CN105803582A - Preparation method of gold-bearing ACF (activated carbon fiber) - Google Patents
Preparation method of gold-bearing ACF (activated carbon fiber) Download PDFInfo
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- CN105803582A CN105803582A CN201610211861.3A CN201610211861A CN105803582A CN 105803582 A CN105803582 A CN 105803582A CN 201610211861 A CN201610211861 A CN 201610211861A CN 105803582 A CN105803582 A CN 105803582A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a preparation method of a gold-bearing ACF (activated carbon fiber). The method comprises the steps as follows: dissolving beta-cyclodextrin in an aqueous solution; adding sodium chloride and chloroauric acid to the aqueous solution, and then inserting positive and negative electrodes connected with a power supply into the solution; performing stirring at a high speed, and obtaining a nanogold solution; treating cleaned viscose in the nanogold solution for certain time to prepare gold-bearing viscose, immersing the viscose in a diammonium hydrogen phosphate aqueous solution, performing charring and activation, and then obtaining the gold-bearing ACF. According to the preparation method, the process is simple, the content of impurities is low, bonding between nanogold and the ACF is firm, and the ACF has outstanding antibacterial performance, catalysis performance and other performance and is widely applied to fields such as medical hygienic materials, air purification, water treatment and the like.
Description
Technical field
The invention belongs to active gold-carrying carbon technical field of fiber preparation, be specifically related to a kind of gold that carries and live
The preparation method of property Carbon fibe.
Background technology
NACF (ACF), also known as fibrous activated carbon, is the high-efficiency activated of excellent performance
Adsorbing material and environment-friendly engineering material, have acid and alkali-resistance, corrosion resistance characteristic, therefore protect at environment
Protect, be catalyzed, the field such as medicine, military project is widely applied.
Active carbon loading silver fiber Patents is more at present, and such as Chinese invention patent, " silver ion is lived
Property carbon antiseptic dressing and preparation method thereof " in (CN 102133420A), disclose a kind of by silver
Solion (such as silver nitrate) and precursor fibre are put in steam pressure container and are heated to
115～130 DEG C, time 10～30 minutes, silver is loaded in precursor fibre, so
The method preparing active carbon loading silver fiber by carbonization, activation.The problem master that this method exists
If the gold ion in solution is difficult to load in precursor fibre, and after carbonization, activation,
Carbon fiber surface gold grain skewness, particle diameter are not of uniform size, and anti-microbial property is poor.Additionally
A kind of rear bearing silver technology, i.e. after fiber carbonization and activation, uses spraying, dipping absorption etc.
Method is at NACF area load silver ion or nanometer silver.As Chinese invention patent is " a kind of
The method of loading nano silvery on activated carbon fiber " in (CN 10138700), disclose one
By electrochemical deposition method method of loading nano silvery on activated carbon fiber, i.e. first with work
Property carbon fiber absorbability Adsorption For Ag ion, then use cathode reduction method be reduced to silver
Simple substance, obtains nanometer silver by controlling operating condition and is directly anchored to activated carbon generating simultaneously
Fiber surface.
The preparation method of active gold-carrying carbon is similar with the preparation method of active carbon loading silver.Current main
In the past road carry Jin Weizhu, as patent of invention " activated carbon supported nano catalyst and preparation and
Application process " in (CN 103932132A), prior to gold solution adds stabilizer, reduction
Aurosol is prepared in agent, then NACF is placed in gold-supported in aurosol treatment fluid.The most such as
Patent of invention " activated carbon is in the preparation method of nano catalyst " (CN 101785997A)
With patent of invention " activated-carbon catalyst of a kind of supported nano-gold metal particles and preparation method thereof and
Application " (CN 104084189A) is all the method using front road to carry gold, its common lacking
Point is that nanometer gold skewness, fastness on NACF are poor, and impurities left is more,
Affect the serviceability of active gold-carrying carbon.
Summary of the invention
The present invention is directed to the production technology of existing active gold-carrying carbon fiber, it is therefore intended that provide one
The preparation method of active gold-carrying carbon fiber.
The present invention realizes especially by techniques below scheme:
The preparation method of a kind of active gold-carrying carbon fiber, specifically includes following steps:
1) select a certain amount of beta-schardinger dextrin-powder to be dissolved in deionized water solution, fully stir
Mix, by changing the temperature of cyclodextrin mass percent and aqueous solution to prepare the ring of variable concentrations
Dextrin solution；
2) in cyclodextrin aqueous solution, add a certain amount of sodium chloride powder, add certain after dissolving
The tetra chlorauric acid of amount, inserts two plate electrodes in mixed solution after stirring, by controlling electricity
Stream size, response time and the size etc. of mixing speed regulation nanogold particle；
3) removal of impurity is gone to prepare nanometer gold aqueous solution after low-speed centrifugal above-mentioned solution.
