it chooses anthracite and is crushed, binder, negative ion powder and smashed anthracite mixing kneading obtain
Mixture A is squeezed into carbon item and carbon item is cut into granular short carbon item by mixture A；
S2: the short carbon item in step S1 is carbonized to obtain anhydrous short carbon item；
S3: anhydrous short carbon item is activated in gas activation agent, and cooling obtains component A；
S4: graphene, surfactant and solvent are mixed and stirred for uniformly, to obtain graphene dispersion solution；
S5: heating after component A is mixed with graphene dispersion solution, and heating time is 1~4 hour, 40~80 DEG C of heating temperature；
Then it dries, drying temperature is 100~200 DEG C, and drying time is 5~15 hours, and the graphite containing negative oxygen ion can be obtained
Alkene composite material.
6. preparation method according to claim 5, which is characterized in that kneading temperature is 65~85 DEG C in step S1, kneading
Time is 15~30 minutes；
The pressure of extrusion process is 190-230kgf/cm in step S12。
7. preparation method according to claim 5, which is characterized in that carburizing temperature is 480~520 DEG C in step S2, is risen
Warm speed is 15~20 DEG C/min, and carbonization time is 1~10 hour.
8. preparation method according to claim 5, which is characterized in that activation temperature is 900~950 DEG C in step S3, living
Change the time 2~10 hours.
9. preparation method according to claim 5, which is characterized in that the concentration of graphene dispersion solution is in step S4
1mg/ml~10mg/ml.
10. preparation method according to claim 5, which is characterized in that component A and graphene dispersion solution are mixed in step S5
Stirring is needed after conjunction 20~60 minutes.
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