CN106238003A - A kind of Kaolin/Chitosan Composites and its preparation method and application - Google Patents
A kind of Kaolin/Chitosan Composites and its preparation method and application Download PDFInfo
- Publication number
- CN106238003A CN106238003A CN201610768174.1A CN201610768174A CN106238003A CN 106238003 A CN106238003 A CN 106238003A CN 201610768174 A CN201610768174 A CN 201610768174A CN 106238003 A CN106238003 A CN 106238003A
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- China
- Prior art keywords
- kaolin
- chitosan
- preparation
- composite
- dimethyl sulfoxide
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Classifications
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
-
- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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 present invention relates to a kind of modified kaolin/Chitosan Composites and its production and use.Described composite contains Kaolin, chitosan and dimethyl sulfoxide.Described preparation method includes: 1) be dissolved in weakly acidic aqueous solution by chitosan, then it is mixed with dimethyl sulfoxide (DMSO), obtains mixed solution；2) by Kaolin and step 1) in the mixed solution that obtains mix, reacting by heating, obtain described composite.Composite of the present invention has good absorption property to copper ion, it is adaptable to waste water processes；It can be prepared at ambient pressure, and reaction condition is gentle, and technique is simple, and preparation process is easy to control, has a good application prospect.
Description
Technical field
The present invention relates to the technical field that Heavy-metal Polluted Environment is repaired, be specifically related to a kind of Kaolin/chitosan and be combined
Material and preparation method thereof and as heavy metal absorbent apply.
Background technology
Heavy metal wastewater thereby refers to arrange in the industrial processes such as mining, metallurgy, machine-building, chemical industry, electronics, instrument
The waste water containing heavy metal gone out.Generally use certain methods that heavy metal in dissolved state in waste water is transformed into the metal of indissoluble
Compound or simple substance, remove, such as neutralization precipitation method, sulphide precipitation, floating through methods such as precipitation or upper flotation from waste water
Partition method, electrodeposit (or floating) method, diaphragm process etc., also have and the heavy metal in waste water do not changed its chemical form
Under conditions of concentrate and separate, such as hyperfiltration, electroosmose process, evaporation and ion exchange etc., these methods all have
There are respective advantage and limitation.
Heavy metal in water body is due to the non-biodegradable of itself, easily to water body and plant migration, rich by organism
Collection, endangers the healthy of the mankind finally by food chain.Therefore, the heavy metal in water body is that a class potential hazard is the biggest
Pollutant.
Chitosan is unique recyclability alkaline polysaccharide in nature, has preferable film property, heat stability and good
Good adsorptivity.Chitosan has chelating adsorption to many materials, the amino in its molecule and the hydroxyl adjacent with amino
Stable chelate can be formed with many kinds of metal ions, therefore can be used for administering heavy metal wastewater thereby or in hydrometallurgy, separating metal
Ion.
Kaolinic principle active component is kaolinite, its aqueous aluminosilicate being made up of multi mineral, crystallization
Formula is 2SiO2·Al2O3·2H2O, wherein H2O exists with-OH form.Kaolin has certain cation commutativity, absorption
Property.Kaolin is widely distributed in China, and cheap, is a kind of preferably natural minerals adsorbent.
Utilize the respective advantage of chitosan, Kaolin, prior art has had tried to chitosan loaded at Kaolin
On, prepare composite adsorbing material, i.e. can improve kaolinic utilization rate, the use cost of chitosan can be reduced again, make
It has higher adsorption effect within the specific limits (see Liu Rong perfume etc., " the chromium slag contaminated underground of kaoline loaded treatment with chitosan
Water ", Treatment of Industrial Water, the 5th phase of volume 32,2012).But the chitosan loaded rate of this composite adsorbing material is relatively low, compound
Material absorbability is more weak.
Summary of the invention
An object of the present invention is to provide a kind of modified kaolin/Chitosan Composites.
A further object of the present invention is to provide the preparation method of a kind of modified kaolin/Chitosan Composites.
It is still another object of the present invention to provide the application of a kind of modified kaolin/Chitosan Composites.
The object of the invention is achieved by following technical solution:
A kind of modified kaolin/Chitosan Composites, it is characterised in that described composite contains Kaolin, shell gathers
Sugar and dimethyl sulfoxide.
According to the present invention, described chitosan and dimethyl sulfoxide load on the kaolin.
According to the present invention, described Kaolin is preferably Coaseries kaolin, with coal symbiosis, association.Described kaolinic particle diameter
It is preferably: (200 mesh sieve) below 75 μm.