4) it is placed in, by cleaning clean viscose rayon, the nanometer gold that mass concentration is 0.01～1g/l
Impregnation process 20～30min in aqueous solution, the viscose glue obtaining being loaded with nanometer gold after dehydration is fine
Dimension；
5) aubergine is carried gold viscose rayon and be placed in the phosphoric acid that mass concentration is 10～40g/l
Hydrogen two aqueous ammonium soaks 5～10h；Through dehydration, dry after, temperature be 500～
In the nitrogen atmosphere of 600 DEG C, carbonization processes 20～30min, it is thus achieved that gold loaded carbon fiber；
6) it is warming up to 900～1200 DEG C again, is passed through nitrogen and pressure is 0.5～0.8Mpa
Steam, activation processing 20～30min, obtain a kind of active gold-carrying carbon fiber.
Further technical scheme as the present invention: described beta-schardinger dextrin-matter in aqueous
Amount percent is 0.1～25wt%.
Further technical scheme as the present invention: the temperature of described aqueous solution be 25～
100 DEG C, mixing time 2～8h, 100～500 revs/min.
Further technical scheme as the present invention: described sodium chloride concentration in aqueous
It is 0.05～10wt%.
Further technical scheme as the present invention: described tetra chlorauric acid rubs with beta-schardinger dextrin-
That ratio is 1:10～9.5:10.
Described size of current is 0.01～1A, the response time 0.5～10h, stirring speed
Spend 100～2000 revs/min.
Nano-Au solution of the present invention is for fields such as antibacterial, catalysis.
The present invention passes through electrochemical modification beta-schardinger dextrin-so that it is possess reproducibility and stability, with
Preparation uniform particle sizes, stable in properties, the nano-Au solution of function excellence.Again nanometer gold is loaded
After on viscose rayon, carbonization-activation obtains active gold-carrying carbon fiber.
The invention have the benefit that
1) utilize electrochemical modification cyclodextrin to have good reproducibility and stability, prepare nanometer
Goldc grains footpath is little, SOLUTION PROPERTIES is stable, and cyclodextrin is free from admixture residual after carbonization-activation.
2) active gold-carrying carbon fiber can effectively overcome part population to use nano silver antibacterial material mistake
The shortcoming of easy allergy in journey, nanometer gold has more preferable stability and biocompatibility simultaneously.
3) front road carries after gold carbonization-activation again, and nanometer gold is good with Carbon fibe binding strength.
Accompanying drawing explanation
Fig. 1 is the non-active gold-carrying carbon fiber scanning electron microscope (SEM) photograph of the present invention.
Fig. 2 is the active gold-carrying carbon fiber scanning electron microscope (SEM) photograph of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, the following stated, is only to this
The preferred embodiment of invention, not does the restriction of other forms to the present invention, any familiar
Professional and technical personnel is changed to become on an equal basis possibly also with the technology contents of the disclosure above
The Equivalent embodiments changed.Every without departing from the present invention program content, the technology according to the present invention is real
Any simple modification that confrontation following example are done or equivalent variations, all fall within the guarantor of the present invention
In the range of protecting.
Embodiment 1,
The preparation method of a kind of nano-Au solution, concretely comprises the following steps: select 5g beta-schardinger dextrin-powder
End is dissolved in 95g deionized water, and the temperature of aqueous solution is 80 DEG C, stirs under 200 revs/min
Mix 6h to preparing transparent beta-cyclodextrin aqueous solution；2g sodium chloride powder is added beta-schardinger dextrin-
In aqueous solution, it is completely dissolved to sodium chloride powder after continuing stirring 0.5h；Again by 0.5g tetrachloro
Auric acid adds in the beta-schardinger dextrin-aqueous solution containing sodium chloride, and stirring 5min will be connected to after dissolving
The positive and negative electrode of power supply inserts in this solution, and regulation electric current, to 0.5A, increases mixing speed extremely
1000 revs/min, after reaction 2h, prepared solution is put in centrifuge, 1000 revs/min
Under be centrifuged 10min after go the removal of impurity to prepare nano-Au solution.
