CN100382887C - A kind of preparation method of activated carbon fiber adsorption material - Google Patents
A kind of preparation method of activated carbon fiber adsorption material Download PDFInfo
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- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 5
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- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
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- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
本发明公开了一种活性碳纤维吸附材料的制备方法，包括如下步骤：(1)将粘胶纤维在碱金属盐或碱土金属盐溶液和磷酸的混合水溶液中浸渍5～24小时；(2)风干后加热至200℃～500℃；(3)在惰性气体条件下加热至700℃～1100℃，同时从500℃～700℃开始通入水蒸汽，活化处理0.5～5小时，冷却之后得到大孔活性碳纤维。所获得的活性碳纤维表面大孔孔径在50～600nm，同时，原料价格便宜，工艺简单，便于工业化生产。
The invention discloses a preparation method of activated carbon fiber adsorption material, comprising the following steps: (1) immersing viscose fiber in the mixed aqueous solution of alkali metal salt or alkaline earth metal salt solution and phosphoric acid for 5-24 hours; (2) air drying (3) Heating to 700°C to 1100°C under inert gas conditions, and at the same time, starting to pass water vapor from 500°C to 700°C, activation treatment for 0.5 to 5 hours, and obtaining macroporous activity after cooling carbon fiber. The large pores on the surface of the obtained active carbon fiber have a diameter of 50-600nm, and at the same time, the raw material is cheap, the process is simple, and it is convenient for industrial production.
Description
技术领域technical field
本发明涉及一种活性碳纤维吸附材料的制备方法，特别是涉及一种表面富含大孔(孔径＞50nm)的粘胶基活性碳纤维的制备方法。The invention relates to a method for preparing an activated carbon fiber adsorption material, in particular to a method for preparing a viscose-based activated carbon fiber whose surface is rich in macropores (pore diameter > 50nm).
背景技术Background technique
活性炭纤维(Activated Carbon Fiber，ACF)是二十世纪60年代初研制成功并逐渐工业化的一种高效吸附功能材料。材料表面不同的孔径能赋予活性碳纤维不同的吸附性能。一般来说ACF的孔径大小为所吸附物质的大小的2倍左右时才可施展出最佳的吸附能力。而根据国际纯理论与化学联合会(IUPAC)的孔径分类标准：孔径小于2nm的为微孔，介于2nm和50nm的为中孔，大于50nm的为大孔。Activated Carbon Fiber (ACF) is a high-efficiency adsorption functional material that was successfully developed in the early 1960s and gradually industrialized. The different pore sizes on the surface of the material can endow the activated carbon fibers with different adsorption properties. Generally speaking, the best adsorption capacity can only be exhibited when the pore size of ACF is about 2 times the size of the adsorbed substance. According to the pore size classification standard of the International Union of Pure Theory and Chemistry (IUPAC): micropores with a pore size less than 2nm, mesopores with a pore size between 2nm and 50nm, and macropores with a pore size greater than 50nm.
目前研制和生产的ACF多为2nm以下的微孔型，仅适于气体和小分子量液体分子的吸附。有一些研究通过改变预处理条件和工艺方法，也仅仅制得了平均孔径几个纳米的中孔型ACF，还未见有孔径大于5nm的产品和相关技术。而目前中微孔型ACF对于尺寸在几十～几百nm的大尺寸物质的吸附效果极差。因此要想吸附生物大分子、有机电解质以及病毒(如流感病毒直径为80～120nm，冠状病毒75～160nm，)等物质必须使用表面富含大孔的ACF。Most of the ACFs developed and produced at present are microporous types below 2nm, which are only suitable for the adsorption of gas and small molecular weight liquid molecules. Some studies have only produced mesoporous ACF with an average pore diameter of a few nanometers by changing the pretreatment conditions and process methods, and there are no products and related technologies with a pore diameter larger than 5nm. However, the current mesoporous ACF has extremely poor adsorption effect on large-scale substances with a size ranging from tens to hundreds of nm. Therefore, in order to adsorb biological macromolecules, organic electrolytes, and viruses (such as influenza virus with a diameter of 80-120nm and coronavirus with a diameter of 75-160nm), ACF with a surface rich in macropores must be used.
发明内容Contents of the invention
本发明所要解决的技术问题是提供一种大孔型(孔径大于50nm)活性碳纤维的制备方法，以弥补现有技术只能获得微、中孔活性碳纤维的不足。The technical problem to be solved by the present invention is to provide a preparation method of macroporous (aperture greater than 50nm) activated carbon fibers, so as to make up for the deficiency that the prior art can only obtain micro- and mesoporous activated carbon fibers.
