CN107029676A - A kind of preparation method of carboxymethyl chitosan organo montmorillonite heavy metal absorbent - Google Patents
A kind of preparation method of carboxymethyl chitosan organo montmorillonite heavy metal absorbent Download PDFInfo
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- CN107029676A CN107029676A CN201710297906.8A CN201710297906A CN107029676A CN 107029676 A CN107029676 A CN 107029676A CN 201710297906 A CN201710297906 A CN 201710297906A CN 107029676 A CN107029676 A CN 107029676A
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- Prior art keywords
- organo montmorillonite
- heavy metal
- carboxymethyl chitosan
- preparation
- metal absorbent
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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
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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
Abstract
The invention discloses a kind of preparation method of carboxymethyl chitosan organo montmorillonite heavy metal absorbent, step includes：Organo montmorillonite is configured to heating stirring at suspension, 70~80 DEG C, insulation obtains A in 0.5~1 hour；Carboxymethyl chitosan is dissolved in the water to obtain B；A and B is mixed, is sufficiently stirred for after 2~3 hours carrying out humid heat treatment at 70~80 DEG C.Heavy metal absorbent produced by the present invention has the characteristics of pH scope of applications are wide, has more preferable absorption property compared to chitosan organo montmorillonite heavy metal absorbent.
Description
Technical field
It is a kind of carboxymethyl chitosan-organo montmorillonite huge sum of money specifically the invention belongs to technical field of function materials
Belong to the preparation method of adsorbent.
Background technology
The threat of toxic heavy metal in air, soil, water is increasingly becoming global problem, therefore effectively removing has
Malicious heavy metal technology turns into a challenging job.It is normal that high molecular heavy metals ion adsorbent has become a kind of comparison
Under heavy metal containing wastewater treatment medicament, normal temperature within the scope of wider pH can with Hg in waste water, Cd, Cu, Pb, Mn, Ni, Zn,
The contents of many kinds of heavy metal ion such as Cr are reacted rapidly, generate water insoluble flocky precipitate, and precipitation is fast, easily filtering, and stability is high, spirit
Quick property is high, so as to reach the mesh of Adsorption heavy metal ion, has obtained widely should in industries such as plating, electronics, wiring boards
With.At the same time, there is the problem of efficiency and heat endurance are poor, contamination resistance is low, service life is not long in organic adsorbent,
And can be only achieved optimal separating effect it is generally necessary to be used cooperatively with other methods.It is inorganic to inhale compared with organic adsorbent
Attached dose has the advantages that adsorption efficiency height, good chemical stability, acid and alkali-resistance and organic solvent, service life are long.Therefore will be organic
It is a study hotspot in heavy metal adsorption field with the composite that inorganic adsorbent is combined to form.
Carboxymethyl chitosan is that chitosan spreads out with a kind of water soluble chitosan made from chloroacetate reaction in the basic conditions
Biology, due to the broken regularity for having changed its crystal of the introducing of carboxymethyl so that crystallinity is substantially reduced, and adds drawing for hydrophilic radical
Enter, water solubility is significantly improved compared with chitosan, can be dissolved in wider pH range, therefore application expands.Carboxymethyl chitosan
Contain-OH ,-NH in molecule2, the group such as-COOH, can more effectively complexation of metal ions compared with chitosan.
Chinese patent CN101524635B discloses a kind of preparation side of chitosan-organic montmorillonite nano composite material
Method, it is by the method for intercalation by chitosan loaded in the organo montmorillonite piece interlayer with layer structure, obtained nanometer
Composite combines the organic and respective advantage of inorganic adsorbent.However, chitosan can not be directly dissolved in the aqueous solution, can only
It is dissolved in acid solution, and under acid solution, chitosan is easily degraded and the amino on its surface is main with-NH3 +Form
In the presence of being not easy to complexing of metal ion, largely limit its application in wastewater treatment field of purification, and be combined
The absorption property of material need further raising.
