CN106984271B - For removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion - Google Patents
For removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion Download PDFInfo
- Publication number
- CN106984271B CN106984271B CN201710354557.9A CN201710354557A CN106984271B CN 106984271 B CN106984271 B CN 106984271B CN 201710354557 A CN201710354557 A CN 201710354557A CN 106984271 B CN106984271 B CN 106984271B
- Authority
- CN
- China
- Prior art keywords
- polyvinyl alcohol
- methyl orange
- preparation
- fluorine ion
- compound adsorbent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- 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, it provides a kind of for removing the preparation method of 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, then it is synthesized carbon/alumina composite material through hydro-thermal reaction, then impregnated through diluted acid or dilute alkaline soln by in-situ preparation polyvinyl alcohol/aluminium salt compound, part aluminium oxide is removed, the compound adsorbent is finally prepared.Preparation method of the present invention is economic and environment-friendly, and can realize it is compound in carbon/alumina molecule level, to obtain the porous structure carbon/alumina composite adsorbent for all having preferable adsorption effect to methyl orange in aqueous solution and fluorine ion.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of for removing the efficient of Methyl Orange in Wastewater and fluorine ion
The preparation method of compound adsorbent.
Background technique
The characteristics of high organic content, high chroma, high toxicity and water quality complexity are dyeing waste waters, if direct emission can be right
Environment causes serious pollution.There are many kinds of the minimizing technologies of organic dyestuff at present, such as: chemical coagulation process, biochemical method, electricity
Chemical method, oxidizing process, biological treatment, absorption method etc..But these methods all there are problems that it is some can not be ignored, such as go
Influence except inefficient, expensive and material itself to environment, thus be restricted in practical 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 carrying out adsorption treatment to methyl orange in water using absorption method, the performance of adsorbent is made with it
It is standby to be even more important.A large amount of new adsorbent occurs successively, such as activated alumina, active carbon, hydroxyapatite, rare earth metal oxygen
Compound, molecular sieve etc..But existing adsorbent is not able to satisfy requirement still, there are manufacturing costs high, preparation process complexity, suction
The attached low disadvantage of amount.Polyvinyl alcohol is a kind of water-soluble material, containing a large amount of hydroxyl group, and it also have it is nontoxic, good
The cell adhesiveness of good biocompatibility and very little, is widely used in field of biomedicine.But pure polyvinyl alcohol is to first in waste water
The adsorbance of base orange is low, it is difficult to which the high-efficiency adsorbent as methyl orange uses, and need to be modified to polyvinyl alcohol.It is common modified
Method be by polyvinyl alcohol and other to methyl orange have high adsorption effect component it is compound.Early-stage study shows aluminium oxide to arsenic
There is preferable adsorption effect, as being expected to be prepared has high absorption to methyl orange by alumina load on polyvinyl alcohol
The compound adsorbent of effect.
Fluorine is the essential trace elements of the human body, and suitable fluorine facilitates human health.However, long-term drinking fluorine content > 1.0
The water of mg/L is easy to suffer from spot tooth disease；Long-term drinking fluorine content > 4.0 mg/L water, then can lead to fluorosis of bone.In order to guarantee the mankind
Health, need to high fluorine waste water carry out defluorinate processing, the method for common removing fluor in water is also using adsorbent.
Summary of the invention
The purpose of the present invention is to provide a kind of for removing the high efficiency composition adsorbent of Methyl Orange in Wastewater and fluorine ion
Preparation method, preparation route is simple, and the compound adsorbent prepared in waste water methyl orange and fluorine ion have
There is efficient removal effect.
To achieve the above object, the present invention adopts the following technical scheme:
It is a kind of to take water as a solvent for removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion,
Use polyvinyl alcohol for carbon source, aluminium salt is inorganic addO-on therapy, then in-situ preparation polyvinyl alcohol/aluminium salt compound is passed through
Hydro-thermal reaction synthesizes carbon/alumina composite material, then impregnates through diluted acid or dilute alkaline soln, removes part aluminium oxide, final to prepare
Obtain the compound adsorbent that good adsorption effect is all had to methyl orange in aqueous solution and fluorine ion.
