CN106732335A - A kind of kaolinite for the treatment of field of Environment Protection water body and preparation method thereof - Google Patents
A kind of kaolinite for the treatment of field of Environment Protection water body and preparation method thereof Download PDFInfo
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- CN106732335A CN106732335A CN201611186817.8A CN201611186817A CN106732335A CN 106732335 A CN106732335 A CN 106732335A CN 201611186817 A CN201611186817 A CN 201611186817A CN 106732335 A CN106732335 A CN 106732335A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
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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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- Chemical Kinetics & Catalysis (AREA)
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- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
Abstract
The invention discloses a kind of kaolinic preparation method for the treatment of field of Environment Protection water body, mainly include the following steps that:(1)Rinsing, crushing kaolinite;(2)Prepare nano-kaolinite powder;(3)Prepare hydration kaolinite;(4)Prepare silver nitrate solution;(5)Prepare Nano Silver hydration kaolinite;(6)60Coradiation;(7)Prepare Nano Silver hydration kaolinite nanometer powder.The kaolinite high adsorption capacity being prepared from using the method, it is easy to popularization and application.
Description
Technical field
The present invention relates to field of Environment Protection, more particularly to a kind of kaolinite and its preparation side for the treatment of field of Environment Protection water body
Method.
Background technology
With the growth in the living standard of people and developing rapidly for economy, what environment for the survival of mankind was subject to pollutes
Also it is more and more serious.The characteristics of especially heavy metal usually has irreversibility to water body.Therefore, how Heavy Metals in Waters is made
Removal be up to state standards and increasingly paid attention to by numerous researchers.The method for removing Heavy Metals in Waters ion includes thing
Reason method, chemical method, biological method etc., wherein, chemisorbed is paid attention to as a kind of efficient processing method.So
And, because the R&D costs of adsorbent are high, the research and development time is long and inefficient etc., defect makes it difficult to be pushed away on a large scale
Wide application.
Kaolinite is a kind of natural silicate clay mineral, and kaolinite has very big specific surface area, due to alumina eight
Trivalent aluminium ion in the body of face is adsorbed by magnesium ion or calcium ion isomorphous substitution, lamella negatively charged in sheet surfaces
Inorganic cation is keeping electroneutral.This design feature can make to make strongly between the pollutant such as it and organic matter, heavy metal
With so as to reach the purpose of Adsorption pollutant.In recent years, with the development of science and technology, kaolinite is widely used in
Synthesize various types of molecular sieves, nano material and sorbing material etc..
However, kaolinite is directly applied into water body treatment, in particular for the treatment of Heavy Metals in Waters, it is impossible to reach
Gratifying effect, therefore kaolinic absorption property how is improved, it is even more important for field of Environment Protection sewerage disposing.
The content of the invention
Regarding to the issue above, the purpose of the present invention aims to provide a kind of kaolinite for the treatment of field of Environment Protection water body.
The purpose of the present invention is achieved by the following technical programs:A kind of kaolinite for the treatment of field of Environment Protection water body
Preparation method, mainly include the following steps that:
(1)Rinsing, crushing kaolinite:Kaolinite is crushed using stone mill pulverizer, the kaolinite after crushing is used into ultrasound point
30min ~ 60min is dissipated, removal particle diameter finally gives the kaolinite stone flour that grain diameter is 200 mesh ~ 150 mesh more than the particle of 200 mesh
End;
(2)Prepare nano-kaolinite powder:Will be by step(1)Kaolinite stone powder obtained by treatment is placed in electric arc furnaces and heats,
After being heated to 1200 ~ 1600 DEG C of 8 ~ 12h of insulation with the heating rate of 20 ~ 30 DEG C/min, nano-kaolinite powder is obtained;
(3)Prepare hydration kaolinite:Will be by step(2)Hydrazine hydrate is added in the nano-kaolinite powder that treatment is obtained, is hydrated
Hydrazine is 50 with the weight ratio of nano-kaolinite powder:2 ~ 3, after slightly stirring, be placed in reactor negative pressure impregnation reaction 24h ~
72h, the scope of negative pressure impregnation is 1000 ~ 3500KPa;It is subsequently placed on high speed freezing centrifuge with 10000rpm/min removals
Layer liquid, adds 75 DEG C for the treatment of 12h of absolute ethyl alcohol to remove hydrazine hydrate in solid sediment, obtain the nano hydrated kaolinite of hydrazine hydrate
Stone;
(4)Prepare silver nitrate solution:10g silver nitrate crystals are weighed in 100ml ultra-pure waters, lucifuge and in 4 DEG C after stirring and dissolving
