CN105921118A - Sodium alginate / hydroxyapatite composite gel with nano-pore structure and preparation method and application thereof - Google Patents
Sodium alginate / hydroxyapatite composite gel with nano-pore structure and preparation method and application thereof Download PDFInfo
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- CN105921118A CN105921118A CN201610209198.3A CN201610209198A CN105921118A CN 105921118 A CN105921118 A CN 105921118A CN 201610209198 A CN201610209198 A CN 201610209198A CN 105921118 A CN105921118 A CN 105921118A
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- sodium alginate
- hydroxyapatite
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- pluralgel
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28014—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
- B01J20/28047—Gels
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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
- B01J20/28078—Pore diameter
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention relates to a preparation method of a sodium alginate / hydroxyapatite composite gel. The method comprises the following steps: 1) dispersing hydroxyapatite in deionized water, adding sodium alginate, and mixing evenly to obtain a sodium alginate / hydroxyapatite suspension; 2) imbibing the suspension from the step 1), and dropwise adding the suspension into a container containing a crosslinking agent under assisted ultrasonic dispersion to obtain the sodium alginate / hydroxyapatite composite gel with nano-pore structure. The invention has the advantages that the sound chemical ultrasonic hole effect is employed to obtain the sodium alginate / hydroxyapatite composite gel with nano-pore structure, so as to improve the adsorption and removal of heavy metal ions in wastewater. The method of the invention does not need an additional pore forming agent, directly uses the micro air bubbles generated by the ultrasonic hole effect to endow the material with nano hole structure, and has the advantages of simple operation, no pollution and low cost.
Description
Technical field
The present invention relates to a kind of method utilizing ultrasonic wave added to prepare sodium alginate/hydroxyapatite pluralgel, obtained sodium alginate/hydroxyapatite pluralgel has nano-pore structure, there is the highest removal of heavy metal ions ability, can be used for sewage disposal, the heavy metal ion in Adsorption water.
Background technology
Along with socioeconomic fast development, the garbage containing heavy metal ion of the discharge such as industrial activity such as process hides, mining, electronics, plating and petrochemical industry is the most appropriately processed the most frequently is just directly discharged in environment, causes serious soil and water pollution.Heavy metal ion exists the most for a long time, will not be metabolized, and the life to people causes lasting harm.Wherein, heavy metal water pollutes especially serious, and the heavy metal ion causing water to pollute mainly has copper, lead, cadmium etc..If heavy metal ion harmful in water body, anion, Organic substance etc. are not effectively treated, it will bring serious ecological problem, the health of people can be caused serious harm.Therefore, the important subject that the method for heavy metal ions in sewage is current sewage disposal is effectively removed in research.
At present, the processing method of heavy metal containing sewage mainly has ion-exchange resin, evaporation concentration method, hyperfiltration, electroosmose process, chemical precipitation method, electrolysis, solvent extraction, membrane separation process, active carbon adsorption etc..These method great majority have its limitation, as evaporation and concentration send out, ion-exchange resin and activated carbon method cost high, chemical precipitation method is not suitable for the removal of heavy metal ion under low concentration and can produce time primary sludge etc..By comparison, absorption method has to the removal of heavy metal ions in sewage that adsorbance is big, efficiency is high, speed is fast and the feature such as easy and simple to handle is widely used, and becomes a kind of important method processing heavy metal ion.
Hydroxyapatite and sodium alginate all have the ability of heavy metal ion in excellent removal water, both compositions the pluralgel adsorbent being mixed with out has had both features concurrently.The removal ability of its heavy metal ion is in addition to having much relations with two kinds of component contents, its absorbability also can be had a huge impact by the microstructure (such as biphase dispersity, pore structure) of pluralgel, particularly having the adsorbent of nano-pore structure, heavy metal ion shows higher absorbability.Therefore the pore structure regulating and controlling pluralgel is also the effective way improving its absorbability.
Summary of the invention
The technical problem to be solved be obtain biphase uniform mixing, scattered on the basis of, the nanorize of pluralgel pore structure is achieved by ultrasonic void effect, the obtained sodium alginate with nano-pore structure/hydroxyapatite pluralgel can be as a kind of removal of heavy metal ions agent, for sewage disposal.