Take clean viscose rayon 5g, be placed in the nanometer gold aqueous solution that mass concentration is 0.4g/l
Middle impregnation process 30min, obtains being loaded with the viscose rayon of nanometer gold after dehydration；Aubergine is carried
Gold viscose rayon is placed in the ammonium dibasic phosphate aqueous solution that mass concentration is 30g/l immersion 6h；
After dehydration, drying, in the nitrogen atmosphere that temperature is 600 DEG C, carbonization processes 30min, obtains
Obtain gold loaded carbon fiber；It is warming up to 1000 DEG C again, is passed through nitrogen and the water that pressure is 0.6Mpa steams
Gas, activation processing 30 minutes, obtain active gold-carrying carbon fiber.
Embodiment 2,
The preparation method of a kind of nano-Au solution, concretely comprises the following steps: select 10g beta-schardinger dextrin-powder
End is dissolved in 90g deionized water, and the temperature of aqueous solution is 90 DEG C, stirs under 400 revs/min
Mix 6h to preparing transparent beta-cyclodextrin aqueous solution；5g sodium chloride powder is added beta-schardinger dextrin-
In aqueous solution, it is completely dissolved to sodium chloride powder after continuing stirring 1h；Again by 0.8g tetrachloro gold
Acid adds in the beta-schardinger dextrin-aqueous solution containing sodium chloride, and stirring 5min will be connected to electricity after dissolving
The positive and negative electrode in source inserts in this solution, and regulation electric current, to 0.8A, increases mixing speed to 1500
Rev/min, reaction 4h after prepared solution is put in centrifuge, under 1000 revs/min from
The removal of impurity is gone to prepare nano-Au solution after heart 10min.
Take clean viscose rayon 5g, be placed in the nanometer gold aqueous solution that mass concentration is 0.4g/l
Middle impregnation process 30min, obtains being loaded with the viscose rayon of nanometer gold after dehydration；Aubergine is carried
Gold viscose rayon is placed in the ammonium dibasic phosphate aqueous solution that mass concentration is 30g/l immersion 6h；
After dehydration, drying, in the nitrogen atmosphere that temperature is 600 DEG C, carbonization processes 30min, obtains
Obtain gold loaded carbon fiber；It is warming up to 1000 DEG C again, is passed through nitrogen and the water that pressure is 0.6Mpa steams
Gas, activation processing 30 minutes, obtain active gold-carrying carbon fiber.
Embodiment 3,
The preparation method of a kind of nano-Au solution, concretely comprises the following steps: select 2g beta-schardinger dextrin-powder
End is dissolved in 98g deionized water, and the temperature of aqueous solution is 80 DEG C, stirs under 200 revs/min
Mix 6h to preparing transparent beta-cyclodextrin aqueous solution；1g sodium chloride powder is added beta-schardinger dextrin-
In aqueous solution, it is completely dissolved to sodium chloride powder after continuing stirring 0.5h；Again by 0.2g tetrachloro
Auric acid adds in the beta-schardinger dextrin-aqueous solution containing sodium chloride, and stirring 5min will be connected to after dissolving
The positive and negative electrode of power supply inserts in this solution, and regulation electric current, to 0.5A, increases mixing speed extremely
1000 revs/min, after reaction 2h, prepared solution is put in centrifuge, 1000 revs/min
Under be centrifuged 10min after go the removal of impurity to prepare nano-Au solution.
Take clean viscose rayon 5g, be placed in the nanometer gold aqueous solution that mass concentration is 0.4g/l
Middle impregnation process 30min, obtains being loaded with the viscose rayon of nanometer gold after dehydration；Aubergine is carried
Gold viscose rayon is placed in the ammonium dibasic phosphate aqueous solution that mass concentration is 30g/l immersion 6h；
After dehydration, drying, in the nitrogen atmosphere that temperature is 600 DEG C, carbonization processes 30min, obtains
Obtain gold loaded carbon fiber；It is warming up to 1000 DEG C again, is passed through nitrogen and the water that pressure is 0.6Mpa steams
Gas, activation processing 30 minutes, obtain active gold-carrying carbon fiber.
Embodiment 4,
The qualification being correlated with embodiment 1 gained nano-Au solution, sees Figure of description
1-2。
Claims (5)
1. the preparation method of an active gold-carrying carbon fiber, it is characterised in that comprise the following steps:
1) select a certain amount of beta-schardinger dextrin-powder to be dissolved in deionized water solution, fully stir
Mix, by changing the temperature of cyclodextrin mass percent and aqueous solution to prepare the ring of variable concentrations
Dextrin solution；
2) in cyclodextrin aqueous solution, add a certain amount of sodium chloride powder, add certain after dissolving
The tetra chlorauric acid of amount, inserts two plate electrodes in mixed solution after stirring, control electric current big
Little, response time and mixing speed, size of current is 0.01-1A, response time 0.5-10h,
Mixing speed 100-2000 rev/min；
3) removal of impurity is gone to prepare nanometer gold aqueous solution after low-speed centrifugal above-mentioned solution.
