CN110669284B - Graphene composite material and preparation method thereof, and prepared product and application thereof - Google Patents
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Abstract
The invention relates to a graphene composite material and a preparation method thereof, and a prepared product and application thereof. The graphene composite material comprises a melt-blown resin matrix, and a rare earth element component and a graphene oxide component which are doped in the melt-blown resin matrix; the content of the graphene oxide component is 0.01 wt% -1 wt% of the melt-blown resin matrix; the rare earth element component is insoluble or insoluble in water, and the content of the rare earth element component is one millionth to five thousandths of the mass of the melt-blown resin matrix. The invention also relates to a finished product obtained by melting the composite material and physically combining the composite material with a macroporous braided fabric and/or a macroscopic porous carrier; and the application of the graphene composite material or the manufactured product in sewage treatment. The product improves the sewage treatment effect of different concentrations, different pollution degrees and even a small amount of heavy metal salt, and has stable and broad-spectrum sewage treatment capability of adapting to complex conditions.
Description
Technical Field
The invention relates to the field of graphene composite materials, in particular to a graphene composite material and a preparation method thereof, and a prepared product and application thereof.
Background
In recent years, along with the development of social modernization, the water quality conditions in many areas at home and abroad are reduced, for example, refractory blue-green algae appear in Taihu lake and nested lake, and water treatment and ecological restoration become important points of social attention. Aiming at serious eutrophication water body, the biological method is a method which is frequently adopted and has high efficiency, low cost and small secondary pollution, and the traditional water treatment technical system still stays in numerous biotechnological improvements and materialization technical grafting. The future water treatment technology is based on the aspects of micro breakthrough, structural design and the like, has a water environment micro regulation and control target in the aspect of micro mechanism application, and has ecological compatibility of water treatment and a water environment in the aspect of macro guidance. The research and development of the method are mainly characterized in that a technology, a process and equipment which are simpler, more efficient and more sustainable in engineering application are created by creating a new technology and a core product for water treatment of the next generation of terminal.
The design that the ecological base of sectional type passes through the cascade structure, it divide into comparatively loose part and comparatively closely knit part, place according to the regular order of biological bacterial colony development and motion, in loose part to fibre braided structure can realize settling of particulate matter and do benefit to the alga growth and reproduction to the at utmost, promote species diversification and in denser part, then form the region that the anaerobe survived through closely knit fibre braided structure, can also form between the two and form the facultative colony. Thereby constructing an ideal 'aerobic-facultative-anaerobic' environment, realizing the processes of high-efficiency nitrogen and phosphorus removal and organic matter degradation, and leading the biological membrane to be capable of naturally falling off. The maximum effectiveness of the ecological base lies in the regulation of the biological activity of bacterial colonies, and the breakthrough of understanding on the micro process is required to be realized by combining materials with engineering technology and continuously practicing and exploring the engineering technology to integrate relevant coupling theory and technology, principle and application.
Graphene (graphene) is a material with various excellent properties appearing in recent years, such as highest electrical conductivity, highest thermal conductivity, best electron mobility, good transparency and the like, and when the graphene (graphene) is used as a filler of a resin matrix, the graphene (graphene) not only has obvious reinforcing effect [ L.Valentini,2018], but also can bring a plurality of new functions to a composite material, such as conductivity [ Marc ao A.Milani,2013, Jin-Yong Dong, Yuan Liu,2015], electromagnetic shielding performance [ Wei-Li Song,2014, Sima Kashi,2016, Yu-Dong Shi,2019], anti-icing performance [ L.Valentini, S.Bittolo Bon, M.Hern Idendez, M.A.Lopez-Manchado, N.M.Pugno,2018] and the like. The graphene has unique adjustable performance and unique performance after being cooperatively adjusted and controlled with other materials, is combined with a rare earth material, and can greatly improve the biological activity through bias voltage. The graphene has the greatest advantage that the conductivity can be increased to a certain degree, and the corresponding structure and function design can be carried out according to specific application requirements.
