阅读说明：本技术 一种碳纳米管/铁网光热材料的制备方法及应用 (Preparation method and application of carbon nanotube/iron mesh photo-thermal material ) 是由 姚忠平 顾燕然 徐云松 姜兆华 于 2021-10-08 设计创作，主要内容包括：一种碳纳米管/铁网光热材料的制备方法及应用,它涉及一种光热材料的制备方法及应用。本发明的目的是要解决现有光热转换材料存在制备方法复杂、转换效率低和循环性能差的缺点。一、铁网预处理；二、制备碳纳米管/铁网光热材料；三、表面处理。一种碳纳米管/铁网光热材料作为光热转换材料应用于太阳能蒸汽发生装置中,用于蒸发水。当光照强度为1kW·m～(-2)时,使用本发明制备的碳纳米管/铁网光热材料的水蒸发速率可达到1.77kg·m～(-2)·h～(-1)。本发明可获得一种碳纳米管/铁网光热材料。(A preparation method and application of a carbon nano tube/iron mesh photo-thermal material relate to a preparation method and application of a photo-thermal material. The invention aims to solve the defects of complex preparation method, low conversion efficiency and poor cycle performance of the conventional photothermal conversion material. Firstly, pretreating an iron net; secondly, preparing a carbon nano tube/iron mesh photo-thermal material; and thirdly, surface treatment. A carbon nanotube/iron net photothermal material is used as photothermal conversion material in a solar steam generator for evaporating water. When the illumination intensity is 1 kW.m ‑2 The water evaporation rate of the carbon nano tube/iron net photo-thermal material prepared by the invention can reach 1.77 kg.m ‑2 ·h ‑1 . The invention can obtain the carbon nano tube/iron net photo-thermal material.)

1. A preparation method of a carbon nanotube/iron mesh photothermal material is characterized in that the preparation method of the carbon nanotube/iron mesh photothermal material is completed according to the following steps:

firstly, pretreating an iron net:

cutting the iron net to obtain the cut iron net; immersing the cut iron net into concentrated hydrochloric acid for ultrasonic treatment, taking out the iron net, sequentially and respectively ultrasonically cleaning the iron net in deionized water and absolute ethyl alcohol, and finally drying to obtain a pretreated iron net;

secondly, preparing the carbon nano tube/iron mesh photo-thermal material:

covering melamine on the upper surface and the lower surface of the pretreated iron net, placing the iron net in a tubular furnace, and performing high-temperature treatment under the protection of nitrogen atmosphere to obtain a carbon nano tube/iron net photo-thermal material;

thirdly, surface treatment:

and taking the carbon nano tube/iron mesh photo-thermal material out of the tubular furnace, and then carrying out surface treatment by using oleic acid steam to finish the preparation method of the carbon nano tube/iron mesh photo-thermal material.

2. The method as claimed in claim 1, wherein the size of the iron net in the first step is 80 mesh, and the diameter of the cut iron net is 2 cm.

3. The method according to claim 1, wherein the concentration of the concentrated hydrochloric acid in the step one is 1.5mol/L to 2 mol/L.

4. The method for preparing carbon nanotube/iron mesh photothermal material according to claim 1, wherein in the first step, the cut iron mesh is put into concentrated hydrochloric acid for ultrasonic treatment for 5min to 10min, the ultrasonic power is 200W to 300W, the cut iron mesh is taken out and sequentially cleaned in deionized water and absolute ethyl alcohol for 10min to 20min, the ultrasonic power is 200W to 300W, and finally, a blower is used for drying to obtain the pretreated iron mesh.

5. The method for preparing the carbon nanotube/iron mesh photothermal material according to claim 1, wherein the mass ratio of the iron mesh to the melamine after the pretreatment in the second step is 1: 5.

6. The method of claim 1, wherein the high temperature treatment temperature in the second step is 600 ℃ to 900 ℃.

7. The method for preparing carbon nanotube/iron mesh photothermal material according to claim 1, wherein the time of the high temperature treatment in the second step is 1.5h to 2 h.

8. The method for preparing the carbon nanotube/iron mesh photothermal material according to claim 1, wherein the ratio of the mass of oleic acid to the diameter of the carbon nanotube/iron mesh photothermal material in the third step is 1.5g:2 cm.