The content of the invention
It is an object of the invention to provide a kind of preparation side of carboxymethyl chitosan-organo montmorillonite heavy metal absorbent
Method, the characteristics of organic and inorganic adsorbent is not only combined each by adsorbent made from this method, and further improve
The adsorption capacity of adsorbent.
The present invention is achieved through the following technical solutions：
A kind of preparation method of carboxymethyl chitosan-organo montmorillonite heavy metal absorbent, comprises the following steps：
(1) organo montmorillonite is configured to heating stirring at suspension, 70~80 DEG C, is incubated 0.5~1 hour；
(2) carboxymethyl chitosan is dissolved in the water；
(3) product of step (1) and step (2) is mixed, be sufficiently stirred for 2~3 hours at 70~80 DEG C；
(4) step (3) products therefrom is subjected to humid heat treatment.
Wherein the mass ratio of carboxymethyl chitosan and organo montmorillonite is 1:1~1:5.
It is preferred that, step (1) organo montmorillonite is by cetyl trimethylammonium bromide, octadecyl trimethyl chlorination
Organic montmorillonite obtained by ammonium or didecyl Dimethy ammonium chloride.
It is preferred that, step (2) carboxymethyl chitosan is that range of viscosities gathers in 170~250mpa ﹒ s water-soluble carboxymethyl shell
Sugar.
It is preferred that, step (3) stirring condition is 150r/min.
It is preferred that, the condition of step (4) humid heat treatment is 121 DEG C, 20min.
It is preferred that, the mass ratio 1 of carboxymethyl chitosan and organo montmorillonite:3.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) carboxymethyl chitosan is polyampholyte, because the introducing of carboxyl, improves its dissolubility in water,
Expand the pH scopes of materials'use.
(2) because carboxyl can add the absorption of material with the metallic ion coordination in solution, the introducing of carboxyl
Site density, improves adsorption capacity.
Embodiment
Below by embodiment, the present invention is described in further detail.
Embodiment 1：
The present embodiment provides a kind of preparation method of crosslinked carboxymethyl chitosan-organo montmorillonite heavy metal absorbent, bag
Include following steps：
(1) 3.6g is modified gained organo montmorillonite through cetyl trimethylammonium bromide and is configured to suspension, 70~80
Heating stirring at DEG C, is incubated 0.5~1 hour；
(2) 1.2g carboxymethyl chitosans are dissolved in the water.
(3) product of step (1) and step (2) is mixed, 70~80 DEG C, stir 2~3 hours under 150r/min；
(4) by 121 DEG C of step (3) products therefrom, humid heat treatment is carried out under 20min.
Embodiment 2：
The present embodiment provides a kind of preparation method of crosslinked carboxymethyl chitosan-organo montmorillonite heavy metal absorbent, bag
Include following steps：
(1) 3.6g is modified gained organo montmorillonite through OTAC and is configured to suspension, 70~80
Heating stirring at DEG C, is incubated 0.5~1 hour；
(2) 3.6g carboxymethyl chitosans are dissolved in the water；
(3) product of step (1) and step (2) is mixed, 70~80 DEG C, stir 2~3 hours under 200r/min；
(4) by 121 DEG C of step (3) products therefrom, humid heat treatment is carried out under 20min.
Embodiment 3：
The present embodiment provides a kind of preparation method of crosslinked carboxymethyl chitosan-organo montmorillonite heavy metal absorbent, bag
Include following steps：
(1) 4.5g is configured to suspension, 70~80 through organo montmorillonite obtained by didecyl Dimethy ammonium chloride
Heating stirring at DEG C, is incubated 0.5~1 hour；
(2) 0.9g carboxymethyl chitosans are dissolved in the water；
(3) product of step (1) and step (2) is mixed, 70~80 DEG C, stir 2~3 hours under 100r/min；
(4) by 121 DEG C of step (3) products therefrom, humid heat treatment is carried out under 20min.
