CN106984271A - For the preparation method for the compound adsorbent for removing Methyl Orange in Wastewater and fluorine ion - Google Patents
For the preparation method for the compound adsorbent for removing Methyl Orange in Wastewater and fluorine ion Download PDFInfo
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- CN106984271A CN106984271A CN201710354557.9A CN201710354557A CN106984271A CN 106984271 A CN106984271 A CN 106984271A CN 201710354557 A CN201710354557 A CN 201710354557A CN 106984271 A CN106984271 A CN 106984271A
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- polyvinyl alcohol
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- compound adsorbent
- methyl orange
- carbon
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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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- 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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- 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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- 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 is directed to existing environmental problem, there is provided a kind of preparation method for being used to remove the compound adsorbent of Methyl Orange in Wastewater and fluorine ion, it uses polyvinyl alcohol for carbon source, aluminium salt is inorganic addO-on therapy, in-situ preparation polyvinyl alcohol/aluminium salt compound, then synthesizes carbon/alumina composite material, then soak through diluted acid or dilute alkaline soln by it through hydro-thermal reaction, part aluminum oxide is removed, the compound adsorbent is finally prepared.Preparation method of the present invention is economic and environment-friendly, and can realize being combined in carbon/alumina molecule level, so as to obtain being respectively provided with methyl orange in the aqueous solution and fluorine ion loose structure carbon/alumina composite adsorbent of preferable adsorption effect.
Description
Technical field
The invention belongs to chemical technology field, and in particular to a kind of to be used to remove the efficient of Methyl Orange in Wastewater and fluorine ion
The preparation method of compound adsorbent.
Background technology
The characteristics of content of organics height, high chroma, high toxicity and water quality complexity are dyeing waste waters, if directly discharge meeting pair
Environment causes serious pollution.There is the minimizing technology of a variety of organic dyestuff at present, such as：Chemical coagulation process, biochemical process, electricity
Chemical method, oxidizing process, biological treatment, absorption method etc..But all be present the problem of some can not be ignored in these methods, such as go
Except the influence of inefficient, costly and material to environment in itself, thus it is restricted in actual applications.
In these methods, absorption method technique is most simple, and cost consumption is minimum, thus is widely used, be currently used for
The important method of wastewater treatment.When methyl orange carries out adsorption treatment in using absorption method to water, the performance of adsorbent is made with it
It is standby to be even more important.Substantial amounts of new adsorbent occurs successively, such as activated alumina, activated carbon, hydroxyapatite, rare earth metal oxygen
Compound, molecular sieve etc..But existing adsorbent can not still meet use requirement, there is high manufacturing cost, preparation technology complexity, inhale
The attached low shortcoming of amount.Polyvinyl alcohol is a kind of water-soluble material, containing substantial amounts of oh group, and it is also with nontoxic, good
Good biocompatibility and the cell adhesiveness of very little, are widely used in biomedical sector.But pure polyvinyl alcohol is to first in waste water
The adsorbance of base orange is low, it is difficult to use, polyvinyl alcohol need to be modified as the high-efficiency adsorbent of methyl orange.Conventional modification
Method is that with other there is the component of high adsorption effect to be combined to methyl orange polyvinyl alcohol.Early-stage Study shows aluminum oxide to arsenic
There is preferable adsorption effect, if by alumina load on polyvinyl alcohol, being expected to prepare has high adsorb to methyl orange
The compound adsorbent of effect.
Fluorine is the essential trace elements of the human body, and appropriate fluorine contributes to health.However, drinking Oil repellent for a long time>1.0
Mg/L water, easily suffers from spot tooth disease；Drink Oil repellent for a long time>4.0 mg/L water, then can cause fluorosis of bone.In order to ensure the mankind
Health, it is necessary to high fluorine waste water carry out defluorinate processing, the method for conventional removing fluor in water is also to use adsorbent.
