CN108380175B - A kind of carbonic acid gas lanthanum-halloysite composite material and its preparation method and application - Google Patents
A kind of carbonic acid gas lanthanum-halloysite composite material and its preparation method and application Download PDFInfo
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- CN108380175B CN108380175B CN201810165746.6A CN201810165746A CN108380175B CN 108380175 B CN108380175 B CN 108380175B CN 201810165746 A CN201810165746 A CN 201810165746A CN 108380175 B CN108380175 B CN 108380175B
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0207—Compounds of Sc, Y or Lanthanides
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
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- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
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- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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Abstract
The invention discloses a kind of carbonic acid gas lanthanum-halloysite composite materials and its preparation method and application.The present invention uniformly mixes natural nano tubulose galapectite mineral with carbonic acid gas lanthanum precursor solution, the composite material of the uniform load carbonic acid gas lanthanum inside and outside halloysite nanotubes is prepared with the methods of low-temperature burning by vacuumizing, both the meso-hole structure of galapectite had been remained, its inner cavity is not blocked again, 100mgP/g is up to the saturated extent of adsorption of phosphate anion, can be used for adsorbing phosphate anion or is used to prepare dephosphorization adsorbent.The preparation method of composite material of the present invention also has many advantages, such as that low energy consumption, easy to operate, short preparation period, has a good application prospect.
Description
Technical field
The invention belongs to technical field of environmental pollution treatment, it is more particularly related to a kind of for adsorbing phosphate radical
Carbonic acid gas lanthanum-halloysite composite material of ion and its preparation method and application.
Background technique
Lanthanum is the common adsorbent for repairing eutrophication water, principle be mainly in water phosphate radical given birth in conjunction with lanthanum
At the lanthanum orthophosphate for being insoluble in water, by phosphate radical from water body fast eliminating.It is most at present to contain lanthanum since lanthanum nano particle is easy to reunite
Adsorbent material is that lanthanum is carried in carrier, to reduce lanthanum nanoparticle agglomerates, strengthens its contact and absorption to phosphate radical.
Diameter of carrier is small, and porosity is big, is conducive to lanthanum-containing materials with nanoscale in its area load, therefore carrier material characteristic (including
Partial size, pore structure and its physicochemical properties etc.) it will affect the load of lanthanum nano particle, and then adsorbent material containing lanthanum is influenced to dirt
Contaminate the absorption of object.The research about lanthanum support materials absorption phosphate radical makes important progress at present.
Such as Chinese patent (application number CN201510721249.6) is using biomass anion exchange resin as carrier, at it
Upper load nano lanthanum oxide forms biomass-based nano lanthanum oxide dephosphorization compound adsorbent；In addition, there is document report with zeolite, life
Object carbon, expanded graphite, Coaseries kaolin are carrier, and lanthanum oxide-carrying or lanthanum hydroxide are as dephosphorization adsorbent.However, above inhale
Attached dose lower to the adsorbance of phosphorus, is below 70mg P/g adsorbent.The main reason for phosphorus adsorbance is low include: charcoal,
Mostly in micro-meter scale, these carrier dimensions are excessive to be unfavorable for surface lanthanum and phosphoric acid piece-root grafting for expanded graphite and Coaseries kaolin etc.
Touching；Furthermore zeolite is microcellular structure, and lanthanum load is easy blocking duct, hinders absorption of the lanthanum to phosphate radical.Therefore it is badly in need of lanthanum-carried
Afterwards with the adsorbing agent carrier of higher phosphorous adsorbance.
Galapectite is nanotube-shaped aluminosilicate mineral material, and outstanding feature is in nanoscale, and has special Jie
Hole and hollow tubular structure.In addition, galapectite is cheap compared with the materials such as zeolite and active carbon, it to be used for Phosphateadsorption
Cost is relatively low.It is mainly used for medicament slow release and gas catalytic field currently as the galapectite of carrier, but in Phosphateadsorption side
Face has not been reported.
Summary of the invention
It is an object of the invention to: for the above-mentioned existing supported porous material of lanthanum deficiency present in making and using,
A kind of carbonic acid gas lanthanum-halloysite composite material and its preparation method and application is provided.
