CN105944697A - Preparation method of attapulgite repairing material suitable for heavy metal pollution of water bodies - Google Patents
Preparation method of attapulgite repairing material suitable for heavy metal pollution of water bodies Download PDFInfo
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- CN105944697A CN105944697A CN201610497485.9A CN201610497485A CN105944697A CN 105944697 A CN105944697 A CN 105944697A CN 201610497485 A CN201610497485 A CN 201610497485A CN 105944697 A CN105944697 A CN 105944697A
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- Prior art keywords
- attapulgite
- solution
- described step
- heavy metal
- polyacrylonitrile
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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
-
- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
-
- 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
-
- 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
-
- 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
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
-
- 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 discloses a preparation method of an attapulgite repairing material suitable for heavy metal pollution of water bodies. The preparation method comprises the following specific steps: grinding attapulgite, performing screening, adding a hydrochloric acid solution, performing acidifying, modifying the acid activation attapulgite with a bis-(gamma-[(triethoxysily)propyl])-tetrasulfide KH-858 silane coupling agent, and adding the attapulgite modified with the silane coupling agent into a polyacrylonitrile solution so as to obtain a polyacrylonitrile/attapulgite composite membrane. Through the adoption of the repairing material for heavy metal of the water bodies, prepared by the method disclosed by the invention, the specific surface of attapulgite crystals is increased through acidifying treatment, and the adsorption capacity is effectively improved; a new network structure is formed through the modification of the silane coupling agent; besides, the organic modified attapulgite is added to the polyacrylonitrile solution to prepare the polyacrylonitrile/attapulgite composite membrane, so that the heavy metal in the water bodies can be effectively adsorbed.
Description
Technical field
The invention belongs to water pollution and administer field, particularly relate to a kind of heavy metal pollution of water body of being applicable to
The preparation method of attapulgite repair materials.
Background technology
The heavy metal discharged with waste water, even if concentration is little, it is possible to accumulate in algae and bed mud, by fish and shellfish
Class body surface adsorbs, and produces food chain and concentrates, thus causes public hazards.In water body, metal is favourable or harmful not only takes
Certainly in kind, the physicochemical property of metal, but also depend on the concentration of metal and the valence state of existence and form,
Even if useful metallic element concentration exceedes a certain numerical value also has violent toxicity, animals and plants are made to be poisoned, very
To dead.Metallo-organic compound (such as organic mercury, Organic leadP, organo-arsenic, organotin etc.) is than corresponding
Metal inorganic compound toxicity is much better than;The metal of soluble state is bigger than the toxicity of particulate form metal again.
Attapulgite also known as Paligorskite or Palygorskite, be a kind of have chain layer structure containing Shuifu County's magnesium alumino metasilicate
Salt clay mineral.Its structure belongs to 2:1 type clay mineral.In each 2:1 unit structure layer, tetrahedron is brilliant
Sheet angle is pushed up direction at a certain distance and is overturned, cambium layer chain.Lead to parallel with chain is formed at tetrahedron bar interband
Road, filling zeolite water and water of crystallization in passage.
Summary of the invention
It is an object of the invention to provide the system of a kind of attapulgite repair materials being applicable to heavy metal pollution of water body
Preparation Method, by adding double-(the silica-based propyl group of γ-triethoxy) tetrasulfide in the attapulgite to acidifying
KH-858 is silane coupler modified, and organically-modified attapulgite is joined polyacrylonitrile solution is made poly-
Acrylonitrile/attapulgite composite membrane, can be with the heavy metal in active adsorption water body.
The present invention is achieved by the following technical solutions:
The preparation method of a kind of attapulgite repair materials being applicable to heavy metal pollution of water body, including following concrete
Step:
Step (1), attapulgite is ground and sieves, obtain attapulgite powder;
Step (2), by described step (1) attapulgite powder add hydrochloric acid solution acidifying, solid-to-liquid ratio is
1:1.5, water-bath concussion certain time, obtains being acidified attapulgite solution;
Step (3), it is vacuum dried taking precipitation after the acidifying attapulgite solution centrifugal in described step (2)
To acidifying attapulgite powder;
Step (4), the acidifying attapulgite powder obtained in described step (3) is joined double-(γ-three second
The silica-based propyl group of epoxide) in tetrasulfide KH-858 silane coupler solution, be positioned in electric jacket be heated to molten
Isothermal reaction 4h after liquid boiling, stops heating, obtains organically-modified by this solution for vacuum sucking filtration post-drying afterwards
Concave-convex rod particle;
Step (5), polyacrylonitrile powder is dissolved in dimethyl sulfoxide it is configured to polyacrylonitrile solution, poly-
Acrylonitrile concentration is 12%, adds obtain in described step (4) coupling agent modified in polyacrylonitrile solution
Attapulgite powder obtains polyacrylonitrile/attapulgite solution, and this modified attapulgite concentration is 5%, with scraper by poly-third
Alkene nitrile/attapulgite solution the most uniformly paints the thick film for 50-80 μm, by this glass plate at 80 DEG C
It is positioned in vacuum drying oven drying 24-48h, afterwards by this film washing and drying, prepares polyacrylonitrile/attapulgite
Composite membrane.