The rare earth elements are 17 elements including scandium, yttrium and lanthanide elements in the periodic table of elements, and due to the change characteristics of f-layer electrons, the photoelectric and catalytic properties of the rare earth elements are very excellent, the rare earth content in China is rich, and the application research of the rare earth elements is very active. Research shows that the trace amount of RE element (ppm level) has exciting effect on the activity of saccharomycete, macro fungi, Brucella, glutamic acid bacillus, Rhodopseudomonas, tubercle bacillus, Bacillus thuringiensis and other microbes, and the RE element can combine with GTP, glutamyl synthetase and other microbes in colibacillus to speed up energy conversion and transfer energy directly to colibacillus alkaline phosphatase to promote the growth of bacteria and the decomposition of carbon source matter in substrate culture material. When the content is increased, the effect of suppressing the reaction is obtained.
Disclosure of Invention
The invention relates to a graphene composite material, which comprises a melt-blown resin matrix, and a rare earth element component and a graphene oxide component which are doped in the melt-blown resin matrix;
the content of the graphene oxide component is 0.01 wt% -1 wt% of the melt-blown resin matrix;
the rare earth element component is insoluble or insoluble in water, and the content of the rare earth element component is one millionth to five thousandths of the mass of the melt-blown resin matrix.
According to an aspect of the present invention, the present invention also relates to a method for preparing a graphene composite material, comprising:
A) carrying out spray drying and assembling on graphene feed liquid obtained by uniformly dispersing the rare earth element component and the graphene oxide component to obtain modified graphene;
incorporating the modified graphene into the melt-blown resin matrix using physical blending;
or;
B) carrying out spray drying and assembling on the dispersion liquid of the graphene oxide component to obtain a graphene assembly;
the mixture of the rare earth element component and the graphene assembly is incorporated into the melt blown resin matrix using physical blending.
The invention also relates to a finished product obtained by melting the graphene composite material and physically combining the graphene composite material with at least one of a macroporous braided fabric, a foaming product and a macroscopic porous carrier; and the application of the graphene composite material or the manufactured product in sewage treatment.
The graphene composite material and the finished product prepared from the graphene composite material have improved sewage treatment effects on sewage with different concentrations and different pollution degrees and even containing a small amount of heavy metal salt, and have stable and broad-spectrum sewage treatment capability suitable for complex conditions.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an electron micrograph of the product prepared in example 1;
FIG. 2 is an electron micrograph of the product prepared in example 2;
FIG. 3 is an electron micrograph of the product prepared in example 3.
Detailed Description
Reference will now be made in detail to embodiments of the invention, one or more examples of which are described below. Each example is provided by way of explanation, not limitation, of the invention. In fact, it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. For instance, features illustrated or described as part of one embodiment, can be used on another embodiment to yield a still further embodiment.
It is therefore intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. Other objects, features and aspects of the present invention are disclosed in or are apparent from the following detailed description. It is to be understood by one of ordinary skill in the art that the present discussion is a description of exemplary embodiments only, and is not intended as limiting the broader aspects of the present invention.
The invention relates to a graphene composite material, which comprises a melt-blown resin matrix, and a rare earth element component and a graphene oxide component which are doped in the melt-blown resin matrix;
the graphene oxide component is present in an amount of 0.01 wt% to 1 wt%, such as 0.05 wt%, 0.1 wt%, 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.6 wt%, 0.7 wt%, 0.8 wt%, or 0.9 wt%, of the melt blown resin matrix;
the rare earth element component is insoluble or water-insoluble and is contained in an amount of one part per million to five per thousand, for example, one ten thousandth or one ten thousandth, based on the mass of the melt-blown resin matrix.
Wherein the rare earth element component and the graphene oxide component are incorporated into the melt-blown resin matrix in the form of modified graphene generated by both or in the form of a mixture of an assembly of the graphene oxide component and the rare earth element component.
In some embodiments, the active ingredient of the rare earth element component is one or more of lanthanum, praseodymium, gadolinium, terbium, lutetium, cerium, neodymium.