9. The method for preparing carbon nanotube/iron mesh photothermal material according to claim 1, wherein the temperature of the surface treatment with oleic acid vapor in the third step is 140 ℃ and the treatment time is 1 h.

10. The use of the carbon nanotube/iron mesh photothermal material prepared by the preparation method according to claim 1, wherein a carbon nanotube/iron mesh photothermal material is used as a photothermal conversion material in a solar steam generation device for evaporating water.

Technical Field

The invention relates to a preparation method and application of a photo-thermal material.

Background

The fresh water is the material basis for human life, and the solar energy is low in cost, clean and renewable. The solar energy is captured to heat and evaporate water at a water-air interface to obtain water vapor, so that fresh water is obtained, and the photo-thermal conversion efficiency is greatly improved. Therefore, the preparation of the interface photo-thermal material with excellent performance has important significance. However, the existing photothermal conversion material has the defects of complex preparation method, low conversion efficiency, poor cycle performance and the like.

Disclosure of Invention

The invention aims to overcome the defects of complex preparation method, low conversion efficiency and poor cycle performance of the conventional photothermal conversion material, and provides a preparation method and application of a carbon nano tube/iron mesh photothermal material.

A preparation method of a carbon nano tube/iron mesh photo-thermal material is completed according to the following steps:

firstly, pretreating an iron net:

cutting the iron net to obtain the cut iron net; immersing the cut iron net into concentrated hydrochloric acid for ultrasonic treatment, taking out the iron net, sequentially and respectively ultrasonically cleaning the iron net in deionized water and absolute ethyl alcohol, and finally drying to obtain a pretreated iron net;

secondly, preparing the carbon nano tube/iron mesh photo-thermal material:

covering melamine on the upper surface and the lower surface of the pretreated iron net, placing the iron net in a tubular furnace, and performing high-temperature treatment under the protection of nitrogen atmosphere to obtain a carbon nano tube/iron net photo-thermal material;

thirdly, surface treatment:

and taking the carbon nano tube/iron mesh photo-thermal material out of the tubular furnace, and then carrying out surface treatment by using oleic acid steam to finish the preparation method of the carbon nano tube/iron mesh photo-thermal material.

A carbon nanotube/iron net photothermal material is used as photothermal conversion material in a solar steam generator for evaporating water.

The invention has the advantages that:

(1) the preparation method is simple and feasible, the preparation speed is high, and the cost is low;

(2) the photo-thermal material prepared by the invention has excellent hydrophobicity;

(3) the photo-thermal conversion material prepared by the invention is black in appearance, and is beneficial to converting light energy into heat energy;

(4) the invention utilizes the reaction of the iron net and the melamine at high temperature, grows the carbon nano tube on the surface of the iron net, is used as the photo-thermal conversion material to be applied to the solar steam generating device for evaporating water, and the prepared carbon nano tube/iron net photo-thermal material is the photo-thermal conversion material with high water evaporation rate, low cost and high cycle stability;

(5) when the illumination intensity is 1kW/m²The water evaporation rate of the carbon nano tube/iron net photo-thermal material prepared by the invention can reach 1.77 kg.m^-2·h^-1。

The invention can obtain the carbon nano tube/iron net photo-thermal material.

Drawings

Fig. 1 is a water evaporation rate of the carbon nanotube/iron mesh photothermal material, in which "■" is a blank with no interfacial evaporation material, "●" is the carbon nanotube/iron mesh photothermal material prepared in example one, ". tangle-solidup" is the carbon nanotube/iron mesh photothermal material prepared in example two, and "xxx" is the carbon nanotube/iron mesh photothermal material prepared in example three; ". diamond-solid" is the carbon nanotube/iron mesh photothermal material prepared in example four;

fig. 2 is a graph of the surface temperature of the carbon nanotube/iron mesh photothermal material according to the time, in which "■" is a blank without the interfacial evaporation material, "●" is the carbon nanotube/iron mesh photothermal material prepared in example one, ". tangle-solidup" is the carbon nanotube/iron mesh photothermal material prepared in example two, and "xxx" is the carbon nanotube/iron mesh photothermal material prepared in example three; ". diamond-solid" is the carbon nanotube/iron mesh photothermal material prepared in example four;

fig. 3 is a water evaporation rate of the carbon nanotube/iron mesh photothermal material prepared in example three, wherein "■" is the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled 1 time, "●" is the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled 2 times, ". tangle-solidup" is the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled 3 times, ". txt" is the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled 4 times, ". diamond-solid" is the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled 5 times,blank control without interface evaporation material;