Further, described step (1) uses 180 mesh screen.
Further, described step (2) adds the concentrated hydrochloric acid that concentration is 37% in distilled water and be configured to 5mol/L
Hydrochloric acid solution, in described step (2), bath temperature is 40 DEG C, water-bath concussion the time be 3-5h.
Further, in described step (3), centrifuging temperature is 40 DEG C, and centrifugal rotational speed is 9000g, time centrifugal
Between be 20min.
Further, described step (4) adds double-(the silica-based propyl group of γ-triethoxy) in toluene solution
Tetrasulfide KH-858 is configured to silane coupler solution, wherein, and silane coupler KH-858 and described step
The mass ratio of the acidifying attapulgite powder suddenly obtained in (3) is 1:5.5.
Further, drying temperature in described step (4) is 105 DEG C, and drying time is 4h.
Further, described step (5) uses milli-Q water 3-5 time, described step (5) is dried
Temperature is 50-80 DEG C, and drying time is 24h.
The method have the advantages that
Heavy metal in water repair materials prepared by the inventive method, makes attapulgite crystal ratio by acidification
Surface increases, and is effectively increased absorbability;Silane coupler can produce a large amount of silicone hydroxyl when hydrolysis,
These silicone hydroxyl can produce condensation with attapulgite surface silanol group, or the silicone hydroxyl of silane coupler is certainly
Body is condensed, and is covered in attapulgite surface, its configuration of surface modified and character, forms new network structure;
Organically-modified attapulgite is joined simultaneously and polyacrylonitrile solution is made polyacrylonitrile/attapulgite composite membrane,
Can be with the heavy metal in active adsorption water body.
Detailed description of the invention
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described enforcement
Example is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention,
All other embodiments that those of ordinary skill in the art are obtained under not making creative work premise,
Broadly fall into the scope of protection of the invention.
Embodiment 1
Step (1), by milled for attapulgite 180 mesh sieves, obtain attapulgite powder;
Step (2), distilled water add the concentrated hydrochloric acid that concentration is 37% and are configured to the hydrochloric acid solution of 5mol/L,
Attapulgite powder in step (1) adds hydrochloric acid solution acidifying, and solid-to-liquid ratio is 1:1.5,40 DEG C of water-bath shakes
Swing 3h, obtain being acidified attapulgite solution;
Step (3), by the acidifying attapulgite solution in step (2) in 40 DEG C, centrifugal 20min under 9000g,
Take precipitation vacuum drying to obtain being acidified attapulgite powder;
Step (4), toluene solution add double-(the silica-based propyl group of γ-triethoxy) tetrasulfide KH-858
It is configured to silane coupler solution, pours in flask, wherein, silane coupler KH-858 and step (3)
In obtain acidifying attapulgite powder mass ratio be 1:5.5;
The acidifying attapulgite powder obtained in step (3) is joined in silane coupler solution, flask is put
It is placed in electric jacket and is heated to isothermal reaction 4h after solution boiling, stop heating;
Drying will be positioned in 105 DEG C of baking ovens after coupling agent modified attapulgite powder solution for vacuum sucking filtration
4h obtains there is modified attapulgite granule;
Step (5), polyacrylonitrile powder is dissolved in dimethyl sulfoxide it is configured to polyacrylonitrile solution, poly-
Acrylonitrile concentration is 12%, adds coupling agent modified attapulgite powder and obtain polyacrylonitrile in polyacrylonitrile solution
/ attapulgite solution, this modified attapulgite concentration is 5%, with scraper by polyacrylonitrile/attapulgite solution at glass
Uniformly paint the film that thickness is 80 μm on plate, at 80 DEG C, this glass plate is positioned in vacuum drying oven drying 24h;
This film is taken off from glass plate, with milli-Q water 5 times, puts into drying 24h in 50 DEG C of baking ovens,
Prepare polyacrylonitrile/attapulgite composite membrane.