为了解决上述技术问题，本发明所采用的技术方案是：一种活性碳纤维吸附材料的制备方法，包括如下步骤：(1)将粘胶纤维在碱金属盐或碱土金属盐溶液和磷酸的混合水溶液中浸渍5～24小时；(2)风干后加热至200～500℃；(3)再在惰性气体条件下加热至700～1100℃，同时从500℃～700℃开始通入水蒸汽，活化处理0.5～5小时，冷却之后得到所说的大孔活性碳纤维。In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is: a kind of preparation method of activated carbon fiber adsorption material, comprises the following steps: (1) mix viscose fiber in the mixed aqueous solution of alkali metal salt or alkaline earth metal salt solution and phosphoric acid (2) air-dried and heated to 200-500°C; (3) heated to 700-1100°C under inert gas conditions, and at the same time, water vapor was introduced from 500°C-700°C, and the activation treatment was 0.5 After ~5 hours, the macroporous activated carbon fibers were obtained after cooling.
其中，所述的碱金属盐或碱土金属盐的浓度为1mol/l～饱和浓度。Wherein, the concentration of the alkali metal salt or alkaline earth metal salt is 1 mol/l~saturation concentration.
所述的磷酸的浓度为5wt％～40wt％。The concentration of the phosphoric acid is 5wt%-40wt%.
所述的碱金属盐或碱土金属盐溶液和磷酸溶液的配比为1∶1～5。The ratio of the alkali metal salt or alkaline earth metal salt solution to the phosphoric acid solution is 1:1-5.
作为优选的技术方案：所述的碱金属盐或碱土金属盐包括磷酸二氢钠、磷酸氢二钠、氯化钠、氯化钾、氯化镁、硝酸钠、硝酸钾、硝酸镁中的一种或几种。As a preferred technical solution: the alkali metal salt or alkaline earth metal salt includes one of sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium chloride, potassium chloride, magnesium chloride, sodium nitrate, potassium nitrate, magnesium nitrate or Several kinds.
所述的碱金属盐或碱土金属盐优选的浓度为1mol/l～3.0mol/l。The preferred concentration of the alkali metal salt or alkaline earth metal salt is 1 mol/l-3.0 mol/l.
浸渍后的粘胶纤维在空气中自然风干。The impregnated viscose fibers are dried naturally in the air.
所述的惰性气体为氮气、氦气、氩气中的一种或其混合物，优选的惰性气体为氮气。The inert gas is one of nitrogen, helium, argon or a mixture thereof, and the preferred inert gas is nitrogen.
所述的粘胶纤维在浸渍之前，先在去离子水或蒸馏水中清洗。The viscose fiber is washed in deionized water or distilled water before dipping.
本发明的有益效果是：所制得的大孔活性碳纤维的表面孔径大小可通过盐溶液的浓度进行控制，盐的摩尔浓度为1mol/l～饱和浓度，优选的浓度为1mol/l～3.0mol/l。在此条件下，所获得的活性碳纤维表面大孔孔径在50～600nm。同时，原料价格便宜，工艺简单，便于工业化生产。The beneficial effects of the present invention are: the surface pore size of the prepared macroporous activated carbon fiber can be controlled by the concentration of the salt solution, the molar concentration of the salt is 1mol/l～saturation concentration, and the preferred concentration is 1mol/l～3.0mol /l. Under this condition, the large pores on the surface of the activated carbon fibers obtained have a diameter of 50-600 nm. At the same time, the raw material is cheap, the process is simple, and it is convenient for industrialized production.
附图说明Description of drawings
图1为表面富含大孔的活性碳纤维电镜照片Figure 1 is an electron micrograph of activated carbon fibers rich in macropores on the surface
具体实施方式Detailed ways
下面结合附图对本发明作进一步详细阐述。参照附图1The present invention will be described in further detail below in conjunction with the accompanying drawings. Refer to attached drawing 1
实施例1Example 1
将粘胶纤维先在去离子水中清洗，晾干。将1mol/l的磷酸二氢钠盐溶液和5wt％ H3PO4溶液以1∶1的比例混合，再将清洗晾干后的粘胶原丝置于此溶液中静置5小时，取出自然风干后放入预氧化炉中，在200℃加热，恒温1小时。然后置入碳化活化炉中，在N2保护下以20℃/min的速率升温到700℃，恒温30min，并从500℃开始通入水蒸汽活化，冷却后得到大孔型活性碳纤维。比表面积为1027m2/g。其电镜照片如图1，所获得的大孔型活性碳纤维表面布满大孔(100nm＜孔径＜600nm)，且孔型较圆。Wash the viscose fiber in deionized water first, and let it dry. Mix 1mol/l sodium dihydrogen phosphate solution and 5wt% H3PO4 solution at a ratio of 1:1, then place the cleaned and dried viscose filaments in this solution and let it stand for 5 hours, take out the natural After air-drying, put it into a pre-oxidation furnace, heat at 200° C., and keep the temperature constant for 1 hour. Then put it into a carbonization activation furnace, raise the temperature to 700°C at a rate of 20°C/min under the protection of N2 , keep the temperature constant for 30 minutes, and start to pass water vapor from 500°C for activation, and obtain macroporous activated carbon fibers after cooling. The specific surface area is 1027m 2 /g. Its electron micrograph is shown in Figure 1, and the surface of the obtained macroporous activated carbon fiber is covered with macropores (100nm<aperture<600nm), and the hole type is relatively round.
