CN106179240A - A kind of preparation method of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material - Google Patents

A kind of preparation method of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material Download PDF

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Publication number
CN106179240A
CN106179240A CN201610560599.3A CN201610560599A CN106179240A CN 106179240 A CN106179240 A CN 106179240A CN 201610560599 A CN201610560599 A CN 201610560599A CN 106179240 A CN106179240 A CN 106179240A
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CN
China
Prior art keywords
raw material
absorption agent
carbon fiber
aeroge
flexible fiber
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Pending
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CN201610560599.3A
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Chinese (zh)
Inventor
李坚
万才超
焦月
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Northeast Forestry University
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Northeast Forestry University
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Priority to CN201610560599.3A priority Critical patent/CN106179240A/en
Publication of CN106179240A publication Critical patent/CN106179240A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28047Gels
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

Abstract

The preparation method of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material, the present invention relates to the preparation method of carbon fiber aeroge circulation absorption agent.The invention solves the problems that tradition adsorbing material oil absorbency low, without or weakly stable selectivity, recycle the problem such as ability.Method: flexible fiber is kneaded into bulk and is placed in container, the container that will be equipped with flexible fiber is placed in high temperature pyrolysis device, is passed through noble gas in high temperature pyrolysis device;Under the protection of noble gas; first the temperature of high temperature pyrolysis device risen to 200 DEG C~800 DEG C and is incubated, then the temperature of high temperature pyrolysis device be warming up to 1000 DEG C~2000 DEG C and be incubated, then high temperature pyrolysis unit temp is down to 400 DEG C~800 DEG C; after cooling, through naturally cooling to room temperature.The present invention is for the preparation method of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material.

