CN108393064A - A kind of modification infusorial earth material and preparation method thereof of absorption dyestuff direct scarlet 4BS - Google Patents
A kind of modification infusorial earth material and preparation method thereof of absorption dyestuff direct scarlet 4BS Download PDFInfo
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- CN108393064A CN108393064A CN201810061623.8A CN201810061623A CN108393064A CN 108393064 A CN108393064 A CN 108393064A CN 201810061623 A CN201810061623 A CN 201810061623A CN 108393064 A CN108393064 A CN 108393064A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- B01J20/28054—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 surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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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
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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
-
- 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
Abstract
The present invention provides a kind of modification infusorial earth materials and preparation method thereof of absorption dyestuff direct scarlet 4BS, the modification infusorial earth material is using diatomite as base stock, it first passes through pickling and obtains acid activation diatomite, magnetic diatomite is prepared by hydrothermal synthesis method again, the magnetic diatomite is mixed with halogenated phosphates (CPC), deionized water, absolute ethyl alcohol and ammonium hydroxide, the uniform liquid of black is obtained, simultaneously ethyl orthosilicate is added dropwise in mechanical agitation（TEOS）, 5 ~ 7 h are then continuously stirred, the modified material deionized water and washes of absolute alcohol that will be obtained are dried in vacuum drying chamber, obtain the modification infusorial earth material.Modified magnetic diatomite material after modification has many advantages, such as stable chemical property, easily recycling, separation, preferably improves diatomaceous absorption property, the dyestuff direct scarlet 4BS especially in handling waste water shows unique advantage.
Description
Technical field
The invention belongs to inorganic composite materials technical field, more particularly to a kind of modification of absorption dyestuff direct scarlet 4BS
Diatomite material and preparation method thereof.
Background technology
Dyeing is the main pollution in one of more industrial department of China's water consumption, waste discharge amount and China
One of source, waste water are largely discharged into natural water, necessarily lead to the severe exacerbation of natural water.Due in dyeing waste water
Dyestuff much be the complicated organic matter containing azo bond, poly aromatic rings, it is toxic difficult to degrade, can carcinogenic, teratogenesis, mutagenesis, can be right
Human health generates extreme influence.Therefore, the dyestuff being effectively treated in waste water is constantly subjected to concern both domestic and external.
As a kind of environmentally friendly and cheap adsorbent, diatomite includes the micropore of a large amount of distribution rules
Road, so having the characteristics that large specific surface area, absorption property are strong, density is low, rich reserves.But there is also some to lack for diatomite
Point limits its use value, as in diatomite original soil containing accompanying impurities, dispersibility is strong and settleability is weak, it is fast to be difficult to realize
Speed is separated by solid-liquid separation, this just affects diatomaceous absorption property and recycling and reuse.
Invention content
In view of the above-mentioned problems, the object of the present invention is to provide a kind of modification infusorial earth material and preparation method thereof, it is described to change
Property diatomite material does not remove only the accompanying impurities in diatomite original soil, and the modified magnetic diatomite material after modification
Have many advantages, such as stable chemical property, easily recycling, separation, preferably improves diatomaceous absorption property, especially locating
Dyestuff direct scarlet 4BS in reason waste water shows unique advantage.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of preparation method of modification infusorial earth material, includes the following steps：
Using diatomite as base stock, first passes through pickling and obtain acid activation diatomite, then magnetism is prepared by hydrothermal synthesis method
The magnetic diatomite is mixed with halogenated phosphates (CPC), deionized water, absolute ethyl alcohol and ammonium hydroxide, is obtained by diatomite
Simultaneously ethyl orthosilicate is added dropwise in the liquid uniform to black, mechanical agitation（TEOS）, 5 ~ 7 h are then continuously stirred, will be obtained
Modified material deionized water and washes of absolute alcohol, dried in vacuum drying chamber, obtain the modification infusorial earth
Material.
Further, diatomaceous pickling processes the specific steps are：First diatomite original soil is dried, by dried diatom
Soil is placed in constant temperature acid in sulfuric acid solution and boils, and is then cooled to room temperature, and is rinsed to neutrality using deionized water, is obtained after drying described
Acid activation diatomite.
Further, the hydrothermal synthesis method the specific steps are：Ferric trichloride is dissolved in ethylene glycol and obtains mixed liquor, then
The acid activation diatomite is put into mixed liquor, magnetic agitation, polyethylene glycol, anhydrous sodium acetate is then added
（CH3COONa）, continue to be formed as yellowish-brown liquid after stirring is mutually melted, liquid be transferred in stainless steel ptfe autoclave
It is sealed, is positioned in baking oven and reacts, reaction terminates to be cooled to room temperature, and black product ultra-pure water and absolute ethyl alcohol are floated respectively
It washes, after product is vacuum dried, obtains the magnetic diatomite.