FIG. 4 is a surface temperature infrared image of the carbon nanotube/iron mesh photothermal material prepared in the third embodiment;

fig. 5 is an XRD chart, in which 1 is the carbon nanotube/iron mesh photothermal material prepared in the first example, 2 is the carbon nanotube/iron mesh photothermal material prepared in the second example, and 3 is the carbon nanotube/iron mesh photothermal material prepared in the third example; 4, the carbon nano tube/iron net photo-thermal material prepared in the fourth embodiment;

FIG. 6 is an SEM image of a carbon nanotube/iron mesh photothermal material prepared according to one embodiment;

FIG. 7 is an SEM image of the carbon nanotube/iron mesh photothermal material prepared in the second embodiment;

FIG. 8 is an SEM image of the carbon nanotube/iron mesh photothermal material prepared in the third example;

FIG. 9 is an SEM image of the carbon nanotube/iron mesh photothermal material prepared in the fourth example;

FIG. 10 is a graph showing a contact angle test of a photo-thermal material of carbon nanotube/iron mesh prepared in the second three steps of the example;

fig. 11 is a contact angle test chart of the carbon nanotube/iron mesh photothermal material prepared in the third step of the example.

Detailed Description

The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.

The first embodiment is as follows: the preparation method of the carbon nanotube/iron mesh photothermal material of the embodiment is completed according to the following steps:

firstly, pretreating an iron net:

cutting the iron net to obtain the cut iron net; immersing the cut iron net into concentrated hydrochloric acid for ultrasonic treatment, taking out the iron net, sequentially and respectively ultrasonically cleaning the iron net in deionized water and absolute ethyl alcohol, and finally drying to obtain a pretreated iron net;

secondly, preparing the carbon nano tube/iron mesh photo-thermal material:

covering melamine on the upper surface and the lower surface of the pretreated iron net, placing the iron net in a tubular furnace, and performing high-temperature treatment under the protection of nitrogen atmosphere to obtain a carbon nano tube/iron net photo-thermal material;

thirdly, surface treatment:

and taking the carbon nano tube/iron mesh photo-thermal material out of the tubular furnace, and then carrying out surface treatment by using oleic acid steam to finish the preparation method of the carbon nano tube/iron mesh photo-thermal material.

The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the specification of the iron net in the step one is an 80-mesh screen, and the diameter of the cut iron net is 2 cm. Other steps are the same as in the first embodiment.

The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the concentration of the concentrated hydrochloric acid in the first step is 1.5-2 mol/L. The other steps are the same as in the first or second embodiment.

The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: and in the first step, the cut iron net is put into concentrated hydrochloric acid for ultrasonic treatment for 5-10 min, the ultrasonic power is 200-300W, the iron net is taken out and sequentially subjected to ultrasonic cleaning in deionized water and absolute ethyl alcohol for 10-20 min, the ultrasonic power is 200-300W, and finally a blower is used for drying to obtain the pretreated iron net. The other steps are the same as those in the first to third embodiments.

The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and the mass ratio of the iron net to the melamine after pretreatment in the second step is 1: 5. The other steps are the same as those in the first to fourth embodiments.

The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the temperature of the high-temperature treatment in the second step is 600-900 ℃. The other steps are the same as those in the first to fifth embodiments.

The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the time of the high-temperature treatment in the step two is 1.5-2 h. The other steps are the same as those in the first to sixth embodiments.

The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: in the third step, the ratio of the mass of the oleic acid to the diameter of the carbon nano tube/iron mesh photothermal material is 1.5g:2 cm. The other steps are the same as those in the first to seventh embodiments.

The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the temperature of the surface treatment by using the oleic acid steam in the third step is 140 ℃, and the treatment time is 1 h. The other steps are the same as those in the first to eighth embodiments.

The detailed implementation mode is ten: the embodiment is that the carbon nano tube/iron net photo-thermal material is applied to a solar steam generating device as a photo-thermal conversion material and is used for evaporating water.

