CN105214619A - A kind of preparation method of organic bentonite gel adsorbent - Google Patents
A kind of preparation method of organic bentonite gel adsorbent Download PDFInfo
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- CN105214619A CN105214619A CN201510642993.7A CN201510642993A CN105214619A CN 105214619 A CN105214619 A CN 105214619A CN 201510642993 A CN201510642993 A CN 201510642993A CN 105214619 A CN105214619 A CN 105214619A
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Abstract
A kind of preparation method of bentonite plural gel adsorbent, relate to a kind of preparation method of bentone adsorbent, the method first with halogenated phosphates (CPC) for modifier, modification is carried out to sodium bentonite, after preparing halogenated phosphates organobentonite (CPC-B), with AlCl
3for crosslinking agent, sodium carboxymethylcellulose (CMC) is utilized to carry out twice-modified to CPC-B, obtained halogenated phosphates/sodium carboxymethylcellulose organic bentonite gel adsorbent (CPC/CMC-B).The halogenated phosphates that the present invention obtains/sodium carboxymethylcellulose organic bentonite gel adsorbent (CPC/CMC-B), have absorption property good, removal effect is obvious, and adsorption operations is easy, the few rate of recovery of loss is high, is a kind of environment-friendly molded adsorbent with applications well prospect.
Description
Technical field
The present invention relates to a kind of preparation method of bentone adsorbent, particularly relate to a kind of preparation method of organic bentonite gel adsorbent.
Background technology
Bentonite is a kind of clay mineral be widely distributed, take montmorillonite as main component, its structure cell is made up of 2 layers of Si-O tetrahedron therebetween one deck Al-O octahedron, the standard 2 sharing oxygen atom height of formation orderly between tetrahedron and octahedron ties up lamella, therefore specific area is large, has very strong adsorptivity and ion exchangeable.And energy the force rate natural earth raising tens even hundred times of water pollutant is removed through the bentonite of modification, there is good application prospect in the treatment of waste water.
CPC-B is trickle Powdered of particle, specific area is large, adsorptivity and ion-exchange performance high, but it has swellability, transparent performance is poor, adopts such These powdered adsorbents to carry out sewage disposal, solid-liquid is difficult to be separated and have a large amount of situation about running off, recycling cannot reach desirable effect, therefore in recent years These powdered adsorbents is carried out forming processes, and is applied to wastewater treatment and becomes main direction of studying.Gel is the one of formed absorbent, containing numerous functional groups in its crosslinked network structure, by the effects such as ion-exchange, hydrogen bond, Van der Waals force and organic matter and corrupt split thus the concentration of decreasing pollution thing.CPC-/CMC-B gel adsorber prepared by the present invention, on single organic modified bentonite basis, the sodium carboxymethylcellulose (CMC) of environment-protecting asepsis is adopted to carry out gelation process further, this performance of the adsorbent is good, and overcoming above-mentioned These powdered adsorbents defect in the application, is a kind of superior adsorbent of novel also tool environmental protection concept.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of organic bentonite gel adsorbent, the halogenated phosphates that the present invention obtains/sodium carboxymethylcellulose organic bentonite gel adsorbent (CPC/CMC-B), there is absorption property good, removal effect is obvious, adsorption operations is easy, the few rate of recovery of loss is high, is a kind of environment-friendly molded adsorbent with applications well prospect.
The object of the invention is to be achieved through the following technical solutions:
A kind of preparation method of organic bentonite gel adsorbent, described method first with halogenated phosphates (CPC) for modifier, modification is carried out to sodium bentonite, after preparing halogenated phosphates organobentonite (CPC-B), take AlCl3 as crosslinking agent, sodium carboxymethylcellulose (CMC) is utilized to carry out twice-modified to CPC-B, obtained halogenated phosphates/sodium carboxymethylcellulose organic bentonite gel adsorbent (CPC/CMC-B); Comprise following concrete steps:
(1) bentonite acid etching: bentonite and deionized water make medicinal bentonite suspension, regulates pH=1-2, and 70 DEG C of constant temperature water baths stir 3h, washing, centrifugal, dry, broken after to cross 100 mesh sieves for subsequent use;
(2) preparation of CPC-B: according to the mass fraction, preparation bentonite and CPC proportioning are the medicinal bentonite suspension of 4:1, regulate pH=10,3h is stirred in 70 DEG C of waters bath with thermostatic control, wash with alcohol after washing, wash filter cake while suction filtration, 105 DEG C of oven dry, filter cake grinds 100 orders and sieves, and obtains CPC-B organobentonite;
(3) preparation of CPC/CMC – B: according to the mass fraction, prepare the even magma that CPC-B and CMC proportioning is 1:4 at bath temperature 60 DEG C, the AlCl3 utilizing concentration to be 0.1mol/L is crosslinking agent, after cross-linking reaction a period of time, 25-40 DEG C of oven dry, obtains CPC/CMC-B gel adsorber.
