CN107754863A - The preparation method of alum acid iron support type bafta - Google Patents
The preparation method of alum acid iron support type bafta Download PDFInfo
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- CN107754863A CN107754863A CN201711229395.2A CN201711229395A CN107754863A CN 107754863 A CN107754863 A CN 107754863A CN 201711229395 A CN201711229395 A CN 201711229395A CN 107754863 A CN107754863 A CN 107754863A
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- bafta
- acid iron
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Abstract
A kind of preparation method of alum acid iron support type bafta, belongs to field of material preparation, it is characterised in that：Bafta is soaked with deionized water, is placed in ethanolic aqueous system, is ultrasonically treated, is washed with deionized after taking-up, is then dried for standby；In three-necked flask equipped with ethanolic aqueous system, regulation system pH value adds silane coupler, and ultrasound is fully hydrolyzed silane coupler；Alum acid iron powder body is added, continues ultrasound and surface modification is carried out to alum acid iron；Then sodium hydroxide solution regulation system pH value is used, three-necked flask is placed in oil bath, the bafta extracted through deionized water wetting is put under mechanical stirring and dries；Then drying, alum acid iron support type bafta is obtained through washing again.The important medium for making alum acid iron and bafta strong bonded is used as using silane coupler KH560, alum acid iron/bafta this new catalyst can successfully be prepared by dipping, and alum acid iron is evenly distributed in fabric face, to the catalytic degradation better performances of quadracycline.
Description
Technical field
The invention belongs to field of material preparation, more particularly to a kind of preparation method of alum acid iron support type bafta.
Background technology
Global is about every year 100,000 ~ 200,000 ton using the total amount of antibiotic, and the antibiotic for wherein at least having 50% is used
In animal husbandry and aquaculture.In animal husbandry, because tetracycline has the advantages that broad spectrum activity, of high quality and at a reasonable price, and at low dose
It can promote the growth of livestock and poultry during amount addition, and can be used to treat disease during high dose, it is had become output and is faced
The larger antibiotic of bed usage amount.Tetracycline can be used for multi-infection disease, for example, respiratory tract, nasal sinus, tympanitis, uropoiesis and
Enteron aisle, it can also be used to gonorrhoea is treated, but because their side effect, unstability in different environments, particularly in water ring
Continuous accumulation in border, it is set to obtain widely paying close attention in world wide.
Traditional photocatalysis research is often carried out in suspended state system, and because catalyst granules is tiny, proportion is also smaller, passes
The separation method of system, which such as filters, precipitates, flocculating, centrifuges operation is difficult to be separated, reclaims and regeneration, simultaneously
Catalyst easily cohesion and poisoning, it is impossible to realize continuous operation, thus produce substantial amounts of iron containing sludge, water body can be caused secondary
Pollution.The alum acid iron particle being suspended in reaction system can not only produce to light in use absorbs barrier effect, and
The irradiation depth of light source can be influenceed.The research to suspended state photocatalytic system is mainly carried out in laboratory at present, it is difficult to real
The commercial Application of existing scale.
The content of the invention
A kind of the present invention is intended to provide preparation method of alum acid iron support type bafta.
The preparation method of alum acid iron support type bafta of the present invention, comprises the following steps：
（1）Bafta is soaked with deionized water, is placed in 100mL ethanol-water systems, 60min is ultrasonically treated, is spent after taking-up
Ion water washing, is then dried for standby；（2）In three-necked flask equipped with ethanol-water system, regulation system pH value, silicon is added
Alkane coupling agent, ultrasonic 30min are fully hydrolyzed silane coupler；（3）Alum acid iron powder body is added, continues ultrasonic 30min to alum acid
Iron carries out surface modification；（4）Then sodium hydroxide solution regulation system pH value is used, three-necked flask is placed in oil bath, in machinery
The bafta that the lower input of stirring is extracted through deionized water wetting is dried；（5）Then drying, the load of alum acid iron is obtained through washing again
Type bafta.
The preparation method of alum acid iron support type bafta of the present invention, step（1）Second in the ethanol-water system
Alcohol is 9 with water volume ratio:1.
The preparation method of alum acid iron support type bafta of the present invention, step（1）The drying temperature is 80 DEG C.
The preparation method of alum acid iron support type bafta of the present invention, step（2）The regulation pH is by ice vinegar
Acid or ammoniacal liquor are adjusted.
The preparation method of alum acid iron support type bafta of the present invention, step（4）The churned mechanically stirring speed
Spend for 200 turns/min.
The preparation method of alum acid iron support type bafta of the present invention, step（4）The baking step is first through 80
DEG C preliminary drying, then 120 DEG C bake.
The preparation method of alum acid iron support type bafta of the present invention, using silane coupler KH560 as making alum
The important medium of sour iron and bafta strong bonded, alum acid iron/bafta this new catalytic can successfully be prepared by dipping
Agent, and alum acid iron is evenly distributed in fabric face, to the catalytic degradation better performances of quadracycline.