Saved backup in environment;
(5)Prepare Nano Silver hydration kaolinite:By step(3)In the obtained nano hydrated kaolinite of hydrazine hydrate and step(4)In
The silver nitrate solution mixing for obtaining, is placed in reacting 72h in 30 ~ 50 DEG C of environment, wherein, the nano hydrated kaolinite of hydrazine hydrate and nitre
The volume ratio of sour silver solution is 1:150~180;
(6)60Coradiation:By step(5)In be prepared from Nano Silver hydration kaolinite irradiated by Co 60 device, spoke
It is 35 ~ 40KGy according to dosage, exposure time is 30min ~ 60min;
(7)Prepare Nano Silver hydration kaolinite nanometer powder:By step(6)After treatment Nano Silver hydration kaolinite mixed liquor from
The heart is separated, and removes liquid level, and solids of sedimentation layer takes out to be placed in crucible and is placed into 1200 DEG C of calcining 6h in Muffle furnace, after insulation 1h
Obtain Nano Silver hydration kaolinite nanometer powder.
Preferably, step(1)In kaolinite grain diameter preferably 170 mesh that obtain.
Preferably, step(3)Middle hydrazine hydrate is 50 with the weight ratio of nano-kaolinite powder:3, pressure during negative pressure impregnation
It is 2000KPa.
Preferably, step(5)The middle nano hydrated kaolinite of hydrazine hydrate is 1 with the volume ratio of silver nitrate solution:160.
Preferably, step(6)Middle 60Coradiation dosage is 36.5KGy, and exposure time is 45min.
Relative to prior art, beneficial effects of the present invention:One kind that the present invention is provided is for the treatment of field of Environment Protection water body
Kaolinic preparation method, preparation method process is simple, it is only necessary to can obtain being hydrated kaolinite by simple mixing
Stone;Additionally, during Nano Silver hydration kaolinite is prepared, due to without the addition chemicals toxic to human body or water body
Poisonous and hazardous material will not be produced during matter, therefore use, with environmental-protecting performance;Finally, Co 60 is employed to preparation
Into Nano Silver hydration kaolinite solution irradiated, improve kaolinic absorption property.It is of the invention a kind of for environmental protection
The kaolinic preparation method of field water body treatment is simple to operate, traditional water treatment technology can be effectively combined, with fine
Actual application value and large-scale promotion application prospect.
Brief description of the drawings
Fig. 1 is the processing step flow chart for preparing kaolinic method.
Specific embodiment
The invention will be further described with the following Examples.
Such as Fig. 1 of embodiment 1, is a kind of kaolinic preparation for the treatment of field of Environment Protection water body of the present embodiment offer
The processing step of method, comprises the following steps:
(1)Rinsing, crushing kaolinite:Kaolinite is crushed using stone mill pulverizer, the kaolinite after crushing is used into ultrasound point
45min is dissipated, removal particle diameter further filters out the kaolinite particle that particle diameter is 170 mesh more than the particle of 200 mesh;
(2)Prepare nano-kaolinite powder:Will be by step(1)Kaolinite stone powder obtained by treatment is placed in electric arc furnaces and heats,
After being heated to 1200 DEG C of insulation 12h with the heating rate of 20 ~ 30 DEG C/min, nano-kaolinite powder is obtained;
(3)Prepare hydration kaolinite:Will be by step(2)Hydrazine hydrate is added in the nano-kaolinite powder that treatment is obtained, is hydrated
Hydrazine is 50 with the weight ratio of nano-kaolinite powder:3, after slightly stirring, it is placed in negative pressure impregnation reaction 36h, negative pressure in reactor
The pressure of dipping is 2000KPa;It is subsequently placed on high speed freezing centrifuge and supernatant liquid is removed with 10000rpm/min, solid sinks
Add 75 DEG C for the treatment of 12h of absolute ethyl alcohol to remove hydrazine hydrate in starch, obtain the nano hydrated kaolinite of hydrazine hydrate;
(4)Prepare silver nitrate solution:10g silver nitrate crystals are weighed in 100ml ultra-pure waters, lucifuge and in 4 DEG C after stirring and dissolving
Saved backup in environment;
(5)Prepare Nano Silver hydration kaolinite:By step(3)In the obtained nano hydrated kaolinite of hydrazine hydrate and step(4)In
The silver nitrate solution mixing for obtaining, is placed in reacting 72h in 45 DEG C of environment, wherein, the nano hydrated kaolinite of hydrazine hydrate and nitric acid
The volume ratio of silver-colored solution is 1:160;
(6)60Coradiation:By step(5)In be prepared from Nano Silver hydration kaolinite irradiated by Co 60 device, spoke
It is 36.5KGy according to dosage, exposure time is 45min;
(7)Prepare Nano Silver hydration kaolinite nanometer powder:By step(6)After treatment Nano Silver hydration kaolinite mixed liquor from
The heart is separated, and removes liquid level, and solids of sedimentation layer takes out to be placed in crucible and is placed into 1200 DEG C of calcining 6h in Muffle furnace, after insulation 1h
Obtain Nano Silver hydration kaolinite nanometer powder.