In order to achieve the above-mentioned object of the invention, the present invention provides a kind of preparation sides of carbonic acid gas lanthanum-halloysite composite material
Method comprising following steps:
S1, galapectite is added in carbonic acid gas lanthanum precursor solution, ultrasound obtains galapectite and carbonic acid gas lanthanum presoma
The suspension of solution；The carbonic acid gas lanthanum precursor solution is by lanthanum nitrate hexahydrate, glycine and water according to 1~5:1:3~25
Mass ratio mix；The ratio of the volume of the quality of the galapectite and the carbonic acid gas lanthanum precursor solution is 100~
1000:1；
S2, the suspension is vacuumized, is dried, obtaining drying sample；
S3, the drying sample is placed in tube furnace, under nitrogen atmosphere, 250~450 DEG C of 1~3h of reaction, obtains carbonic acid
Oxygen lanthanum-halloysite composite material.
Cardinal principle of the invention is: by vacuumizing, high concentration lanthanum nitrate and glycine solution being made to be filled in Ai Luo
In stone nanotube；After material is dry, react combustion adjuvant glycine and lanthanum nitrate using combustion method, synthesize lanthanum nano thin-film and
Grain.A large amount of nitrogen are generated in reaction, and to be conducive to carbonic acid gas lanthanum evenly dispersed inside and outside galapectite pipe；It is enriched in addition, galapectite has
Aluminium hydroxyl and silicone hydroxyl, with lanthanum pipe surfaces externally and internally formed Si/Al-O-La key, be conducive to carbonic acid gas lanthanum nano material in pipe
It is uniformly distributed outside.Therefore, that galapectite composite adsorbing material had both remained halloysite nanotubes to the carbonic acid gas lanthanum-prepared was unique
Mesoporous framework again can inside and outside pipe uniform load carbonic acid gas lanthanum nano thin-film and particle.
A kind of optimal technical scheme of preparation method as carbonic acid gas lanthanum-halloysite composite material of the present invention, described angstrom
The purity of Lip river stone is greater than 80%.
A kind of optimal technical scheme of preparation method as carbonic acid gas lanthanum-halloysite composite material of the present invention is described super
The time of sound is 10~30min.
A kind of optimal technical scheme of preparation method as carbonic acid gas lanthanum-halloysite composite material of the present invention, the pumping
Vacuum time is 10~30min, and is repeated 3~5 times.
A kind of optimal technical scheme of preparation method as carbonic acid gas lanthanum-halloysite composite material of the present invention, the baking
Dry is 1~5h of drying at 80~150 DEG C.
A kind of optimal technical scheme of preparation method as carbonic acid gas lanthanum-halloysite composite material of the present invention, the nitrogen
The flow velocity of gas is 100~200ml/min.
The present invention also provides a kind of carbonic acid gas lanthanum-halloysite composite materials, are prepared by above-mentioned preparation method
It arrives.
It is verified by experiments, carbonic acid gas lanthanum-halloysite composite material of the present invention is to the absorption with higher of phosphate radical pollutant
Amount, at room temperature its to the saturated extent of adsorption of phosphate radical up to 100mgP/g or more, therefore, carbonic acid gas lanthanum-galapectite of the present invention
Composite material can be used for adsorbing phosphate anion, or be used to prepare dephosphorization adsorbent.
Compared with the existing technology, the invention has the advantages that and the utility model has the advantages that
(1) present invention makes full use of the unique mesoporous hollow tubular structure of galapectite, is received by vacuumizing to fill in pipe
For rice carbonic acid gas lanthanum without blocking inner tube, this is conducive to pollutant diffusion and mass transfer.In addition, the present invention makes full use of galapectite surface rich
The silicone hydroxyl and aluminium hydroxyl contained makes itself and lanthanum generate chemical bond, and loading inside and outside galapectite pipe of lanthanum is allowed to be optimized.
