CN109174066A - A kind of preparation method of nano lanthanum oxide de-fluoridation adsorbent - Google Patents
A kind of preparation method of nano lanthanum oxide de-fluoridation adsorbent Download PDFInfo
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- CN109174066A CN109174066A CN201811293478.2A CN201811293478A CN109174066A CN 109174066 A CN109174066 A CN 109174066A CN 201811293478 A CN201811293478 A CN 201811293478A CN 109174066 A CN109174066 A CN 109174066A
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- lanthanum
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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
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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
- B01J20/28002—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 physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
Abstract
The present invention relates to a kind of Nano-lanthanum hydroxide de-fluoridation adsorbent and preparation method thereof, method includes the following steps: 1, reactor vessel is placed in 10 ~ 35 DEG C of ice water, deionized water is added into reactor vessel;2, it takes lanthanum nitrate solid powder to be added into deionized water described in step 1, is stirred dissolution with blender;3, after lanthanum nitrate dissolution, it is slowly added to sodium hydroxide solution, adjusts pH to 8.5-9.0;At this time;4, the solution that step 3 is prepared is rinsed repeatedly with deionized water;5, the slurries for washing step 4, are dehydrated with centrifuge, are then dried;6, grinding screening obtains lanthanum hydroxide dry powder;7, lanthanum hydroxide dry powder is mixed with microcrystalline cellulose, hypromellose b, is granulated through wet granulator and spheronizator.The preparation process of the defluorinating agent is simple, and obtained product absorption fluorine ion is more efficient, and the regeneration period is longer.
Description
The invention belongs to technical field of waste water processing, and in particular to a kind of Nano-lanthanum hydroxide de-fluoridation adsorbent and its preparation
Method.
Background technique
" endemia fluorosis " is to compare typical location property fluorine poisoning disease, is that one, environmental geochemistry field is more popular
One research topic.
Fluorine is a kind of essential micronutrient element of human body, is the chemical substance for participating in human homergy, can be with
The calcification for promoting tooth and bone, mould all the having certain effect of conduction and participation metabolism for nervous excitation.But human body
After taking in excessive fluorine, fluorine poisoning will occur, cause the lesion of tooth and bone to lead to " fluorosis of bone " and " den tal fluorosis ", seriously
The deformation of person's four limbs, spinal curvature, muscular atrophy and paralysis, can also cause the diseases such as anaemia.
" endemia fluorosis " is exactly one of more universal with the exceeded related fluorine poisoning disease of underground water fluoride, this disease
Disease can cause human body greatly to injure.In addition, reduction is answered there are also studies have shown that fluorine can influence the normal activity of nervous centralis
Swash property, and can lessen one's memory, lassitude is easy to fatigue, cause insomnia etc..So Drinking Water in China standard
(GB5749-85) and in groundwater quality standard (GB/T14848-93) it provides, the fluorine content in drinking water must not exceed
1.0mg/L, suitable concentration are 0.5~1.0mg/L.Currently, fluorine lesion population in China spreads 27, the whole nation up to more than 7,200 ten thousand people
Provinces, municipalities and autonomous regions.In addition to underground water fluoride content is exceeded, the industries such as semiconductor, LED can also be produced due to the needs of circuit-board processes
Raw a large amount of fluorine-containing industrial wastewater.In order to solve the fluorine ion excessive problem in waste water, it has been proposed that and practiced a variety of fluorine from
The processing method of several frequently seen fluoride waste is described below in subprocessing method:
1, chemical precipitation method
Coagulant sedimentation mainly passes through adds Polyferric Sulfate, aluminum sulfate or lime in water, so that it is generated fluoride precipitating, then leads to
The methods of filtering or sedimentation, are separated from water sediment, to achieve the purpose that fluorine removal.But it is handled by coagulant sedimentation
Effect it is unstable, especially underground water may cause the exceeded phenomenon of water outlet aluminium, iron.
Flocculation sedimentation processing cost is larger, and generation sludge quantity is more, and fluoride ion removing effect is by stirring condition, sedimentation time etc.
SO in operation factors and water4 2-、Cl-Equal anion effects are big, and effluent quality is not sufficiently stable.
2, film process
In order to solve environment friendly and economy.In recent years, reverse osmosis membrane technology of Fluoride Removal is using relatively broad, it mainly by
In pressure more higher than osmotic pressure, change natural direction the solvent of concentrated solution is pressed to semi-transparent coating solution on one side, to reach
The purpose of substance separation.But reverse osmosis operation, cost of investment are high, in addition requirement of the film process for influent quality is compared
Height, operation difficulty are larger.
