CN103769050A - Electrochemical method for preparing activated carbon fibers with photocatalysis function - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 18
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 9
- 229920000049 Carbon (fiber) Polymers 0.000 title abstract description 31
- 238000002848 electrochemical method Methods 0.000 title description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 20
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000004070 electrodeposition Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
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- 238000004140 cleaning Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 32
- 238000001179 sorption measurement Methods 0.000 abstract description 22
- 238000011069 regeneration method Methods 0.000 abstract description 12
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 10
- 230000008929 regeneration Effects 0.000 abstract description 8
- 239000003344 environmental pollutant Substances 0.000 abstract description 6
- 231100000719 pollutant Toxicity 0.000 abstract description 6
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- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 24
- 102100027310 Bromodomain adjacent to zinc finger domain protein 1A Human genes 0.000 description 18
- 101000937778 Homo sapiens Bromodomain adjacent to zinc finger domain protein 1A Proteins 0.000 description 18
- 238000005868 electrolysis reaction Methods 0.000 description 10
- 239000004917 carbon fiber Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000000746 purification Methods 0.000 description 7
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000002156 adsorbate Substances 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 3
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
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- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- BCHZICNRHXRCHY-UHFFFAOYSA-N 2h-oxazine Chemical group N1OC=CC=C1 BCHZICNRHXRCHY-UHFFFAOYSA-N 0.000 description 1
- 101100269321 Arabidopsis thaliana AFC1 gene Proteins 0.000 description 1
- 101100258032 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) STE24 gene Proteins 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明属于活性炭纤维制备领域，具体涉及一种具有光催功能活性炭纤维的制备方法。 The invention belongs to the field of preparation of activated carbon fibers, and in particular relates to a preparation method of activated carbon fibers with photocatalytic function.
背景技术 Background technique
活性炭纤维因其孔隙结构发达、吸附力强、表面官能团丰富、化学惰性等优点，被广泛应用于气体吸附净化、污染水体治理、饮用水净化以及食品工业、化学工业等领域。但由于活性炭纤维品种少、技术含量低、缺少功能化高品质专用活性炭纤维，制约我国活性炭纤维行业迈向更高层次的应用。将活性炭纤维改性处理，研制出能够对污染物进行高效、深度净化的功能活性炭纤维，是降低活性炭纤维的使用成本、扩大其使用范围、提高其利用效率的有效途径，是活性炭纤维行业未来发展的方向。 Due to its developed pore structure, strong adsorption capacity, rich surface functional groups, and chemical inertness, activated carbon fibers are widely used in gas adsorption purification, polluted water treatment, drinking water purification, food industry, chemical industry and other fields. However, due to the lack of activated carbon fiber varieties, low technical content, and lack of functional high-quality special activated carbon fibers, my country's activated carbon fiber industry is restricted from moving towards a higher level of application. Modification of activated carbon fibers to develop functional activated carbon fibers that can efficiently and deeply purify pollutants is an effective way to reduce the cost of activated carbon fibers, expand their scope of use, and improve their utilization efficiency. It is the future development of the activated carbon fiber industry. direction.
