CN103638904A - Preparation method for high-adsorptivity organic bentonite - Google Patents
Preparation method for high-adsorptivity organic bentonite Download PDFInfo
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- CN103638904A CN103638904A CN201310603850.6A CN201310603850A CN103638904A CN 103638904 A CN103638904 A CN 103638904A CN 201310603850 A CN201310603850 A CN 201310603850A CN 103638904 A CN103638904 A CN 103638904A
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- bentonite
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Abstract
The invention discloses a new method for enhancing the adsorption performance of organic bentonite. The method comprises: performing original soil grinding and crushing on bentonite, performing lithium ion exchange, then utilizing a certain amount of organic cations to exchange part of lithium ions, finally performing heating processing, so as to migrating interlayer lithium ions into bentonite lamella and further to obtain the organic bentonite adsorption material with good adsorption performance. The method provided by the invention is characterized by pre-exchanging organic cations to bentonite interlayer, utilizing the pillared effect of the organic cations to prevent bentonite layer structure from collapsing, then performing heating charge-reducing treatment, so as to furthest retaining the interlayer adsorption space and improve the specific surface area and adsorption sites of organic bentonite, and further enhance the adsorption performance of organic bentonite to toxic organic pollutants. The preparation method provided by the invention helps to reduce the sewage processing cost of organic bentonite and thus has wide application prospect in pollution control.
Description
Technical field
The present invention relates to a kind of high absorption property method for preparing organobentonite, belong to alta-mud modification processing technology field.
Background technology
Bentonite is a kind of clay rock that montmorillonite (Montmorillonite) is essential mineral of take.Montmorillonite is a kind of layer aluminosilicate mineral with two-dimensional nanostructure, by aluminium of two silicon-oxy tetrahedron therebetween (magnesium) oxygen (hydrogen-oxygen) are octahedra, forms.Because isomorphous replacement effect montmorillonite lamella has permanent negative electrical charge, need to reach charge balance at its interlamination region Liquidity limit.Under natural conditions, montmorillonite interlamination region cation is mainly the inorganic ions (as calcium ion, sodium ion) with strong hydration capability, so montmorillonite interlamination region is hydrophilic environment, to toxic organic compound adsorption capacity extreme difference.But these inorganic cations can be exchanged by organic cation, and then change the hydrophilic environment of interlamination region and strengthen bentonite absorption property.Conventional organic cation can be the cationic surfactant (as cetyltrimethyl ammonium ion) containing long carbochain, or undersized organic cation (as tetramethyl ammonium).After organic cation exchange, prepared modified product is called as organobentonite.Generally speaking, the principle that small size organic cation clearing house obtains organobentonite absorption organic molecule is adsorption effect, and adsorption capacity is mainly determined by its specific area.Therefore increasing organobentonite specific area is to improve the key of its absorption property.
At present bentonite being subtracted to electric charge processing is the effective ways that increase organobentonite specific area and absorption property.Be exactly particularly first with undersized lithium ion exchanged, to go out the original inorganic cation of montmorillonite interlamination region, then under heating condition, lithium ion migration enters montmorillonite lamella and compensates its negative electrical charge, finally carries out organic cations exchange again.Thus, in montmorillonite interlamination region, less organic cation gets final product the negative electrical charge of full remuneration montmorillonite, the occupied space of organic cation is few so, has more silicon-oxy tetrahedron simultaneously and exposes, and this can improve organobentonite specific area and adsorption site.Obviously, the amount that lithium ion migration enters montmorillonite lamella is more, and the organic cation of required compensation montmorillonite negative electrical charge is fewer, and the silicon-oxy tetrahedron of exposure is more many is more conducive to increase organobentonite specific area and absorption property.General increase heating-up temperature and prolongation heat time are conducive to increase the migration amount of lithium ion.But, there is very large randomness in the transition process of lithium ion, therefore in heating process, the migration amount of part lamella lithium ion can be much larger than other lamella, that is to say, lithium ion in part montmorillonite interlamination region may the overwhelming majority can migration enter lamella, and this will cause subsiding of montmorillonite part layer structure, and then causes the corresponding interlamination region can not be as Adsorption of Organic site.Therefore, to subtract charge method limited to promoting organobentonite absorption property effect for tradition.
Summary of the invention
For addressing the above problem, the present invention proposes and a kind ofly can prevent montmorillonite layer structural collapse, prepare high absorption property bentonite new method.
Object of the present invention is providing a kind of high absorption property method for preparing organobentonite.
The technical solution used in the present invention is:
A high absorption property method for preparing organobentonite, comprises the following steps:
1) add in lithium salt solution after bentonite is ground, carry out lithium ion exchanged, then dry, pulverize acquisition lithium bentonite;
2) by adding organic cation solution in lithium bentonite, carry out organic cation exchange, then dry, pulverize the organobentonite that obtains preliminary treatment;
3) organobentonite of preliminary treatment is heated to 10～20h at 150～180 ℃, make lithium ion enter bentonitic lamellar structure, make organobentonite.
