CN109420481A - A kind of modified MMT/C nano-complex and preparation method thereof - Google Patents
A kind of modified MMT/C nano-complex and preparation method thereof Download PDFInfo
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- CN109420481A CN109420481A CN201710755785.7A CN201710755785A CN109420481A CN 109420481 A CN109420481 A CN 109420481A CN 201710755785 A CN201710755785 A CN 201710755785A CN 109420481 A CN109420481 A CN 109420481A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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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- 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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- 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
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
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- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
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- Geochemistry & Mineralogy (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of modified MMT/C nano-complex and preparation method thereof, by 10-20 parts of montmorillonite through purifying and sodium after, and 10-50 parts of glucose, using montmorillonite carbon made from hydrothermal carbonization method (MMT C) composite material.The compound, impurity content is low, and high to heavy metal adsorption amount, environmental pollution is small, simple process, high production efficiency；With great social benefit and environmental benefit.
Description
Technical field
The present invention relates to montmorillonite composite material technical field, specifically a kind of modified MMT/C nano-complex and its
Preparation method.
Background technique
In recent decades, with the continuous development of China's industry, such as metal plating industry, mining, fertilizer industry, print
Dye-works, tannery, insecticide factory, paper mill, textile industry etc., more and more heavy metal wastewater therebies are directly or indirectly discharged into ring
In border, especially in some remote sites.Unlike organic pollutant, heavy metal cannot be degraded by biology, and be easy in life
Enrichment, can also convert into the bigger methyl compound of toxicity in object, more than will cause to seriously threaten to organism after a certain amount of.
For example lead can cause nervous system damage, can also damage kidney, liver and reproductive system and basic cell work and big
Brain function；Nickel is more than that its critical level may be brought other than digestive discomfort, also will cause serious lung and kidney problems, and
Skin dermatitis.Therefore, the concern which results in people to heavy metal pollution of water body.
Clay is referred to as " universal material ", is increasingly paid attention to by people.It is according to statistics, reachable for bentonitic purposes
More than 400 kinds, purification and decoloration agent, binder, thixotropic agent, suspending agent, stabilizer, filling material, feed, catalyst etc. can be done, extensively
For fields such as agriculture, light industry and cosmetics, drugs.In China, although bentonite resource is very rich, add up exploitation
Amount is less than the l% of proved reserves, is the situation of a kind of " low go out high into " in the international market, i.e., outlet after-product (raw ore,
Casting use, drilling well use, low-grade atlapulgite etc.), import high-grade products (washing powder softener, high-grade organoclay etc.).Although swollen
Moisten the native exploitation in terms of purification of water quality and sewage treatment and using oneself through having made some progress, but it is efficiently honest and clean to still need to exploitation
Valence, physicochemical properties are stable and can be with industrialized adsorbent or flocculant.Modification to clay, and its to pollutant
Absorption research is more and more, has become one of heat subject.
It is although cheap and easy to get in clay mineral, but in the progress of absorption heavy metal, there is also some problems and
Problem: 1) clay mineral is impure more, such as metal oxide, organic matter, causes its limited sorption capacity；2) some clays
Mineral needs are further processed and could use, and if bentonite needs to purify, concave convex rod needs brilliant beam dissociation；3) powdered viscous
Soil is swollen after water suction, forms mud, it is difficult to be separated by solid-liquid separation, while cause secondary pollution to environment；4) clay mineral surface
Functional group is few, and specific surface area is little, smaller to heavy metal adsorption amount.
Summary of the invention
The purpose of the present invention is to provide a kind of modified MMT/C nano-complex and preparation method thereof, the compound
Impurity content is low, high to heavy metal adsorption amount, and environmental pollution is small.
Realizing the technical solution of the object of the invention is:
A kind of modified MMT/C nano-complex, is made of the raw material of following weight:
10-20 parts of montmorillonite；
10-50 parts of glucose.
The glucose is Dextrose Monohydrate.
A kind of preparation method of modified MMT/C nano-complex, specifically comprises the following steps:
1) purifying of montmorillonite:
10-20 parts of montmorillonite powder are taken, ultrapure water is added, quickly stirs evenly, is then allowed to stand, after being layered, by bottom residues
It outwells, stays upper layer turbid solution stand-by, 4 times repeatedly, upper layer turbid solution obtained above be centrifuged at a high speed 5
Minute, supernatant liquor is outwelled, layer slurries of keeping on file are stand-by, 3 times repeatedly, are finally dried to obtain the montmorillonite of high-purity；
2) sodium of montmorillonite
The montmorillonite of high-purity after purification in step 1) is taken, ultrapure water is added, is slowly stirred to form uniform mixed liquor, chlorination is added
Sodium solid, after at the uniform velocity stirring 12 h, be centrifuged at a high speed mixed liquor, outwells supernatant liquor after 10 minutes.Again it adds identical
The NaCl solution of concentration 4 times repeatedly, guarantees that the cation exchange site point of montmorillonite is saturated by Na+ ion, will obtain
Sodium-based montmorillonite be centrifuged repeatedly flushing with ultrapure water, until centrifugation after supernatant liquor barium nitrate solution negative test can not examine
Until measuring chloride ion, 200 mesh sieve are finally crossed after 60 DEG C of drying in oven 12h, mechanical disruption, obtain dry powder
Last shape sodium-based montmorillonite (Na-MMT)；
3) preparation of function dough MMT/C nanocomposite
Na-MMT made from step 2 is added in ultrapure water, 1 h of ultrasonic disperse is then slowly added into glucose 10-50
Part, magnetic agitation 50min forms uniform mixed liquor, mixed liquor is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, filling rate is about 85%, tightens container, is put into 200 DEG C of baking oven and reacts 24 h, and wait hydrothermal reaction kettles to be cooled to room temperature, from
The isolated product of the heart is alternately rinsed 4 times with ultrapure water and ethyl alcohol, removes responseless glucose, dry by 60 °C
Dry, grinding, crosses 200 mesh sieve, obtains montmorillonitic clay/carbon composite (MMT/C)；
By above-mentioned steps, modified MMT/C nano-complex is successfully prepared.