The present invention is adopted the technical scheme that to realize above-mentioned target: has the preparation method of the sodium alginate/hydroxyapatite pluralgel of nano-pore structure, comprises the following steps:
1) hydroxyapatite is scattered in deionized water, adds sodium alginate, mix homogeneously, obtain sodium alginate/hydroxyapatite suspensions；
2) aspiration step 1) in the suspension that obtains, under ultrasonic disperse assists, be added drop-wise to fill in the container of cross-linking agent, obtain the Na-alginate/hydroxyapatite pluralgel with nano-pore structure.
By such scheme, the preparation method of described hydroxyapatite is: according to mol ratio Ca/P=1.67, ammonium dibasic phosphate aqueous solution is poured into rapidly in the aqueous solution of calcium nitrate at 80 DEG C, and to mixed solution and dripping ammonia, it is uniformly mixed, after reacting 1 hour, is centrifuged and is precipitated thing, after deionized water rinsing 3 times, it is re-dispersed in water.
By such scheme, dropping ammonia controls the pH value 10-11 of solution.
Being 1:4-1:1 by the mass ratio of such scheme, hydroxyapatite and sodium alginate, the concentration of sodium alginate/hydroxyapatite suspensions is 0.00167-0.00668g/mL.
By such scheme, step 2) ratio between volume aspirated and the cross-linking agent volume of described sodium alginate/hydroxyapatite mixture is 1:50-1:100.
By such scheme, described cross-linking agent be mass fraction be calcium chloride solution and the mixed solution of dehydrated alcohol of 5%, its volume ratio is 4:1.
By such scheme, step 2) in ultrasonic time be 4 minutes.
The sodium alginate with the nano-pore structure/hydroxyapatite pluralgel of above-mentioned any preparation method gained.
By such scheme, described pluralgel is three-dimensional through network structure, and on it, nanoporous size is 10-80nm.
The described sodium alginate with nano-pore structure/hydroxyapatite pluralgel is as adsorbent for heavy metal application in sewage disposal.
The invention have the advantage that and utilize the ultrasonic void effect of sonochemistry, obtain the sodium alginate/hydroxyapatite pluralgel with nano-pore structure, the ability of its Adsorption heavy metal ions in sewage can be improved.The method of the present invention is not required to additional pore former, directly utilizes the micro-bubble imparting material nano pore structure that ultrasonic void effect produces, has operating procedure simple, and process is pollution-free, feature with low cost.
Detailed description of the invention
Below by embodiment, the present invention is described in more detail, but this explanation will not be construed as limiting the invention.
Embodiment 1
First, preparing calcium nitrate aqueous solution, concentration is 0.0334mol/L；Preparation ammonium dibasic phosphate aqueous solution, concentration is 0.02mol/L；According to mol ratio Ca/P=1.67, at 80 DEG C, 100mL ammonium dibasic phosphate aqueous solution is poured into rapidly in 100mL calcium nitrate aqueous solution, and to mixed solution and dripping ammonia, control pH value of solution is 10-11, it is uniformly mixed, after maintaining reaction temperature to be 80 DEG C of reaction 1h, is centrifuged and obtains white depositions, after deionized water rinsing 3 times, it is re-dispersed in 200mL deionized water.Then by the mass ratio of hydroxyapatite and sodium alginate be 1:1 add sodium alginate, at 80 DEG C stir, after being sufficiently mixed, the concentration obtaining sodium alginate/hydroxyapatite mixture is 0.00167g/mL.0.5mL sodium alginate/hydroxyapatite mixture is drawn with liquid-transfering gun, under high-energy ultrasonic Probe Ultrasonic Searching dispersion assosting effect, instilling 50mL mass fraction is in the calcium chloride of 5% and the mixed cross-linker (volume ratio is 4:1) of ethanol, obtain sodium alginate/hydroxyapatite pluralgel, supersound process 4 minutes.Scanning electron microscopic observation shows, pluralgel has the hole of 10-60nm, presents three-dimensional through network structure.Being placed in by the pluralgel of acquisition in copper ion aqueous solution (400mg/L), concussion absorption 1 hour under room temperature, the adsorbance to copper ion is 1.4g/g.