由于活性炭纤维对污染物的吸附主要以微孔填充为主，吸附量有限，短时间内即可达吸附饱和而失去吸附能力，吸附饱和的活性炭纤维成为二次污染源，须对其进行再生处理方可再次利用。目前活性炭纤维再生方法总体上可以分为两类：一是设法使吸附质脱附，即通过创造与低负荷相对应的条件(引入物质或能量使吸附质分子与活性炭纤维之间的作用力减弱或消失)，除去吸附质；二是依靠热分解或氧化还原反应破坏吸附质的结构，除去吸附质。传统的再生方法主要有热再生、化学药品再生、溶剂再生、生物再生等，但由于其存在效率低、耗费高、操作条件苛刻、工艺复杂等缺陷，传统再生方法已不能满足现在工业发展的需求。因此研究一种在常温、常压、低耗费、高效率、操作工艺单简的再生方法成为国内外研究的热点。 Since the adsorption of pollutants by activated carbon fibers is mainly based on micropore filling, the adsorption capacity is limited, and the adsorption saturation can be reached in a short time and the adsorption capacity is lost. The saturated activated carbon fibers become a secondary pollution source and must be regenerated. Can be reused. At present, the activated carbon fiber regeneration methods can be generally divided into two categories: one is to try to desorb the adsorbate, that is, by creating conditions corresponding to the low load (introducing substances or energy to weaken the force between the adsorbate molecules and the activated carbon fiber). or disappear) to remove the adsorbate; the second is to rely on thermal decomposition or redox reaction to destroy the structure of the adsorbate and remove the adsorbate. Traditional regeneration methods mainly include thermal regeneration, chemical regeneration, solvent regeneration, biological regeneration, etc., but due to their defects such as low efficiency, high cost, harsh operating conditions, and complicated processes, traditional regeneration methods can no longer meet the needs of current industrial development. . Therefore, researching a regeneration method at normal temperature, normal pressure, low consumption, high efficiency, and simple operation process has become a research hotspot at home and abroad.
发明内容 Contents of the invention
本发明的目的在于提供一种具有光催功能活性炭纤维的制备方法。本发明制得的光催化功能活性炭纤维具有光催化功能和吸附功能，且在光照下活性炭纤维可原位再生。 The purpose of the present invention is to provide a preparation method of activated carbon fiber with photocatalytic function. The photocatalytic functional activated carbon fiber prepared by the invention has photocatalytic function and adsorption function, and the activated carbon fiber can be regenerated in situ under illumination.
为实现上述目的，本发明采用如下技术方案： To achieve the above object, the present invention adopts the following technical solutions:
采用电化学法制备固载石墨相氮化碳的活性炭纤维，包括以下步骤： Prepare the active carbon fiber of immobilized graphitic phase carbon nitride by electrochemical method, comprising the following steps:
（1）将具有导电性、且电阻率小于80kΩ/m的活性炭纤维，用2wt.%的盐酸煮沸清洗后，再用蒸馏水洗涤至中性，于烘箱中烘24h； (1) After boiling and cleaning activated carbon fibers with electrical conductivity and resistivity less than 80kΩ/m with 2wt.% hydrochloric acid, they are washed with distilled water until neutral, and baked in an oven for 24 hours;
（2）将步骤（1）的活性炭纤维置于二氰二胺的N,N二甲基甲酰胺溶液中浸泡24h； (2) Soak the activated carbon fiber in step (1) in N,N dimethylformamide solution of dicyandiamide for 24 hours;
（3）固载石墨相氮化碳的过程在电解池中进行，电化学沉积条件：以二氰二胺的N,N二甲基甲酰胺溶液作为电解液，以石墨为阳极，以步骤（2）的活性炭纤维为阴极，电源为直流电源，电解过程电压500~2000V，温度25~30℃，时间1~5h； (3) The process of immobilizing graphite-phase carbon nitride is carried out in an electrolytic cell, and the electrochemical deposition conditions: use N,N dimethylformamide solution of dicyandiamide as electrolyte, graphite as anode, and step ( 2) The active carbon fiber is the cathode, the power supply is DC power supply, the electrolysis process voltage is 500~2000V, the temperature is 25~30℃, and the time is 1~5h;
（4）从电解池中取出阴极的活性炭纤维，用蒸馏水充分洗涤、烘干，即制得固载石墨相氮化碳的活性炭纤维。 (4) The activated carbon fiber of the cathode is taken out from the electrolytic cell, fully washed with distilled water, and dried to obtain the activated carbon fiber immobilized with graphite phase carbon nitride.
所述的二氰二胺的N,N二甲基甲酰胺溶液中二氰二胺的浓度为0.05~0.15mol/L。 The concentration of dicyandiamine in the N,N dimethylformamide solution of dicyandiamine is 0.05-0.15mol/L.