Further, the mass ratio of the magnetic diatomite and CPC are 1:The mass ratio of 1, the TEOS and CPC are 4:1.
Further, the acid activation diatomite and FeCl3·6H2The mass ratio of O is 1:2.7, the polyethylene glycol with
CH3COONa mass ratioes are 1:3.6.
Further, the churned mechanically temperature is 20 DEG C ~ 30 DEG C, rotating speed 300rpm.
Further, the modification infusorial earth can be applied to absorption dyestuff direct scarlet 4BS.
The present invention having the beneficial effect that compared with prior art：
1, modification infusorial earth material preparation method of the present invention can be disposed effectively by way of pickling first
Accompanying impurities contained in diatomite original soil；Then, magnetization treatment then combines diatomite and Fe3O4The common advantage of MNPs,
Not only there is preferable absorption property to the pollutant in water, while also having Fe3O4The magnetism of MNPs, efficiently solves silicon
The problem of recycling of diatomaceous earth difficulty, separation；
2, the magnetic diatomaceous method of existing preparation is coprecipitation, and is existed by magnetic diatomite made from coprecipitation
The problems such as composition is not uniform enough, magnetic intensity is not high, for the advantage and disadvantage of magnetic diatomite material prepared by coprecipitation, this hair
It is bright to prepare Dispersion on surface Fe using hydrothermal synthesis method3O4The magnetic diatomite of MNPs is closed relative to other methods by hydro-thermal
Cheng Fa, it is only necessary to which a step can prepare magnetic diatomite, easy to operate, and the magnetism of material intensity prepared is good；
3, in modification infusorial earth material preparation method of the present invention, after magnetic diatomite is prepared, further draw
Enter functionalized reagent halogenated phosphates（CPC）, magnetic diatomite is modified, ethyl orthosilicate is continuously added
（TEOS）, ethyl orthosilicate（TEOS）Hydrolysis can be by halogenated phosphates（CPC）It is fixed on magnetic diatomite surface,
Diatomite is surface modified using cationic surfactant on diatomaceous method of modifying, magnetic silicon can be further increased
The specific surface area of diatomaceous earth, and increase its chemism, the presence of halogenated phosphates can make the modified silicon being prepared
Diatomaceous earth material surface carries the ammonium ion of a large amount of positive charges, and direct dyes molecule is mostly azo structure, and includes a variety of bases
Group, such as：Sulfonic group（-SO3H）, hydroxyl（-OH）Equal groups, being dissolved in water can be present in water in the form of anion, directly big
Red 4BS has the feature of direct dyes, due to the sucking action of positive and negative charge, modification infusorial earth material that the present invention is prepared
There is preferable absorption property to direct scarlet 4BS.
Description of the drawings
Fig. 1 is the acid processing diatomite of acidified processing in scanning electron microscope（SEM）Under structural schematic diagram；
Fig. 2 is the modification infusorial earth material in scanning electron microscope（SEM）Under structural schematic diagram；
Fig. 3 is absorption result schematic diagram of the modification infusorial earth material with diatomite original soil to dyestuff direct scarlet 4BS；
Fig. 4 is influence of the adsorption temp to the absorption result of dyestuff direct scarlet.
Specific implementation mode
Embodiment 1
A kind of preparation method of modification infusorial earth material, includes the following steps：
Using diatomite as base stock, first passes through pickling and obtain acid activation diatomite, then magnetism is prepared by hydrothermal synthesis method
The magnetic diatomite is mixed with halogenated phosphates (CPC), deionized water, absolute ethyl alcohol and ammonium hydroxide, is obtained by diatomite
Simultaneously ethyl orthosilicate is added dropwise in the liquid uniform to black, mechanical agitation（TEOS）, 5 ~ 7 h are then continuously stirred, will be obtained
Modified material deionized water and washes of absolute alcohol, dried in vacuum drying chamber, obtain the modification infusorial earth
Material.
Further, diatomaceous pickling processes the specific steps are：First diatomite original soil is dried, by dried diatom
Soil is placed in constant temperature acid in sulfuric acid solution and boils, and is then cooled to room temperature, and is rinsed to neutrality using deionized water, is obtained after drying described
Acid activation diatomite.
Further, the hydrothermal synthesis method the specific steps are：Ferric trichloride is dissolved in ethylene glycol and obtains mixed liquor, then
The acid activation diatomite is put into mixed liquor, magnetic agitation, polyethylene glycol, anhydrous sodium acetate is then added
（CH3COONa）, continue to be formed as yellowish-brown liquid after stirring is mutually melted, liquid be transferred in stainless steel ptfe autoclave
It is sealed, is positioned in baking oven and reacts, reaction terminates to be cooled to room temperature, and black product ultra-pure water and absolute ethyl alcohol are floated respectively
It washes, after product is vacuum dried, obtains the magnetic diatomite.
