CN110026164A - A kind of preparation method of porous fibre composite dephosphorization adsorbent - Google Patents
A kind of preparation method of porous fibre composite dephosphorization adsorbent Download PDFInfo
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- CN110026164A CN110026164A CN201910294006.7A CN201910294006A CN110026164A CN 110026164 A CN110026164 A CN 110026164A CN 201910294006 A CN201910294006 A CN 201910294006A CN 110026164 A CN110026164 A CN 110026164A
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- porous fibre
- fibre composite
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- dephosphorization adsorbent
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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
-
- 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
-
- 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
-
- 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
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
Abstract
The invention discloses a kind of preparation method of porous fibre composite dephosphorization adsorbent, include the following steps: that basalt fibre is added in Fe solution in (1), sufficiently impregnates and obtain the soak containing porous fibre；(2) ethanol solution is added dropwise in soak, the military rock fiber oil bath after immersion is condensed back, obtains the porous fibre of load β-FeOOH；(3) basalt fibre of step (2) load β-FeOOH is impregnated, cleaning, drying, obtains porous fibre composite dephosphorization adsorbent；(4) it regenerates；Porous fibre composite dephosphorization adsorbent prepared by the present invention, which is negative, is loaded with the basalt fibre of β-FeOOH, it reaches 99.5% to the removal rate of low phosphorus in water body, and preparation method is easy to operate, adsorbent is easy to regenerate, powder dephosphorization adsorbent can be also solved to be difficult to settle, be difficult to recycle, the problems such as difficult is recycled, there is wide prospect of the application.
Description
Technical field
The invention belongs to municipal works and environmental project water-treatment technology field, and in particular to one kind is low in water removal for going
The preparation method of the porous fibre composite dephosphorization adsorbent of concentration orthophosphates.
Background technique
Phosphorus is nutrient necessary to most of biology growing in the ecosystem, but the phosphorus concentration in water body is more than
It can cause the eutrophication of water body when 0.02mg/L.Once eutrophication occurs for water body, algal bloom will result in,
Oxygen in water decline, aquatile mortality generate toxic and harmful gas, influence water supply quality etc., this not only can be to life
State environment causes persistence to endanger, and immeasurable loss can be also caused to social economy.Traditional phosphorus removing method mainly includes
Bioanalysis, chemical method and absorption method.In these phosphorus removing methods, phosphorus aqueous concentration: biological phosphate-eliminating > 1.0mg/L；Chemical dephosphorization >
0.50mg/L；Adsorption and dephosphorization < 0.02mg/L, only absorption method can achieve water body occur eutrophication phosphorus controlled concentration (<
0.02mg/L).Therefore exploitation efficient dephosphorization composite material is extremely urgent.
The oxide of iron such as goethite (alpha-feooh), akaganeite (β-FeOOH), lepidocrocite (γ-FeOOH) are soil
The resistant mineral being widely present in earth, water body and deposit, specific surface area with higher and subtle grain structure, to environment
Pollutant in medium has important catharsis, and research finds to have using chemically synthesized FeOOH as adsorbent preferable
Phosphor-removing effect, dephosphorization mechanism be mainly pass through β-FeOOH surface hydroxyl and phosphate anion ligand exchange.But β-
FeOOH powder can make water body become muddy, not easily settled, be difficult to separate with water body because its particle size is small after putting into water body
A series of problems, such as with recycling and difficult recycling, these are insufficient to be also applied in Practical Project as powder adsorbent material
One big obstacle, but also materials industrialization becomes problem.Because not have good pore structure, mechanical strength low by β-FeOOH, need
It is dipped into attachment on porous support, porous carrier and carrying method determine dephosphorization effect composite porous after loading
Fruit.It is not easily settled however, so efficient dephosphorization material is separated because being difficult to water body, become cloudy water body, colour changed into yellow etc. it is a series of
Problem becomes the big obstacle for being applied to it in engineering, but also materials industrialization becomes problem.
Summary of the invention
It is an object of the invention in place of overcome the deficiencies in the prior art, provide a kind of porous fibre composite dephosphorization absorption
The preparation method of agent solves the problems in above-mentioned background technique.