实施例2Example 2
将粘胶纤维先在蒸馏水中清洗，晾干。将2mol/l的磷酸氢二钠盐溶液和5wt％ H3PO4溶液以1∶5的比例混合，再将清洗晾干后的粘胶原丝置于此溶液中静置10小时，取出自然风干后放入预氧化炉中，在300℃加热，恒温1小时。然后置入碳化活化炉中，在氦气保护下以20℃/min的速率升温到800℃，恒温2小时，并从600℃开始通入水蒸汽活化，得到大孔型活性碳纤维。比表面积为1303m2/g，所获得的大孔型活性碳纤维表面布满大孔(50nm＜孔径＜300nm)，且孔型较圆。Wash the viscose fiber in distilled water first and let it dry. Mix 2mol/l disodium hydrogen phosphate solution and 5wt% H3PO4 solution at a ratio of 1:5 , then place the cleaned and dried viscose filaments in this solution for 10 hours, take out the natural After air-drying, put it into a pre-oxidation furnace, heat at 300° C., and keep the temperature constant for 1 hour. Then put it into a carbonization activation furnace, raise the temperature to 800°C at a rate of 20°C/min under the protection of helium, keep the temperature constant for 2 hours, and start to pass water vapor from 600°C for activation to obtain macroporous activated carbon fibers. The specific surface area is 1303m 2 /g, and the surface of the obtained macroporous activated carbon fiber is covered with macropores (50nm<pore diameter<300nm), and the pore type is relatively round.
实施例3Example 3
将粘胶纤维先在去离子水或蒸馏水中清洗，晾干。将3mol/l的氯化钠盐溶液和40wt％ H3PO4溶液以1∶2的比例混合，再将清洗晾干后的粘胶原丝置于此溶液中静置24小时，取出自然风干后放入预氧化炉中，在500℃加热，恒温1小时。然后置入碳化活化炉中，在N2保护下以20℃/min的速率升温到1100℃，恒温1小时，并从700℃开始通入水蒸汽活化，得到大孔型活性碳纤维。比表面积为988m2/g，所获得的大孔型活性碳纤维表面布满大孔(100nm＜孔径＜500nm)，且孔型较圆。Wash the viscose fiber in deionized or distilled water first, and let it dry. Mix 3mol/l sodium chloride salt solution and 40wt% H 3 PO 4 solution in a ratio of 1:2, then place the cleaned and dried viscose filaments in this solution for 24 hours, take it out and let it air dry Then put it into a pre-oxidation furnace, heat at 500°C, and keep the temperature constant for 1 hour. Then put it into a carbonization activation furnace, raise the temperature to 1100°C at a rate of 20°C/min under the protection of N2, keep the temperature for 1 hour, and start to pass water vapor from 700°C for activation to obtain macroporous activated carbon fibers. The specific surface area is 988m 2 /g, and the surface of the obtained macroporous activated carbon fiber is covered with macropores (100nm<pore diameter<500nm), and the pore type is relatively round.