Embodiment 2
The present embodiment is preferred embodiment on the basis of embodiment 1, specifically provides a kind of absorption dyestuff direct scarlet 4BS's
The preparation method of modification infusorial earth material, specific preparation method are as follows：
（1）Diatomaceous pickling processes：Diatomite original soil 20g is taken, dry 1h under the conditions of 110 DEG C, by dried diatomite
It is placed in the sulfuric acid solution that mass fraction is 35%, volume is 200mL, constant temperature acid boils 35min under the conditions of 100 ± 5 DEG C, in acid
5% dilute sulfuric acid is filled into during boiling in right amount to be cooled to room temperature to keep level balance, is rinsed to neutrality using deionized water,
Drying obtains acid activation diatomite at 110 DEG C；
（2）Magnetic diatomite is prepared using hydrothermal synthesis method：Take step（1）The acid activation diatomite 0.2g being prepared, by matter
Amount is than acid activation diatomite：Ferric trichloride（FeCl3·6H2O）It is 1：2.7, ferric trichloride（FeCl3·6H2O）It takes and is dissolved in 16mL
In ethylene glycol, acid activation diatomite is put into mixed liquor, magnetic agitation 10min, polyethylene glycol, anhydrous sodium acetate are added afterwards
（CH3COONa）, polyethylene glycol and anhydrous sodium acetate（CH3COONa）Mass ratio is 1：3.6, mixture continues to stir 20min, mutually
Be formed as yellowish-brown liquid after melting, liquid be transferred in stainless steel ptfe autoclave and is sealed, is positioned in baking oven,
190 DEG C of reaction 8h, reaction terminates to be cooled to room temperature, in liquid dislocation beaker, by black product ultra-pure water and absolute ethyl alcohol point
It does not rinse three times, vacuum drying chamber under the conditions of 60 DEG C of product, dry 5h, obtains the magnetic diatomite；
Wherein, the additive amount of the polyethylene glycol is 0.4g,
（3）The preparation of modification infusorial earth material：According to mass ratio magnetism diatomite：Halogenated phosphates (CPC) are 1:1
Ratio takes magnetic diatomite and halogenated phosphates (CPC) are added to 80 ml deionized waters, 60 ml absolute ethyl alcohols, 1 ml
It in the mixed system of 25% ammonium hydroxide, and is mixed uniformly, obtains the uniform liquid of black；Aforesaid liquid is transferred to tri- mouthfuls of 250ml
It in flask, under 20 DEG C ~ 30 DEG C temperature conditions, is stirred using mechanical agitator, rotating speed is set as 300rpm, and adds dropwise
Enter ethyl orthosilicate（TEOS）, ethyl orthosilicate（TEOS）It is 4 with halogenated phosphates (CPC) mass ratio:1, continuously stir
Mix 5 ~ 7 h；The magnetic diatomite modified material deionized water and washes of absolute alcohol that will be obtained, 60 DEG C in vacuum drying chamber
2h is dried to get to the modification infusorial earth material；
Wherein, the additive amount of the CPC is 0.1g.
Fig. 1, Fig. 2 are scanning electron microscope (SEM) photograph of the diatomite after metal spraying sample preparation, and wherein Fig. 1 is acid processing diatomite, can by Fig. 1
To find out, acid processing diatomite surface only has less impurity, and hole is high-visible, illustrates that diatom is effectively got rid of in pickling
Partial impurities in native original soil；Fig. 2 is the modification infusorial earth material, and as seen from Figure 2, diatomite surface has a large amount of spherical
Object illustrates through hydrothermal synthesis method, a large amount of Fe3O4Micro-ball load is to diatomite surface, due to the load of CPC so that diatomite
Surface becomes coarse.
Embodiment 3
The present embodiment is the application example that the modification infusorial earth material is prepared in embodiment 2, weighs the diatomite of 5mg respectively
The modification infusorial earth material that original soil and 5mg embodiments 2 are prepared, is positioned over a concentration of 50mg/L, and volume is the direct of 50mL
Carry out concussion adsorption reaction in bright red 4BS dye solutions, at being 25 DEG C in temperature and take liquid in the set time, Magneto separate, λ=
Its supernatant absorbance is surveyed at 507nm, calculates its adsorption rate.
As seen from Figure 3, unmodified diatomite to dyestuff direct scarlet 4BS substantially without adsorption effect, it is modified
Treated, and modification infusorial earth material adsorption effect is obviously improved, and can also prove that this modification mode is suitable for waste water
The removal of middle dyestuff direct scarlet 4BS.