A kind of kaolinic preparation method for the treatment of field of Environment Protection water body that the present embodiment of embodiment 2 is provided, including
Following steps:
(1)Rinsing, crushing kaolinite:Kaolinite is crushed using stone mill pulverizer, the kaolinite after crushing is used into ultrasound point
60min is dissipated, the kaolinite stone powder of 200 mesh ~ 180 mesh is filtered out;
(2)Prepare nano-kaolinite powder:Will be by step(1)Kaolinite stone powder obtained by treatment is placed in electric arc furnaces and heats,
After being heated to 1420 DEG C of insulation 9.6h with the heating rate of 20 ~ 30 DEG C/min, nano-kaolinite powder is obtained;
(3)Prepare hydration kaolinite:Will be by step(2)Hydrazine hydrate is added in the nano-kaolinite powder that treatment is obtained, is hydrated
Hydrazine is 50 with the weight ratio of nano-kaolinite powder:2, after slightly stirring, it is placed in negative pressure impregnation reaction 72h, negative pressure in reactor
The pressure of dipping is 1000KPa;It is subsequently placed on high speed freezing centrifuge and supernatant liquid is removed with 10000rpm/min, solid sinks
Add 75 DEG C for the treatment of 12h of absolute ethyl alcohol to remove hydrazine hydrate in starch, obtain the nano hydrated kaolinite of hydrazine hydrate;
(4)Prepare silver nitrate solution:10g silver nitrate crystals are weighed in 100ml ultra-pure waters, lucifuge and in 4 DEG C after stirring and dissolving
Saved backup in environment;
(5)Prepare Nano Silver hydration kaolinite:By step(3)In the obtained nano hydrated kaolinite of hydrazine hydrate and step(4)In
The silver nitrate solution mixing for obtaining, is placed in reacting 72h in 50 DEG C of environment, wherein, the nano hydrated kaolinite of hydrazine hydrate and nitric acid
The volume ratio of silver-colored solution is 1:180;
(6)60Coradiation:By step(5)In be prepared from Nano Silver hydration kaolinite irradiated by Co 60 device, spoke
It is 40KGy according to dosage, exposure time is 30min;
(7)Prepare Nano Silver hydration kaolinite nanometer powder:By step(6)After treatment Nano Silver hydration kaolinite mixed liquor from
The heart is separated, and removes liquid level, and solids of sedimentation layer takes out to be placed in crucible and is placed into 1200 DEG C of calcining 6h in Muffle furnace, after insulation 1h
Obtain Nano Silver hydration kaolinite nanometer powder.