The preparation method of the compound adsorbent includes the following steps:
1) polyvinyl alcohol is added in deionized water, heating stirring dissolution obtains polyvinyl alcohol water solution；
2) aluminium salt is added into step 1) gained polyvinyl alcohol water solution, then the complex solution is imported and contains polytetrafluoro
Hydro-thermal reaction is carried out in the autoclave of ethylene liner, generates carbon/precipitation of alumina object；
3) carbon/precipitation of alumina object obtained by step 2 is impregnated in diluted acid or dilute alkaline aqueous solution, then uses deionization
Water repeated flushing arrives the compound adsorbent to neutrality.
The concentration of polyvinyl alcohol water solution described in step 1) is 5 ~ 10 wt%.
The mass ratio of aluminium salt and polyvinyl alcohol used is 3 ~ 6:1 in step 2；The aluminium salt is aluminum nitrate or aluminium chloride.
The temperature of hydro-thermal reaction is 140 ~ 200 DEG C in step 2,4 ~ 10 h of reaction time.
Diluted acid or dilute alkaline soln used are the hydrochloric acid or sodium hydroxide solution of 0.1 mol/L in step 3)；Its soaking time
For 1 ~ 2 h.
The present invention has the following beneficial effects:
(1) it can be sent out with aluminium ion using polyvinyl alcohol as carbon source using the hydroxyl on polyvinyl alcohol molecule chain in the present invention
Raw strong interaction, so that aluminium ion is homogeneously distributed in final C-base composte material.
(2) aluminium salts such as aluminum nitrate or aluminium chloride used in the present invention can promote polyethylene in aqueous solution at faintly acid
Alcohol thermal degradation at carbon process.
(3) by being impregnated in diluted acid or dilute alkaline soln, further the carbon of preparation/alumina composite material can be carried out
Activation, improves its adsorption effect.
Detailed description of the invention
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 the adsorption effect figure of fluorine ion and methyl orange,
Wherein a is fluorine ion, and b is methyl orange.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution 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 dissolution obtains the polyethylene that concentration is 5 wt%
Alcohol solution；3 g aluminum nitrates are added into polyvinyl alcohol water solution, then import polyvinyl alcohol/aluminum nitrate composite solution high
It presses in reaction kettle, 4 h of hydro-thermal reaction at 140 DEG C, is crushed after taking-up, obtains solid particle；Obtained solid particle is immersed again
2 h are impregnated in the sodium hydrate aqueous solution of 0.1 mol/L, are then rinsed with deionized water to neutrality, and drying is to get to can be used for
The compound adsorbent of Methyl Orange in Wastewater and fluoride ion removing.
Embodiment 2
1 g polyvinyl alcohol is taken to be dissolved in 9 g deionized waters, heating stirring dissolution obtains the polyethylene that concentration is 10 wt%
Alcohol solution；6 g aluminum nitrates are added into polyvinyl alcohol water solution, then import polyvinyl alcohol/aluminum nitrate composite solution high
It presses in reaction kettle, 8 h of hydro-thermal reaction at 180 DEG C, is crushed after taking-up, obtains solid particle；Obtained solid particle is immersed again
1 h is impregnated in the sodium hydrate aqueous solution of 0.1 mol/L, is then rinsed with deionized water to neutrality, and drying is to get to can be used for
The compound adsorbent of Methyl Orange in Wastewater and fluoride ion removing.
Embodiment 3
1 g polyvinyl alcohol is taken to be dissolved in 9 g deionized waters, heating stirring dissolution obtains the polyethylene that concentration is 10 wt%
Alcohol solution；6 g aluminum nitrates are added into polyvinyl alcohol water solution, then import polyvinyl alcohol/aluminum nitrate composite solution high
It presses in reaction kettle, 4 h of hydro-thermal reaction at 200 DEG C, is crushed after taking-up, obtains solid particle；Obtained solid particle is immersed again
1 h is impregnated in the aqueous hydrochloric acid solution of 0.1 mol/L, is then rinsed with deionized water to neutrality, and drying is to get to can be used for waste water
The compound adsorbent of middle methyl orange and fluoride ion removing.