In addition, weighing the modification infusorial earth material that three parts of 5mg embodiments 2 are prepared is respectively put into a concentration of 50mg/L,
Volume is that it is anti-to carry out concussion absorption at being respectively 25 DEG C, 35 DEG C, 45 DEG C in temperature in the direct scarlet 4BS dye solutions of 50mL
It answers, takes liquid, Magneto separate to survey its supernatant absorbance at λ=507nm, calculate its adsorption rate in the set time.
As seen from Figure 4, the adsorption rate of dyestuff is gradually increased with the raising adsorbent of temperature, and the rate of adsorption adds
Soon, illustrate that heating is conducive to the progress of the adsorption process.
Claims (8)
1. a kind of preparation method of modification infusorial earth material, which is characterized in that the preparation method comprises the following steps：
Using diatomite as base stock, first passes through pickling and obtain acid activation diatomite, then magnetism is prepared by hydrothermal synthesis method
The magnetic diatomite is mixed with halogenated phosphates (CPC), deionized water, absolute ethyl alcohol and ammonium hydroxide, is obtained by diatomite
Simultaneously ethyl orthosilicate is added dropwise in the liquid uniform to black, mechanical agitation（TEOS）, 5 ~ 7 h are then continuously stirred, will be obtained
Modified material deionized water and washes of absolute alcohol, dried in vacuum drying chamber, obtain the modification infusorial earth
Material.
2. the preparation method of modification infusorial earth material according to claim 1, which is characterized in that diatomaceous pickling processes
The specific steps are：First diatomite original soil is dried, dried diatomite, which is placed in constant temperature acid in sulfuric acid solution, to be boiled, and postcooling
It to room temperature, is rinsed to neutrality using deionized water, the acid activation diatomite is obtained after drying.
3. the preparation method of modification infusorial earth material according to claim 1, which is characterized in that the hydrothermal synthesis method
The specific steps are：Ferric trichloride is dissolved in ethylene glycol and obtains mixed liquor, then the acid activation diatomite is put into mixed liquor, magnetic
Power stirs, and polyethylene glycol, anhydrous sodium acetate is then added（CH3COONa）, continue to be formed as yellowish-brown liquid after stirring is mutually melted,
Liquid is transferred in stainless steel ptfe autoclave and is sealed, is positioned in baking oven and reacts, reaction terminates to be cooled to room temperature,
Black product ultra-pure water and absolute ethyl alcohol are rinsed respectively, after product is vacuum dried, obtain the magnetic diatomite.
4. the preparation method of modification infusorial earth material according to claim 1, which is characterized in that it is described magnetism diatomite and
The mass ratio of CPC is 1:The mass ratio of 1, the TEOS and CPC are 4:1.
5. the preparation method of modification infusorial earth material according to claim 2, which is characterized in that the acid activation diatomite
And FeCl3·6H2The mass ratio of O is 1:2.7, the polyethylene glycol and CH3COONa mass ratioes are 1:3.6.
6. the preparation method of modification infusorial earth material according to claim 1, which is characterized in that the churned mechanically temperature
Degree is 20 DEG C ~ 30 DEG C, rotating speed 300rpm.
7. a kind of modification infusorial earth material, which is characterized in that the modification infusorial earth material is by any one of claim 1-6
What the preparation method was prepared.
8. a kind of application of modification infusorial earth material as claimed in claim 7, which is characterized in that the modification infusorial earth can answer
For adsorbing dyestuff direct scarlet 4BS.
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| CN115504726A (en) * | 2022-09-20 | 2022-12-23 | 安徽理工大学 | Preparation method of slow-release hydrophobic microcapsule and hydrophobic concrete |
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| CN110228857A (en) * | 2019-06-04 | 2019-09-13 | 成都纳海川环境工程有限公司 | The preparation method of fullerene modification scale dispersing agent for floor heating circulation water |
| CN111871413A (en) * | 2020-01-09 | 2020-11-03 | 长春工业大学 | Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition |
| CN111514847A (en) * | 2020-05-15 | 2020-08-11 | 辽宁科隆精细化工股份有限公司 | Preparation method of modified diatomite and application of modified diatomite in salt-containing wastewater treatment |
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| CN115121249A (en) * | 2022-05-29 | 2022-09-30 | 北京工业大学 | Preparation method and application of magnetic sodium iron silicate/hematite composite photocatalyst |
| CN115121249B (en) * | 2022-05-29 | 2024-03-12 | 北京工业大学 | Preparation method and application of magnetic sodium iron silicate/hematite composite photocatalyst |
| CN115504726A (en) * | 2022-09-20 | 2022-12-23 | 安徽理工大学 | Preparation method of slow-release hydrophobic microcapsule and hydrophobic concrete |
| CN115504726B (en) * | 2022-09-20 | 2023-09-08 | 安徽理工大学 | Preparation method of slow-release hydrophobic microcapsule and hydrophobic concrete |
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