CN106861621A - A kind of La2O3/Fe2O3The preparation technology of carbon fibre material - Google Patents
A kind of La2O3/Fe2O3The preparation technology of carbon fibre material Download PDFInfo
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- CN106861621A CN106861621A CN201710184510.2A CN201710184510A CN106861621A CN 106861621 A CN106861621 A CN 106861621A CN 201710184510 A CN201710184510 A CN 201710184510A CN 106861621 A CN106861621 A CN 106861621A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid 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
- B01J20/28023—Fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to the higher value application of discarded object, more particularly to a kind of preparation method of functionalization sorbing material is applied to wastewater treatment field of Environment Protection, a kind of La2O3/Fe2O3Carbon fibre material, is matrix with discarded bafta, and using sol-gal process in the lanthanum-carried iron metal composite oxide of surface of cotton fabric, whole preparation process step is simple, easy to operate, the characteristics of the carbon material adsorbent of preparation has low cost, performance good.
Description
Technical field
The present invention relates to the higher value application of discarded object, more particularly to a kind of preparation method of functionalization sorbing material, tool
Body is a kind of La2O3/Fe2O3The preparation technology of carbon fibre material, is applied to wastewater treatment field of Environment Protection.
Background technology
About 26,000,000 tons of the waste textile that China produces, recovery has only been obtained less than 10% and has been reused, and other are big
Underground or burning are all embedded in, underground is imbedded, not only land occupation resource, chemical ＆ blended fabric is not easy to be degraded in underground, and
Colouring particles and fabric in fabric harmful substance in itself etc. can also contaminated soil and water resource, cause soil deterioration, water ring
Border is degraded.At present, the method for waste textile recycling mainly has：Machinery, physics, chemistry, heat energy and solvent are returned
Receipts method.The main component of bafta is cellulose, and content of cellulose accounts for 90%-94%, and C constituent contents are accounted in cellulose
44%, it is phosphorus content highest natural polymer, also hemicellulose, soluble saccharide, pectin, wax, fat in addition
Fat, nitrogen substance, ash grade, can be as the raw materials for production of activated carbon.Can largely be disappeared as carbon source prepares carbon material with cotton fiber
Consumption waste cotton fabric, the product added value for obtaining is high compared with the product added value that other method is obtained, and is not in machine cuts
Dust pollution during for regenerated fiber, and the acid or alkali environment of regenerated celulose fibre and paper-making process pollutes, and is a kind of environment
The reuse method of friendly.Carbon product active oxygen-containing functional group because surface is rich in, can combine to form with different kinds of ions or group
New carbon, makes it have a wide range of applications space in other field.
The content of the invention
It is carbon source with discarded bafta for the relatively low situation of the recycling of current waste textile, it is solidifying by colloidal sol
The lanthanum metal oxide of glue method carried with doped iron, calcining obtains fibrous lanthanum iron metal composite oxide carbon material, for going
Except the pollutant in waste water.To reach above-mentioned purpose, using following technical proposals：
A kind of La2O3/Fe2O3The preparation technology of carbon fibre material, is matrix with discarded bafta, using sol-gal process in cotton
The lanthanum-carried iron metal composite oxide of fabric face.Comprise the following steps：
（1）The pretreatment of discarded bafta：By waste cotton cloth as in distilled water, sodium hypochlorite and NaOH are added, stood
Clear water rinses low temperature drying afterwards, and the cotton chip for being cut into 2-3cm is stand-by；
（2）It is metal oxide-loaded：Metal salt mixture is dissolved in distilled water, ammonia is slowly added dropwise after adding citric acid solution
Water is 5-7 to the pH of solution, yellow gel is obtained after persistently stirring certain hour, to adding step in yellow gel（1）Gained
Cotton chip soaks, low temperature drying after dipping at least 48h；
（3）La2O3/Fe2O3The preparation of carbon fibre material：After the cotton chip of metal oxide-impregnated gel is wrapped up with tinfoil
La is can obtain after 1-2 is calcined in Muffle furnace2O3/Fe2O3Carbon fibre material.
Preferably, the mass concentration of sodium hypochlorite is 1% -3%, and the mass concentration of NaOH is 3% -5%, dwell temperature
It it is 80 DEG C -90 DEG C, the time of standing is 1-2h, and the temperature of low temperature drying is 50 DEG C.3. one kind according to claim 1
La2O3/Fe2O3Carbon fibre material, it is characterised in that：Step（2）Middle cotton chip is with the mass ratio of metal salt mixture：1：
3.25—1：6.85, the mixture of the molysite of the soluble lanthanum salt in metal salt mixture position and solubility.