In some embodiments, the rare earth element component is selected from:
a) a rare earth element precursor capable of reacting with any one of a biological, biological metabolite, non-biological acid/base to slowly release a rare earth element; and
b) stearates, sulfates, molybdophosphates of rare earth elements not belonging to the rare earth elements defined in a).
a) The components in the formula (I) can specifically comprise one or a mixture of more of a carbonate, an amorphous oxide bonding state, a heteropolyacid salt and other reagents capable of slowly releasing rare earth ions, an acid-extractable or hydrolyzable reagent such as an oxide and a sulfide, and an oleate, a stearate, an octoate (and other low molecular weight organic acid salts) and a humus adsorption type rare earth reagent. The components can promote various microorganisms such as ammoniated microorganisms, fungi, actinomycetes and cellulolytic bacteria, and promote the growth of various plants (preferably algae) such as anabaena, crypthecodinium cohnii, microcystis and moon-sprout; and may slowly release rare earth elements in the above-mentioned biological or environmental acid/base interaction. The released rare earth elements can improve the photosynthetic oxygen release activity by promoting the synthesis of chlorophyll a, can also promote the absorption and utilization of phosphorus, potassium and other elements and the nitrogen metabolism process of plants, greatly enhances the stress resistance of the plants, has more influence on the activity of the microcystis than on the crescent moon, is favorable for the microcystis to become an advantageous species in lakes, and can greatly improve the activity of the artificial grass by the mode. The rare earth is applied in low amount to enhance the resistance of plants to adverse conditions such as high temperature, low temperature, salinization, mineral deficiency and the like, so that the artificial grass material obtained by the process has stable and broad-spectrum sewage treatment capability of adapting to complex conditions
b) The stearate (preferably lanthanum stearate), sulfate, molybdenum phosphate and other insoluble salts in the graphene composite material have low toxicity, and the thermal stability and lubricity are excellent, so that the graphene composite material can be used for degrading environmental-friendly products such as plastics and can also be used in PVC transparent food packaging materials, and therefore, the graphene composite material can also be used as an auxiliary component to be added to improve the chemical performance of the graphene composite material.
In some embodiments, the melt blown resin matrix is selected from one or more of polypropylene resin, polyethylene resin, nylon resin, dacron resin, and polyurethane resin.
In some embodiments, the meltblown resin matrix is a degradable resin such as a thermal degradation type, a photodegradation type, a biodegradation type, and/or a metallocene resin.
In some embodiments, the graphene oxide is prepared via Hummers or Brodie methods, preferably Hummers. Currently, in the methods for preparing graphene oxide by chemical methods, the Hummers method is the most widely used method, and compared with the Brodie method, the Hummers method has less reaction time and does not generate toxic gases such as chlorine and the like.
According to an aspect of the present invention, the present invention also relates to a method for preparing a graphene composite material, comprising:
A) carrying out spray drying and assembling on graphene feed liquid obtained by uniformly dispersing the rare earth element component and the graphene oxide component to obtain modified graphene;
incorporating the modified graphene into the melt-blown resin matrix using physical blending;
or;
B) carrying out spray drying and assembling on the dispersion liquid of the graphene oxide component to obtain a graphene assembly;
the mixture of the rare earth element component and the graphene assembly is incorporated into the melt blown resin matrix using physical blending.
In some embodiments, the physical blending is melt blending such as twin screw, banburying, but is not limited to these processes.
In some embodiments, the temperature of the spray drying is 175 ℃ to 240 ℃, also selected from 180 ℃ to 230 ℃, such as 190 ℃, 200 ℃, 210 ℃, 220 ℃.
The air speed of the spray drying may be, for example, 50m3/h～300m3And the wind speed can be calibrated according to the yield.
According to an aspect of the invention, the invention also relates to a manufactured product, which is fused from the graphene composite material as described above, and is at least one of a macroporous braid, a foamed product with a pore size between 0.5 μm and 10 μm, and a macro porous support with a pore size between 20 μm and 500 μm.
In some embodiments, the foamed product has a pore size of 1 μm to 8 μm.
In some embodiments, the macropore support has a pore size in the range of 50 μm to 200 μm.
In some embodiments, the macroporous woven fabric is selected from nylon.