In step 1) and step 2, the high speed centrifugation, centrifugation rate is 5000 r/min.
In step 2, the montmorillonite of high-purity and the mass ratio of sodium chloride are 10:1.
The utility model has the advantages that modified MMT/C nano-complex prepared by the present invention, impurity content is low, to heavy metal adsorption amount
Height, environmental pollution is small, simple process, high production efficiency；With great social benefit and environmental benefit.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below, but is not limitation of the invention.
Embodiment 1
200 g of montmorillonite powder is weighed, 2000 m L of ultrapure water is added, quickly stirs evenly, is then allowed to stand, it, will after being layered
Bottom residues are outwelled, and stay upper layer turbid solution stand-by, and 4 times repeatedly.Upper layer turbid solution obtained above is subjected to high speed
(5000 r/min) is centrifugated 5 minutes, outwells supernatant liquor, layer slurries of keeping on file are stand-by, 3 times repeatedly, finally do
The dry montmorillonite for obtaining high-purity.100g high-purity montmorillonite powder is added in the large beaker of 1500 m L, is added super
1000 m L of pure water, is slowly stirred to form uniform mixed liquor, is then 10:1 according to mass ratio, solid sodium chloride is added
10 g, remain a constant speed 12 h of stirring, and high speed (5000 r/min) is centrifugated mixed liquor, it is clear to outwell upper layer after 10 minutes
Liquid.
Again the Na Cl solution for adding same concentrations, 4 times repeatedly, guarantees the cation exchange site of montmorillonite
Point is by Na+
Ion saturation.Obtained sodium-based montmorillonite is centrifuged repeatedly flushing with ultrapure water, until the supernatant liquor nitre after centrifugation
Until sour barium solution negative test can not detect chloride ion.200 are finally crossed after 60 DEG C of drying in oven 12h, mechanical disruption
Mesh sieve obtains dry powdered sodium-based montmorillonite (Na-MMT).
2) preparation of function dough MMT/C nanocomposite
MMT/C nanocomposite is synthesized using Dextrose Monohydrate as carbon source by a step hydrothermal carbonization method.By 1.5 g Na-
MMT
It is added in 85m L ultrapure water, 1 h of ultrasonic disperse is then slowly added into 5.5 g Dextrose Monohydrates, magnetic agitation
50 min form uniform disperse system.Above-mentioned mixed liquor is transferred to the polytetrafluoroethyllining lining that a volume is 100 m L
Stainless steel cauldron in, filling rate is about 85%, tightens container, is put into 200 DEG C of baking oven and reacts 24 h.Etc. hydro-thermals it is anti-
Kettle is answered to be cooled to room temperature, the product being centrifugally separating to obtain alternately is rinsed 4 times with ultrapure water and ethyl alcohol, removed responseless
Glucose.By 60 °C of dryings, grinding, 200 mesh sieve are crossed, montmorillonitic clay/carbon composite (MMT/C) is obtained.
Claims (6)
1. a kind of modified MMT/C nano-complex, which is characterized in that be made of the raw material of following weight:
10-20 parts of montmorillonite；
10-50 parts of glucose.
2. a kind of modified MMT/C nano-complex according to claim 1, which is characterized in that the glucose is
Dextrose Monohydrate.
3. a kind of preparation method of modified MMT/C nano-complex, which is characterized in that specifically comprise the following steps:
The purifying of montmorillonite:
10-20 parts of montmorillonite powder are taken, ultrapure water is added, quickly stirs evenly, is then allowed to stand, after being layered, by bottom residues
It outwells, stays upper layer turbid solution stand-by, 4 times repeatedly, upper layer turbid solution obtained above be centrifuged at a high speed 5
Minute, supernatant liquor is outwelled, layer slurries of keeping on file are stand-by, 3 times repeatedly, are finally dried to obtain the montmorillonite of high-purity；
The sodium of montmorillonite
The montmorillonite of high-purity after purification in step 1) is taken, ultrapure water is added, is slowly stirred to form uniform mixed liquor, chlorination is added
Sodium solid, after at the uniform velocity stirring 12 h, be centrifuged at a high speed mixed liquor, outwells supernatant liquor after 10 minutes.