Additionally need periodically carry out film replacement but reverse osmosis technology since cost of investment, operating cost are higher,
3, ion-exchange
Ion-exchange is by the way that exchange interaction occurs using the polluted heavy metals ion in ion exchange resin and water body, weight
Metal is cemented out from water body, and then achievees the purpose that removal.
At present there are various defects in the treatment process of fluoride waste, this technology solves conventional adsorbent suction
Attached capacity is low, regenerates difficult problem, while this technology operation is easy, and raw material cost is low, and absorption is stablized, and will not make to water body
At secondary pollution.
4, traditional absorption method
Traditional absorbent filter medium includes active carbon, activated alumina etc., but the drawbacks of traditional filtrate is, filtrate adsorption capacity is small,
Treatment effeciency is low, the processing time is long;Exchange capacity declines after some media regenerations, reuses ineffective.
Therefore, need that a kind of adsorption efficiency is higher, regeneration period longer fluorine ion absorber and preparation method thereof, with
Fluorine ion absorption in waste water.
Summary of the invention
The object of the present invention is to provide a kind of Nano-lanthanum hydroxide de-fluoridation adsorbent and preparation method thereof, the systems of the defluorinating agent
Standby simple process, obtained product absorption fluorine ion is more efficient, and the regeneration period is longer, solves existing in the prior art ask
Topic.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of preparation method of Nano-lanthanum hydroxide de-fluoridation adsorbent, comprising the following steps:
Step 1: reactor vessel is placed in 10 ~ 35 DEG C of ice water, deionized water is added into reactor vessel;
Step 2: lanthanum nitrate solid powder is taken to be added into deionized water described in step 1, dissolution is stirred with blender;
Step 3: being slowly added to sodium hydroxide solution after lanthanum nitrate dissolution, pH to 8.5-9.0 is adjusted;At this point, low temperature deionization
Water: lanthanum nitrate: the mass ratio of sodium hydroxide is (5-7): (2-4): (0.4-1);
Step 4: being rinsed the solution that step 3 is prepared repeatedly to conductivity with deionized water in 1 ms/cm or less;
Step 5: the slurries that step 4 is washed, are dehydrated with centrifuge, are then dried at 60-90 DEG C using baking oven
It is dry;
Step 6: grinding and passing through the sieve screening of 10-100 mesh, lanthanum hydroxide dry powder is obtained;
Step 7: lanthanum hydroxide dry powder is mixed with microcrystalline cellulose, hypromellose b, through wet granulator and round as a ball
Machine is granulated, wherein lanthanum hydroxide: microcrystalline cellulose: the mass ratio of hypromellose is (4-5): (1-3): (2-
4).
Further, the grain diameter after step 7 is granulated is 1.8 ~ 2.5mm.
According to Nano-lanthanum hydroxide de-fluoridation adsorbent obtained by above-mentioned preparation method.
Compared with prior art, beneficial effects of the present invention are as follows:
(1) de-fluoridation adsorbent of the invention environmental protection: the fluorine after absorption secondary will not be revealed, and filtrate itself is not soluble in water, will not be right
Water outlet causes secondary pollution.
(2) de-fluoridation adsorbent long service life of the invention: Performances of Novel Nano-Porous meter level adsorbent material has very strong absorption regeneration
Can, pass through the regeneration of regenerated liquid.
(3) de-fluoridation adsorbent stability of the invention is high: since nano material activity is strong, large specific surface area, and this fluorine removal material
Adsorption capacity is stablized after material repeatedly regenerates, and does not reduce substantially.
(4) de-fluoridation adsorbent of the invention use, regeneration technology are simple: the application of this material engineering is easy, it can be achieved that entirely certainly
Dynamicization operation, in addition, this material only needs a kind of neutral regenerated liquid progress regeneration technology simple.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) photograph (SEM) photo that nanometer fluorine ion absorber is made in the embodiment of the present invention 1.
Fig. 2 is transmission electron microscope (TEM) figure that nanometer fluorine ion absorber is made in the embodiment of the present invention 1.
Fig. 3 is energy disperse spectroscopy (EDS) figure that nanometer fluorine ion absorber is made in the embodiment of the present invention 1.
Fig. 4 is the X-ray diffraction (XRD) figure that nanometer fluorine ion absorber is made in the embodiment of the present invention 1.
Fig. 5 is the experimental data figure that nanometer fluorine ion absorber is made in the embodiment of the present invention 1.