In some embodiments, the macro-porous support is selected from one or more of a sponge, meltblown cotton, nonwoven fabric, nylon mesh, and activated carbon.
In some embodiments, the method of physically bonding is one or a combination of woven, segmented, and sandwich bonding to each other.
In some embodiments, the article of manufacture is a hydraulic product.
In some embodiments, the hydraulic product is artificial grass or a floating island.
According to an aspect of the invention, the invention also relates to the use of a graphene composite material as described above, or of a manufactured article as described above, in sewage treatment.
Embodiments of the present invention will be described in detail with reference to examples.
Example 1
1) Preparing raw material graphene: taking graphene oxide dispersion liquid prepared by a Hummers method, adjusting the concentration of the graphene oxide dispersion liquid to be 1g/L, mixing and adding rare earth components such as lanthanum stearate, cerium oxide (molar ratio is 1: 1) and the like which are slowly released along with the environment, wherein the content of the rare earth components is 10 wt% of the content of graphene;
and (3) carrying out spray drying to obtain modified graphene ultrafine powder, setting the temperature at 200 ℃, adjusting the wind speed, and finally obtaining the modified graphene ultrafine powder with the yield of 18 g/h.
2) Selecting biodegradable PP melt-blown resin with the density of 0.88-0.91 g/cm3The melt index is 1500 +/-100 g/10 min; the graphene rare earth mixed powder sample is added through the degradation process, and the addition amount is 0.1 wt%.
3) Melt spinning through a spinneret (Japan Carson) with the aperture of 0.35mm, wherein the melt-blowing temperature is 255-270 ℃, and the feeding amount is 6-15 kg/h; at the same time, 0.1 wt% of nylon is added into the mixture through nylon spinning, and the mixture is woven into a felt, so that the aperture of the felt is 35 mu m.
4) Sandwiching the two layers of nylon felt prepared in the step 3) into fused silk spray cotton to obtain experimental artificial grass, and treating the experimental artificial grass in a cut-off water pool of Suzhou river for 3 months at the temperature of 25 ℃. The COD content is determined to be reduced by about 15 percent compared with the traditional ecological base.
Example 2
1) Preparing raw material graphene: taking graphene oxide dispersion liquid prepared by a Hummers method, adjusting the concentration of the graphene oxide dispersion liquid to be 1g/L, and performing ultrasonic treatment for 1h and then performing centrifugal separation on the modified graphene oxide;
and (3) carrying out spray drying to obtain modified graphene ultrafine powder, setting the temperature at 200 ℃, adjusting the air speed, and finally obtaining the modified graphene ultrafine powder with the yield of 22 g/h.
2) Selecting biodegradable PP melt-blown resin with the density of 0.88-0.91 g/cm3The melt index is 1500 +/-100 g/10 min; the graphene powder sample and the nano-scale rare earth mixed sample (lanthanum stearate: neodymium oxide: cerium oxide, molar ratio 1: 1: 1) were added through a degradation process, with an addition amount of 0.1 wt%.
3) Melt spinning through a spinneret (Japan Carson) with the aperture of 0.35mm, wherein the melt-blowing temperature is 255-270 ℃, and the feeding amount is 6-15 kg/h; at the same time, 0.1 wt% of nylon is added into the mixture through nylon spinning, and the mixture is woven into a felt, so that the aperture of the felt is 35 mu m.
4) Sandwiching the two layers of nylon felt prepared in the step 3) into fused silk spray cotton to obtain experimental artificial grass, and treating the experimental artificial grass in a cut-off water pool of Suzhou river for 3 months at the temperature of 25 ℃. The COD content is determined to be reduced by about 21.1 percent compared with the traditional ecological base.
Example 3
1) Preparing raw material graphene: taking graphene oxide dispersion liquid prepared by a Hummers method, adjusting the concentration of the graphene oxide dispersion liquid to be 2g/L, and mixing and adding rare earth components such as gadolinium oleate, terbium oxide (molar ratio of 1: 4) and the like which are slowly released along with the environment, wherein the content of the rare earth components is 1 wt% of the content of graphene;
and (3) carrying out spray drying to obtain modified graphene ultrafine powder, setting the temperature at 230 ℃, and adjusting the wind speed to obtain the final yield of 24 g/h.