Embodiment 2
First, preparing calcium nitrate aqueous solution, concentration is 0.0334mol/L；Preparation ammonium dibasic phosphate aqueous solution, concentration is 0.02mol/L；According to mol ratio Ca/P=1.67, at 80 DEG C, 100mL ammonium dibasic phosphate aqueous solution is poured into rapidly in 100mL calcium nitrate aqueous solution, and to mixed solution and dripping ammonia, control pH value of solution is 10-11, it is uniformly mixed, after maintaining reaction temperature to be 80 DEG C of reaction 1h, is centrifuged and obtains white depositions, after deionized water rinsing 3 times, it is re-dispersed in 200mL deionized water.Then by the mass ratio of hydroxyapatite and sodium alginate be 1:4 add sodium alginate, at 80 DEG C stir, after being sufficiently mixed, the concentration obtaining sodium alginate/hydroxyapatite mixture is 0.00668g/mL.1.0mL sodium alginate/hydroxyapatite mixture is drawn with liquid-transfering gun, under high-energy ultrasonic Probe Ultrasonic Searching dispersion assosting effect, instilling 50mL mass fraction is in the calcium chloride of 5% and the mixed cross-linker (volume ratio is 4:1) of ethanol, obtain sodium alginate/hydroxyapatite pluralgel, supersound process 4 minutes.Scanning electron microscopic observation shows, pluralgel has the hole of 20-80nm, presents three-dimensional through network structure.Being placed in by the pluralgel of acquisition in copper ion aqueous solution (400mg/L), concussion absorption 1 hour under room temperature, the adsorbance to copper ion is 1.2g/g.
Claims (10)
1. there is the preparation method of the sodium alginate/hydroxyapatite pluralgel of nano-pore structure, comprise the following steps:
1) hydroxyapatite is scattered in deionized water, adds sodium alginate, mix homogeneously, obtain sodium alginate/hydroxyl phosphorus
Lime stone suspension；
2) aspiration step 1) in the suspension that obtains, under ultrasonic disperse assists, be added drop-wise to fill in the container of cross-linking agent,
To the Na-alginate/hydroxyapatite pluralgel with nano-pore structure.
2. the preparation method of the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel as described in claim 1, its
The preparation method being characterised by described hydroxyapatite is: according to mol ratio Ca/P=1.67, by phosphoric acid hydrogen two at 80 DEG C
Aqueous ammonium is poured into rapidly in the aqueous solution of calcium nitrate, and to mixed solution and dripping ammonia, is uniformly mixed, and reaction 1 is little
Shi Hou, is centrifuged and is precipitated thing, after deionized water rinsing 3 times, be re-dispersed in water.
3. the preparation method of the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel as described in claim 2, its
It is characterised by that dripping ammonia controls the pH value 10-11 of solution.
4. the preparation method of the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel as described in claim 1, its
The mass ratio being characterised by hydroxyapatite and sodium alginate is 1:4-1:1, and the concentration of sodium alginate/hydroxyapatite suspensions is
0.00167-0.00668g/mL。
5. the preparation method of the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel as described in claim 1, its
It being characterised by step 2) ratio between volume aspirated and the cross-linking agent volume of described sodium alginate/hydroxyapatite mixture is 1:
50-1:100.
6. the preparation method of the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel as described in claim 1, its
The cross-linking agent being characterised by described be mass fraction be calcium chloride solution and the mixed solution of dehydrated alcohol of 5%, its volume ratio is
4:1。
7. the preparation method of the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel as described in claim 1, its
Be characterised by step 2) in ultrasonic time be 4 minutes.
8. the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel of any preparation method of claim 1-7 gained.
9. the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel as described in claim 8, it is characterised in that institute
The pluralgel stated is three-dimensional through network structure, and on it, nanoporous size is 10-80nm.