The following examples were used to demonstrate the beneficial effects of the present invention:

the first embodiment is as follows: a preparation method of a carbon nano tube/iron mesh photo-thermal material is completed according to the following steps:

firstly, pretreating an iron net:

cutting the iron net to obtain the cut iron net; immersing the cut iron net into a hydrochloric acid solution with the concentration of 2mol/L for ultrasonic treatment for 5min, wherein the ultrasonic power is 200W, taking out the iron net, sequentially and respectively ultrasonically cleaning the iron net in deionized water and absolute ethyl alcohol for 10min, wherein the ultrasonic power is 200W, and finally drying the iron net by using a blower to obtain a pretreated iron net;

the diameter of the cut iron net in the step one is 2cm, and the specification is an 80-mesh screen;

secondly, preparing the carbon nano tube/iron mesh photo-thermal material:

covering melamine on the upper surface and the lower surface of the pretreated iron net, then placing the iron net in a tubular furnace, and carrying out high-temperature treatment under the protection of nitrogen atmosphere, wherein the temperature of the high-temperature treatment is 600 ℃, and the time of the high-temperature treatment is 2 hours, so as to obtain the carbon nano tube/iron net photo-thermal material;

the mass ratio of the iron net to the melamine after pretreatment in the second step is 1: 5;

thirdly, surface treatment:

taking the carbon nanotube/iron mesh photothermal material out of the tubular furnace, and then carrying out surface treatment by using oleic acid steam, wherein the temperature of the surface treatment is 140 ℃, and the time of the surface treatment is 1h, so that the preparation method of the carbon nanotube/iron mesh photothermal material is completed;

the dosage of the oleic acid in the step three is 1.5 g.

Example two: the present embodiment is different from the first embodiment in that: the temperature of the high-temperature treatment in the second step is 700 ℃. Other steps and parameters are the same as those in the first embodiment.

Example three: the present embodiment is different from the first embodiment in that: the temperature of the high-temperature treatment in the second step is 800 ℃. Other steps and parameters are the same as those in the first embodiment.

Example four: the present embodiment is different from the first embodiment in that: the temperature of the high-temperature treatment in the second step is 900 ℃. Other steps and parameters are the same as those in the first embodiment.

And (3) evaporation test:

simulating sunlight by using a xenon lamp as a simulation light source, adjusting the distance between the xenon lamp and a sample to be measured, and determining the illumination intensity of light irradiating the sample to be 1 kW.m by using an irradiator^-2. The samples prepared in examples one to three were placed above the liquid level of the container containing water, and the initial mass of the entire container was recorded with an electronic balance with a precision of one in ten thousandth. The test was then started by turning on the light source and recording the readings of the electronic balance every 10min for 1 h. In addition, during the water evaporation test, an infrared thermal imager was used to record the surface temperature of the sample at different times. After the light source is turned on, the temperature is recorded every certain time until the surface temperature of the sample is kept stable in multiple recordings.

Fig. 1 is a water evaporation rate of the carbon nanotube/iron mesh photothermal material, in which "■" is a blank with no interfacial evaporation material, "●" is the carbon nanotube/iron mesh photothermal material prepared in example one, ". tangle-solidup" is the carbon nanotube/iron mesh photothermal material prepared in example two, and "xxx" is the carbon nanotube/iron mesh photothermal material prepared in example three; ". diamond-solid" is the carbon nanotube/iron mesh photothermal material prepared in example four;

as can be seen from FIG. 1, the water evaporation rate of the carbon nanotube/iron mesh photothermal material increased with the increase of the high-temperature treatment temperature, and the photothermal conversion effect of the carbon nanotube/iron mesh photothermal material obtained by the high-temperature treatment at 800 ℃ was the best in the third example, and reached 1.77 kg.m^-2·h^-1Has better photo-thermal conversion performance and has positive effect on water evaporation.

Fig. 2 is a graph of the surface temperature of the carbon nanotube/iron mesh photothermal material according to the time, in which "■" is a blank without the interfacial evaporation material, "●" is the carbon nanotube/iron mesh photothermal material prepared in example one, ". tangle-solidup" is the carbon nanotube/iron mesh photothermal material prepared in example two, and "xxx" is the carbon nanotube/iron mesh photothermal material prepared in example three; ". diamond-solid" is the carbon nanotube/iron mesh photothermal material prepared in example four;

as can be seen from fig. 2, the surface temperature of the carbon nanotube/iron mesh sample rises faster with the increase of the high temperature treatment temperature, and the results of the second, third and fourth examples are not very different, and the final surface rise temperature is about 24 ℃.