Embodiment 4
1 g polyvinyl alcohol is taken to be dissolved in 9 g deionized waters, heating stirring dissolution obtains the polyethylene that concentration is 10 wt%
Alcohol solution；3 g aluminium chloride are added into polyvinyl alcohol water solution, then import polyvinyl alcohol/aluminium chloride composite solution high
It presses in reaction kettle, 4 h of hydro-thermal reaction at 180 DEG C, is crushed after taking-up, obtains solid particle；Obtained solid particle is immersed again
1 h is impregnated in the aqueous hydrochloric acid solution of 0.1 mol/L, is then rinsed with deionized water to neutrality, and drying is to get to can be used for waste water
The compound adsorbent of middle methyl orange and fluoride ion removing.
Embodiment 5
1 g polyvinyl alcohol is taken to be dissolved in 15 g deionized waters, heating stirring dissolution obtains the poly- second that concentration is 6.25 wt%
Enol aqueous solution；5 g aluminium chloride are added into polyvinyl alcohol water solution, then import polyvinyl alcohol/aluminium chloride composite solution
In autoclave, hydro-thermal reaction 8h at 160 DEG C is crushed after taking-up, obtains solid particle；Obtained solid particle is immersed again
1 h is impregnated in the sodium hydrate aqueous solution of 0.1 mol/L, is then rinsed with deionized water to neutrality, and drying is to get to can be used for
The compound adsorbent of Methyl Orange in Wastewater and fluoride ion removing.
The experiment of fluorine ion determining adsorption:
Each 0.1 g of compound adsorbent prepared by Example 1-5, being added separately to 500 mL fluorinion concentrations is 10
It in the aqueous solution of mg/L, is then placed in water-bath constant temperature oscillator, vibrates 7 h at 150 rpm respectively, then use M519 type fluorine
Ionometer measures the concentration of fluorine ion, and calculates adsorbance according to the following formula:
Fluorine ion adsorbance (mg/g)=(Ci−Ce)V/m×1000 mg F−/ g,
Wherein, CiIt (mg/L) is F in waste water−Initial concentration；Ce(mg/L) be adsorption equilibrium when F−Initial concentration；V
(L) be fluoride waste volume；M (g) is sorbent used quality.
Adsorption of Methyl Orange measurement experiment:
Methyl orange solution is diluted to various concentration (10 mg/L, 8 mg/L, 6 mg/L, 4 mg/L, 2mg/L, 1 mg/
L its absorbance), and at 465 nm is measured, using absorbance as ordinate, methyl orange concentration is that abscissa draws standard curve,
And obtain its regression equation.
Each 0.12 g of compound adsorbent for weighing embodiment 1-5 preparation, is added separately to 30 mL, 100 mg/L's
In methyl orange solution, after adsorbing 110min in the constant temperature oscillator under 25 DEG C, 150 rpm, solution is taken out through Buchner funnel
Filter takes filtrate to measure its UV absorption intensity at 465 nm, and according to its concentration of gained regression equation calculation, finds out 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 the compound adsorbent of 1. embodiment 1-5 of table preparation
Seen from table 1, present invention gained compound adsorbent has good adsorption effect to fluorine ion and methyl orange.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (5)
1. a kind of for removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion, it is characterised in that: use
Polyvinyl alcohol is carbon source, and aluminium salt is inorganic addO-on therapy, through hydrothermal synthesis carbon/alumina composite material, then by it through diluted acid or
Dilute alkaline soln impregnates, and the composite adsorption that good adsorption effect is all had to methyl orange in aqueous solution and fluorine ion is finally prepared
Agent；
It specifically comprises the following steps:
1) polyvinyl alcohol is added in deionized water, heating stirring dissolution obtains polyvinyl alcohol water solution；
2) aluminium salt is added into step 1) 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, generates carbon/precipitation of alumina object；
3) carbon/precipitation of alumina object obtained by step 2 is impregnated in diluted acid or dilute alkaline aqueous solution, then anti-with deionized water
It is multiple to rinse to neutrality to get the compound adsorbent is arrived.
2. it is according to claim 1 for removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion,
It is characterized by: the concentration of polyvinyl alcohol water solution described in step 1) is 5 ~ 10 wt%.
3. it is according to claim 1 for removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion,
It is characterized by: the mass ratio of aluminium salt and polyvinyl alcohol used is 3 ~ 6:1 in step 2；The aluminium salt is aluminum nitrate or chlorination
Aluminium.