The preparation method of described a kind of organic bentonite gel adsorbent, the bentonite described in step (1) is that the sodium original washing powder powder bentonite after acidleach process crosses 100 mesh sieves.
The preparation method of described a kind of organic bentonite gel adsorbent, bentonite described in step (2) and CPC quality proportioning are 4:1.
The preparation method of described a kind of organic bentonite gel adsorbent, the adjustment pH described in step (2) is for be adjusted to 10 by pH.
The preparation method of described a kind of organic bentonite gel adsorbent, the ethanol wash described in step (2) is the ethanol wash with 30%.
The preparation method of described a kind of organic bentonite gel adsorbent, CPC-B and CMC mass ratio 1:4 described in step (3).
The preparation method of described a kind of organic bentonite gel adsorbent, described in step (3), bath temperature is 60 DEG C.
The preparation method of described a kind of organic bentonite gel adsorbent, described in step (3), low temperature drying is 25-40 DEG C.
Described a kind of organic bentonite gel adsorbent, sem analysis display CPC-B organobentonite is irregular laminated structure, and laminated structure outline line is more more clear than original soil, and slicing layer thickness is also obviously thinner than original soil.The SEM photo of CPC/CMC-B gel shows to define obvious cross-linked structure, and inside has a large amount of holes.
Described a kind of organic bentonite gel adsorbent, the X-ray diffraction spectrogram display of CPC-B and CPC/CMC-B: the 2 θ angles of CPC-B are 3.9200 °, d001=2.2522nm; Main diffraction peak comparatively original soil offsets to low-angle direction, illustrate cation between former bentonite bed replace by organic cation, be modified as organobentonite, interlamellar spacing also has obvious increase, but the structure (cell configuration etc.) of modification to other parts of bentonite does not have an impact.The diffraction maximum of CPC/CMC-B is then between sodium base soil and CPC-B, and 2 θ angles are 4.3487 °, d001=1.9847nm; Sheaf space is occupied owing to entering interlayer through cross-linking reaction rear section cross-linked structure, thus reducing layer spacing.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention;
Fig. 2 is the surface texture adopting ESEM (SEM) to analyze sodium base original soil in the embodiment of the present invention 1, and multiplication factor is 10,000 times;
Fig. 3 adopts ESEM (SEM) to analyze CPC-B bentonite surface texture in the embodiment of the present invention 1, multiplication factor is 20,000 times;
Fig. 4 is the surface texture adopting ESEM (SEM) to analyze CPC-B/CMC bentonite gel adsorbent in the embodiment of the present invention 1, and multiplication factor is 20,000 times;
Fig. 5 is the X-ray diffraction spectrogram of original soil in the embodiment of the present invention 1, CPC-B organobentonite and CPC-B/CMC gel adsorber.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Composition principle:
Natural earth is a kind of lamellar aluminosilicate, combine by electrostatic interaction between layers, there is isomorphous substitution widely in tetrahedron and octahedron, Si4+ in tetrahedron is often substituted by Al3+, Al3+ in octahedron is often substituted by Mg2+, Fe3+, Fe2+, Ni2+, Li+ etc., make interlayer produce weak negative electrical charge, thus there is some cationic ability of absorption.Organic modifiers CPC can insert between the lamella of bentonite montmorillonite, changes bentonite bed spacing and specific area, improves bentonitic adsorption capacity.CMC is a kind of food additives of asepsis environment-protecting, utilizes its thickening property that the organobentonite CPC-B of single modification is made magma, adds crosslinking agent AlCl3, and the carboxyl generation crosslinked action of Al3+ and CMC produces cross-linked structure and the gel of netted hole.