Description

A kind of preparation of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material Method
Technical field
The present invention relates to the preparation method of carbon fiber aeroge circulation absorption agent.
Background technology
Animal and plant have been given in environmental pollution caused by Oil spills, chemistry leakage and industrial organic sewage discharge Living environment bring the destruction being difficult to reverse.At present, the process of organic wastewater still relies on the physics of various adsorbent, change Learn adsorption.Conventional adsorbent such as silica gel, activated alumina etc. are because of limited sorption capacity, complicated process of preparation, adsorption conditions Limit, without problems such as (or weak) adsorptive selectivity, recycling ability, it is difficult to meet the need of large-scale treatment of Organic Wastewater Ask.Activated carbon is a kind of more conventional adsorbent.Having hydrophobic material with carbon element as one, the hydrophobicity of itself is it Providing genetic prerequisite as oil-water separation material, but activated carbon is on the high side, this just have impact on its answering in water processes With and promote.Additionally, due to activated carbon is very big to the removal effect difference of water pollutant, cause it that kind of adsorbate is had Bigger restriction.Activated carbon is shorter for service life, needs periodic replacement, too increases cost.Therefore, people more favor in green Colour circle is protected, with low cost, high adsorption, reusable edible and have the adsorbing material of adsorptive selectivity.
Summary of the invention
The present invention is to solve that tradition adsorbing material oil absorbency is low, without (or weak) adsorptive selectivity, recycling ability Etc. problem, and provide the preparation method of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material.
The preparation method of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material is according to following steps Carry out:
One, flexible fiber being kneaded into bulk to be placed in container, the container that will be equipped with flexible fiber is placed in high temperature pyrolysis dress In putting, in high temperature pyrolysis device, it is passed through noble gas 5min~20min;
Two, under the protection of noble gas, it is 0.1 DEG C/min~20 DEG C/min with heating rate, by high temperature pyrolysis device Temperature first rise to 200 DEG C~800 DEG C, and under conditions of temperature is 200 DEG C~800 DEG C, be incubated 1h~10h, then with Heating rate is 0.1 DEG C/min~20 DEG C/min, and by 200 DEG C~800 DEG C, the temperature of high temperature pyrolysis device is warming up to 1000 DEG C ~2000 DEG C, and under conditions of temperature is 1000 DEG C~2000 DEG C, it is incubated 1h~10h, then is 0.1 DEG C/min with rate of temperature fall ~20 DEG C/min, high temperature pyrolysis unit temp is down to 400 DEG C~800 DEG C by 1000 DEG C~2000 DEG C, after cooling, through the coldest But to room temperature, the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material is obtained.
The invention has the beneficial effects as follows: the carbon fiber aeroge that, prepared by the present invention has the hydrophobic performance of excellence, contact Angle can reach 151 °, and therefore this carbon fiber aeroge has good adsorptive selectivity, can separate organic liquor from aqueous solution Body.
Two, the carbon fiber aeroge that prepared by the present invention has a higher adsorption rate, adsorbable own wt 23~51 times Organic solvent and waste oil.
Three, the carbon fiber aeroge that prepared by the present invention can be recycled, and the organic liquid sucked in adsorbent can be according to having The type of machine liquid use burn, extrude, the means such as extraction are separated, after being used for multiple times, adsorbance change is not quite.
Four, the preparation method that the present invention provides is simple, quickly, it is not necessary to expensive device, raw material sources are extensive, with low cost And environment-friendly and green, preparation method safety is high, will not cause environment pollution.
The present invention is for the preparation method of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material.
Accompanying drawing explanation
Fig. 1 is the photomacrograph figure of natural bamboo fibres;
Fig. 2 is the photomacrograph of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of embodiment one preparation Figure;
Fig. 3 is the scanning electron microscope (SEM) photograph of natural bamboo fibres;
Fig. 4 is the scanning electron microscope of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of embodiment one preparation Figure;
Fig. 5 is the water contact angle of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of embodiment one preparation Test figure;
Fig. 6 is that the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of embodiment one preparation is to various organic The adsorption rate of liquid, 1 is acetylacetone,2,4-pentanedione, and 2 is benzene, and 3 is chloroform, and 4 is dimethylformamide, and 5 is ethanol, and 6 is acetic acid second Ester, 7 is heptane, and 8 is machine oil, and 9 is oleic acid, and 10 is carbon tetrachloride, and 11 is toluene;
Fig. 7 is carbon fiber aeroge circulation absorption agent the following for benzene with flexible fiber as raw material of embodiment one preparation Ring absorption test, 1 is adsorption process, and 2 is combustion process, and 3 is quality of adsorption, and 4 is residual mass;
Carbon fiber aeroge circulation absorption agent the following for ethanol with flexible fiber as raw material of Fig. 8 embodiment one preparation Ring absorption test, 1 is adsorption process, and 2 is extrusion process, and 3 is quality of adsorption, and 4 is residual mass;
The carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of Fig. 9 embodiment one preparation circulation to machine oil Absorption test, 1 is adsorption process, and 2 is extraction and combustion process, and 3 is quality of adsorption, and 4 is residual mass.
Detailed description of the invention
Technical solution of the present invention is not limited to the detailed description of the invention of act set forth below, also include each detailed description of the invention it Between combination in any.
Detailed description of the invention one: a kind of carbon fiber aeroge circulation with flexible fiber as raw material described in present embodiment The preparation method of adsorbent follows the steps below:
One, flexible fiber being kneaded into bulk to be placed in container, the container that will be equipped with flexible fiber is placed in high temperature pyrolysis dress In putting, in high temperature pyrolysis device, it is passed through noble gas 5min~20min;
Two, under the protection of noble gas, it is 0.1 DEG C/min~20 DEG C/min with heating rate, by high temperature pyrolysis device Temperature first rise to 200 DEG C~800 DEG C, and under conditions of temperature is 200 DEG C~800 DEG C, be incubated 1h~10h, then with Heating rate is 0.1 DEG C/min~20 DEG C/min, and by 200 DEG C~800 DEG C, the temperature of high temperature pyrolysis device is warming up to 1000 DEG C ~2000 DEG C, and under conditions of temperature is 1000 DEG C~2000 DEG C, it is incubated 1h~10h, then is 0.1 DEG C/min with rate of temperature fall ~20 DEG C/min, high temperature pyrolysis unit temp is down to 400 DEG C~800 DEG C by 1000 DEG C~2000 DEG C, after cooling, through the coldest But to room temperature, the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material is obtained.
Present embodiment provides the benefit that: the carbon fiber aeroge that, prepared by present embodiment has the hydrophobic of excellence Performance, contact angle can reach 151 °, and therefore this carbon fiber aeroge has good adsorptive selectivity, can divide from aqueous solution From organic liquid.