Preferably, the mol ratio of lanthanum salt and molysite is 1:3—3:1.
Preferably, lanthanum salt is lanthanum nitrate, and the molysite is iron chloride, and the mol ratio of the lanthanum nitrate and iron chloride is 1:
3—3:1。
Preferably, the amount of the material of citric acid is the amount sum of lanthanum salt and molysite material.
Preferably, the calcining heat of fiber carbon material is 350 DEG C -650 DEG C.
Preferably, the calcining heat of fiber carbon material is 530 DEG C.
The present invention this have the advantage that compared with prior art：
Proposing a kind of discarded bafta carries out the approach of higher value application, by being improved to iron atom is adulterated in lanthanum-oxides
Reactivity, the synthesis temperature of metal oxide is reduced by the way that metal composite oxide is supported on bafta.
The application is matrix with discarded bafta, and Bian mixes the lanthanum-oxides carbon materials of iron with sol-gal process synthetic fibers shape
Material, the lanthanum-oxides carbon material of the iron of incorporation makes lanthanum element form defect so as to improve the adsorption capacity of adsorbent.
Brief description of the drawings：
Fig. 1 is waste cotton cloth, unmodified carbon fiber and La2O3/Fe2O3Carbon fiber compares the removal effect of rhodamine；
Fig. 2 is waste cotton cloth, unmodified carbon fiber and La2O3/Fe2O3Carbon fiber compares the removal effect of fluorine ion；
Fig. 3 is the La of different mol ratio example doping2O3/Fe2O3Carbon fiber compares the removal effect of rhodamine.
Specific embodiment
Embodiment 1
200mL deionized waters are taken in beaker, 2g sodium hypochlorite, 10g NaOH is added.Cotton 3g is put into 85 DEG C in solution
1h is boiled, clear water washing and filtering is used after solution turned yellow, cotton strap is cut into chip after 50 DEG C of low temperature dryings；By six hydrations of 2mmol
Lanthanum nitrate and 2mmol iron chloride are dissolved in 15mL deionized waters under magnetic stirring, and lanthanum is 1 with the mol ratio of iron：1, then
The citric acid of 4mmol is added in above-mentioned solution；Then, to ammoniacal liquor is slowly added dropwise in above-mentioned solution, regulation solution ph is arrived
6；After lasting stirring about 20 minutes, yellow transparent colloid substance is obtained；Cotton chip is soaked into 48h in above-mentioned colloidal sol, so
50 DEG C of low temperature dryings, after drying, the cotton chip of metal oxide-impregnated gel are wrapped up after the horse at 650 DEG C with tinfoil afterwards
Not calcined in stove 2 hours and can obtain La2O3/Fe2O3Carbon fiber；
Cotton directly is cut into fringe to be put into crucible, the Muffle furnace calcining that crucible is placed on 650 DEG C is not changed for 2 hours
The carbon fiber of property；
The cotton chip of 0.1g, unmodified carbon fiber and La are taken respectively2O3/Fe2O3Carbon fiber adds sieve of 50ml 150mg/L
Filtered after 24h is shaken in red bright solution, take supernatant liquor and calculate removal using the remaining rhodamine concentration of spectrophotometry
La is found after rate2O3/Fe2O3Carbon fiber, apparently higher than cotton fiber and unmodified carbon fiber, is tied to the removal ability of rhodamine
Fruit is as shown in Figure 1.
Embodiment 2
200mL deionized waters are taken in beaker, 3g sodium hypochlorite, 8g NaOH is added.Cotton 3g is cut into and is put into solution
85 DEG C are boiled 1h, and clear water washing and filtering is used after solution turned yellow, and cotton strap is cut into chip after 50 DEG C of low temperature dryings；By the six of 2mmol
Nitric hydrate lanthanum and 2mmol iron chloride are dissolved in 15mL deionized waters under magnetic stirring, and lanthanum is 1 with the mol ratio of iron：1,
Then the citric acid of 4mmol is added in above-mentioned solution, then, to ammoniacal liquor is slowly added dropwise in above-mentioned solution, adjusts solution
PH value is to 7；After lasting stirring about 20 minutes, yellow transparent colloid substance is obtained；Cotton chip is soaked in above-mentioned colloidal sol
50h, then 50 DEG C of low temperature dryings；After drying, the cotton chip of metal oxide-impregnated gel is wrapped up after 550 with tinfoil
DEG C Muffle furnace in calcining 1.5 hours i.e. can obtain La2O3/Fe2O3Carbon fiber；
Cotton directly is cut into fringe to be put into crucible, the Muffle furnace calcining that crucible is placed on 550 DEG C is not changed for 2 hours
The carbon fiber of property；
The cotton chip of 0.1g, unmodified carbon fiber and La are taken respectively2O3/Fe2O3Carbon fiber adds the fluorine of 50ml 200mg/L
Filtered after 24h is shaken in solion, take supernatant liquor and determine remaining fluorinion concentration using fluoride ion electrode method, calculating is gone
Except finding La after rate2O3/Fe2O3Carbon fiber to the removal ability of fluorine ion apparently higher than cotton fiber and unmodified carbon fiber,
Result is as shown in Figure 2.