Present invention also offers the preparation method of a kind of modification of chitosan/kaolin composite material, comprise the following steps:
1) chitosan is dissolved in weakly acidic aqueous solution, then it is mixed with dimethyl sulfoxide (DMSO), obtain mixed solution；
2) by Kaolin and step 1) in the mixed solution that obtains mix, reacting by heating, obtain modified kaolin/chitosan
Composite.
According to the present invention, in step 1) in, the method in weakly acidic aqueous solution that dissolves the chitosan in can be prior art
In any known process, such as, in the range of temperature is 50～100 DEG C (such as 60～80 DEG C) stir 5～8h.Described weak acid
The mass concentration of aqueous solution is 0.5～3wt%, preferably 1wt%.Described weak acid includes but not limited to acetic acid, metasilicic acid, carbonic acid
Deng；Preferably acetic acid.
According to the present invention, in step 1) in, described chitosan is in the mixed solution containing chitosan and dimethyl sulfoxide
Mass concentration be 10～50g/L, preferably 20g/L.The volume ratio of described weakly acidic aqueous solution and dimethyl sulfoxide be 0:10～
5:5, preferably 1:9 and 2:8.
According to the present invention, in step 2) in, described Kaolin is at the mixed solution containing chitosan and dimethyl sulfoxide
In mass concentration be 100～500g/L, preferably 200g/L.Described reaction temperature is 60～150 DEG C, preferably 80～130 DEG C, example
Such as 90 DEG C, 100 DEG C.Response time is preferably 4～10 hours, more preferably 6～8 hours.
According to the present invention, in step 2) in, described Kaolin the most first carries out pretreatment, and the method for described pretreatment is,
Being pulverized and sieved by Kaolin, described grit number of crossing is preferably 10～300 mesh, more preferably 200 mesh (～75 μm).Preferably sieve after bake
Dry (such as under the conditions of 80 DEG C).
According to the present invention, in step 2) in, after described reaction terminates, by reactant liquor centrifugation, obtain solid, then will be solid
Body washing, dry (such as 50 DEG C vacuum drying), obtain modified kaolin/Chitosan Composites.
According to the present invention, described preparation method comprises the following steps:
1) adding chitosan in aqueous acetic acid, 80 DEG C are stirred 5～8 hours, mix with dimethyl sulfoxide afterwards,
To mixed solution.
2) take Kaolin to pulverize and sieve, join step 1) in the mixed solution that obtains, little in 100 DEG C of heated and stirred 6
It is centrifuged time after, makes solid precipitation separate from liquid, abandoning supernatant, then washing of precipitate (is such as washed with deionized water
Wash 3 times), it is dried (such as 50 DEG C vacuum drying), grinds, obtain modified kaolin/Chitosan Composites of the present invention.
In the composite of the present invention, chitosan, dimethyl sulfoxide preferably disperse and are compounded in kaolin surface or layer
Between；Dimethyl sulfoxide can be directly inserted into Coaseries kaolin interlayer, kaolinic interlamellar spacing is widened, thus improves composite wood
The absorbability of material.And dimethyl sulfoxide enters Kaolin interlayer to chitosan and serves important instrumentality, in preparation
In, by adding dimethyl sulfoxide, utilize physics and chemisorption, polar micromolecules dimethyl sulfoxide to be directly inserted into coal
It is Kaolin interlayer, and the chitosan simultaneously carrying low-molecular-weight secretly is inserted into the stratiform Coaseries kaolin with two-dimensional space structure
Interlamination region, make the load factor of chitosan be improved.
Modified kaolin/the Chitosan Composites of the present invention has chitosan loaded rate height, compound absorbing material absorption
The features such as ability is strong.Contaminant metal ions in energy active adsorption heavy metal wastewater thereby, such as Cu2+, can be applicable to containing metal from
The waste water of son processes.Particularly, under conditions of simulated wastewater, to Cu2+Adsorbing and removing effect is obvious, and initial concentration is by it
The Cu of 50mg/L2+Adsorption rate is up to 19%～26%.The process of actual waste water has a good application prospect.
Present invention also offers the purposes of described modified kaolin/Chitosan Composites, it is used for Adsorption of Heavy Metals, example
Such as Adsorption of Heavy Metals in sewage disposal.Preferably, described composite is for the absorption of copper ion.
The beneficial effects of the present invention is:
1. modified kaolin/the Chitosan Composites of the present invention has higher chitosan loaded rate, high adsorption capacity.