Embodiment 2
Step (1), by milled for attapulgite 180 mesh sieves, obtain attapulgite powder;
Step (2), distilled water add the concentrated hydrochloric acid that concentration is 37% and are configured to the hydrochloric acid solution of 5mol/L,
Attapulgite powder in step (1) adds hydrochloric acid solution acidifying, and solid-to-liquid ratio is 1:1.5,40 DEG C of water-bath shakes
Swing 5h, obtain being acidified attapulgite solution;
Step (3), by the acidifying attapulgite solution in step (2) in 40 DEG C, centrifugal 20min under 9000g,
Take precipitation vacuum drying to obtain being acidified attapulgite powder;
Step (4), toluene solution add double-(the silica-based propyl group of γ-triethoxy) tetrasulfide KH-858
It is configured to silane coupler solution, pours in flask, wherein, silane coupler KH-858 and step (3)
In obtain acidifying attapulgite powder mass ratio be 1:5.5;
The acidifying attapulgite powder obtained in step (3) is joined in silane coupler solution, flask is put
It is placed in electric jacket and is heated to isothermal reaction 4h after solution boiling, stop heating;
Drying will be positioned in 105 DEG C of baking ovens after coupling agent modified attapulgite powder solution for vacuum sucking filtration
4h obtains there is modified attapulgite granule;
Step (5), polyacrylonitrile powder is dissolved in dimethyl sulfoxide it is configured to polyacrylonitrile solution, poly-
Acrylonitrile concentration is 12%, adds coupling agent modified attapulgite powder and obtain polyacrylonitrile in polyacrylonitrile solution
/ attapulgite solution, this modified attapulgite concentration is 5%, with scraper by polyacrylonitrile/attapulgite solution at glass
Uniformly paint the film that thickness is 50 μm on plate, at 80 DEG C, this glass plate is positioned in vacuum drying oven drying 48h;
This film is taken off from glass plate, with milli-Q water 3 times, puts into drying 24h in 80 DEG C of baking ovens,
Prepare polyacrylonitrile/attapulgite composite membrane.
Embodiment 3
Step (1), by milled for attapulgite 180 mesh sieves, obtain attapulgite powder;
Step (2), distilled water add the concentrated hydrochloric acid that concentration is 37% and are configured to the hydrochloric acid solution of 5mol/L,
Attapulgite powder in step (1) adds hydrochloric acid solution acidifying, and solid-to-liquid ratio is 1:1.5,40 DEG C of water-bath shakes
Swing 4h, obtain being acidified attapulgite solution;
Step (3), by the acidifying attapulgite solution in step (2) in 40 DEG C, centrifugal 20min under 9000g,
Take precipitation vacuum drying to obtain being acidified attapulgite powder;
Step (4), toluene solution add double-(the silica-based propyl group of γ-triethoxy) tetrasulfide KH-858
It is configured to silane coupler solution, pours in flask, wherein, silane coupler KH-858 and step (3)
In obtain acidifying attapulgite powder mass ratio be 1:5.5;
The acidifying attapulgite powder obtained in step (3) is joined in silane coupler solution, flask is put
It is placed in electric jacket and is heated to isothermal reaction 4h after solution boiling, stop heating;
Drying will be positioned in 105 DEG C of baking ovens after coupling agent modified attapulgite powder solution for vacuum sucking filtration
4h obtains there is modified attapulgite granule;
Step (5), polyacrylonitrile powder is dissolved in dimethyl sulfoxide it is configured to polyacrylonitrile solution, poly-
Acrylonitrile concentration is 12%, adds coupling agent modified attapulgite powder and obtain polyacrylonitrile in polyacrylonitrile solution
/ attapulgite solution, this modified attapulgite concentration is 5%, with scraper by polyacrylonitrile/attapulgite solution at glass
Uniformly paint the film that thickness is 65 μm on plate, at 80 DEG C, this glass plate is positioned in vacuum drying oven drying 36h;
This film is taken off from glass plate, with milli-Q water 4 times, puts into drying 24h in 65 DEG C of baking ovens,
Prepare polyacrylonitrile/attapulgite composite membrane.
Heavy metal in water repair materials prepared by the inventive method, makes attapulgite crystal ratio by acidification
Surface increases, and is effectively increased absorbability;Silane coupler can produce a large amount of silicone hydroxyl when hydrolysis,
These silicone hydroxyl can produce condensation with attapulgite surface silanol group, or the silicone hydroxyl of silane coupler is certainly
Body is condensed, and is covered in attapulgite surface, its configuration of surface modified and character, forms new network structure;
Organically-modified attapulgite is joined simultaneously and polyacrylonitrile solution is made polyacrylonitrile/attapulgite composite membrane,
Can be with the heavy metal in active adsorption water body.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art
Described specific embodiment is made various amendment or supplements or use similar mode to substitute, as long as
Without departing from inventing or surmounting scope defined in the claims, protection scope of the present invention all should be belonged to.