This point can be confirmed by SEM and X-ray diffraction experiment.The surface texture of sem analysis original soil, CPC-B and CPC/CMC-B, wherein Fig. 2 and Fig. 3 is respectively original soil and CPC-B bentonite SEM photo.Contrast picture can be found out, modified organobentonite is irregular laminated structure, and laminated structure outline line is more more clear than original soil, and slicing layer thickness is also obviously thinner than original soil.Fig. 4 is the SEM photo of CPC-B/CMC gel adsorber, comparison diagram 3 and Fig. 4 can find out, the two presents diverse two kinds of configuration states, Fig. 3 is lamellar structure, and material surface defines obvious cross-linked structure as seen from Figure 4, inside has a large amount of holes, and the formation of gel network is described.
The X-ray diffraction spectrogram of original soil, CPC-B organobentonite and CPC-B/CMC gel adsorber, analysis result shows: according to X-ray diffraction condition and Bragg equation: 2dsin θ=n λ show that sodium bentonite 2 θ angle is 5.9400 °, d001=1.4867nm; The 2 θ angles of CPC-B are 3.9200 °, d001=2.2522nm; Modified through CPC, main diffraction peak offsets to low-angle direction, illustrate cation between former bentonite bed replace by organic cation, be modified as organobentonite, interlamellar spacing also has obvious increase, but the structure (cell configuration etc.) of modification to other parts of bentonite does not have an impact.The diffraction maximum of CPC-B/CMC, then between sodium base soil and CPC-B, occupies sheaf space owing to entering interlayer through cross-linking reaction rear section cross-linked structure, thus reducing layer spacing.
The preparation method of CPC/CMC-B gel adsorber
(1) bentonite acid etching: appropriate bentonite and deionized water make medicinal bentonite suspension, regulates pH=1-2, and 70 DEG C of constant temperature water baths stir 3h, washing, centrifugal, dry, broken after 100 mesh sieves for subsequent use.
(2) preparation of CPC-B: according to the mass fraction, preparation bentonite and CPC proportioning are the medicinal bentonite suspension of 4:1, regulate pH=10,3h is stirred in 70 DEG C of waters bath with thermostatic control, wash with alcohol after washing, wash filter cake while suction filtration, 105 DEG C of oven dry, filter cake grinds 100 orders and sieves, and obtains CPC-B organobentonite.
(3) preparation of CPC/CMC-B: according to the mass fraction, prepare the even magma that CPC-B and CMC proportioning is 1:4 at bath temperature 60 DEG C, the AlCl3 utilizing concentration to be 0.1mol/L is crosslinking agent, after cross-linking reaction a period of time, 25-40 DEG C of oven dry, obtains CPC/CMC-B gel adsorber.
Claims (10)
1. the preparation method of an organic bentonite gel adsorbent, it is characterized in that, described method first with halogenated phosphates (CPC) for modifier, modification is carried out to sodium bentonite, after preparing halogenated phosphates organobentonite (CPC-B), be crosslinking agent with AlCl3, utilize sodium carboxymethylcellulose (CMC) to carry out twice-modified to CPC-B, obtained halogenated phosphates/sodium carboxymethylcellulose organic bentonite gel adsorbent (CPC/CMC-B); Comprise following concrete steps:
(1) bentonite acid etching: bentonite and deionized water make medicinal bentonite suspension, regulates pH=1-2, and 70 DEG C of constant temperature water baths stir 3h, washing, centrifugal, dry, broken after to cross 100 mesh sieves for subsequent use;
(2) preparation of CPC-B: according to the mass fraction, preparation bentonite and CPC proportioning are the medicinal bentonite suspension of 4:1, regulate pH=10,3h is stirred in 70 DEG C of waters bath with thermostatic control, wash with alcohol after washing, wash filter cake while suction filtration, 105 DEG C of oven dry, filter cake grinds 100 orders and sieves, and obtains CPC-B organobentonite;
(3) preparation of CPC/CMC – B: according to the mass fraction, prepare the even magma that CPC-B and CMC proportioning is 1:4 at bath temperature 60 DEG C, the AlCl3 utilizing concentration to be 0.1mol/L is crosslinking agent, after cross-linking reaction a period of time, 25-40 DEG C of oven dry, obtains CPC/CMC-B gel adsorber.