Embodiment 3
200mL deionized waters are taken in beaker, 3g sodium hypochlorite, 10g NaOH is added.Cotton 3g is cut into and is put into solution
80 DEG C are boiled 1h, and clear water washing and filtering is used after solution turned yellow, and cotton strap is cut into chip after 50 DEG C of low temperature dryings；By the six of 2mmol
Nitric hydrate lanthanum and 2mmol iron chloride are dissolved in 15mL deionized waters under magnetic stirring, and lanthanum is 1 with the mol ratio of iron：1,
Then the citric acid of 4mmol is added in above-mentioned solution, then, to ammoniacal liquor is slowly added dropwise in above-mentioned solution, adjusts solution
PH value is to 5；After lasting stirring about 20 minutes, yellow transparent colloid substance is obtained；Cotton chip is soaked in above-mentioned colloidal sol
52h, then 50 DEG C of low temperature dryings；After drying, the cotton chip of metal oxide-impregnated gel is wrapped up after 350 with tinfoil
DEG C Muffle furnace in calcining 2 hours i.e. can obtain La2O3/Fe2O3Carbon fiber；
Take the La of 0.1g2O3/Fe2O3Filtered after shaking 24h in the rhodamine liquor of carbon fiber addition 50ml 100mg/L, taken
Layer clear liquid finds La after calculating clearance using the remaining rhodamine concentration of spectrophotometry2O3/Fe2O3Carbon fiber is to sieve
Red bright clearance is 92%；
Take the La of 0.1g2O3/Fe2O3Filtered after shaking 24h in the fluoride solution of carbon fiber addition 50ml 100mg/L, taken
Layer clear liquid determines remaining fluorinion concentration using fluoride ion electrode method, and La is found after calculating clearance2O3/Fe2O3Carbon fiber pair
The clearance of fluorine ion is 94%.
Embodiment 4
200mL deionized waters are taken in beaker, 2g sodium hypochlorite, 10g NaOH is added.Cotton 3g is cut into and is put into solution
85 DEG C are boiled 1h, and clear water washing and filtering is used after solution turned yellow, and cotton strap is cut into chip after 50 DEG C of low temperature dryings；By total mol concentration
Be the lanthanum nitrate hexahydrate of 4mmol and being dissolved under magnetic stirring in 15mL deionized waters for iron chloride, lanthanum and iron mole
Than being respectively 1：1 or 1：2 or 1：3 or 2：1 or 3：1；Then the citric acid of 4mmol is added in above-mentioned solution, then, upwards
State and be slowly added dropwise in solution ammoniacal liquor, regulation solution ph is to 7；After lasting stirring about 20 minutes, yellow transparent is obtained gluey
Material；Cotton chip is soaked into 54h in above-mentioned colloidal sol, then 50 DEG C of low temperature dryings；After drying, metal oxide-impregnated is coagulated
The cotton chip tinfoil parcel of glue 2 hours is that can obtain La after being calcined in 500 DEG C of Muffle furnace2O3/Fe2O3Carbon fiber；
Take the La of 0.1g difference lanthanum iron mol ratios2O3/Fe2O3Shaken in the rhodamine liquor of carbon fiber addition 50ml 100mg/L
Filtered after 24h, take supernatant liquor and calculate clearance using the remaining rhodamine concentration of spectrophotometry, as shown in Figure 3,
Understand that preferred lanthanum is 1 with the mol ratio of iron：2.
Claims (8)
1. a kind of La2O3/Fe2O3The preparation technology of carbon fibre material, it is characterised in that：It is matrix with discarded bafta, using molten
Sol-gel is comprised the following steps in the lanthanum-carried iron metal composite oxide of surface of cotton fabric：
The pretreatment of discarded bafta：During sodium hypochlorite and NaOH added into distilled water, wiring solution-forming, by waste cotton cloth extremely
A period of time is stood in solution, clear water rinsing low temperature drying after standing, the cotton chip for being cut into 2-3cm is stand-by；
It is metal oxide-loaded：Metal salt mixture is dissolved in distilled water, ammoniacal liquor is slowly added dropwise after adding citric acid solution
PH to solution is 5-7, yellow gel is obtained after persistently stirring certain hour, to adding step in yellow gel（1）Gained cotton
Cloth chip soaks, low temperature drying after dipping at least 48h；
La2O3/Fe2O3The preparation of carbon fibre material：The cotton chip of metal oxide-impregnated gel is wrapped up after horse with tinfoil
La is can obtain after 1-2 is not calcined in stove2O3/Fe2O3Carbon fibre material.