2) Selecting photodegradable polyester melt-blown resin with the density of 1.20-1.33 g/cm3The melt index is 1700 +/-100 g/10 min; adding a graphene rare earth mixed powder sample through a degradation process, wherein the addition amount of the graphene rare earth mixed powder sample is0.2wt％。
3) Spinning was carried out as in example 1, except that the nylon added was replaced with polypropylene.
Adding the molten silk-spraying cotton prepared in the step 3) into the non-woven fabric in sections to obtain the experimental artificial grass.
Example 4
1) Preparing raw material graphene: taking graphene oxide dispersion liquid prepared by a Hummers method, adjusting the concentration of the graphene oxide dispersion liquid to be 1g/L, and performing ultrasonic treatment for 1h and then performing centrifugal separation on the modified graphene oxide;
and (3) carrying out spray drying to obtain modified graphene ultrafine powder, setting the temperature at 180 ℃, and adjusting the wind speed to obtain the final yield of 22 g/h.
2) Selecting metallocene PP melt-blown resin with the density of 0.95-1.01 g/cm3The melt index is 1450 +/-100 g/10 min; the graphene powder sample and a nano-scale rare earth mixed sample (lutetium octoate: neodymium sulfate: terbium oxide, molar ratio 1: 1: 1) are added in a degradation process, and the addition amount is 0.1 wt%.
3) Spinning was carried out as in example 1.
4) The material obtained by melt-blowing the composite material in the mode is compounded with a macroporous braided fabric or used as a bottom raw material of an artificial island in contact with water.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A graphene composite material comprises a melt-blown resin matrix, and a rare earth element component and a graphene oxide component which are doped in the melt-blown resin matrix;
the content of the graphene oxide component is 0.01 wt% -1 wt% of the melt-blown resin matrix;
the rare earth element component is insoluble or insoluble water, and the content of the rare earth element component is one millionth to five thousandths of the mass of the melt-blown resin matrix;
the rare earth element component is selected from:
a) a rare earth element precursor capable of reacting with any one of a biological, biological metabolite, non-biological acid/base to slowly release a rare earth element; and
b) stearates, sulfates, molybdophosphates of rare earth elements not belonging to the rare earth elements defined in a).
2. The graphene composite material according to claim 1, wherein the melt-blown resin matrix is selected from one or more of polypropylene resin, polyethylene resin, nylon resin, polyester resin, and polyurethane resin.
3. The graphene composite material according to claim 1 or 2, wherein the melt-blown resin matrix is a degradable resin and/or a metallocene resin.
4. The method for preparing the graphene composite material according to any one of claims 1 to 3, comprising:
A) carrying out spray drying and assembling on graphene feed liquid obtained by uniformly dispersing the rare earth element component and the graphene oxide component to obtain modified graphene;
incorporating the modified graphene into the melt-blown resin matrix using physical blending;
or;
B) carrying out spray drying and assembling on the dispersion liquid of the graphene oxide component to obtain a graphene assembly;
the mixture of the rare earth element component and the graphene assembly is incorporated into the melt blown resin matrix using physical blending.
5. The method for preparing the graphene composite material according to claim 4, wherein the temperature of the spray drying is 180 ℃ to 230 ℃.
6. A finished product obtained by melting the graphene composite material as claimed in any one of claims 1 to 3 and physically combining the graphene composite material with at least one of a macroporous braided fabric, a foamed product with a pore size of 0.5-10 μm and a macroscopic porous carrier with a pore size of 20-500 μm.
7. The article of manufacture of claim 6 wherein the physical bonding is one or a combination of woven, segmented, and sandwich bonded to each other.
8. The manufactured product according to claim 6 or 7, characterized in that it is a water craft product.
9. The manufacture of claim 8 wherein the hydraulic product is artificial grass or a floating island.
10. Use of the graphene composite material according to any one of claims 1 to 3 or the manufactured product according to any one of claims 6 to 9 in sewage treatment.
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