A kind of kaolinic preparation method for the treatment of field of Environment Protection water body that the present embodiment of embodiment 3 is provided, including
Following steps:
(1)Rinsing, crushing kaolinite:Kaolinite is crushed using stone mill pulverizer, the kaolinite after crushing is used into ultrasound point
30min is dissipated, the kaolinite stone powder of 160 mesh ~ 150 mesh is filtered out;
(2)Prepare nano-kaolinite powder:Will be by step(1)Kaolinite stone powder obtained by treatment is placed in electric arc furnaces and heats,
After being heated to 1600 DEG C of insulation 8h with the heating rate of 20 ~ 30 DEG C/min, nano-kaolinite powder is obtained;
(3)Prepare hydration kaolinite:Will be by step(2)Hydrazine hydrate is added in the nano-kaolinite powder that treatment is obtained, is hydrated
Hydrazine is 50 with the weight ratio of nano-kaolinite powder:3, after slightly stirring, it is placed in negative pressure impregnation reaction 24h, negative pressure in reactor
The pressure of dipping is 3500KPa;It is subsequently placed on high speed freezing centrifuge and supernatant liquid is removed with 10000rpm/min, solid sinks
Add 75 DEG C for the treatment of 12h of absolute ethyl alcohol to remove hydrazine hydrate in starch, obtain the nano hydrated kaolinite of hydrazine hydrate;
(4)Prepare silver nitrate solution:10g silver nitrate crystals are weighed in 100ml ultra-pure waters, lucifuge and in 4 DEG C after stirring and dissolving
Saved backup in environment;
(5)Prepare Nano Silver hydration kaolinite:By step(3)In the obtained nano hydrated kaolinite of hydrazine hydrate and step(4)In
The silver nitrate solution mixing for obtaining, is placed in reacting 72h in 30 DEG C of environment, wherein, the nano hydrated kaolinite of hydrazine hydrate and nitric acid
The volume ratio of silver-colored solution is 1:150;
(6)60Coradiation:By step(5)In be prepared from Nano Silver hydration kaolinite irradiated by Co 60 device, spoke
It is 35KGy according to dosage, exposure time is 60min;
(7)Prepare Nano Silver hydration kaolinite nanometer powder:By step(6)After treatment Nano Silver hydration kaolinite mixed liquor from
The heart is separated, and removes liquid level, and solids of sedimentation layer takes out to be placed in crucible and is placed into 1200 DEG C of calcining 6h in Muffle furnace, after insulation 1h
Obtain Nano Silver hydration kaolinite nanometer powder.
Test example is hydrated kaolinite nanometer powder to containing heavy metal using the Nano Silver that embodiment 1 ~ 3 is prepared from
Water body is processed, and copper, lead, arsenic, cadmium and the mercury ion water sample 1000ml of 1000mg/L are taken respectively, is delivered wherein unprocessed
Kaolinite and after treatment Nano Silver hydration kaolinite nanometer powder, be placed at normal temperatures vibration case in 200rpm/
Min vibrates 6h, then detects each heavy metal ion content in above-mentioned water sample, different clearances is obtained, as a result such as the institute of table 1
Show.
The result table of comparisons of table 1.As table 1 result data display, using preparation method of the invention prepare and
Into Nano Silver be hydrated kaolinite nanometer powder, heavy metal has significant removal effect, and adsorption capacity is significantly carried
Height, the removal adsorption capacity particularly with mercury metal ion is strong compared with remaining metal ion.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of scope is protected, although being explained to the present invention with reference to preferred embodiment, one of ordinary skill in the art should
Work as understanding, technical scheme can be modified or equivalent, without deviating from the reality of technical solution of the present invention
Matter and scope.
Claims (5)
1. it is a kind of for field of Environment Protection water body treatment kaolinic preparation method, it is characterised in that mainly include the following steps that:
(1)Rinsing, crushing kaolinite:Kaolinite is crushed using stone mill pulverizer, the kaolinite after crushing is used into ultrasound point
30min ~ 60min is dissipated, removal particle diameter finally gives the kaolinite stone flour that grain diameter is 200 mesh ~ 150 mesh more than the particle of 200 mesh
End;
(2)Prepare nano-kaolinite powder:Will be by step(1)Kaolinite stone powder obtained by treatment is placed in electric arc furnaces and heats,
After being heated to 1200 ~ 1600 DEG C of 8 ~ 12h of insulation with the heating rate of 20 ~ 30 DEG C/min, nano-kaolinite powder is obtained;