The content of the invention
It is an object of the invention to provide a kind of high efficiency composition adsorbent for being used to remove Methyl Orange in Wastewater and fluorine ion
Preparation method, its syntheti c route is simple, and the compound adsorbent prepared has to the methyl orange and fluorine ion in waste water
There is efficient removal effect.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method for being used to remove the compound adsorbent of Methyl Orange in Wastewater and fluorine ion, it is used using water as solvent
Polyvinyl alcohol is carbon source, and aluminium salt is inorganic addO-on therapy, in-situ preparation polyvinyl alcohol/aluminium salt compound, then by it through hydro-thermal
Reaction synthesis carbon/alumina composite material, then soaked through diluted acid or dilute alkaline soln, part aluminum oxide is removed, is finally prepared
The compound adsorbent of good adsorption effect is respectively provided with to methyl orange in the aqueous solution and fluorine ion.
The preparation method of the compound adsorbent comprises the following steps：
1）Polyvinyl alcohol is added in deionized water, heating stirring dissolving obtains polyvinyl alcohol water solution；
2）Toward step 1）Aluminium salt is added in gained polyvinyl alcohol water solution, then the complex solution is imported and contains polytetrafluoroethylene (PTFE)
Hydro-thermal reaction is carried out in the autoclave of liner, carbon/precipitation of alumina thing is generated；
3）By step 2）Gained carbon/precipitation of alumina thing is soaked in diluted acid or dilute alkaline aqueous solution, then anti-with deionized water
Rinse again to neutrality, that is, obtain the compound adsorbent.
Step 1）Described in polyvinyl alcohol water solution concentration be 5 ~ 10 wt%.
Step 2）The mass ratio of middle aluminium salt and polyvinyl alcohol used is 3 ~ 6:1；The aluminium salt is aluminum nitrate or aluminium chloride.
Step 2）The temperature of middle hydro-thermal reaction is 140 ~ 200 DEG C, the h of reaction time 4 ~ 10.
Step 3）In used diluted acid or dilute alkaline soln be 0.1 mol/L hydrochloric acid or sodium hydroxide solution；Its soak time
For 1 ~ 2 h.
The present invention has following beneficial effect：
（1）Using polyvinyl alcohol as carbon source in the present invention, can occur using the hydroxyl on polyvinyl alcohol molecule chain with aluminium ion strong
Interaction so that aluminium ion equal distributed mutually in final C-base composte material.
（2）The aluminium salts such as the aluminum nitrate or aluminium chloride that are used in the present invention can promote polyethylene in aqueous into faintly acid
Process of the alcohol thermal degradation into carbon.
（3）By being soaked in diluted acid or dilute alkaline soln, further carbon/alumina composite material of preparation can be carried out
Activation, improves its adsorption effect.
Brief description of the drawings
Fig. 1 is the microscopic appearance figure of compound adsorbent prepared by embodiment 1.
Fig. 2 be compound adsorbent prepared by embodiment 1 under different time to fluorine ion and the adsorption effect figure of methyl orange,
Wherein a is fluorine ion, and b is methyl orange.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention
Technical scheme is described further, but the present invention is not limited only to this.
Embodiment 1
1 g polyvinyl alcohol is taken to be dissolved in 19 g deionized waters, heating stirring dissolving obtains the polyvinyl alcohol water that concentration is 5 wt%
Solution；3 g aluminum nitrates are added into polyvinyl alcohol water solution, it is anti-that polyvinyl alcohol/aluminum nitrate composite solution then is imported into high pressure
Answer in kettle, the h of hydro-thermal reaction 4 at 140 DEG C, crushed after taking-up, obtain solid particle；Gained solid particle is immersed 0.1 again
2 h are soaked in mol/L sodium hydrate aqueous solution, then with deionized water rinsing to neutrality, drying obtains can be used for waste water
The compound adsorbent of middle methyl orange and fluoride ion removing.
Embodiment 2
1 g polyvinyl alcohol is taken to be dissolved in 9 g deionized waters, heating stirring dissolving obtains the polyvinyl alcohol water that concentration is 10 wt%
Solution；6 g aluminum nitrates are added into polyvinyl alcohol water solution, it is anti-that polyvinyl alcohol/aluminum nitrate composite solution then is imported into high pressure
Answer in kettle, the h of hydro-thermal reaction 8 at 180 DEG C, crushed after taking-up, obtain solid particle；Gained solid particle is immersed 0.1 again
1 h is soaked in mol/L sodium hydrate aqueous solution, then with deionized water rinsing to neutrality, drying obtains can be used for waste water
The compound adsorbent of middle methyl orange and fluoride ion removing.