本发明的显著优点在于：本发明制得的活性炭纤维不仅具有吸附功能，而且具有光催化功能。其在黑暗或光线不足的情况下依靠活性炭纤维的吸附功能净化污染物；在光照充足的情况下吸附功能及光催化功能均可净化污染物，还可实现活性炭纤维吸附功能的原位再生，大大降低再生过程人力、物力、财力耗费。该活性炭纤维的研制成功对于缓解我国活性炭纤维供应量不足具有重要的作用。 The remarkable advantage of the present invention is that: the activated carbon fiber prepared by the present invention not only has the function of adsorption, but also has the function of photocatalysis. It relies on the adsorption function of activated carbon fibers to purify pollutants in the dark or insufficient light; in the case of sufficient light, both the adsorption function and the photocatalytic function can purify pollutants, and can also realize the in-situ regeneration of the adsorption function of activated carbon fibers, greatly Reduce manpower, material and financial resources in the regeneration process. The successful development of the activated carbon fiber plays an important role in alleviating the insufficient supply of activated carbon fiber in my country.
附图说明 Description of drawings
图1为ACF1及ACF0的XRD谱； Fig. 1 is the XRD spectrum of ACF1 and ACF0;
图2为ACF1及ACF0的FTIR谱； Figure 2 is the FTIR spectrum of ACF1 and ACF0;
图3为AFC1及ACF0的吸附脱附曲线图； Fig. 3 is the adsorption-desorption curve diagram of AFC1 and ACF0;
图4为在光照及暗吸附条件下ACF1及ACF0对甲醛的净化效果； Figure 4 is the purification effect of ACF1 and ACF0 on formaldehyde under light and dark adsorption conditions;
图5为光照条件下ACF1及ACF0重复使用6次对甲醛的去除效果。 Figure 5 shows the removal effect of ACF1 and ACF0 on formaldehyde after repeated use for 6 times under light conditions.
注：本发明制备的光催化功能活性炭纤维(标记为:ACF1)，而对照样活性炭纤维(标记为:ACF0)。 Note: The photocatalytic functional activated carbon fiber (marked as: ACF1) prepared by the present invention, and the control activated carbon fiber (marked as: ACF0).
具体实施方式 Detailed ways
实施例1Example 1
1) 将具有导电性、且电阻率小于80kΩ/m的活性炭纤维，用2%的盐酸煮沸清洗，后再用蒸馏洗涤至中性，并至于烘箱烘干24h； 1) The activated carbon fibers with conductivity and resistivity less than 80kΩ/m are boiled and cleaned with 2% hydrochloric acid, then washed by distillation until neutral, and dried in an oven for 24 hours;
2)将步骤1)中的活性炭纤维置于0.05mol/L二氰二胺的N,N二甲基甲酰胺溶液中浸泡24h； 2) Soak the activated carbon fiber in step 1) in a N,N dimethylformamide solution of 0.05mol/L dicyandiamide for 24 hours;
3)固载石墨相氮化碳的过程在电解池中进行，电化学沉积条件：以0.05mol/L二氰二胺的N,N二甲基甲酰胺溶液作为电解液，以石墨为阳极，以步骤2)的活性炭纤维为阴极，电源为直流电源，电解过程电压2000V，电解过程温度25℃，电解时间1h。 3) The process of immobilizing graphite-phase carbon nitride is carried out in an electrolytic cell. Electrochemical deposition conditions: use 0.05mol/L dicyandiamine N,N dimethylformamide solution as electrolyte, graphite as anode, The activated carbon fiber in step 2) is used as the cathode, the power supply is a DC power supply, the electrolysis process voltage is 2000V, the electrolysis process temperature is 25°C, and the electrolysis time is 1h.
4) 从电解池中取出阴极的活性炭纤维，并用蒸馏水充分洗涤、烘干，即制得固载石墨相氮化碳具有光催化功能的活性炭纤维。 4) Take out the active carbon fiber of the cathode from the electrolytic cell, wash and dry it fully with distilled water, and then obtain the active carbon fiber with photocatalytic function of immobilized graphite phase carbon nitride.