4. adding the NaCl solution of same concentrations again, 4 times repeatedly, guarantee the cation exchange site point quilt of montmorillonite
Na+ ion saturation, is centrifuged repeatedly flushing with ultrapure water for obtained sodium-based montmorillonite, until the supernatant liquor nitric acid after centrifugation
Until the negative test of barium solution can not detect chloride ion, 200 mesh are finally crossed after 60 DEG C of drying in oven 12h, mechanical disruption
Sieve obtains dry powdered sodium-based montmorillonite (Na-MMT)；
3) preparation of function dough MMT/C nanocomposite
Na-MMT made from step 2 is added in ultrapure water, 1 h of ultrasonic disperse is then slowly added into glucose 10-50
Part, magnetic agitation 50min forms uniform mixed liquor, mixed liquor is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, filling rate is about 85%, tightens container, is put into 200 DEG C of baking oven and reacts 24 h, and wait hydrothermal reaction kettles to be cooled to room temperature, from
The isolated product of the heart is alternately rinsed 4 times with ultrapure water and ethyl alcohol, removes responseless glucose, dry by 60 °C
Dry, grinding, crosses 200 mesh sieve, obtains montmorillonitic clay/carbon composite (MMT/C)；
By above-mentioned steps, modified MMT/C nano-complex is successfully prepared.
5. a kind of preparation method of modified MMT/C nano-complex according to claim 3, which is characterized in that step
1) and in step 2, the high speed centrifugation, centrifugation rate is 5000 r/min.
6. a kind of preparation method of modified MMT/C nano-complex according to claim 3, which is characterized in that step
2) in, the montmorillonite of high-purity and the mass ratio of sodium chloride are 10:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710755785.7A CN109420481A (en) | 2017-08-29 | 2017-08-29 | A kind of modified MMT/C nano-complex and preparation method thereof |
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| CN201710755785.7A CN109420481A (en) | 2017-08-29 | 2017-08-29 | A kind of modified MMT/C nano-complex and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496599A (en) * | 2019-07-25 | 2019-11-26 | 南方科技大学 | Compound adsorbent and the preparation method and application thereof |
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| CN101774599A (en) * | 2009-01-08 | 2010-07-14 | 浙江海力生制药有限公司 | Modified na-montmorillonite, preparation method and application thereof |
| CN103263896A (en) * | 2013-05-30 | 2013-08-28 | 新疆大学 | Cellulose-based polymer/montmorillonite nano composite adsorption material and preparation method thereof |
| CN104841373A (en) * | 2015-04-21 | 2015-08-19 | 蚌埠德美过滤技术有限公司 | Montmorillonite/nanometer titanium dioxide composite adsorption filtering agent and preparation method thereof |
| CN105921108A (en) * | 2016-05-28 | 2016-09-07 | 中国科学院新疆理化技术研究所 | Preparation method and application of montmorillonoid and carbon composite material |
| CN106861607A (en) * | 2017-03-17 | 2017-06-20 | 武汉理工大学 | A kind of preparation method of the modified carbon/montmorillonite Composite sorbing material of organic-inorganic |
| CN107987290A (en) * | 2017-11-23 | 2018-05-04 | 内蒙古农业大学 | A kind of nano lignocellulose/montmorillonite composite material and its preparation and application |
-
2017
- 2017-08-29 CN CN201710755785.7A patent/CN109420481A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774599A (en) * | 2009-01-08 | 2010-07-14 | 浙江海力生制药有限公司 | Modified na-montmorillonite, preparation method and application thereof |
| CN103263896A (en) * | 2013-05-30 | 2013-08-28 | 新疆大学 | Cellulose-based polymer/montmorillonite nano composite adsorption material and preparation method thereof |
| CN104841373A (en) * | 2015-04-21 | 2015-08-19 | 蚌埠德美过滤技术有限公司 | Montmorillonite/nanometer titanium dioxide composite adsorption filtering agent and preparation method thereof |
| CN105921108A (en) * | 2016-05-28 | 2016-09-07 | 中国科学院新疆理化技术研究所 | Preparation method and application of montmorillonoid and carbon composite material |
| CN106861607A (en) * | 2017-03-17 | 2017-06-20 | 武汉理工大学 | A kind of preparation method of the modified carbon/montmorillonite Composite sorbing material of organic-inorganic |
| CN107987290A (en) * | 2017-11-23 | 2018-05-04 | 内蒙古农业大学 | A kind of nano lignocellulose/montmorillonite composite material and its preparation and application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496599A (en) * | 2019-07-25 | 2019-11-26 | 南方科技大学 | Compound adsorbent and the preparation method and application thereof |
| CN110496599B (en) * | 2019-07-25 | 2022-08-23 | 南方科技大学 | Composite adsorbent and preparation method and application thereof |
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