Embodiment 3
1 g polyvinyl alcohol is taken to be dissolved in 9 g deionized waters, heating stirring dissolving obtains the polyvinyl alcohol water that concentration is 10 wt%
Solution；6 g aluminum nitrates are added into polyvinyl alcohol water solution, it is anti-that polyvinyl alcohol/aluminum nitrate composite solution then is imported into high pressure
Answer in kettle, the h of hydro-thermal reaction 4 at 200 DEG C, crushed after taking-up, obtain solid particle；Gained solid particle is immersed 0.1 again
1 h is soaked in mol/L aqueous hydrochloric acid solution, then with deionized water rinsing to neutrality, drying obtains can be used for first in waste water
The compound adsorbent of base orange and fluoride ion removing.
Embodiment 4
1 g polyvinyl alcohol is taken to be dissolved in 9 g deionized waters, heating stirring dissolving obtains the polyvinyl alcohol water that concentration is 10 wt%
Solution；3 g aluminium chloride are added into polyvinyl alcohol water solution, it is anti-that polyvinyl alcohol/aluminium chloride composite solution then is imported into high pressure
Answer in kettle, the h of hydro-thermal reaction 4 at 180 DEG C, crushed after taking-up, obtain solid particle；Gained solid particle is immersed 0.1 again
1 h is soaked in mol/L aqueous hydrochloric acid solution, then with deionized water rinsing to neutrality, drying obtains can be used for first in waste water
The compound adsorbent of base orange and fluoride ion removing.
Embodiment 5
1 g polyvinyl alcohol is taken to be dissolved in 15 g deionized waters, heating stirring dissolving obtains the polyvinyl alcohol that concentration is 6.25 wt%
The aqueous solution；5 g aluminium chloride are added into polyvinyl alcohol water solution, polyvinyl alcohol/aluminium chloride composite solution is then imported into high pressure
In reactor, hydro-thermal reaction 8h at 160 DEG C crushes after taking-up, obtains solid particle；Gained solid particle is immersed 0.1 again
1 h is soaked in mol/L sodium hydrate aqueous solution, then with deionized water rinsing to neutrality, drying obtains can be used for waste water
The compound adsorbent of middle methyl orange and fluoride ion removing.
Fluorine ion determining adsorption is tested：
Each 0.1 g of compound adsorbent prepared by Example 1-5, is added separately to 500 mL fluorinion concentrations for 10 mg/
In the L aqueous solution, be then placed in water-bath constant temperature oscillator, vibrate 7 h under 150 rpm respectively, then with M519 types fluorine from
The concentration of son meter measurement fluorine ion, and adsorbance is calculated according to below equation：
Fluorine ion adsorbance (mg/g)=(Ci−Ce)V/m×1000 mg F−/ g,
Wherein, Ci(mg/L) it is F in waste water−Initial concentration；Ce(mg/L) F when for adsorption equilibrium−Initial concentration；V (L)
It is the volume of fluoride waste；M (g) is sorbent used quality.
Adsorption of Methyl Orange determination experiment：
Methyl orange solution is diluted to various concentrations（10 mg/L、8 mg/L、6 mg/L、4 mg/L、2mg/L、1 mg/L）, and
Its absorbance is determined under 465 nm, using absorbance as ordinate, methyl orange concentration is that abscissa draws standard curve, and is obtained
Its regression equation.
Each 0.12 g of compound adsorbent of embodiment 1-5 preparations is weighed, is added separately to the mg/L's of 30 mL 100
In methyl orange solution, adsorbed in the constant temperature oscillator under 25 DEG C, 150 rpm after 110min, solution is taken out through Buchner funnel
Filter, takes filtrate to determine its UV absorption intensity at 465 nm, and according to its concentration of gained regression equation calculation, obtains balance and inhale
Attached amount.