Embodiment
The preparation method of alum acid iron support type bafta of the present invention, comprises the following steps：
（1）Bafta is soaked with deionized water, is placed in 100mL ethanol-water systems, 60min is ultrasonically treated, is spent after taking-up
Ion water washing, is then dried for standby；（2）In three-necked flask equipped with ethanol-water system, regulation system pH value, silicon is added
Alkane coupling agent, ultrasonic 30min are fully hydrolyzed silane coupler；（3）Alum acid iron powder body is added, continues ultrasonic 30min to alum acid
Iron carries out surface modification；（4）Then sodium hydroxide solution regulation system pH value is used, three-necked flask is placed in oil bath, in machinery
The bafta that the lower input of stirring is extracted through deionized water wetting is dried；（5）Then drying, the load of alum acid iron is obtained through washing again
Type bafta.
The preparation method of alum acid iron support type bafta of the present invention, step（1）Second in the ethanol-water system
Alcohol is 9 with water volume ratio:1.Step（1）The drying temperature is 80 DEG C.Step（2）The regulation pH is by glacial acetic acid or ammonia
Water is adjusted.Step（4）The churned mechanically mixing speed is 200 turns/min.Step（4）The baking step is first to pass through
80 DEG C of preliminary dryings, then 120 DEG C bake.Alum acid iron powder body is most strong to quadracycline adsorption capacity in 10min, prolonging over time
Long, absorption gradually tends to saturation, absorption-desorption balance is reached after about 30min, the 30min changes of quadracycline later are with before
Person is compared to smaller.Meanwhile bafta has been also up to absorption-desorption balance in 30min.Therefore it can be pointed out that alum acid iron
Powder is with bafta to can be balanced when the adsorption time of quadracycline is 30min with reaching absorption-desorption.If only may be used
Light is seen without using catalyst, and its degradation rate is no more than 5% after reacting 120min.And alum acid iron support type bafta is used to pass through
Also the photocatalysis of the degradation rate, i.e. alum acid iron support type bafta to quadracycline can only be slightly improved after 120min reactions
Performance is not high, and its degradation rate after 120min is no more than 10%, and this is due to that alum acid iron load factor is not high caused.Class Fenton body
System is the same as above compared with both, it is obtained significantly in 30min to the catalytic degradation speed and catalysis degradation modulus of quadracycline
Improve, the class Fenton's reaction of alum acid iron support type bafta has more to the degradation effect of quadracycline than its light-catalyzed reaction
Advantage, degradation rate just reaches 48.58% during 30min.
Photocatalysis generates HO to alum acid iron under visible light, and Fe and V can induce hydrogen peroxide to produce HO, both
Synergy substantially increases the oxidative degradation to quadracycline.On the one hand support type bafta is the hydrochloric acid for improving absorption
The effective area of tetracycline, on the other hand it is to absorb more photons to produce more HO free radicals.Degradation rate during 30min
Just it is 67.39%, by 120min reaction, the degradation rate of quadracycline reaches 97.63%.Illustrate the support type being prepared
Bafta is good to the catalytic degradation effect of quadracycline, has certain Research Significance.Open loop and and cotton in the basic conditions
Hydroxyl on fabric forms covalent bond, is firmly attached to fabric face.And alum acid iron is all mainly logical in blank sample and KH550
Cross hydrogen bond and be attached to bafta, while stirring, be easy to come off again, so load factor is below KH560.And in blank sample
Solvent be all deionized water, this can preferably make bafta hygroscopic swelling, improve the load of alum acid iron to a certain extent
Rate.After catalytic degradation, blank sample and there is a certain degree of peeling using the powder on KH550 fabric, exist certain
Defect, do not changed using weight after the fabric reaction after KH560.In summary, alum acid iron is carried on into cotton by KH560 to knit
More preferable catalytic degradation effect can be reached on thing.As the increase of the ratio of system reclaimed water, its catalytic degradation performance are also gradual
Improve, illustrate that the presence of water is particularly important to TC catalytic degradation performance to improving product.This is due to that the increase of water is advantageous to
The hygroscopic swelling of cotton fiber, adsorption and diffusion and attachment of the alum acid iron in fabric face are further improved, so as to improve alum acid iron
Load capacity, i.e. the performance of catalytic degradation TC is improved.
