CN101734651B - Preparation method of fibrous porous carbon for purification of drinking water - Google Patents
Preparation method of fibrous porous carbon for purification of drinking water Download PDFInfo
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- CN101734651B CN101734651B CN2010101101196A CN201010110119A CN101734651B CN 101734651 B CN101734651 B CN 101734651B CN 2010101101196 A CN2010101101196 A CN 2010101101196A CN 201010110119 A CN201010110119 A CN 201010110119A CN 101734651 B CN101734651 B CN 101734651B
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Abstract
The invention provides a preparation method of fibrous porous carbon for purification of drinking water, belonging to the technical field of preparation of new materials and the cross technical fields of cellulose science, carbon material and resource environment. The method is characterized by taking viscose fiber as a raw material, and preparing the fibrous porous carbon by the steps of pretreating, charring, activating, secondary charring and secondary activating of the raw material. By soaking the viscose fiber in diammonium hydrogen phosphate, the charring yield can be effectively improved. Through charring, activating, secondary charring and secondary activating, the fibrous porous carbon with a high specific surface area can be prepared. The invention has the effects and advantages that by soaking the viscose fiber in the diammonium hydrogen phosphate, the yield of the porous carbon can be improved so as to reduce the product price, and the prepared fibrous porous carbon has high and controllable specific surface area and good purifying effect on drinking water.
Description
Technical field
The present invention designs a kind of preparation method who is used for the fibrous porous carbon of drink water purifying.It mainly is to be raw material with the viscose fiber, prepares the fibrous porous carbon that specific surface area is big, drink water purifying is effective through pre-treatment, charing, activation, secondary charing and re-activation.
Background technology
The raw water quality at most water sources such as China's rivers,lakes and seas even underground water is relatively poor relatively and pollute and to be on the rise.Because the main at present coagulation that adopts in the most water treatment plants of China, precipitation is filtered, and conventional water treatment processes such as liquid chlorine sterilization are limited to the removal effect of organic pollutant etc., is difficult to adapt to the water quality of continuous deterioration, is difficult to reach up-to-date drinking water standard.The prosperity of fibrous porous carbon pore texture, there is a large amount of oxygen-containing functional groups on the surface, specific surface area is big, high adsorption capacity, and have certain intensity and good form, be difficult for pulverizing, the pressure-losses is little in water treatment, packing layer is blockage phenomenon easily not, and regeneration is relatively easy, is expected to play a positive role in drink water purifying.But fibrous porous carbon yield in the preparation is lower, generally 10～18%, thereby causes higher its industrial applications in tap water that restricted of preparation cost.If protofibril is flooded the carbonization yield that pre-treatment can improve raw fibre, thereby reduce the cost of final porous charcoal product, be expected to promote its large-scale application in tap water.
Summary of the invention
The present invention seeks to design a kind of fibrous porous carbon that is used for drink water purifying, it is raw material with the viscose fiber, makes through dipping pre-treatment, charing, activation, secondary charing and re-activation, and its technical characterstic is that the step and the processing condition of its preparation are as follows:
(1). raw fibre is cut into the sample of 150mm * 150mm, and in 110 ℃ of oven dry 3h, taking-up is weighed;
(2). it is to soak 5～30min in 1～40% the Secondary ammonium phosphate that fiber after will drying immerses the concentration for preparing in advance, and sample takes out extruding from solution, dry 10h at 110～150 ℃ then, weighs;
(3). soak and dried viscose fiber is warming up to 800～900 ℃ with 2～10 ℃/min under nitrogen or helium atmosphere, constant temperature 0.5～2h carries out charing, and the fiber carbonization yield that soaks through Secondary ammonium phosphate is 1.1～2.4 times when being untreated;
(4). with water vapour is activated media, in 700～950 ℃ of following activation treatment 10～120min, obtains having the fibrous porous carbon of certain initial hole after the cooling in nitrogen or helium atmosphere;
(5). this fibrous porous carbon is placed under nitrogen or the helium atmosphere, temperature rise rate is 10～20 ℃/min, carrying out the secondary charing at 800～900 ℃ of following constant temperature 30～120min, is that activated media carries out re-activation again with water vapour, can make the high-specific surface area fibrous porous carbon.
This fibrous porous carbon has good decontamination effect improving to tap water, tap water not up to standard behind this fibrous porous carbon purifying, COD
MnAll reduce to below 1.5 by 3.5 before purifying, satisfy COD in the tap water latest national standards fully
MnBe not higher than 3 standard.
Embodiment
Come enumeration technical characterstic of the present invention below in conjunction with specific embodiment.