4. it is according to claim 1 for removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion,
It is characterized by: the temperature of hydro-thermal reaction is 140 ~ 200 DEG C in step 2,4 ~ 10 h of reaction time.
5. it is according to claim 1 for removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion,
It is characterized by: diluted acid or dilute alkaline soln used are the hydrochloric acid or sodium hydroxide solution of 0.1 mol/L in step 3)；When it is impregnated
Between be 1 ~ 2 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106984271A CN106984271A (en) | 2017-07-28 |
| CN106984271B true CN106984271B (en) | 2019-07-09 |
Family
ID=59420260
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710354557.9A Expired - Fee Related 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 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106984271B (en) |
Families Citing this family (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 |
-
2017
- 2017-05-19 CN CN201710354557.9A patent/CN106984271B/en not_active Expired - Fee Related
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 |
|---|
| 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;Beibei Fang等;《RSC Advances》;20151215;第6卷;全文 |
| 水热法合成LiFePO4及其性能研究;张伟;《中国优秀硕士学位论文全文数据库》;20130215(第2期);全文 |
| 活性炭负载铝吸附去除水中氟离子的研究;谌任平等;《三峡环境与生态》;20130731;第35卷(第4期);全文 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106984271A (en) | 2017-07-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107715855B (en) | It is a kind of for organic dyestuff and the porous carbon materials of fluoride wastewater treatment and preparation method thereof | |
| CN107694510B (en) | Method for removing methylene blue in printing and dyeing wastewater by two-dimensional magnetic MXene | |
| JP2018518551A (en) | Porous cyclodextrin polymer material and method for producing and using the same | |
| CN104163479B (en) | A kind of method adopting three-diemsnional electrode to remove nitrate nitrogen in water and device thereof | |
| CN109289884A (en) | A kind of silver-silver orthophosphate-tungstic acid tri compound nano-photocatalyst material and its preparation method and application | |
| CN104492391B (en) | A kind of preparation method of chitosan-modified albumin nanospheres heavy-metal adsorption material | |
| CN109261133A (en) | A kind of ferromagnetism composite balls and its application being easily recycled | |
| CN106311163B (en) | A kind of preparation method of the chitosan of arsenic-adsorbing/iron hydroxide compound adsorbent | |
| CN107321333A (en) | A kind of preparation method for the hydrogel microsphere for adsorbing dye ions | |
| CN107597143A (en) | A kind of metal nanoparticle is uniformly embedded into the controllable method for preparing of the elctro-catalyst of mesoporous carbon spheres internal structure | |
| CN106984271B (en) | For removing the preparation method of the compound adsorbent of Methyl Orange in Wastewater and fluorine ion | |
| CN110115272A (en) | A kind of Cu nanoparticle coupling graphene hydrogel composite material and its preparation method and application | |
| CN114307941B (en) | Aminated surface defect sphalerite material, preparation method and application thereof in degradation of perfluorinated compounds | |
| CN105664879B (en) | Composite adsorption film, preparation method and applications | |
| CN114570406A (en) | Carbon nitride composite photocatalytic material for organic sewage remediation and preparation method thereof | |
| CN107159094B (en) | The method of tetracycline in magnetic magnesium hydroxide adsorbent removal waste water | |
| CN110327896A (en) | A kind of magnetism poly-dopamine/carboxymethyl chitosan adsorbent and the preparation method and application thereof | |
| CN115321657B (en) | Hydrophobic chitosan-polyaluminium chloride Hmcs-PAC composite flocculant and preparation and application thereof | |
| CN103769061B (en) | The synthetic method of a kind of collagen load hyper-branched polyester/metal ion fluoride adsorbent | |
| CN106219666A (en) | A kind of Pt doping In2o3the method of PFOA in photocatalytic degradation water | |
| CN110357223A (en) | A kind of synergistically modified cerium oxide combination electrode of zinc bismuth and its preparation method and application | |
| CN102247810B (en) | Method for surface modification of chitosan and application of chitosan subjected to surface modification | |
| WO2016197397A1 (en) | Preparation method and use of photocatalytic degradation-adsorption material | |
| CN107413169A (en) | A kind of formaldehyde absorbent of the doped nano titanium dioxide containing Ternary copper and preparation method thereof | |
| CN107497394B (en) | A kind of Fe-Mg-La tri compound fluorine ion absorber and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190709 |