With the increase of alum acid iron dosage, the degradation rate and degradation rate of quadracycline gradually step up, after 120min its
Degradation rate is more or less the same.Because with the increase of alum acid iron, it is more in the load capacity of surface of cotton fabric, then photocatalysis with
Caused HO is more under class Fenton's reaction, and the efficiency of oxidative degradation quadracycline is higher, and catalysis degradation modulus are higher.When alum acid
When iron addition increases to 0.15g by 0.05g, its degradation efficiency to quadracycline gradually steps up, the degradation rate after 30min
47.75% is brought up to from 35.34%；And when continuing to increase to 0.20g, though being also improved, increased amplitude is much smaller than the former,
Degradation rate after 30min is 51.49%, only improves 3.74%.In view of the effective rate of utilization and production cost of alum acid iron, choosing
The optimum addition for taking alum acid iron is 0.15g.With the raising of temperature, support type bafta is gradual to TC catalytic degradation performance
It is improved, when temperature is 80 DEG C, degradation rate is maximum.Continue to improve load temperature, degradation rate reduces on the contrary, this be by
Too high in now temperature, self-crosslinking occurs for KH560, and system KH560 is reduced, and alum acid iron is with covalently cross-linked to negative on bafta
Carrying capacity reduces, and is more that can be come off again from fabric by Hydrogenbond, stage so that alum acid iron/bafta is to TC
Catalytic degradation performance also decline therewith.It can be seen that there is a little film to produce in experimentation, this has been also further demonstrated that
It is theoretical.Also a kind of is probably that the temperature of now system has reached the azeotropic point of ethanol-water system, although along with stirring,
It is system still in unstable state, temperature is higher, and the alum acid iron powder body motion of fabric face diffusive skin is more violent, easier
Again away from fabric face, so as to cause load capacity relatively low.With the extension of load time, the alum acid iron loaded on bafta is got over
It is more, it is higher to the catalysis degradation modulus and degradation rate of quadracycline.Load is can be seen that from degradation rate when reacting 30min
Ultimate load has been nearly reached after 9h, has continued to increase load time, has no and significantly improve for catalysis degradation modulus.Therefore, it is
Reduction real cost of production, can to choose 9h be the optimum load time.By optimizing load work of the alum acid iron powder body to bafta
Skill condition, tentatively obtaining its optimum load technique is：Bath raio 1:120, the volume ratio of ethanol and water is 1 in system:9, alum acid iron
Dosage is 0.15g, and KH560 addition is 0.5%, is loaded 9 hours in 80 DEG C.
Claims (6)
1. a kind of preparation method of alum acid iron support type bafta, it is characterised in that comprise the following steps：（1）Will with deionized water
Bafta soaks, and is placed in 100mL ethanol-water systems, is ultrasonically treated 60min, is washed with deionized after taking-up, then dries
It is standby；（2）In three-necked flask equipped with ethanol-water system, regulation system pH value adds silane coupler, and ultrasonic 30min makes
Silane coupler is fully hydrolyzed；（3）Alum acid iron powder body is added, continues ultrasonic 30min and surface modification is carried out to alum acid iron；（4）So
Sodium hydroxide solution regulation system pH value is used afterwards, and three-necked flask is placed in oil bath, put under mechanical stirring through deionized water
Soak the bafta drying extracted；（5）Then drying, alum acid iron support type bafta is obtained through washing again.
2. the preparation method of alum acid iron support type bafta according to claim 1, it is characterised in that：Step（1）It is described
Ethanol and water volume ratio in ethanol-water system are 9:1.
3. the preparation method of alum acid iron support type bafta according to claim 2, it is characterised in that：Step（1）It is described
Drying temperature is 80 DEG C.
4. the preparation method of alum acid iron support type bafta according to claim 3, it is characterised in that：Step（2）It is described
Adjusting pH is adjusted by glacial acetic acid or ammoniacal liquor.
5. the preparation method of alum acid iron support type bafta according to claim 4, it is characterised in that：Step（4）It is described
Churned mechanically mixing speed is 200 turns/min.
6. the preparation method of alum acid iron support type bafta according to claim 5, it is characterised in that：Step（4）It is described
Baking step is first through 80 DEG C of preliminary drying, then 120 DEG C bake.
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| CN201711229395.2A CN107754863A (en) | 2017-11-29 | 2017-11-29 | The preparation method of alum acid iron support type bafta |
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| CN201711229395.2A CN107754863A (en) | 2017-11-29 | 2017-11-29 | The preparation method of alum acid iron support type bafta |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110904677A (en) * | 2019-11-14 | 2020-03-24 | 南通大学 | Cotton fabric for photocatalytic degradation of azo dye and preparation method thereof |
| CN111268751A (en) * | 2019-11-29 | 2020-06-12 | 南通天虹银海实业有限公司 | Preparation method of polyacid-based yarn for catalyzing organic pollutants |
| CN111330362A (en) * | 2020-03-11 | 2020-06-26 | 天津大学 | Natural polymer-based functional air filtering material and preparation method thereof |
| CN112371182A (en) * | 2020-11-30 | 2021-02-19 | 南通大学 | Preparation method of fiber-based bismuth vanadate composite photocatalytic material |
-
2017
- 2017-11-29 CN CN201711229395.2A patent/CN107754863A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110904677A (en) * | 2019-11-14 | 2020-03-24 | 南通大学 | Cotton fabric for photocatalytic degradation of azo dye and preparation method thereof |
| CN110904677B (en) * | 2019-11-14 | 2022-04-22 | 南通大学 | Cotton fabric for photocatalytic degradation of azo dye and preparation method thereof |
| CN111268751A (en) * | 2019-11-29 | 2020-06-12 | 南通天虹银海实业有限公司 | Preparation method of polyacid-based yarn for catalyzing organic pollutants |
| CN111330362A (en) * | 2020-03-11 | 2020-06-26 | 天津大学 | Natural polymer-based functional air filtering material and preparation method thereof |
| CN112371182A (en) * | 2020-11-30 | 2021-02-19 | 南通大学 | Preparation method of fiber-based bismuth vanadate composite photocatalytic material |
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