2. a kind of La according to claim 12O3/Fe2O3The preparation technology of carbon fibre material, it is characterised in that：Hypochlorous acid
The mass concentration of sodium is 1% -3%, and the mass concentration of NaOH is 3% -5%, and dwell temperature is 80 DEG C -90 DEG C, standing when
Between be 1-2h, the temperature of low temperature drying is 50 DEG C.
3. a kind of La according to claim 12O3/Fe2O3The preparation technology of carbon fibre material, it is characterised in that：Step（2）
Middle cotton chip is with the mass ratio of metal salt mixture：1：3.25—1：6.85, the soluble lanthanum salt in metal salt mixture position
With the mixture of soluble molysite.
4. a kind of La according to claim 32O3/Fe2O3The preparation technology of carbon fibre material, it is characterised in that：The lanthanum
The mol ratio of salt and molysite is 1:3—3:1.
5. a kind of La according to claim 3 or 42O3/Fe2O3The preparation technology of carbon fibre material, it is characterised in that：It is described
Lanthanum salt is lanthanum nitrate, and the molysite is iron chloride, and the mol ratio of the lanthanum nitrate and iron chloride is 1:3—3:1.
6. a kind of La according to claim 42O3/Fe2O3The preparation technology of carbon fibre material, it is characterised in that：Citric acid
Material amount be lanthanum salt and molysite material amount sum.
7. a kind of La according to claim 12O3/Fe2O3The preparation technology of carbon fibre material, it is characterised in that：Fibrous carbon
The calcining heat of material is 350 DEG C -650 DEG C.
8. a kind of La according to claim 72O3/Fe2O3The preparation technology of carbon fibre material, it is characterised in that：Fibrous carbon
The calcining heat of material is 530 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107790139A (en) * | 2017-09-29 | 2018-03-13 | 华纺股份有限公司 | A kind of preparation method of ferrocerium Heterogeneous Composite activated carbon fiber |
| CN109036866A (en) * | 2018-08-09 | 2018-12-18 | 盐城工学院 | A kind of flexible fabric base electrode material and preparation method thereof |
| CN109231280A (en) * | 2018-10-12 | 2019-01-18 | 山东理工大学 | A kind of preparation method of rice-shaped di-iron trioxide composite cotton fabric carbon fibre material |
| CN109420512A (en) * | 2017-09-04 | 2019-03-05 | 中国科学院上海硅酸盐研究所 | A kind of catalysis material and its preparation method and application based on phosphoric acid modification |
| CN109569733A (en) * | 2018-11-30 | 2019-04-05 | 华纺股份有限公司 | A kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst and preparation method |
| CN109692700A (en) * | 2018-11-30 | 2019-04-30 | 华纺股份有限公司 | A kind of threadiness support type g-C3N4/Ag2WO4Catalysis material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109420512A (en) * | 2017-09-04 | 2019-03-05 | 中国科学院上海硅酸盐研究所 | A kind of catalysis material and its preparation method and application based on phosphoric acid modification |
| CN107790139A (en) * | 2017-09-29 | 2018-03-13 | 华纺股份有限公司 | A kind of preparation method of ferrocerium Heterogeneous Composite activated carbon fiber |
| CN109036866A (en) * | 2018-08-09 | 2018-12-18 | 盐城工学院 | A kind of flexible fabric base electrode material and preparation method thereof |
| CN109231280A (en) * | 2018-10-12 | 2019-01-18 | 山东理工大学 | A kind of preparation method of rice-shaped di-iron trioxide composite cotton fabric carbon fibre material |
| CN109569733A (en) * | 2018-11-30 | 2019-04-05 | 华纺股份有限公司 | A kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst and preparation method |
| CN109692700A (en) * | 2018-11-30 | 2019-04-30 | 华纺股份有限公司 | A kind of threadiness support type g-C3N4/Ag2WO4Catalysis material and preparation method thereof |
| CN109692700B (en) * | 2018-11-30 | 2021-09-07 | 华纺股份有限公司 | Fibrous load type g-C3N4/Ag2WO4The photocatalytic material and the preparation method thereof |
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