Embodiment 1
Viscose fiber is cut into the sample of 150mm * 150mm, and in 110 ℃ of oven dry 3h, taking-up is weighed.It is to soak 5min in 10% the Secondary ammonium phosphate that fiber after the oven dry is immersed the concentration prepare in advance, and sample takes out extruding from solution, dry 10h at 110 ℃ then, weighs; Immersion and dried viscose fiber are warming up to 900 ℃ with 4 ℃/min under nitrogen atmosphere, constant temperature 2h carries out charing, and the fiber carbonization yield that soaks through Secondary ammonium phosphate is 44%, is 2.4 times of untreatment fiber carbonization yield 18%; With water vapour is activated media, and in 750 ℃ of following activation treatment 30min, obtaining specific surface area after the cooling is 673m in nitrogen atmosphere
2The fibrous porous carbon of/g; This fibrous porous carbon is placed under the nitrogen atmosphere, and temperature rise rate is 10 ℃/min, carries out the secondary charing at 820 ℃ of following constant temperature 60min, is that activated media carries out re-activation at 820 ℃ of following constant temperature 120min again with water vapour, and can make specific surface area is 2685m
2The fibrous porous carbon of/g.This fibrous porous carbon has good decontamination effect improving to tap water, tap water not up to standard behind this fibrous porous carbon purifying, COD
MnReduce to 1.5 by 3.5 before purifying, satisfy COD in the tap water latest national standards fully
MnBe not higher than 3 standard.
Embodiment 2
With gained dipping charing sample among the embodiment 1 is raw material, is activated media with water vapour, and in 850 ℃ of following activation treatment 30min, obtaining specific surface area after the cooling is 1250m in nitrogen atmosphere
2The fibrous porous carbon of/g; This fibrous porous carbon is placed under the nitrogen atmosphere, and temperature rise rate is 10 ℃/min, carries out the secondary charing at 820 ℃ of following constant temperature 60min, is that activated media carries out re-activation at 820 ℃ of following constant temperature 120min again with water vapour, and can make specific surface area is 2963m
2The fibrous porous carbon of/g.This fibrous porous carbon has good decontamination effect improving to tap water, tap water not up to standard behind this fibrous porous carbon purifying, COD
MnReduce to 1.3 by 3.5 before purifying, satisfy COD in the tap water latest national standards fully
MnBe not higher than 3 standard.
Embodiment 3
With gained dipping charing sample among the embodiment 1 is raw material, is activated media with water vapour, and in 950 ℃ of following activation treatment 30min, obtaining specific surface area after the cooling is 1702m in nitrogen atmosphere
2The fibrous porous carbon of/g; This fibrous porous carbon is placed under the nitrogen atmosphere, and temperature rise rate is 10 ℃/min, carries out the secondary charing at 820 ℃ of following constant temperature 60min, is that activated media carries out re-activation at 820 ℃ of following constant temperature 120min again with water vapour, and can make specific surface area is 3218m
2The fibrous porous carbon of/g.This fibrous porous carbon has good decontamination effect improving to tap water, tap water not up to standard behind this fibrous porous carbon purifying, COD
MnReduce to 1.1 by 3.5 before purifying, satisfy COD in the tap water latest national standards fully
MnBe not higher than 3 standard.
Embodiment 4
Viscose fiber is cut into the sample of 150mm * 150mm, and in 110 ℃ of oven dry 3h, taking-up is weighed.It is to soak 5min in 5% the Secondary ammonium phosphate that fiber after the oven dry is immersed the concentration prepare in advance, and sample takes out extruding from solution, dry 10h at 110 ℃ then, weighs; Immersion and dried viscose fiber are warming up to 900 ℃ with 4 ℃/min under nitrogen atmosphere, constant temperature 2h carries out charing, and the fiber carbonization yield that soaks through Secondary ammonium phosphate is 42%, is 2.3 times of untreatment fiber carbonization yield 18%; With water vapour is activated media, and in 800 ℃ of following activation treatment 30min, obtaining specific surface area after the cooling is 830m in nitrogen atmosphere
2The fibrous porous carbon of/g; This fibrous porous carbon is placed under the nitrogen atmosphere, and temperature rise rate is 10 ℃/min, carries out the secondary charing at 820 ℃ of following constant temperature 60min, is that activated media carries out re-activation at 820 ℃ of following constant temperature 120min again with water vapour, and can make specific surface area is 2815m
2The fibrous porous carbon of/g.This fibrous porous carbon has good decontamination effect improving to tap water, tap water not up to standard behind this fibrous porous carbon purifying, COD
MnReduce to 1.4 by 3.5 before purifying, satisfy COD in the tap water latest national standards fully
MnBe not higher than 3 standard.