2. the preparation method of a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, the bentonite described in step (1) is that the sodium original washing powder powder bentonite after acidleach process crosses 100 mesh sieves.
3. the preparation method of a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, bentonite described in step (2) and CPC quality proportioning are 4:1.
4. the preparation method of a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, the adjustment pH described in step (2) is for be adjusted to 10 by pH.
5. the preparation method of a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, the ethanol wash described in step (2) is the ethanol wash with 30%.
6. the preparation method of a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, CPC-B and CMC mass ratio 1:4 described in step (3).
7. the preparation method of a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, described in step (3), bath temperature is 60 DEG C.
8. the preparation method of a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, described in step (3), low temperature drying is 25-40 DEG C.
9. a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, sem analysis display CPC-B organobentonite is irregular laminated structure, and laminated structure outline line is more more clear than original soil, and slicing layer thickness is also obviously thinner than original soil;
The SEM photo of CPC/CMC-B gel shows to define obvious cross-linked structure, and inside has a large amount of holes.
10. a kind of organic bentonite gel adsorbent according to claim 1, is characterized in that, the X-ray diffraction spectrogram display of CPC-B and CPC/CMC-B: the 2 θ angles of CPC-B are 3.9200 °, d001=2.2522nm; Main diffraction peak comparatively original soil offsets to low-angle direction, illustrate cation between former bentonite bed replace by organic cation, be modified as organobentonite, interlamellar spacing also has obvious increase, but the structure (cell configuration etc.) of modification to other parts of bentonite does not have an impact;
The diffraction maximum of CPC/CMC-B is then between sodium base soil and CPC-B, and 2 θ angles are 4.3487 °, d001=1.9847nm; Sheaf space is occupied owing to entering interlayer through cross-linking reaction rear section cross-linked structure, thus reducing layer spacing.
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Cited By (4)
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| CN105621523A (en) * | 2016-03-18 | 2016-06-01 | 沈阳化工大学 | Method for treating phenolic waste water through gel adsorbent |
| CN108393071A (en) * | 2018-03-21 | 2018-08-14 | 广东电网有限责任公司电力科学研究院 | A kind of compound adsorbent and preparation method thereof |
| CN108905539A (en) * | 2018-07-24 | 2018-11-30 | 裴文韬 | A kind of preparation method of composite bentonite desiccant |
| CN109277087A (en) * | 2018-09-28 | 2019-01-29 | 芜湖市鹏磊新材料有限公司 | A kind of preparation method of the modified nanometer cellulose bentonite composite material for treatment of dyeing wastewater |
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| US6827959B1 (en) * | 1999-01-12 | 2004-12-07 | Sud-Chemie Ag | Mycotoxin adsorbents |
| CN103464123A (en) * | 2013-09-29 | 2013-12-25 | 沈阳化工大学 | Preparation method of CTMAB/CPAM/bentonite compound intercalation materials |
| CN104475016A (en) * | 2014-11-13 | 2015-04-01 | 蚌埠德美过滤技术有限公司 | Surfactant modified active carbon filter material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621523A (en) * | 2016-03-18 | 2016-06-01 | 沈阳化工大学 | Method for treating phenolic waste water through gel adsorbent |
| CN108393071A (en) * | 2018-03-21 | 2018-08-14 | 广东电网有限责任公司电力科学研究院 | A kind of compound adsorbent and preparation method thereof |
| CN108905539A (en) * | 2018-07-24 | 2018-11-30 | 裴文韬 | A kind of preparation method of composite bentonite desiccant |
| CN109277087A (en) * | 2018-09-28 | 2019-01-29 | 芜湖市鹏磊新材料有限公司 | A kind of preparation method of the modified nanometer cellulose bentonite composite material for treatment of dyeing wastewater |
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Application publication date: 20160106 |