(2) present invention when uniform load carbonic acid gas lanthanum, using combustion process for preparing, utilizes nitric acid inside and outside halloysite nanotubes
Lanthanum and glycine under lower maturing temperature (250~450 DEG C) react, and obtain carbonic acid gas lanthanum-galapectite composite adsorption material
Material.The advantages such as the preparation method has simple process, and the reaction time is short advantageously reduce the manufacturing cycle of material and reduce production
Energy consumption.
(3) the carbonic acid gas lanthanum-galapectite composite adsorbing material prepared by the method for the invention, since lanthanum is in galapectite pipe
With the uniform load outside pipe, carbonic acid gas lanthanum-galapectite composite adsorbing material has higher adsorbance to phosphorus, under room temperature,
100mgP/g adsorbent or more is reached to the adsorbance of phosphorus.
Detailed description of the invention
Fig. 1 is carbonic acid gas lanthanum-galapectite composite adsorbing material X-ray diffractogram in the embodiment of the present invention 1.
Fig. 2 is carbonic acid gas lanthanum-galapectite composite adsorbing material transmission electron microscope picture in the embodiment of the present invention 2.
Fig. 3 is carbonic acid gas lanthanum-galapectite composite adsorbing material phosphorus adsorption isotherm in the embodiment of the present invention 3.
Specific embodiment
In order to be more clear the purpose of the present invention, technical solution and advantageous effects, with reference to embodiments, to this
Invention is further elaborated.It should be understood that embodiment described in this specification is just for the sake of this hair of explanation
It is bright, be not intended to limit the present invention, parameter, ratio of embodiment etc. can adaptation to local conditions make a choice and substance had no to result
It influences.It in embodiment unless otherwise specified, is this field conventional reagent and method and step.
Embodiment 1
1) 10g galapectite is mixed with 10g lanthanum nitrate hexahydrate and 2g glycine, 50ml deionized water, ultrasound is added
10min。
2) gained suspension in step 1) is placed in 500mL bottle,suction and vacuumizes 10min, be repeated 3 times, it then will be suspended
Liquid is placed in baking oven, is dried 2 hours under the conditions of 80 DEG C, is obtained drying sample.
3) gained drying sample in step 2) is placed in tube furnace, 30min is purged for the nitrogen of 100ml/min with flow velocity
Afterwards, constant temperature 2h under the conditions of 300 DEG C, obtains carbonic acid gas lanthanum-halloysite composite material.
Gained carbonic acid gas lanthanum-halloysite composite material structure is measured using X-ray diffraction (XRD), as a result table
It is bright, occur belonging to the characteristic diffraction peak of carbonic acid gas lanthanum in X ray diffracting spectrum (Fig. 1).
Carbonic acid gas lanthanum-halloysite composite material phosphorus adsorption capacity is tested using batch adsorption experiment, as a result
Show under room temperature, is 135mgP/g adsorbent to Phosphateadsorption amount.
Embodiment 2
1) 20g galapectite is mixed with 15g lanthanum nitrate hexahydrate and 15g glycine, 50ml deionized water, ultrasound is added
20min。
2) gained suspension in step 1) is placed in 500mL bottle,suction and vacuumizes 15min, be repeated 3 times, it then will be suspended
Liquid is placed in baking oven, is dried 5 hours under the conditions of 120 DEG C, is obtained drying sample.
3) gained drying sample in step 2) is placed in tube furnace, 30min is purged for the nitrogen of 150ml/min with flow velocity
Afterwards, constant temperature 2h under the conditions of 400 DEG C, obtains carbonic acid gas lanthanum-halloysite composite material.
Find that carbonic acid gas lanthanum is in galapectite inner and outer pipes uniform load (Fig. 2) by transmission electron microscope (TEM) analysis.Using batch
Secondary adsorption experiment tests carbonic acid gas lanthanum-halloysite composite material phosphorus adsorption capacity, is to Phosphateadsorption amount
125mgP/g adsorbent.
Embodiment 3
1) 30g galapectite is mixed with 18g lanthanum nitrate hexahydrate and 9g glycine, 30ml deionized water, ultrasound is added
30min。
2) gained suspension in step 1) is placed in 250mL bottle,suction and vacuumizes 30min, be repeated 3 times, it then will be suspended
Liquid is placed in baking oven, is dried 4 hours under the conditions of 130 DEG C, is obtained drying sample.