2. the composite of the present invention has that preparation technology is simple, reaction condition is gentle, technological parameter is easily controllable, raw material
Aboundresources, the advantage such as cheap.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction phenogram, (a) be Kaolin original soil, (b) be the modified kaolin/shell of embodiment 1 preparation
Polysaccharide composite material, (c) are the modified kaolin/Chitosan Composites of embodiment 2 preparation.
Fig. 2 is the modified kaolin/Chitosan Composites scanning electron microscope/X-ray energy spectrum (SEM/ of embodiment 1 preparation
EDS) phenogram.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Accompanying drawing, the present invention is described in more detail.But those skilled in the art know, the invention is not limited in accompanying drawing and following reality
Execute example.
Embodiment 1
The preparation of modified kaolin/Chitosan Composites
1) take Coaseries kaolin attrition grinding, cross 200 mesh sieves, dry under the conditions of 80 DEG C, standby.
2) taking 2.0g chitosan in round-bottomed flask, adding 20mL volume fraction is the aqueous acetic acid of 1%, in 80 DEG C of constant temperature
Strong stirring 6h in oil bath, after cooling, stirs and is slowly added to 80mL DMSO mixing.
3) 20g Coaseries kaolin is joined step 2) in the solution containing chitosan and DMSO for preparing, in
100 DEG C of heated and stirred 6h, room temperature stand and centrifugation, make solid precipitation separate from solution, then precipitation is spent from
Sub-water washs 3 times, in 50 DEG C of vacuum drying, obtains described composite after grinding uniformly.
The X-ray diffractogram of the composite of embodiment 1 preparation sees Fig. 1, and (a) is Kaolin original soil, (b) in FIG
The composite prepared for the present embodiment (embodiment 1).By (a) and (b) it can be seen that at the diffraction that the angle of diffraction is about 12 °
The intensity at peak has weakened, and the characteristic diffraction peak that part is corresponding to (001) crystal face moves to the low angle direction of about 7 °
Dynamic, illustrate modified DMSO and chitosan intercalation to Kaolin interlayer so that Kaolin interlamellar spacing becomes greatly, by original
0.72nm increases to about 1.12nm.
Scanning electron microscope/X-ray energy spectrum (SEM/EDS) phenogram of the composite of embodiment 1 preparation sees Fig. 2.By Fig. 2
In it can be seen that containing the element such as S and N ,-NH during wherein N comes from chitosan in composite2Functional group, S comes from
DMSO, from its distribution situation it can be seen that chitosan and DMSO are evenly distributed in kaolinic surface and interlayer.
Embodiment 2
The preparation of modified kaolin/Chitosan Composites
1) take Coaseries kaolin attrition grinding, cross 200 mesh sieves, dry under the conditions of 80 DEG C, standby.
2) taking 2.0g chitosan in round-bottomed flask, adding 10mL volume fraction is the aqueous acetic acid of 1%, in 80 DEG C of constant temperature
Strong stirring 6h in oil bath, after cooling, stirs and is slowly added to 90mL DMSO mixing.
3) 20g Coaseries kaolin is joined step 2) in the solution containing chitosan and DMSO for preparing, in
100 DEG C of heated and stirred 6h, room temperature stand and centrifugation, make solid precipitation separate from solution, then precipitation is spent from
Sub-water washs 3 times, in 50 DEG C of vacuum drying, obtains described composite after grinding uniformly.
The X-ray diffractogram of the composite of embodiment 2 preparation sees Fig. 2, and (a) is Kaolin original soil, (c) in fig. 2
The composite prepared for the present embodiment (embodiment 2).By (c) it can be seen that its composite prepared with embodiment 1
X-ray diffractogram (b) be similar to, the intensity in the diffraction maximum that the angle of diffraction is about 12 ° has weakened, and part (001) crystal face
Corresponding characteristic diffraction peak moves to the low angle direction of about 7 °, illustrates that modified DMSO and chitosan intercalation are to high
Between the soil layer of ridge, so that Kaolin interlamellar spacing is increased to about 1.12nm by original 0.72nm.
Scanning electron microscope/X-ray energy spectrum (SEM/EDS) phenogram of the composite of embodiment 2 preparation and embodiment 1 class
Seemingly.
It is right modified kaolin/Chitosan Composites prepared by embodiment 1 and 2 and Kaolin original soil to be carried out respectively
Cu2+Simulated solution static adsorption contrast experiment, wherein Cu2+Cu in simulated solution2+Initial concentration be 50mg/L, experimental result
It is shown in Table 1.
Table 1 modified kaolin/Chitosan Composites is to Cu2+Absorption property contrast and experiment
Above, embodiments of the present invention are illustrated.But, the present invention is not limited to above-mentioned embodiment.All
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. done, should be included in the guarantor of the present invention
Within the scope of protecting.