The technical solution adopted by the present invention to solve the technical problems is: providing a kind of porous fibre composite dephosphorization absorption
The preparation method of agent, includes the following steps:
(1) preparation of the soak containing porous fibre: by FeCl3·6H2O is dissolved in distilled water, and the concentration for configuring Fe is
The Fe solution of 2~5wt%；The basalt fibre of 1~4wt%, sufficiently 0.5~2h of immersion are added in Fe solution, is contained
The soak of porous fibre；
(2) load the preparation of the porous fibre of β-FeOOH: it is molten that dehydrated alcohol is added dropwise in the soak of step (1)
Liquid, sustained oscillation during dropwise addition, being added dropwise to concentration of alcohol is 40~80wt%, shakes and impregnates 0.5~2h；It takes out after impregnating
The concentration that is placed in of military rock fiber be in 95~98wt% ethanol solution, under the conditions of 40~120 DEG C oil bath be condensed back 4~
For 24 hours, the porous fibre of load β-FeOOH is obtained；
(3) it loads the collection of the porous fibre of β-FeOOH: the porous fibre for the load β-FeOOH that step (2) obtains is set
It is impregnated in ultrapure water, then cleaning, drying, obtain porous fibre composite dephosphorization adsorbent, the porous fibre composite dephosphorization
The load factor of β-FeOOH is 10~80wt% in adsorbent.
In a preferred embodiment of the present invention, 17.8~30wt%SiO is contained in the basalt fibre2。
In a preferred embodiment of the present invention, the basalt fibre is cut into porous fibre block, having a size of 4.9~
8.0mm3。
4. a kind of preparation method of porous fibre composite dephosphorization adsorbent according to claim 1, it is characterised in that:
Oil bath is condensed back 12h under the conditions of 90 DEG C in the step (2).
In a preferred embodiment of the present invention, basalt fibre after impregnating ultrapure water in the step (3), with distillation
It is 4~7 that water, which is cleaned to filtrate pH is rinsed,.
In a preferred embodiment of the present invention, basalt fibre after cleaning is dried at 60~120 DEG C in the step (3)
Dry 10~12h.
In a preferred embodiment of the present invention, the load factor of β-FeOOH is in the porous fibre composite dephosphorization adsorbent
50~80wt%.
In a preferred embodiment of the present invention, this preparation method further includes step (4) porous fibre composite dephosphorization adsorbent
Regeneration: pass through Klorvess Liquid parsing regeneration.
The technical program compared with the background art, it has the following advantages:
1. the basalt fibre that the present invention is utilized has the extremely strong multi-pore structure of water-retaining property, and β-FeOOH fixation is attached
In gap structure, porous fibre composite adsorbing material is made, is conducive to the phosphate radical in the active constituent and water in material
It comes into full contact with, making molding porous material in water has certain mechanical strength, and it is strong to can be applied to certain water impact
The water body environment of degree, while ensure that adsorbent has superior adsorption capacity, it solves β-FeOOH powder body material and is actually answering
With easy turbid water body in the process, the disadvantage for being not readily separated, recycling difficulty；
2. operation of the present invention is simple and easy and the removal effect of centering low phosphorus is significant；
3. β-FeOOH Preferential adsorption phosphate anion and can not generate sludge in water body in the present invention, furthermore can be used
Klorvess Liquid carries out parsing regeneration to the porous fibre composite dephosphorization adsorbent, increases utilization rate and repeatability.
Detailed description of the invention
Fig. 1 is the pictorial diagram of porous fibre composite dephosphorization adsorbent of the present invention.
Fig. 2 is that the SEM of unsupported preceding basalt porous fibre block schemes.
The SEM of Fig. 3 porous fibre composite dephosphorization adsorbent of the present invention schemes.
Specific embodiment
Embodiment 1
A kind of preparation method of porous fibre composite dephosphorization adsorbent of the present embodiment, includes the following steps:
In 3wt%FeCl3·6H2It is impregnated in O and contains 17.8wt%SiO2Porous block basalt fiber cotton, basalt is fine
The dosage of vinylon and cotton blend is 2wt%；Then 50wt% dehydrated alcohol is added dropwise, impregnates 1h after shaking when being added dropwise uniformly, then takes
Out through FeCl3The basalt cotton that solution impregnated is set in a round bottom flask, and 96wt% dehydrated alcohol is added, under the conditions of 90 DEG C
Oil bath is condensed back 6h, and as 0.5-2h is impregnated in ultrapure water, the basalt fibre for loading upper β-FeOOH is then obtained by filtration
Cotton；It is put into baking oven after finally being rinsed with distilled water flushing 5~8 times to flushing filtrate PH=4~7 and dries 12h extremely drying at 60 DEG C,
Porous basalt fiber as shown in figures 1 and 3 is obtained except pictorial diagram and the SEM figure of phosphorus composite material, Fig. 2 is unsupported preceding profound
The SEM of military rock porous fibre block schemes.