Comparative example 1：
The present embodiment provides a kind of preparation method of chitosan-organo montmorillonite heavy metal absorbent, comprises the following steps：
(1) 3.6g is modified gained organo montmorillonite through cetyl trimethylammonium bromide and is configured to suspension, 70~80
Heating stirring at DEG C, is incubated 0.5~1 hour；
(2) 1.2g chitosans are dissolved in the water；
(3) product of step (1) and step (2) is mixed, 70~80 DEG C, stir 2~3 hours under 150r/min；
(4) by 121 DEG C of step (3) products therefrom, humid heat treatment is carried out under 20min；
Comparative example 2：
The present embodiment provides a kind of preparation method of chitosan-organo montmorillonite heavy metal absorbent, comprises the following steps：
(1) 3.6g is configured to suspension, 70~80 through organo montmorillonite obtained by didecyl Dimethy ammonium chloride
Heating stirring at DEG C, is incubated 0.5~1 hour；
(2) 1.2g chitosans are dissolved in the water；
(3) product of step (1) and step (2) is mixed, 70~80 DEG C, stir 2~3 hours under 150r/min；
(4) by 121 DEG C of step (3) products therefrom, humid heat treatment is carried out under 20min；
Using test：
Carboxymethyl chitosan-organo montmorillonite the heavy metal absorbent and comparative example 1~2 prepared respectively to embodiment 1~3
The performance of chitosan-organo montmorillonite heavy metal absorbent processing metal plating waste water detected that specific testing procedure is such as
Under：
The above-mentioned heavy metal absorbent 1.0g prepared is taken respectively, is added to the galvanizer that 100ml contains heavy metal ion
Industry waste water, adjusts the pH=5.7 of solution, at room temperature oscillation treatment 8 hours.After having handled, absorbent filtering is gone out, by atom
Emission spectrometry determines heavy metal ion (Pb in the front and rear metal plating waste water of absorption2+、Ni2+、Cd2+) concentration change.Test knot
Fruit is as shown in table 1.
Table 1
Carboxymethyl chitosan-organo montmorillonite efficient heavy prepared by the present invention is can be seen that from the experimental result of table 1
Much better than chitosan-organo montmorillonite heavy metal absorbent of the effect of adsorbent Adsorption of Heavy Metals ion.
It is described above, be only presently preferred embodiments of the present invention, any formal limitation not done to the present invention, it is every according to
According to the present invention technical spirit above example is made any simple modification, equivalent variations, each fall within the present invention protection
Within the scope of.
Claims (6)
1. the preparation method of a kind of carboxymethyl chitosan-organo montmorillonite heavy metal absorbent, it is characterised in that including following step
Suddenly：
(1) organo montmorillonite is configured to heating stirring at suspension, 70~80 DEG C, is incubated 0.5~1 hour；
(2) carboxymethyl chitosan is dissolved in the water；
(3) product of step (1) and step (2) is mixed, be sufficiently stirred for 2~3 hours at 70~80 DEG C；
(4) step (3) products therefrom is subjected to humid heat treatment；
The wherein mass ratio 1 of carboxymethyl chitosan and organo montmorillonite:1~1:5.
2. a kind of preparation method of carboxymethyl chitosan-organo montmorillonite heavy metal absorbent according to claim 1, its
It is characterised by：Step (1) organo montmorillonite is by cetyl trimethylammonium bromide, OTAC
Or the organic montmorillonite obtained by didecyl Dimethy ammonium chloride.
3. a kind of preparation side of carboxymethyl chitosan-organo montmorillonite heavy metal absorbent according to claim 1 or 2
Method, it is characterised in that：Step (2) carboxymethyl chitosan is water-soluble carboxymethyl of the range of viscosities in 170~250mpa ﹒ s
Chitosan.