Claims (10)
1. modified kaolin/Chitosan Composites, it is characterised in that: described composite contains Kaolin, chitosan
And dimethyl sulfoxide.
Composite the most according to claim 1, it is characterised in that: described Kaolin is preferably Coaseries kaolin, described
Kaolinic particle diameter is preferably below 75 μm.
3. the preparation method of the composite described in claim 1 or 2, including:
1) chitosan is dissolved in weakly acidic aqueous solution, then it is mixed with dimethyl sulfoxide (DMSO), obtain mixed solution；
2) by Kaolin and step 1) in the mixed solution that obtains mix, reacting by heating, obtain modified kaolin/chitosan and be combined
Material.
Preparation method the most according to claim 3, it is characterised in that: step 1) in, dissolve the chitosan in weak acid water-soluble
Method in liquid is: stir 5～8h in the range of temperature is 50～100 DEG C (such as 60～80 DEG C).
5. according to the preparation method described in claim 3 or 4, it is characterised in that: in step 1) in, the matter of described weakly acidic aqueous solution
Amount concentration is 0.5～3wt%, preferably 1wt%；Described weak acid is preferably acetic acid, metasilicic acid, carbonic acid etc.；
Preferably, in step 1) in, described chitosan mass concentration in the mixed liquor containing chitosan and dimethyl sulfoxide
It is 10～50g/L, preferably 20g/L.Described weakly acidic aqueous solution is 0:10～5:5, preferably 1:9 with the volume ratio of dimethyl sulfoxide
And 2:8.
6. according to the preparation method described in claim 3 or 4, it is characterised in that: in step 2) in, described Kaolin is containing
Mass concentration in the mixed solution of chitosan and dimethyl sulfoxide is 100～500g/L, preferably 200g/L.Described reaction temperature
It is 60～150 DEG C, preferably 80～130 DEG C, such as 90 DEG C, 100 DEG C；The described response time be preferably 4～10h, more preferably 6～
8h。
7. according to the preparation method described in claim 3 or 4, it is characterised in that: in step 2) in, described Kaolin first carries out pre-
Processing, the method for described pretreatment is, is pulverized and sieved by Kaolin, and described grit number of crossing is preferably 10～300 mesh, more preferably
200 mesh (～75 μm).
Preferably, in step 2) in, after described reaction terminates, by reactant liquor centrifugation, obtain solid, then solid is washed,
It is dried (such as 50 DEG C vacuum drying), obtains modified kaolin/Chitosan Composites.
8. according to the preparation method described in claim 3 or 4, it is characterised in that: described preparation method comprises the following steps:
1) add chitosan in aqueous acetic acid, 80 DEG C of stirrings 5～8h, mix with dimethyl sulfoxide afterwards, mixed
Solution；
2) take Kaolin to pulverize and sieve, join step 1) in the mixed solution that obtains, after 100 DEG C of heated and stirred 6h from
The heart, makes solid precipitation separate from liquid, abandoning supernatant, then by washing of precipitate (being such as washed with deionized 3 times),
It is dried (such as 50 DEG C vacuum drying), grinds, obtain described modified kaolin/Chitosan Composites.
9. the purposes of the composite described in claim 1 or 2, it is characterised in that: for Adsorption of Heavy Metals, such as at sewage
Adsorption of Heavy Metals in reason.Preferably, described composite is for the absorption of copper ion.
10. a method of wastewater treatment, it is characterised in that: use the composite described in claim 1 or 2 to process waste water,
Preferably, described waste water is containing Cu2+Waste water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265750A (en) * | 2018-08-28 | 2019-01-25 | 安徽江淮汽车集团股份有限公司 | A kind of antibacterial agent and preparation method thereof |
| CN109467385A (en) * | 2018-01-15 | 2019-03-15 | 杭州创屹机电科技有限公司 | A kind of antibacterial environment protection 3D printing ceramic material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109467385A (en) * | 2018-01-15 | 2019-03-15 | 杭州创屹机电科技有限公司 | A kind of antibacterial environment protection 3D printing ceramic material and preparation method thereof |
| CN109467385B (en) * | 2018-01-15 | 2021-09-03 | 杭州创屹机电科技有限公司 | Antibacterial environment-friendly 3D printing ceramic material and preparation method thereof |
| CN109265750A (en) * | 2018-08-28 | 2019-01-25 | 安徽江淮汽车集团股份有限公司 | A kind of antibacterial agent and preparation method thereof |
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