4) it is placed in, by cleaning clean viscose rayon, the nanometer gold that mass concentration is 0.01～1g/l
Impregnation process 20～30min in aqueous solution, the viscose glue obtaining being loaded with nanometer gold after dehydration is fine
Dimension；
5) aubergine is carried gold viscose rayon and be placed in the phosphoric acid that mass concentration is 10～40g/l
Hydrogen two aqueous ammonium soaks 5～10h；Through dehydration, dry after, temperature be 500～
In the nitrogen atmosphere of 600 DEG C, carbonization processes 20～30min, it is thus achieved that gold loaded carbon fiber；
6) it is warming up to 900-1200 DEG C again, is passed through nitrogen and pressure is 0.5～0.8Mpa
Steam, activation processing 20～30min, obtain a kind of active gold-carrying carbon fiber.
The preparation method of a kind of nano-Au solution the most according to claim 1, its feature
It is: beta-schardinger dextrin-mass percent in aqueous is 0.1～25wt%.
The preparation method of a kind of nano-Au solution the most according to claim 1, its feature
It is: the temperature of aqueous solution is 25～100 DEG C, mixing time 2～8h, 100～500 turns/
Minute.
The preparation method of a kind of nano-Au solution the most according to claim 1, its feature
It is: sodium chloride concentration in aqueous is 0.05～10wt%.
The preparation method of a kind of nano-Au solution the most according to claim 1, its feature
It is: tetra chlorauric acid is 1:10～9.5:10 with the mol ratio of beta-schardinger dextrin-.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109647052A (en) * | 2018-12-04 | 2019-04-19 | 山西绿建科技有限公司 | A kind of preparation method of antibacterial air conditioner filter element material |
| CN116371428A (en) * | 2023-03-29 | 2023-07-04 | 南通大学 | Solid acid catalyst for depolymerizing waste plastics and preparation method thereof |
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| CN103225134A (en) * | 2013-05-09 | 2013-07-31 | 张家港耐尔纳米科技有限公司 | Preparation method of silver-loaded active carbon fibers |
| CN104841949A (en) * | 2015-05-20 | 2015-08-19 | 上海韬鸿化工科技有限公司 | Nanometer silver glue preparation method |
| CN105417492A (en) * | 2015-11-04 | 2016-03-23 | 安徽师范大学 | Method for preparing beta-cyclodextrin-gold nano-particles and method for detecting cholesterol |
-
2016
- 2016-04-06 CN CN201610211861.3A patent/CN105803582B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837465A (en) * | 2010-05-10 | 2010-09-22 | 张家港耐尔纳米科技有限公司 | Preparation method of nanometer sliver colloid solution |
| CN103225134A (en) * | 2013-05-09 | 2013-07-31 | 张家港耐尔纳米科技有限公司 | Preparation method of silver-loaded active carbon fibers |
| CN104841949A (en) * | 2015-05-20 | 2015-08-19 | 上海韬鸿化工科技有限公司 | Nanometer silver glue preparation method |
| CN105417492A (en) * | 2015-11-04 | 2016-03-23 | 安徽师范大学 | Method for preparing beta-cyclodextrin-gold nano-particles and method for detecting cholesterol |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109647052A (en) * | 2018-12-04 | 2019-04-19 | 山西绿建科技有限公司 | A kind of preparation method of antibacterial air conditioner filter element material |
| CN116371428A (en) * | 2023-03-29 | 2023-07-04 | 南通大学 | Solid acid catalyst for depolymerizing waste plastics and preparation method thereof |
| CN116371428B (en) * | 2023-03-29 | 2024-05-17 | 南通大学 | Solid acid catalyst for depolymerizing waste plastics and preparation method thereof |
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Effective date of registration: 20200731 Address after: Groups 22 and 23, shuangmeng village, Xianfeng street, Tongzhou District, Nantong City, Jiangsu Province 226300 Patentee after: Nantong chuangtong daily necessities Co., Ltd Address before: 226019 Jiangsu city of Nantong province sik Road No. 9 Patentee before: NANTONG University |