Two, the carbon fiber aeroge that prepared by present embodiment has higher adsorption rate, adsorbable own wt 23~51 Organic solvent again and waste oil.
Three, the carbon fiber aeroge that prepared by present embodiment can be recycled, and the organic liquid sucked in adsorbent can root Use according to the type of organic liquid burn, extrude, the means such as extraction are separated, after being used for multiple times, adsorbance change is not quite.
Four, the preparation method that present embodiment provides is simple, quickly, it is not necessary to expensive device, and raw material sources are extensive, cost Cheap and environment-friendly and green, preparation method safety is high, will not cause environment pollution.
Detailed description of the invention two: present embodiment is unlike detailed description of the invention one: the flexibility described in step one Fiber is bamboo fibre, cotton fiber or flaxen fiber.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment is unlike one of detailed description of the invention one or two: institute in step one The container stated is quartz curette, porcelain Noah's ark or tube-type receptacle.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: present embodiment is unlike one of detailed description of the invention one to three: institute in step one The high temperature pyrolysis device stated is tube furnace, Muffle furnace or pyrolysis oven.Other is identical with detailed description of the invention one to three.
Detailed description of the invention five: present embodiment is unlike one of detailed description of the invention one to four: in step 2 with Heating rate is 5 DEG C/min, and first the temperature of tube furnace is risen to 500 DEG C.Other is identical with detailed description of the invention one to four.
Detailed description of the invention six: present embodiment is unlike one of detailed description of the invention one to five: in step 2 Under conditions of temperature is 500 DEG C, it is incubated 1h.Other is identical with detailed description of the invention one to five.
Detailed description of the invention seven: present embodiment is unlike one of detailed description of the invention one to six: in step 2 with Heating rate is 5 DEG C/min, and by 500 DEG C, tube furnace temperature is warming up to 1000 DEG C.Other and detailed description of the invention one to six phase With.
Detailed description of the invention eight: present embodiment is unlike one of detailed description of the invention one to seven: in step 2 Under conditions of temperature is 1000 DEG C, it is incubated 2h.Other is identical with detailed description of the invention one to seven.
Detailed description of the invention nine: present embodiment is unlike one of detailed description of the invention one to eight: in step 2 with Rate of temperature fall is 5 DEG C/min, and by 1000 DEG C, tube furnace temperature is down to 500 DEG C.Other is identical with detailed description of the invention one to eight.
Detailed description of the invention ten: present embodiment is unlike one of detailed description of the invention one to nine: will in step one Flexible fiber is kneaded into bulk and is placed in container, and the container that will be equipped with flexible fiber is placed in tube furnace, is passed through in tube furnace Noble gas 15min.Other is identical with detailed description of the invention one to nine.
Employing following example checking beneficial effects of the present invention:
Embodiment one:
The preparation method of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material described in the present embodiment Follow the steps below:
One, flexible fiber being kneaded into bulk to be placed in container, the container that will be equipped with flexible fiber is placed in tube furnace, to Tube furnace is passed through noble gas 15min;
Two, under the protection of noble gas, it is 5 DEG C/min with heating rate, first the temperature of tube furnace is risen to 500 DEG C, and under conditions of temperature is 500 DEG C, it is incubated 1h, is then 5 DEG C/min with heating rate, by the temperature of tube furnace by 500 DEG C it is warming up to 1000 DEG C, and under conditions of temperature is 1000 DEG C, is incubated 2h, then is 5 DEG C/min with rate of temperature fall, by tube furnace Temperature is down to 500 DEG C by 1000 DEG C, after cooling, through naturally cooling to room temperature, obtains the carbon fiber gas with flexible fiber as raw material Gel circulation absorption agent;
Flexible fiber described in step one is natural bamboo fibres;Container described in step one is quartz curette.
Utilize the carbon fiber aeroge using flexible fiber as raw material prepared by embodiment one as circulation absorption agent to various The machine liquid of common are carries out adsorbing, circulation absorption test, and test result is as follows:
Fig. 1 is the photomacrograph figure of natural bamboo fibres, and as seen from the figure, this fiber has good flexibility, and meeting preparation needs Ask.
Fig. 2 is the photomacrograph of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of embodiment one preparation Figure, as seen from the figure, this carbon fiber aeroge circulation absorption agent is the black cylinder that shape is regular, it was demonstrated that this carbon fiber aeroge Circulation absorption agent has good forming ability.
Fig. 3 is the scanning electron microscope (SEM) photograph of natural bamboo fibres, and as seen from the figure, the diameter of this fiber is about 10~25 μm.
Fig. 4 is the scanning electron microscope of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of embodiment one preparation Figure, as seen from the figure, after high temperature pyrolysis processes, the diameter of fiber substantially reduces to 3~10 μm.
Fig. 5 is the water contact angle of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of embodiment one preparation Test figure, as seen from the figure, this carbon fiber aeroge circulation absorption agent has good hydrophobicity, and water contact angle is up to 151 °.
Fig. 6 is that the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of embodiment one preparation is to various organic The adsorption rate of liquid, 1 is acetylacetone,2,4-pentanedione, and 2 is benzene, and 3 is chloroform, and 4 is dimethylformamide, and 5 is ethanol, and 6 is acetic acid second Ester, 7 is heptane, and 8 is machine oil, and 9 is oleic acid, and 10 is carbon tetrachloride, and 11 is toluene;As seen from the figure, this carbon fiber aeroge circulation The adsorbable own wt of adsorbent 23~the organic solvent of 51 times and waste oil.
Fig. 7 is carbon fiber aeroge circulation absorption agent the following for benzene with flexible fiber as raw material of embodiment one preparation Ring absorption test, 1 is adsorption process, and 2 is combustion process, and 3 is quality of adsorption, and 4 is residual mass;As seen from the figure, through five times Loop test, the absorbability of this carbon fiber aeroge circulation absorption agent is basically unchanged.
Carbon fiber aeroge circulation absorption agent the following for ethanol with flexible fiber as raw material of Fig. 8 embodiment one preparation Ring absorption test, 1 is adsorption process, and 2 is extrusion process, and 3 is quality of adsorption, and 4 is residual mass;As seen from the figure, through five times Loop test, this carbon fiber aeroge circulation absorption agent still keeps higher absorbability.
The carbon fiber aeroge circulation absorption agent with flexible fiber as raw material of Fig. 9 embodiment one preparation circulation to machine oil Absorption test, 1 is adsorption process, and 2 is extraction and combustion process, and 3 is quality of adsorption, and 4 is residual mass;As seen from the figure, pass through Five loop tests, the absorbability of this carbon fiber aeroge circulation absorption agent is basically unchanged.