10. the sodium alginate with the nano-pore structure/hydroxyapatite pluralgel described in claim 8 is as heavy metal ion
Adsorbent application in sewage disposal.
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Cited By (9)
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| CN109012622A (en) * | 2018-09-27 | 2018-12-18 | 天津理工大学 | A kind of preparation method and application of the porous composite adsorbing material of nanometer hydroxyapatite/sodium alginate |
| CN109174027A (en) * | 2018-09-19 | 2019-01-11 | 重庆大学 | The preparation method of the fixed aluminium pillared bentonite adsorbent of sodium alginate and its method for adsorbing phosphate radical |
| US20190329217A1 (en) * | 2018-04-27 | 2019-10-31 | Washington University | Engineered calcium alginate and uses thereof |
| CN111217598A (en) * | 2018-11-27 | 2020-06-02 | 中国科学院大连化学物理研究所 | Hydroxyapatite forming method, hydroxyapatite and application |
| CN113171753A (en) * | 2021-04-27 | 2021-07-27 | 西南科技大学 | Preparation of sodium alginate-zirconium phosphate composite beads and adsorption application of sodium alginate-zirconium phosphate composite beads in nuclear waste liquid |
| CN113332960A (en) * | 2021-03-23 | 2021-09-03 | 中南大学 | Supported apatite composite adsorption material and preparation method and application thereof |
| CN113388151A (en) * | 2021-07-16 | 2021-09-14 | 浙江理工大学 | Preparation method of nano cellulose fiber-sodium alginate-hydroxyapatite flame-retardant aerogel |
| CN114307994A (en) * | 2022-01-17 | 2022-04-12 | 郑州大学 | Preparation method and application of hydrogel adsorbent for Au (III) recovery |
| CN115254042A (en) * | 2022-07-26 | 2022-11-01 | 青岛农业大学 | Preparation and application of modified sodium alginate composite ball for removing heavy metal ions in water |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190329217A1 (en) * | 2018-04-27 | 2019-10-31 | Washington University | Engineered calcium alginate and uses thereof |
| CN109174027A (en) * | 2018-09-19 | 2019-01-11 | 重庆大学 | The preparation method of the fixed aluminium pillared bentonite adsorbent of sodium alginate and its method for adsorbing phosphate radical |
| CN109012622A (en) * | 2018-09-27 | 2018-12-18 | 天津理工大学 | A kind of preparation method and application of the porous composite adsorbing material of nanometer hydroxyapatite/sodium alginate |
| CN111217598A (en) * | 2018-11-27 | 2020-06-02 | 中国科学院大连化学物理研究所 | Hydroxyapatite forming method, hydroxyapatite and application |
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| CN113332960A (en) * | 2021-03-23 | 2021-09-03 | 中南大学 | Supported apatite composite adsorption material and preparation method and application thereof |
| CN113171753A (en) * | 2021-04-27 | 2021-07-27 | 西南科技大学 | Preparation of sodium alginate-zirconium phosphate composite beads and adsorption application of sodium alginate-zirconium phosphate composite beads in nuclear waste liquid |
| CN113171753B (en) * | 2021-04-27 | 2022-01-28 | 西南科技大学 | Preparation of sodium alginate-zirconium phosphate composite beads and adsorption application of sodium alginate-zirconium phosphate composite beads in nuclear waste liquid |
| CN113388151A (en) * | 2021-07-16 | 2021-09-14 | 浙江理工大学 | Preparation method of nano cellulose fiber-sodium alginate-hydroxyapatite flame-retardant aerogel |
| CN114307994A (en) * | 2022-01-17 | 2022-04-12 | 郑州大学 | Preparation method and application of hydrogel adsorbent for Au (III) recovery |
| CN115254042A (en) * | 2022-07-26 | 2022-11-01 | 青岛农业大学 | Preparation and application of modified sodium alginate composite ball for removing heavy metal ions in water |
| CN115254042B (en) * | 2022-07-26 | 2024-03-01 | 青岛农业大学 | Preparation and application of modified sodium alginate composite ball for removing heavy metal ions in water |
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