实施例2Example 2
1) 将具有导电性、且电阻率小于80kΩ/m的活性炭纤维，用2%的盐酸煮沸清洗，后再用蒸馏洗涤至中性，并至于烘箱烘干24h； 1) The activated carbon fibers with conductivity and resistivity less than 80kΩ/m are boiled and cleaned with 2% hydrochloric acid, then washed by distillation until neutral, and dried in an oven for 24 hours;
2)将步骤1)中的活性炭纤维置于0.15mol/L二氰二胺的N,N二甲基甲酰胺溶液中浸泡24h； 2) Soak the activated carbon fiber in step 1) in 0.15mol/L N,N dimethylformamide solution of dicyandiamide for 24h;
3)固载石墨相氮化碳的过程在电解池中进行，电化学沉积条件：以0.15mol/L二氰二胺的N,N二甲基甲酰胺溶液作为电解液，以石墨为阳极，以步骤2)的活性炭纤维为阴极，电源为直流电源，电解过程电压500V，电解过程温度30℃，电解时间5h。 3) The process of immobilizing graphite phase carbon nitride is carried out in an electrolytic cell, and the electrochemical deposition conditions are as follows: 0.15mol/L N,N dimethylformamide solution of dicyandiamine is used as the electrolyte, and graphite is used as the anode. The activated carbon fiber in step 2) is used as the cathode, the power supply is a DC power supply, the electrolysis process voltage is 500V, the electrolysis process temperature is 30°C, and the electrolysis time is 5h.
4) 从电解池中取出阴极的活性炭纤维，并用蒸馏水充分洗涤、烘干，即制得固载石墨相氮化碳具有光催化功能的活性炭纤维。 4) Take out the active carbon fiber of the cathode from the electrolytic cell, wash and dry it fully with distilled water, and then obtain the active carbon fiber with photocatalytic function of immobilized graphite phase carbon nitride.
实施例3Example 3
1) 将具有导电性、且电阻率小于80kΩ/m的活性炭纤维，用2%的盐酸煮沸清洗，后再用蒸馏洗涤至中性，并至于烘箱烘干24h； 1) The activated carbon fibers with conductivity and resistivity less than 80kΩ/m are boiled and cleaned with 2% hydrochloric acid, then washed by distillation until neutral, and dried in an oven for 24 hours;
2)将步骤1)中的活性炭纤维置于0.10mol/L二氰二胺的N,N二甲基甲酰胺溶液中浸泡24h； 2) Soak the activated carbon fiber in step 1) in 0.10mol/L N,N dimethylformamide solution of dicyandiamide for 24h;
3)固载石墨相氮化碳的过程在电解池中进行，电化学沉积条件：以0.10mol/L二氰二胺的N,N二甲基甲酰胺溶液作为电解液，以石墨为阳极，以步骤2)的活性炭纤维为阴极，电源为直流电源，电解过程电压1000V，电解过程温度28℃，电解时间3h。 3) The process of immobilizing graphite-phase carbon nitride is carried out in an electrolytic cell. Electrochemical deposition conditions: use 0.10mol/L dicyandiamide N,N dimethylformamide solution as electrolyte, graphite as anode, The activated carbon fiber in step 2) is used as the cathode, the power supply is a DC power supply, the electrolysis process voltage is 1000V, the electrolysis process temperature is 28°C, and the electrolysis time is 3h.
4) 从电解池中取出阴极的活性炭纤维，并用蒸馏水充分洗涤、烘干，即制得固载石墨相氮化碳具有光催化功能的活性炭纤维。 4) Take out the active carbon fiber of the cathode from the electrolytic cell, wash and dry it fully with distilled water, and then obtain the active carbon fiber with photocatalytic function of immobilized graphite phase carbon nitride.