Claims (7)
1. the preparation method of the attapulgite repair materials being applicable to heavy metal pollution of water body, it is characterised in that
Comprise the following specific steps that:
Step (1), attapulgite is ground and sieves, obtain attapulgite powder;
Step (2), by described step (1) attapulgite powder add hydrochloric acid solution acidifying, solid-to-liquid ratio is
1:1.5, water-bath concussion certain time, obtains being acidified attapulgite solution;
Step (3), it is vacuum dried taking precipitation after the acidifying attapulgite solution centrifugal in described step (2)
To acidifying attapulgite powder;
Step (4), the acidifying attapulgite powder obtained in described step (3) is joined double-(γ-three second
The silica-based propyl group of epoxide) in tetrasulfide KH-858 silane coupler solution, be positioned in electric jacket be heated to molten
Isothermal reaction 4h after liquid boiling, stops heating, obtains organically-modified by this solution for vacuum sucking filtration post-drying afterwards
Concave-convex rod particle;
Step (5), polyacrylonitrile powder is dissolved in dimethyl sulfoxide it is configured to polyacrylonitrile solution, poly-
Acrylonitrile concentration is 12%, adds obtain in described step (4) coupling agent modified in polyacrylonitrile solution
Attapulgite powder obtains polyacrylonitrile/attapulgite solution, and this modified attapulgite concentration is 5%, with scraper by poly-third
Alkene nitrile/attapulgite solution the most uniformly paints the thick film for 50-80 μm, by this glass plate at 80 DEG C
It is positioned in vacuum drying oven drying 24-48h, afterwards by this film washing and drying, prepares polyacrylonitrile/attapulgite
Composite membrane.
A kind of attapulgite repair materials being applicable to heavy metal pollution of water body the most according to claim 1
Preparation method, it is characterised in that use 180 mesh screen in described step (1).
A kind of attapulgite repair materials being applicable to heavy metal pollution of water body the most according to claim 1
Preparation method, it is characterised in that add the concentrated hydrochloric acid that concentration is 37% in described step (2) in distilled water and join
Being set to the hydrochloric acid solution of 5mol/L, in described step (2), bath temperature is 40 DEG C, water-bath concussion the time be
3-5h。
A kind of attapulgite repair materials being applicable to heavy metal pollution of water body the most according to claim 1
Preparation method, it is characterised in that in described step (3), centrifuging temperature is 40 DEG C, centrifugal rotational speed is 9000g,
Centrifugation time is 20min.
A kind of attapulgite repair materials being applicable to heavy metal pollution of water body the most according to claim 1
Preparation method, it is characterised in that add double-(γ-triethoxysilicane in described step (4) in toluene solution
Base propyl group) tetrasulfide KH-858 is configured to silane coupler solution, wherein, silane coupler KH-858
It is 1:5.5 with the mass ratio of the acidifying attapulgite powder obtained in described step (3).
A kind of attapulgite repair materials being applicable to heavy metal pollution of water body the most according to claim 1
Preparation method, it is characterised in that drying temperature in described step (4) is 105 DEG C, and drying time is 4h.
The preparation of a kind of attapulgite repair materials being applicable to heavy metal pollution of water body the most according to claim 1
Method, it is characterised in that use milli-Q water 3-5 time in described step (5), in described step (5)
Drying temperature and be 50-80 DEG C, drying time is 24h.
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CN107936981A (en) * | 2017-11-15 | 2018-04-20 | 中国环境科学研究院 | Soil heavy metal combined passivator and preparation method thereof, application method and application |
CN108499517A (en) * | 2018-04-17 | 2018-09-07 | 湖南师范大学 | Fiber glass waste modification prepares the method for metal-chelator and the application of metal-chelator |
CN109261129A (en) * | 2018-11-21 | 2019-01-25 | 河西学院 | Attapulgite synergistic adsorbent and its preparation method and application |
CN111659343A (en) * | 2020-06-16 | 2020-09-15 | 明光春计高分子材料有限公司 | Preparation method of attapulgite nanocomposite |
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CN107936981A (en) * | 2017-11-15 | 2018-04-20 | 中国环境科学研究院 | Soil heavy metal combined passivator and preparation method thereof, application method and application |
CN108499517A (en) * | 2018-04-17 | 2018-09-07 | 湖南师范大学 | Fiber glass waste modification prepares the method for metal-chelator and the application of metal-chelator |
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CN109261129B (en) * | 2018-11-21 | 2021-10-29 | 河西学院 | Attapulgite synergistic adsorbent and preparation method and application thereof |
CN111659343A (en) * | 2020-06-16 | 2020-09-15 | 明光春计高分子材料有限公司 | Preparation method of attapulgite nanocomposite |
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