Claims (10)

1. the preparation method of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material, it is characterised in that a kind of with Flexible fiber is that the preparation method of the carbon fiber aeroge circulation absorption agent of raw material follows the steps below:
One, flexible fiber being kneaded into bulk to be placed in container, the container that will be equipped with flexible fiber is placed in high temperature pyrolysis device, Noble gas 5min~20min it is passed through in high temperature pyrolysis device;
Two, under the protection of noble gas, it is 0.1 DEG C/min~20 DEG C/min with heating rate, by the temperature of high temperature pyrolysis device First degree rises to 200 DEG C~800 DEG C, and under conditions of temperature is 200 DEG C~800 DEG C, is incubated 1h~10h, then to heat up Speed is 0.1 DEG C/min~20 DEG C/min, by the temperature of high temperature pyrolysis device by 200 DEG C~800 DEG C be warming up to 1000 DEG C~ 2000 DEG C, and under conditions of temperature is 1000 DEG C~2000 DEG C, be incubated 1h~10h, then with rate of temperature fall be 0.1 DEG C/min~ 20 DEG C/min, high temperature pyrolysis unit temp is down to 400 DEG C~800 DEG C by 1000 DEG C~2000 DEG C, after cooling, through natural cooling To room temperature, obtain the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material.
The preparation side of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that the flexible fiber described in step one is bamboo fibre, cotton fiber or flaxen fiber.
The preparation side of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that the container described in step one is quartz curette, porcelain Noah's ark or tube-type receptacle.
The preparation side of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that the high temperature pyrolysis device described in step one is tube furnace, Muffle furnace or pyrolysis oven.
The preparation side of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that be 5 DEG C/min with heating rate in step 2, first the temperature of tube furnace is risen to 500 DEG C.
The preparation side of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that in step 2 under conditions of temperature is 500 DEG C, is incubated 1h.
The preparation side of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that be 5 DEG C/min with heating rate in step 2, tube furnace temperature is warming up to 1000 DEG C by 500 DEG C.
The preparation side of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that in step 2 under conditions of temperature is 1000 DEG C, is incubated 2h.
The preparation side of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that be 5 DEG C/min with rate of temperature fall in step 2, tube furnace temperature is down to 500 DEG C by 1000 DEG C.
The preparation of a kind of carbon fiber aeroge circulation absorption agent with flexible fiber as raw material the most according to claim 1 Method, it is characterised in that flexible fiber being kneaded in step one bulk and is placed in container, the container that will be equipped with flexible fiber is put In tube furnace, in tube furnace, it is passed through noble gas 15min.
CN201610560599.3A 2016-07-15 2016-07-15 A kind of preparation method of the carbon fiber aeroge circulation absorption agent with flexible fiber as raw material Pending CN106179240A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107243323A (en) * 2017-06-27 2017-10-13 王建军 A kind of fibre based activated Carbon Materials of magnetic bamboo and its preparation method and application
CN108097213A (en) * 2018-01-17 2018-06-01 湖南大学 A kind of arsenic-removing adsorption agent and preparation method thereof

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CN103253649A (en) * 2013-04-19 2013-08-21 东南大学 Preparation method and application of carbon sponge
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CN103146017A (en) * 2013-03-06 2013-06-12 东北林业大学 Method for preparing aerogel by quickly dissolving lignocellulose
CN103253649A (en) * 2013-04-19 2013-08-21 东南大学 Preparation method and application of carbon sponge
CN105601314A (en) * 2015-12-29 2016-05-25 中国石油化工股份有限公司 Preparation method of hydrophobic carbon-fiber aerogel for reclaiming oil spillage

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107243323A (en) * 2017-06-27 2017-10-13 王建军 A kind of fibre based activated Carbon Materials of magnetic bamboo and its preparation method and application
CN107243323B (en) * 2017-06-27 2020-05-08 王建军 Magnetic bamboo fiber based activated carbon material and preparation method and application thereof
CN108097213A (en) * 2018-01-17 2018-06-01 湖南大学 A kind of arsenic-removing adsorption agent and preparation method thereof

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Application publication date: 20161207