3) obtained solid in step 2) is placed in tube furnace, nitrogen flow rate 160ml/min, after nitrogen protection 30min,
Constant temperature 2h under the conditions of 450 DEG C takes out sample, obtains carbonic acid gas lanthanum-halloysite composite material after tube furnace is cooling.
Carbonic acid gas lanthanum-halloysite composite material phosphorus adsorption capacity is tested using batch adsorption experiment, it is right
Phosphateadsorption amount is 120mgP/g adsorbent (Fig. 3).
The announcement and guidance of book according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula carries out change and modification appropriate.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to this
Some modifications and changes of invention should also be as falling into the scope of the claims of the present invention.In addition, although this specification
In use some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (9)
1. a kind of preparation method of carbonic acid gas lanthanum-halloysite composite material, which comprises the steps of:
S1, galapectite is added in carbonic acid gas lanthanum precursor solution, ultrasound obtains galapectite and carbonic acid gas lanthanum precursor solution
Suspension；The carbonic acid gas lanthanum precursor solution is the matter by lanthanum nitrate hexahydrate, glycine and water according to 1~5:1:3~25
Amount ratio mixes；The ratio of the quality of the galapectite and the volume of the carbonic acid gas lanthanum precursor solution is 100~1000:1；
S2, the suspension is vacuumized, is dried, obtaining drying sample；
S3, the drying sample is placed in tube furnace, under nitrogen atmosphere, 250~450 DEG C of 1~3h of reaction, obtains carbonic acid gas
Lanthanum-halloysite composite material.
2. the preparation method of carbonic acid gas lanthanum-halloysite composite material according to claim 1, which is characterized in that described angstrom
The purity of Lip river stone is greater than 80%.
3. the preparation method of carbonic acid gas lanthanum-halloysite composite material according to claim 1, which is characterized in that described super
The time of sound is 10~30min.
4. the preparation method of carbonic acid gas lanthanum-halloysite composite material according to claim 1, which is characterized in that the pumping
Vacuum time is 10~30min, and is repeated 3~5 times.
5. the preparation method of carbonic acid gas lanthanum-halloysite composite material according to claim 1, which is characterized in that the baking
Dry is 1~5h of drying at 80~150 DEG C.
6. the preparation method of carbonic acid gas lanthanum-halloysite composite material according to claim 1, which is characterized in that the nitrogen
The flow velocity of gas is 100~200mL/min.
7. a kind of carbonic acid gas lanthanum-halloysite composite material, which is characterized in that it is by any one power in claim 1~6
Benefit requires the preparation method of the carbonic acid gas lanthanum-halloysite composite material to be prepared.
8. application of the lanthanum of carbonic acid gas described in the claim 7-halloysite composite material in absorption phosphate anion.
9. the lanthanum of carbonic acid gas described in claim 7-halloysite composite material is preparing the application in dephosphorization adsorbent.
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| CN111744454A (en) * | 2020-06-02 | 2020-10-09 | 河北科技师范学院 | Preparation method of composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite |
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| CN113797950B (en) * | 2020-06-17 | 2023-11-14 | 中国石油化工股份有限公司 | Catalyst with low-temperature activity in methane oxidative coupling reaction, and preparation method and application thereof |
| CN112675810B (en) * | 2020-12-02 | 2022-10-11 | 哈尔滨工业大学 | Amorphous high-efficiency phosphorus removal adsorption material, preparation method and water treatment application thereof |
| CN113041992B (en) * | 2021-04-08 | 2022-07-26 | 中国科学院地球化学研究所 | Halloysite-based efficient adsorbent for removing radioactive I-and preparation method thereof |
| CN114100561B (en) * | 2021-12-01 | 2023-05-02 | 中国科学院生态环境研究中心 | Metal modified La 2 O 2 CO 3 Adsorbent, and preparation method and application thereof |
| CN114653341A (en) * | 2022-04-12 | 2022-06-24 | 四川文理学院 | Modified tea residue biochar, preparation method and application thereof |
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