4. a kind of preparation method of carboxymethyl chitosan-organo montmorillonite heavy metal absorbent according to claim 3, its
It is characterised by：Step (3) stirring condition is 150r/min.
5. a kind of preparation method of carboxymethyl chitosan-organo montmorillonite heavy metal absorbent according to claim 4, its
It is characterised by：The condition of step (4) humid heat treatment is 121 DEG C, 20min.
6. a kind of preparation method of carboxymethyl chitosan-organo montmorillonite heavy metal absorbent according to claim 5, its
It is characterised by：The mass ratio 1 of the carboxymethyl chitosan and organo montmorillonite:3.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704620A (en) * | 2018-07-02 | 2018-10-26 | 大连理工大学 | The preparation method and application of chitosan/hydrophobic montmorillonite sorbing material of anion in a kind of processing waste water |
| CN110550689A (en) * | 2019-08-26 | 2019-12-10 | 神美科技有限公司 | Organic-inorganic composite heavy metal ion trapping agent |
| CN110756159A (en) * | 2019-11-06 | 2020-02-07 | 中山职业技术学院 | Preparation method of high-performance modified sodium bentonite nano composite adsorption material |
| CN112779019A (en) * | 2021-01-07 | 2021-05-11 | 何雨昕 | Soil conditioner for enhancing stress resistance of crops and preparation method thereof |
| CN115501860A (en) * | 2022-11-09 | 2022-12-23 | 江西理工大学 | Preparation method of composite modified montmorillonite for adsorbing heavy metal ions of anions/cations |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077795A (en) * | 2006-05-22 | 2007-11-28 | 北京化工大学 | Composite biological adsorption and preparing method thereof |
| CN101524635A (en) * | 2009-03-28 | 2009-09-09 | 大连理工大学 | Method for preparing chitosan/organo montmorillonite nanometer composite material |
| CN105622960A (en) * | 2015-12-30 | 2016-06-01 | 华南理工大学 | Carboxymethyl chitosan/oxidized graphene compounded hydrogel and preparation as well as application thereof |
-
2017
- 2017-04-29 CN CN201710297906.8A patent/CN107029676A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077795A (en) * | 2006-05-22 | 2007-11-28 | 北京化工大学 | Composite biological adsorption and preparing method thereof |
| CN101524635A (en) * | 2009-03-28 | 2009-09-09 | 大连理工大学 | Method for preparing chitosan/organo montmorillonite nanometer composite material |
| CN105622960A (en) * | 2015-12-30 | 2016-06-01 | 华南理工大学 | Carboxymethyl chitosan/oxidized graphene compounded hydrogel and preparation as well as application thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704620A (en) * | 2018-07-02 | 2018-10-26 | 大连理工大学 | The preparation method and application of chitosan/hydrophobic montmorillonite sorbing material of anion in a kind of processing waste water |
| CN108704620B (en) * | 2018-07-02 | 2021-04-20 | 大连理工大学 | Preparation method and application of chitosan/hydrophobic montmorillonite adsorbing material for treating anions in wastewater |
| CN110550689A (en) * | 2019-08-26 | 2019-12-10 | 神美科技有限公司 | Organic-inorganic composite heavy metal ion trapping agent |
| CN110756159A (en) * | 2019-11-06 | 2020-02-07 | 中山职业技术学院 | Preparation method of high-performance modified sodium bentonite nano composite adsorption material |
| CN112779019A (en) * | 2021-01-07 | 2021-05-11 | 何雨昕 | Soil conditioner for enhancing stress resistance of crops and preparation method thereof |
| CN115501860A (en) * | 2022-11-09 | 2022-12-23 | 江西理工大学 | Preparation method of composite modified montmorillonite for adsorbing heavy metal ions of anions/cations |
| CN115501860B (en) * | 2022-11-09 | 2024-02-27 | 江西理工大学 | Preparation method of composite modified montmorillonite for adsorbing negative/positive heavy metal ions |
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