图1为ACF1及ACF0的XRD谱。由图可以看出，ACF1在2θ=27.65o附近有一个较宽的衍射峰，其对应于石墨相氮化碳的(002)晶面衍射峰。另外，ACF1在2θ=13.23o附近有一个较宽的衍射峰，其对应于石墨相氮化碳的(100)晶面衍射峰。 Figure 1 is the XRD spectrum of ACF1 and ACF0. It can be seen from the figure that ACF1 has a broad diffraction peak around 2 θ = 27.65o, which corresponds to the (002) crystal plane diffraction peak of graphitic carbon nitride. In addition, ACF1 has a broad diffraction peak around 2 θ = 13.23o, which corresponds to the (100) crystal plane diffraction peak of graphitic carbon nitride.
图2为ACF1及ACF0的FTIR谱。ACF1在810nm-1的特征吸收峰可归属为嗪环的弯曲振动，1246~1633 nm-1范围内几个强的特征峰对应于CN杂环化合物的特征吸收峰。1326 nm-1和1635 nm-1处的特征吸收峰分别归属为石墨相氮化碳的C-N键和C=N键的弯曲振动吸收峰。1635 nm-1处出现较强的特征吸收峰说明g-C3N4的结晶度较高。3175 nm-1和3432 nm-1的特征吸收峰分别为N-H键和O-H键的伸缩振动吸收峰。 Figure 2 is the FTIR spectra of ACF1 and ACF0. The characteristic absorption peak of ACF1 at 810nm -1 can be attributed to the bending vibration of the oxazine ring, and several strong characteristic peaks in the range of 1246~1633 nm -1 correspond to the characteristic absorption peaks of CN heterocyclic compounds. The characteristic absorption peaks at 1326 nm -1 and 1635 nm -1 are assigned to the bending vibration absorption peaks of CN bond and C=N bond of graphitic carbon nitride, respectively. The strong characteristic absorption peak at 1635 nm -1 indicates that the crystallinity of gC 3 N 4 is high. The characteristic absorption peaks at 3175 nm -1 and 3432 nm -1 are the stretching vibration absorption peaks of NH bond and OH bond, respectively.
图3为ACF1及ACF0样品的N2吸附-脱附曲线图。由图可知，两种样品的吸附等温线均呈现相同的类型，且都具有滞后环。另外，从图还可以看出ACF1的吸附量略小于ACF0。 Figure 3 is the N 2 adsorption-desorption curves of ACF1 and ACF0 samples. It can be seen from the figure that the adsorption isotherms of the two samples are of the same type, and both have hysteresis loops. In addition, it can also be seen from the figure that the adsorption capacity of ACF1 is slightly smaller than that of ACF0.
图4为在光照及暗吸附条件下ACF1及ACF0对甲醛的净化效果。由图可以看出，以该工艺制备的活性炭纤维不仅具有吸附功能，而且还具有光催化功能。在暗吸附条件，ACF1的吸附量略小于ACF0；但是在光照条件下ACF1对甲醛的净化效果显著好于ACF0对甲醛的去除效果。 Figure 4 shows the purification effect of ACF1 and ACF0 on formaldehyde under light and dark adsorption conditions. It can be seen from the figure that the activated carbon fiber prepared by this process not only has the function of adsorption, but also has the function of photocatalysis. Under dark adsorption conditions, the adsorption capacity of ACF1 was slightly smaller than that of ACF0; however, the purification effect of ACF1 on formaldehyde was significantly better than that of ACF0 on formaldehyde under light conditions.
图5为光照条件下ACF1及ACF0重复使用6次对甲醛的净化效果实验，从图可以看出ACF1对甲醛的净化效果明显好于ACF0。在相同条件下ACF1重复使用6后对甲醛的去除率在94%以上，而ACF0重复使用6次后对甲醛去除率仅为4%。 Figure 5 is an experiment on the purification effect of ACF1 and ACF0 on formaldehyde after repeated use for 6 times under light conditions. It can be seen from the figure that the purification effect of ACF1 on formaldehyde is significantly better than that of ACF0. Under the same conditions, the formaldehyde removal rate of ACF1 after repeated use for 6 times was over 94%, while that of ACF0 was only 4% after repeated use for 6 times.
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。 The above descriptions are only preferred embodiments of the present invention, and all equivalent changes and modifications made according to the scope of the patent application of the present invention shall fall within the scope of the present invention.
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