Embodiment 2
Embodiment 2 the difference from embodiment 1 is that: in 2.5wt%FeCl3·6H2It is impregnated in O and contains 17.8wt%SiO2's
The amount of porous basalt cellucotton, basalt fiber cotton is 2wt%, is then added dropwise to 50wt% dehydrated alcohol, is shaken when being added dropwise
1h is impregnated after swinging uniformly, is then taken out through FeCl3The basalt cotton that solution impregnated is set in a round bottom flask, and 96wt% is added
Dehydrated alcohol, oil bath is condensed back 6h under the conditions of 90 DEG C, and the basalt fiber cotton for loading upper β-FeOOH is then obtained by filtration,
It is put into baking oven after finally being rinsed with distilled water flushing 5~8 times to flushing filtrate PH=4~7 and dries 12h at 60 DEG C to drying, obtains
To porous basalt fiber as shown in figures 1 and 3 except pictorial diagram and the SEM figure of phosphorus composite material, Fig. 2 is the unsupported preceding Black Warrior
The SEM of rock porous fibre block schemes.
Embodiment 3
Embodiment 3 the difference from embodiment 1 is that: in 2wt%FeCl3·6H2It is impregnated in O and contains 17.8wt%SiO2It is more
The amount of hole basalt fiber cotton, basalt fiber cotton is 2wt%, is then added dropwise to 50wt% dehydrated alcohol, is shaken when being added dropwise
1h is impregnated after uniformly, is then taken out through FeCl3The basalt cotton that solution impregnated is set in a round bottom flask, add 96wt% without
Water-ethanol, oil bath is condensed back 6h under the conditions of 90 DEG C, the basalt fiber cotton for loading upper β-FeOOH is then obtained by filtration, most
It is put into baking oven after being rinsed afterwards with distilled water flushing 5~8 times to flushing filtrate PH=4~7 and dries 12h at 60 DEG C to drying, obtains
For porous basalt fiber as shown in figures 1 and 3 except pictorial diagram and the SEM figure of phosphorus composite material, Fig. 2 is unsupported preceding basalt
The SEM of porous fibre block schemes.
Embodiment 4
The present embodiment carries out the removal of phosphorus in water using porous fibre composite dephosphorization adsorbent prepared by embodiment 1, including
Following steps: the porous fibre composite dephosphorization adsorbent that 2g embodiment 1 is obtained, the phosphate-buffered that investment 100mL is prepared are molten
In liquid, phosphorous 2.5mg/L (with P element Mass Calculation) adsorbs 48h at 30 DEG C；Sampling, using molybdate spectrophotometry into
Row Phosphate analysis, removal rate of phosphate 99.8%.
Embodiment 5
The present embodiment carries out the removal of phosphorus in water using porous fibre composite dephosphorization adsorbent prepared by embodiment 2, including
Following steps: the phosphate buffer solution that the porous fibre composite dephosphorization adsorbent investment 100mL that 2g embodiment 1 is obtained is prepared
In, phosphorous 2.5mg/L (with P element Mass Calculation) adsorbs 48h at 30 DEG C；Sampling, is carried out using molybdate spectrophotometry
Phosphate analysis, removal rate of phosphate 99.5%.
Embodiment 6
The present embodiment adopts the removal that porous fibre composite dephosphorization adsorbent prepared with embodiment 3 carries out phosphorus in water, including
Following steps: the phosphate buffer solution that porous fibre composite dephosphorization adsorbent investment 100mL prepared by 2g embodiment 3 is prepared
In, phosphorous 2.5mg/L (with P element Mass Calculation) adsorbs 48h at 30 DEG C；Sampling, is carried out using molybdate spectrophotometry
Phosphate analysis, removal rate of phosphate 99.0%.