实施例4Example 4
将粘胶纤维先在去离子水或蒸馏水中清洗，晾干。将氯化镁的饱和盐溶液和10wt％ H3PO4溶液以1∶4的比例混合，再将清洗晾干后的粘胶原丝置于此溶液中静置15小时，取出自然风干后放入预氧化炉中，在400℃加热，恒温30分钟。然后置入碳化活化炉中，在氩气保护下以20℃/min的速率升温到900℃，恒温5小时，并从700℃开始通入水蒸汽活化，得到大孔型活性碳纤维。比表面积为1113m2/g，所获得的大孔型活性碳纤维表面布满大孔(50nm＜孔径＜200nm)，且孔型较圆。Wash the viscose fiber in deionized or distilled water first, and let it dry. Mix the saturated salt solution of magnesium chloride and 10wt% H 3 PO 4 solution at a ratio of 1:4, then place the cleaned and dried viscose filaments in this solution and let it stand for 15 hours, take it out and dry it naturally and put it in a pre- In an oxidation furnace, heat at 400°C and keep the temperature constant for 30 minutes. Then put it into a carbonization activation furnace, raise the temperature to 900°C at a rate of 20°C/min under the protection of argon, keep the temperature constant for 5 hours, and start to pass water vapor from 700°C for activation to obtain macroporous activated carbon fibers. The specific surface area is 1113m 2 /g, and the surface of the obtained macroporous activated carbon fiber is covered with macropores (50nm<pore diameter<200nm), and the pore type is relatively round.
实施例5Example 5
将粘胶纤维先在去离子水或蒸馏水中清洗，晾干。将饱和浓度的氯化镁和磷酸二氢钠的混合盐溶液(氯化镁和磷酸二氢钠的摩尔比为1∶1)和30wt％ H3PO4溶液以1∶3的比例混合，再将清洗晾干后的粘胶原丝置于此溶液中静置24小时，取出自然风干后放入预氧化炉中，在300℃加热恒温30分钟。然后置入碳化活化炉中，在N2保护下以20℃/min的速率升温到1100℃，恒温半小时，并从700℃开始通入水蒸汽活化，得到大孔型活性碳纤维。比表面积为1273m2/g，所获得的大孔型活性碳纤维表面布满大孔(100nm＜孔径＜400nm)，且孔型较圆。Wash the viscose fiber in deionized or distilled water first, and let it dry. Mix the saturated concentration of magnesium chloride and sodium dihydrogen phosphate mixed salt solution (the molar ratio of magnesium chloride and sodium dihydrogen phosphate is 1:1) and 30wt% H 3 PO 4 solution in a ratio of 1:3, then wash and dry The final viscose collagen filaments are placed in this solution and left to stand for 24 hours, taken out and air-dried naturally, then placed in a pre-oxidation furnace, and heated at a constant temperature of 300°C for 30 minutes. Then put it into a carbonization activation furnace, raise the temperature to 1100°C at a rate of 20°C/min under the protection of N2 , keep the temperature constant for half an hour, and start to pass water vapor from 700°C for activation to obtain macroporous activated carbon fibers. The specific surface area is 1273m 2 /g, and the surface of the obtained macroporous activated carbon fiber is covered with macropores (100nm<pore diameter<400nm), and the pore type is relatively round.
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| CN101844070B (en) * | 2010-05-07 | 2013-12-11 | 东华大学 | Porous activated carbon fiber adsorbing material of sheath-core composite structure and preparation thereof |
| CN102153162B (en) * | 2011-04-29 | 2013-10-09 | 南京大学 | Application of activated carbon activated by KOH in adsorption and removal of antibiotics in water |
| CN102874805A (en) * | 2012-09-17 | 2013-01-16 | 浙江海亮环境材料有限公司 | Method for preparing porous carbon for wastewater treatment |
| CN104817417B (en) * | 2015-04-13 | 2017-12-12 | 湖南浏花烟花有限公司 | A kind of method for preparing bamboo charcoal fiber cotton |
| CN104878478A (en) * | 2015-06-08 | 2015-09-02 | 江苏同康特种活性炭纤维面料有限公司 | Activating method of high-strength viscose-based active carbon fiber fabric |
| CN104878479A (en) * | 2015-06-08 | 2015-09-02 | 江苏同康特种活性炭纤维面料有限公司 | Activating method of long-service-life high-strength viscose-based active carbon fiber fabric |
| CN104947361A (en) * | 2015-06-08 | 2015-09-30 | 江苏同康特种活性炭纤维面料有限公司 | Carbonization method for viscose-based carbonized fireproofing fabric with excellent flame resistance |
| CN106111058A (en) * | 2016-06-14 | 2016-11-16 | 时笑阳 | A kind of ion hydrate type adsorbent and its preparation method and application |
| CN112871133A (en) * | 2020-04-21 | 2021-06-01 | 中国科学院大连化学物理研究所 | Preparation method and application of macroporous inorganic functional material for adsorbing inactivated viruses |
| CN118326702B (en) * | 2024-06-17 | 2024-08-27 | 烟台奥森制动材料有限公司 | Preparation method for continuous steam activation of carbon fibers of battery felt |
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