Specific embodiment
The present invention is described in further detail with specific implementation example with reference to the accompanying drawing, but protection model of the invention
Enclose be not limited to it is as described below:
Several specific embodiments of the invention are described below:
Embodiment 1
Reactor vessel is placed in 10 DEG C of ice water by step 1, and deionized water is added into reactor vessel;
130g lanthanum nitrate solid powder is added into above-mentioned low temperature deionized water step 2, is stirred dissolution with blender;
After step 3, dissolution, it is slowly added to sodium hydroxide solution, adjusts pH to 8.5;At this point, water: lanthanum nitrate: the matter of sodium hydroxide
Amount is than being 5:2:0.4;
Step 4 is rinsed step 3 preparation solution repeatedly to conductivity in 1 ms/cm or less with deionized water;
Step 5, the slurries for washing step 4, are dehydrated with centrifuge, are dried at 90 DEG C using baking oven;
Step 6, grinding, and screened by the sieve of 100 mesh, obtain lanthanum hydroxide dry powder;
Step 7 mixes lanthanum hydroxide dry powder with microcrystalline cellulose, hypromellose, through wet granulator and round as a ball
Machine is granulated, wherein lanthanum hydroxide: microcrystalline cellulose: the mass ratio of hypromellose is 4:1:2
Finally grain diameter obtained is 1.6 ~ 2.0mm to above-mentioned steps.
The present embodiment is most preferred embodiment.
Fig. 1 is scanning electron microscope (SEM) photograph (SEM) photo that nanometer fluorine ion absorber is made in the present embodiment;Known to SEM figure originally
The lanthanum hydroxide of method synthesis is nanometer strip, in irregular shape, so that this material be made to have bigger reference area, Jin Erzeng
Strong absorption property.
Fig. 2 is transmission electron microscope (TEM) figure of this implementation nanometer fluorine ion absorber;By TEM figure it can be seen that lanthanum hydroxide
Grain diameter is less than 50 nm.
Fig. 3 and Fig. 4 is respectively energy disperse spectroscopy (EDS) figure and X-ray diffraction (XRD) figure of nanometer fluorine ion absorber, by
Figure can be seen that the new material impurity of synthesis is less, can be seen as relatively pure lanthanum hydroxide particle.
Take lanthanum hydroxide grain products 225g manufactured in the present embodiment be placed in resin adsorption live in, material bulk density is
1.25g/ml, filling rate 80%;The water sample for taking certain waterworks fluorine exceeded adjusts water inlet flow velocity using peristaltic pump, and empty bed stops
Time (EBCT)=4min.
Influent quality parameter are as follows: F-=1.37 mg/L, pH=7.8-8.2.Effluent criteria refers to urban water supply water standard
The mg/L of F-=1.0 in CJT206-2005.
Final experimental data figure is as shown in Figure 5.Experimental result shows, this material fluorine ion suitable for practical water quality
Removal, for highest removal rate up to 99%, it is 2L/g that unit mass material, which handles water,.
Embodiment 2
Reactor vessel is placed in 10 DEG C of ice water by step 1, and deionized water is added to reactor vessel;
130g lanthanum nitrate is added into above-mentioned deionized water step 2, is stirred dissolution with blender;
Step 3 is slowly added to sodium hydroxide solution, and adjusting pH is 9.0;At this point, water: lanthanum nitrate: the mass ratio of sodium hydroxide is
2:1:0.2;
Step 4 is rinsed above-mentioned solution repeatedly to conductivity in 1 ms/cm or less with deionized water;
Step 5, by step 4 wash slurries, be dehydrated at 1500r/min with centrifuge, using baking oven at 60 DEG C into
Row drying;
Step 6, grinding, and screened by the sieve of 100 mesh, obtain lanthanum hydroxide dry powder;
Step 7 mixes lanthanum hydroxide dry powder with microcrystalline cellulose, hypromellose, through wet granulator and round as a ball
Machine is granulated, wherein lanthanum hydroxide: microcrystalline cellulose: the mass ratio of hypromellose is 4.5:2:3;
Final grain diameter obtained is 1.7 ~ 2.2mm through this embodiment.
Embodiment 3
Reactor vessel is placed in 10 DEG C of ice water by step 1;Deionized water is added to reactor vessel;
130g lanthanum nitrate is added into above-mentioned water step 2, is stirred dissolution with blender;
Step 3 is slowly added to sodium hydroxide solution, and adjusting pH is 9.0;At this point, water: lanthanum nitrate: the mass ratio of sodium hydroxide is
7:4:0.1;
Step 4 is rinsed above-mentioned solution repeatedly to conductivity in 1 ms/cm or less with deionized water;
Step 5, the slurries for washing step 4, are dehydrated with centrifuge, are dried at 90 DEG C using baking oven;
Step 6, grinding, and screened by the sieve of 100 mesh, obtain lanthanum hydroxide dry powder;
Step 7 mixes lanthanum hydroxide dry powder with microcrystalline cellulose, hypromellose, through wet granulator and round as a ball
Machine is granulated, wherein lanthanum hydroxide: microcrystalline cellulose: the mass ratio of hypromellose is 5:1:2;
Final grain diameter obtained is 1.9 ~ 2.5mm through this embodiment.