(3)Prepare hydration kaolinite:Will be by step(2)Hydrazine hydrate is added in the nano-kaolinite powder that treatment is obtained, is hydrated
Hydrazine is 50 with the weight ratio of nano-kaolinite powder:2 ~ 3, after slightly stirring, be placed in reactor negative pressure impregnation reaction 24h ~
72h, the scope of negative pressure impregnation is 1000 ~ 3500KPa;It is subsequently placed on high speed freezing centrifuge with 10000rpm/min removals
Layer liquid, adds 75 DEG C for the treatment of 12h of absolute ethyl alcohol to remove hydrazine hydrate in solid sediment, obtain the nano hydrated kaolinite of hydrazine hydrate
Stone;
(4)Prepare silver nitrate solution:10g silver nitrate crystals are weighed in 100ml ultra-pure waters, lucifuge and in 4 DEG C after stirring and dissolving
Saved backup in environment;
(5)Prepare Nano Silver hydration kaolinite:By step(3)In the obtained nano hydrated kaolinite of hydrazine hydrate and step(4)In
The silver nitrate solution mixing for obtaining, is placed in reacting 72h in 30 ~ 50 DEG C of environment, wherein, the nano hydrated kaolinite of hydrazine hydrate and nitre
The volume ratio of sour silver solution is 1:150~180;
(6)60Coradiation:By step(5)In be prepared from Nano Silver hydration kaolinite irradiated by Co 60 device, spoke
It is 35 ~ 40KGy according to dosage, exposure time is 30min ~ 60min;
(7)Prepare Nano Silver hydration kaolinite nanometer powder:By step(6)After treatment Nano Silver hydration kaolinite mixed liquor from
The heart is separated, and removes liquid level, and solids of sedimentation layer takes out to be placed in crucible and is placed into 1200 DEG C of calcining 6h in Muffle furnace, after insulation 1h
Obtain Nano Silver hydration kaolinite nanometer powder.
2. as claimed in claim 1 it is a kind of for field of Environment Protection water body treatment kaolinic preparation method, it is characterised in that step
Suddenly(1)In kaolinite grain diameter preferably 170 mesh that obtain.
3. a kind of kaolinic preparation method for the treatment of field of Environment Protection water body as claimed in claim 1, it is characterised in that
Step(3)Middle hydrazine hydrate is 50 with the weight ratio of nano-kaolinite powder:3, pressure during negative pressure impregnation is 2000KPa.
4. a kind of kaolinic preparation method for the treatment of field of Environment Protection water body as claimed in claim 1, it is characterised in that
Step(5)The middle nano hydrated kaolinite of hydrazine hydrate is 1 with the volume ratio of silver nitrate solution:160.
5. as described in any one of claim 1 ~ 4 it is a kind of for field of Environment Protection water body treatment kaolinic preparation method, its
It is characterised by, step(6)Middle 60Coradiation dosage is 36.5KGy, and exposure time is 45min.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102701229A (en) * | 2012-06-14 | 2012-10-03 | 浙江大学 | Method for preparing 0.84 nm kaolinite hydrate by hydrazine hydrate-kaolinite intercalation complex |
CN103084152A (en) * | 2012-12-20 | 2013-05-08 | 中国科学院合肥物质科学研究院 | Treatment method for effectively improving microstructures and absorption properties of attapulgite and kieselguhr |
CN103271942A (en) * | 2013-05-27 | 2013-09-04 | 浙江大学 | Method for preparing nano silver-kaolinite compound by using hydrated kaolinite as carrier |
CN105126743A (en) * | 2015-08-20 | 2015-12-09 | 南京航空航天大学 | Preparation and recovery methods for magnetic clay adsorption material |
CN105969399A (en) * | 2016-06-06 | 2016-09-28 | 广西美耕生物科技有限公司 | Organic soil activating agent and preparation method thereof |
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2016
- 2016-12-21 CN CN201611186817.8A patent/CN106732335A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102701229A (en) * | 2012-06-14 | 2012-10-03 | 浙江大学 | Method for preparing 0.84 nm kaolinite hydrate by hydrazine hydrate-kaolinite intercalation complex |
CN103084152A (en) * | 2012-12-20 | 2013-05-08 | 中国科学院合肥物质科学研究院 | Treatment method for effectively improving microstructures and absorption properties of attapulgite and kieselguhr |
CN103271942A (en) * | 2013-05-27 | 2013-09-04 | 浙江大学 | Method for preparing nano silver-kaolinite compound by using hydrated kaolinite as carrier |
CN105126743A (en) * | 2015-08-20 | 2015-12-09 | 南京航空航天大学 | Preparation and recovery methods for magnetic clay adsorption material |
CN105969399A (en) * | 2016-06-06 | 2016-09-28 | 广西美耕生物科技有限公司 | Organic soil activating agent and preparation method thereof |
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