Embodiment 5
With gained dipping charing sample among the embodiment 4 is raw material, is activated media with water vapour, and in 700 ℃ of following activation treatment 30min, obtaining specific surface area after the cooling is 450m in nitrogen atmosphere
2The fibrous porous carbon of/g; This fibrous porous carbon is placed under the nitrogen atmosphere, and temperature rise rate is 10 ℃/min, carries out the secondary charing at 820 ℃ of following constant temperature 60min, is that activated media carries out re-activation at 820 ℃ of following constant temperature 120min again with water vapour, and can make specific surface area is 2013m
2The fibrous porous carbon of/g.This fibrous porous carbon has good decontamination effect improving to tap water, tap water not up to standard behind this fibrous porous carbon purifying, COD
MnReduce to 2.0 by 3.5 before purifying, satisfy COD in the tap water latest national standards fully
MnBe not higher than 3 standard.
Embodiment 6
With gained dipping charing sample among the embodiment 4 is raw material, is activated media with water vapour, and in 900 ℃ of following activation treatment 30min, obtaining specific surface area after the cooling is 1604m in nitrogen atmosphere
2The fibrous porous carbon of/g; This fibrous porous carbon is placed under the nitrogen atmosphere, and temperature rise rate is 10 ℃/min, carries out the secondary charing at 820 ℃ of following constant temperature 60min, is that activated media carries out re-activation at 820 ℃ of following constant temperature 120min again with water vapour, and can make specific surface area is 3148m
2The fibrous porous carbon of/g.This fibrous porous carbon has good decontamination effect improving to tap water, tap water not up to standard behind this fibrous porous carbon purifying, COD
MnReduce to 1.2 by 3.5 before purifying, satisfy COD in the tap water latest national standards fully
MnBe not higher than 3 standard.
The invention effect
1. viscose fiber impregnation of phosphoric acid hydrogen two ammoniums can effectively improve its carbonization yield, and corresponding carbonization yield can reach 2.4 times of carbonization yield when being untreated after the dip treating.
2. be feedstock production high-specific surface area fibrous porous carbon with the viscose fiber, its specific surface area can reach 3218m
2/ g, and can effectively regulate and control by processing parameter contrast table areas such as Secondary ammonium phosphate impregnation rate, activation temperatures.
This fibrous porous carbon has good decontamination effect improving to water factory's water inlet.Tap water not up to standard behind this fibrous porous carbon purifying, COD
MnAll reduce to below 1.5 by 3.5 before purifying, satisfy COD in the tap water latest national standards fully
MnBe not higher than 3 standard.
Claims (2)
1. a preparation method who is used for the fibrous porous carbon of drink water purifying is a raw material with the viscose fiber, makes through raw materials pretreatment, charing, activation, secondary charing and re-activation, it is characterized in that the step of its preparation and processing condition are as follows:
(1). in 110 ℃ of oven dry 3h, taking-up is weighed with the raw material viscose fiber;
(2). it is that 1～40% ammonium dibasic phosphate solution soaks 5～30min that the viscose fiber after will drying places concentration, and fiber is taken out from solution and pushes, and at 110～150 ℃ of oven dry 10h, weighs;
(3). soak and dried viscose fiber is warming up to 800～900 ℃ with 2～10 ℃/min under nitrogen or helium atmosphere, constant temperature 0.5～2h carries out charing, and the fiber carbonization yield that soaks through Secondary ammonium phosphate is 1.1～2.4 times of untreatment fiber carbonization yield;
(4). with water vapour is activated media, with fiber after the above-mentioned charing in nitrogen or helium atmosphere in 700～950 ℃ of following activation treatment 10～120min, obtain having the fibrous porous carbon of certain initial hole after the cooling;
(5). the fibrous porous carbon that will have certain initial hole places under nitrogen or the helium atmosphere, temperature rise rate is 10～20 ℃/min, carry out the secondary charing at 800～900 ℃ of following constant temperature 30～120min, be that activated media carries out re-activation again with water vapour, can make the high-specific surface area fibrous porous carbon.
2. a kind of preparation method who is used for the fibrous porous carbon of drink water purifying according to claim 1 is characterized in that the concentration of ammonium dibasic phosphate solution is 5～30%, and loading to the Secondary ammonium phosphate on the fiber and the mass ratio of fibrous material is 5～100%.
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| CN108726576B (en) * | 2018-06-01 | 2019-08-23 | 东莞理工学院 | The continuous preparation porous charcoal/Fe of carbonization-activation oxidation3O4Method |
| CN110562974A (en) * | 2019-10-18 | 2019-12-13 | 中国石油大学(华东) | Preparation method of high-mesoporous-rate wood activated carbon |
| CN113735117A (en) * | 2021-08-25 | 2021-12-03 | 淮北市森化碳吸附剂有限责任公司 | Pressure swing adsorption's active carbon |
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Non-Patent Citations (1)
| Title |
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| 黄正宏等.湿氧化改性多孔炭对低浓度苯和丁酮蒸汽的吸附.《清华大学学报(自然科学版)》.2000,第40卷(第10期),111－115. * |
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