Embodiment 7
The present embodiment is parsed again using the porous fibre composite dephosphorization adsorbent after adsorbing phosphate radical in embodiment 6
It is raw, include the following steps: for the porous fibre composite dephosphorization adsorbent after absorption to be placed in the chlorination that concentration is 0.1~0.5mol/L
It is parsed in potassium solution, shakes 3~12h, take out fiber block, after being washed with distilled water 3~5 times, be placed in 60 DEG C of baking oven drying,
Regeneration porous fibre composite dephosphorization adsorbent is made.
The above is only the preferred embodiment of the present invention, the range implemented of the present invention that therefore, it cannot be limited according to, i.e., according to
Equivalent changes and modifications made by the invention patent range and description, should still be within the scope of the present invention.
Claims (8)
1. a kind of preparation method of porous fibre composite dephosphorization adsorbent, which comprises the steps of:
(1) preparation of the soak containing porous fibre: by FeCl3·6H2O is dissolved in distilled water, configure Fe concentration be 2~
The Fe solution of 5wt%；The basalt fibre of 1~4wt%, sufficiently 0.5~2h of immersion are added in Fe solution, obtains containing porous
The soak of fiber；
(2) it loads the preparation of the porous fibre of β-FeOOH: ethanol solution being added dropwise in the soak of step (1), drip
Sustained oscillation during adding, being added dropwise to concentration of alcohol is 40~80wt%, shakes and impregnates 0.5~2h；Take out the force after impregnating
The concentration that rock fiber is placed in be 95~98wt% ethanol solution in, under the conditions of 40~120 DEG C oil bath be condensed back 4~for 24 hours, obtain
To the porous fibre of load β-FeOOH；
(3) it loads the collection of the porous fibre of β-FeOOH: the porous fibre for the load β-FeOOH that step (2) obtains being placed in super
It is impregnated in pure water, then cleaning, drying, obtains porous fibre composite dephosphorization adsorbent, the porous fibre composite dephosphorization absorption
The load factor of β-FeOOH is 10~80wt% in agent.
2. a kind of preparation method of porous fibre composite dephosphorization adsorbent according to claim 1, it is characterised in that: described
Contain 17.8~30wt%SiO in basalt fibre2。
3. a kind of preparation method of porous fibre composite dephosphorization adsorbent according to claim 2, it is characterised in that: described
Basalt fibre is cut into porous fibre block, having a size of 4.9~8.0mm3。
4. a kind of preparation method of porous fibre composite dephosphorization adsorbent according to claim 1, it is characterised in that: described
Oil bath is condensed back 12h under the conditions of 90 DEG C in step (2).
5. a kind of preparation method of porous fibre composite dephosphorization adsorbent according to claim 1, it is characterised in that: described
Basalt fibre after impregnating ultrapure water in step (3) is wash with distilled water 4~7 to filtrate pH is rinsed.
6. a kind of preparation method of porous fibre composite dephosphorization adsorbent according to claim 1, it is characterised in that: described
Basalt fibre dries 10~12h at 60~120 DEG C after cleaning in step (3).
7. a kind of preparation method of porous fibre composite dephosphorization adsorbent according to claim 1, it is characterised in that: described
The load factor of β-FeOOH is 50~80wt% in porous fibre composite dephosphorization adsorbent.
8. a kind of preparation method of porous fibre composite dephosphorization adsorbent according to claim 1, which is characterized in that also wrap
Include the regeneration of step (4) porous fibre composite dephosphorization adsorbent: by the porous fibre composite dephosphorization adsorbent after absorption phosphorus solution
It is placed in the Klorvess Liquid that concentration is 0.1~0.5mol/L, shakes 3~12h, take out and be washed with distilled water 3~5 postpositions
It is dried in 60 DEG C of baking ovens, regeneration porous fibre composite dephosphorization adsorbent is made.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910294006.7A CN110026164A (en) | 2019-04-12 | 2019-04-12 | A kind of preparation method of porous fibre composite dephosphorization adsorbent |
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| CN201910294006.7A CN110026164A (en) | 2019-04-12 | 2019-04-12 | A kind of preparation method of porous fibre composite dephosphorization adsorbent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115155537A (en) * | 2022-07-28 | 2022-10-11 | 安徽农业大学 | FeOOH functionalized acrylic fiber and preparation method and application thereof |
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