Embodiment 4
Reactor vessel is placed in 30 DEG C of ice water by step 1, and deionized water is added into reactor vessel;
130g lanthanum nitrate solid powder is added into above-mentioned low temperature deionized water step 2, is stirred dissolution with blender;
After step 3, dissolution, it is slowly added to sodium hydroxide solution, adjusts pH to 8.5;At this point, water: lanthanum nitrate: the matter of sodium hydroxide
Amount is than being 5:2:0.4;
Step 4 is rinsed step 3 preparation solution repeatedly to conductivity in 1 ms/cm or less with deionized water;
Step 5, the slurries for washing step 4, are dehydrated with centrifuge, are dried at 90 DEG C using baking oven;
Step 6, grinding, and screened by the sieve of 100 mesh, obtain lanthanum hydroxide dry powder;
Step 7 mixes lanthanum hydroxide dry powder with microcrystalline cellulose, hypromellose, through wet granulator and round as a ball
Machine is granulated, wherein lanthanum hydroxide: microcrystalline cellulose: the mass ratio of hypromellose is 4:1:2
Finally grain diameter obtained is 1.6 ~ 2.0mm to above-mentioned steps.
The contents of the present invention are not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And to any equivalent transformation that technical solution of the present invention is taken, all are covered by the claims of the invention.
Claims (3)
1. a kind of preparation method of Nano-lanthanum hydroxide de-fluoridation adsorbent, which comprises the following steps:
Step 1: reactor vessel is placed in 10 ~ 35 DEG C of ice water, deionized water is added into reactor vessel;
Step 2: lanthanum nitrate solid powder is taken to be added into deionized water described in step 1, dissolution is stirred with blender;
Step 3: being slowly added to sodium hydroxide solution after lanthanum nitrate dissolution, pH to 8.5-9.0 is adjusted;At this point, low temperature deionization
Water: lanthanum nitrate: the mass ratio of sodium hydroxide is (5-7): (2-4): (0.4-1);
Step 4: being rinsed the solution that step 3 is prepared repeatedly to conductivity with deionized water in 1 ms/cm or less;
Step 5: the slurries that step 4 is washed, are dehydrated with centrifuge, are then dried at 60-90 DEG C using baking oven
It is dry;
Step 6: grinding and passing through the sieve screening of 10-100 mesh, lanthanum hydroxide dry powder is obtained;
Step 7: lanthanum hydroxide dry powder is mixed with microcrystalline cellulose, hypromellose b, through wet granulator and round as a ball
Machine is granulated, wherein lanthanum hydroxide: microcrystalline cellulose: the mass ratio of hypromellose is (4-5): (1-3): (2-
4).
2. preparation method according to claim 1, which is characterized in that step 7 be granulated after grain diameter be 1.8 ~
2.5mm。
3. Nano-lanthanum hydroxide de-fluoridation adsorbent obtained by a kind of preparation method according to claim 1.
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Cited By (4)
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CN112427028A (en) * | 2020-11-19 | 2021-03-02 | 成都理工大学 | Cetyl trimethyl ammonium bromide modified nano iron lanthanum material, preparation method and application |
CN113274976A (en) * | 2021-04-28 | 2021-08-20 | 中国矿业大学 | Synthetic method of lanthanum-doped graphene oxide nanocomposite fluorine removal agent |
CN115010179A (en) * | 2021-03-05 | 2022-09-06 | 中南大学 | Method for preparing fluorine-free battery-grade high-purity manganese sulfate by fluorination method |
CN115501856A (en) * | 2022-09-20 | 2022-12-23 | 燕山大学 | Specific fluorine-absorbing agent and preparation method and application method thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112427028A (en) * | 2020-11-19 | 2021-03-02 | 成都理工大学 | Cetyl trimethyl ammonium bromide modified nano iron lanthanum material, preparation method and application |
CN115010179A (en) * | 2021-03-05 | 2022-09-06 | 中南大学 | Method for preparing fluorine-free battery-grade high-purity manganese sulfate by fluorination method |
CN113274976A (en) * | 2021-04-28 | 2021-08-20 | 中国矿业大学 | Synthetic method of lanthanum-doped graphene oxide nanocomposite fluorine removal agent |
CN113274976B (en) * | 2021-04-28 | 2022-10-18 | 中国矿业大学 | Synthetic method of lanthanum-doped graphene oxide nanocomposite fluorine removal agent |
CN115501856A (en) * | 2022-09-20 | 2022-12-23 | 燕山大学 | Specific fluorine-absorbing agent and preparation method and application method thereof |
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Application publication date: 20190111 |