Compound adsorbent obtained by embodiment 1-5 is shown in Table 1 to the adsorption effect of fluorine ion and methyl orange.
The adsorption efficiency of compound adsorbent prepared by the embodiment 1-5 of table 1.
From table 1, present invention gained compound adsorbent has good adsorption effect to fluorine ion and methyl orange.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (6)
1. a kind of preparation method for being used to remove the compound adsorbent of Methyl Orange in Wastewater and fluorine ion, it is characterised in that：Using
Polyvinyl alcohol is carbon source, and aluminium salt is inorganic addO-on therapy, through Hydrothermal Synthesiss carbon/alumina composite material, then by it through diluted acid or
Dilute alkaline soln soaks, and finally prepares the composite adsorption that good adsorption effect is respectively provided with to methyl orange in the aqueous solution and fluorine ion
Agent.
2. the preparation method of compound adsorbent according to claim 1, it is characterised in that：Comprise the following steps：
1）Polyvinyl alcohol is added in deionized water, heating stirring dissolving obtains polyvinyl alcohol water solution；
2）Toward step 1）Aluminium salt is added in gained polyvinyl alcohol water solution, then the complex solution is imported and contains polytetrafluoroethylene (PTFE)
Hydro-thermal reaction is carried out in the autoclave of liner, carbon/precipitation of alumina thing is generated；
3）By step 2）Gained carbon/precipitation of alumina thing is soaked in diluted acid or dilute alkaline aqueous solution, then anti-with deionized water
Rinse again to neutrality, that is, obtain the compound adsorbent.
3. the preparation method according to claim 2 for being used to remove the compound adsorbent of Methyl Orange in Wastewater and fluorine ion,
It is characterized in that：Step 1）Described in polyvinyl alcohol water solution concentration be 5 ~ 10 wt%.
4. the preparation method of compound adsorbent according to claim 2, it is characterised in that：Step 2）Middle aluminium salt is gathered with used
The mass ratio of vinyl alcohol is 3 ~ 6:1；The aluminium salt is aluminum nitrate or aluminium chloride.
5. the preparation method of compound adsorbent according to claim 2, it is characterised in that：Step 2）Middle hydro-thermal reaction
Temperature is 140 ~ 200 DEG C, the h of reaction time 4 ~ 10.
6. the preparation method of compound adsorbent according to claim 2, it is characterised in that：Step 3）In diluted acid used or
Dilute alkaline soln is 0.1 mol/L hydrochloric acid or sodium hydroxide solution；Its soak time is 1 ~ 2 h.
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| CN201710354557.9A CN106984271B (en) | 2017-05-19 | 2017-05-19 | For removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107321324A (en) * | 2017-09-05 | 2017-11-07 | 霍邱金木鱼农业科技有限公司 | A kind of dye discoloration magnetic adsorptive material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663448A (en) * | 2012-09-19 | 2014-03-26 | 天津普兰纳米科技有限公司 | Preparation method of carbon material, obtained carbon material and application thereof |
| CN106512936A (en) * | 2016-11-11 | 2017-03-22 | 镇江市高等专科学校 | Hydrothermal method for preparing fluoride removal adsorbent and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663448A (en) * | 2012-09-19 | 2014-03-26 | 天津普兰纳米科技有限公司 | Preparation method of carbon material, obtained carbon material and application thereof |
| CN106512936A (en) * | 2016-11-11 | 2017-03-22 | 镇江市高等专科学校 | Hydrothermal method for preparing fluoride removal adsorbent and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| BEIBEI FANG等: "Preparation of a hierarchical flower-like g-Al2O3@C composite exhibiting enhanced adsorption performance for congo red by high temperature transformation of g-AlOOH@C precursors", 《RSC ADVANCES》 * |
| 张伟: "水热法合成LiFePO4及其性能研究", 《中国优秀硕士学位论文全文数据库》 * |
| 谌任平等: "活性炭负载铝吸附去除水中氟离子的研究", 《三峡环境与生态》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107321324A (en) * | 2017-09-05 | 2017-11-07 | 霍邱金木鱼农业科技有限公司 | A kind of dye discoloration magnetic adsorptive material and preparation method thereof |
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