The carbon nanotube/iron mesh photothermal material prepared in example three after undergoing the water evaporation test for 1 hour was subjected to the water evaporation test again as the carbon nanotube/iron mesh photothermal material prepared in example three which was cycled for 1 time; the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled for 1 time, was subjected to the water evaporation test again to be used as the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled for 2 times; the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled for 2 times, was subjected to the water evaporation test again to be used as the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled for 3 times; the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled 3 times, was subjected to the water evaporation test again as the carbon nanotube/iron mesh photothermal material prepared in example three, which was cycled 4 times, as shown in fig. 3;

FIG. 3 shows the water evaporation rate of the carbon nanotube/iron mesh photothermal material prepared in example three, wherein "■" is the cycleExample three, in which the number of cycles was 1, "●" was the carbon nanotube/iron mesh photothermal material prepared in example three, in which 2 cycles were performed, ". tangle-solidup" was the carbon nanotube/iron mesh photothermal material prepared in example three, in which 3 cycles were performed, ". xxx" was the carbon nanotube/iron mesh photothermal material prepared in example three, in which 4 cycles were performed, ". diamond-like" was the carbon nanotube/iron mesh photothermal material prepared in example three, in which 5 cycles were performed,blank control without interface evaporation material;

as can be seen from FIG. 3, the photo-thermal material of carbon nanotube/iron mesh prepared in example three after 5 cycles still has a high water evaporation rate, and the photo-thermal material of carbon nanotube/iron mesh prepared in example three after 5 cycles can reach 1.58kg · m^-2·h^-1。

FIG. 4 is a surface temperature infrared image of the carbon nanotube/iron mesh photothermal material prepared in the third embodiment;

as can be seen from fig. 4, the surface temperature of the carbon nanotube/iron mesh photothermal material prepared in example three can be raised from 20.5 ℃ to 44.9 ℃ under the irradiation of xenon lamp.

Fig. 5 is an XRD chart, in which 1 is the carbon nanotube/iron mesh photothermal material prepared in the first example, 2 is the carbon nanotube/iron mesh photothermal material prepared in the second example, and 3 is the carbon nanotube/iron mesh photothermal material prepared in the third example; 4, the carbon nano tube/iron net photo-thermal material prepared in the fourth embodiment;

as can be seen from fig. 5: the main components of the materials prepared in example one are Fe, and the main components of the materials prepared in example two, example three and example four are Fe and Fe₃C。

FIG. 6 is an SEM image of a carbon nanotube/iron mesh photothermal material prepared according to one embodiment;

FIG. 7 is an SEM image of the carbon nanotube/iron mesh photothermal material prepared in the second embodiment;

FIG. 8 is an SEM image of the carbon nanotube/iron mesh photothermal material prepared in the third example;

FIG. 9 is an SEM image of the carbon nanotube/iron mesh photothermal material prepared in the fourth example;

as can be seen from fig. 6 to 9, the surfaces of the samples prepared in the first example are amorphous thick carbon sheets and carbon spheres, and as the treatment temperature increases, carbon nanotubes gradually form on the surface of the iron mesh. Example two prepared samples with small surface diameter carbon nanotubes wrapped in Fe₃C, performing heat treatment; example three prepared samples formed high quality carbon nanotubes with high degree of graphitism on the surface and uniformly dispersed Fe wrapped inside the carbon nanotubes₃C, nano-particles and carbon nano-tubes are basically generated; example four-surface carbon nanotubes were further grown, and the interior of the carbon nanotubes was wrapped with Fe₃And C, nano-particles. .

FIG. 10 is a graph showing a contact angle test of a photo-thermal material of carbon nanotube/iron mesh prepared in the second three steps of the example;

fig. 11 is a contact angle test chart of the carbon nanotube/iron mesh photothermal material prepared in the third step of the example.

As can be seen from fig. 10 to 11, the contact angle of the carbon nanotube/iron mesh treated with oleic acid vapor increases, and the material changes from hydrophilic to hydrophobic, which has a positive effect on the evaporation of water.