Further, the operating process of lithium ion exchanged described in step 1) is: by adding mole in bentonite, be that lithium salts, the quality of 1～3 times of bentonite cation exchange capacity is the water of 40～60 times of bentonites, mix, under 40～80 ℃ of heating conditions, stir 4～6h and carry out cation exchange reaction, then suction filtration, lithium salts and the water of isodose will be added in filter residue again, repeated exchanged process 2～4 times, then suction filtration, distilled water washes clean, 50～80 ℃ of oven dry, are crushed to 100 orders and obtain below lithium bentonite.
Further, described lithium salts is selected from lithium chloride and nitrate.
Further, the operating process of organic cation step 2) exchange is: by adding mole in lithium bentonite, be that organic cation and the quality of bentonite cation exchange capacity 5～40% is the water of 50～100 times of bentonites, mix, under 40～80 ℃ of heating conditions, stir 5～7h and carry out organic cation exchange reaction, then suction filtration, 50～80 ℃ of oven dry of distilled water washes clean, are crushed to the organobentonite that 100 orders obtain preliminary treatment below.
Further, described organic cation chemical structural formula is
, R wherein
1～R
4independently be selected from alkyl, phenyl, the benzyl of C1～C3.
Further, described in
be selected from tetramethylammonium cation, trimethyl benzyl ammonium cation.
The invention has the beneficial effects as follows:
In the present invention, first with undersized lithium ion exchanged, go out the original inorganic cation of bentonite interlamination region, then by organic cation and part lithium ion exchanged, finally under higher temperature, heating moves to its negative electrical charge of montmorillonite lamella internal compensation by lithium ion; Like this, the organic cation that exchanges in advance interlamination region can strut bentonite lamella, firmly pillared between bentonite bed, can effectively prevent organobentonite layer structural collapse, retain to greatest extent domain space between organic bentonite bed, improve bentonite specific area and adsorption site, and then improved bentonite absorption property.
Organobentonite prepared by the present invention is much better than traditional organobentonite to the absorption property of toxicity organic pollution, contributes to reduce organobentonite cost of sewage disposal, and in polluting control, tool has a broad prospect of the use.
Accompanying drawing explanation
Fig. 1 is that organobentonite and the tradition of embodiment 1 preparation subtracts electric charge bentonite XRD spectrum figure;
Fig. 2 is that organobentonite and the tradition of embodiment 1 preparation subtracts electric charge bentonite nitrogen adsorption-desorption curve.
The specific embodiment
A high absorption property method for preparing organobentonite, comprises the following steps:
1) add in lithium salt solution after bentonite is ground, carry out lithium ion exchanged, then dry, pulverize acquisition lithium bentonite;
2) by adding organic cation solution in lithium bentonite, carry out organic cation exchange, then dry, pulverize the organobentonite that obtains preliminary treatment;
3) organobentonite of preliminary treatment is heated to 10～20h at 150～180 ℃, make lithium ion enter bentonitic lamellar structure, make organobentonite.
Preferably, the detailed process of step 1) is: by adding mole in bentonite, be that lithium salts, the quality of 1～3 times of bentonite cation exchange capacity is the water of 40～60 times of bentonites, mix, under 40～80 ℃ of heating conditions, stir 4～6h and carry out cation exchange reaction, then suction filtration, will add lithium salts and the water of isodose again in filter residue, repeated exchanged process 2～4 times, then suction filtration, distilled water washes clean, 50～80 ℃ of oven dry, are crushed to 100 orders and obtain below lithium bentonite.
Preferably, described lithium salts is selected from lithium chloride and nitrate.
Preferably, step 2) detailed process is: by adding mole in lithium bentonite, be that organic cation and the quality of bentonite cation exchange capacity 5～40% is the water of 50～100 times of bentonites, mix, under 40～80 ℃ of heating conditions, stir 5～7h and carry out organic cation exchange reaction, then suction filtration, 50～80 ℃ of oven dry of distilled water washes clean, are crushed to the organobentonite that 100 orders obtain preliminary treatment below.
Preferably, described organic cation chemical structural formula is
, R wherein
1～R
4independently be selected from alkyl, phenyl, the benzyl of C1～C3.
Preferably, described in
be selected from tetramethylammonium cation, trimethyl benzyl ammonium cation.
Preferably, in described lithium bentonite, adding mole is that the organic cation of bentonite cation exchange capacity 10% carries out organic cation exchange reaction.
embodiment 1:
A new method that strengthens organobentonite absorption property, comprises the following steps:
1) by cation exchange capacity, be that the bentonite in powder of 1.06 mmol/g is broken to below 100 orders, getting 10 g, to put into 500 mL concentration be in the lithium chloride solution of 30 mmol/L, under 60 ℃ of heating conditions, stir 4 hours, carry out after lithium ion exchanged, suction filtration, then gained filter residue is continued to add the lithium chloride solution with amount, repeat lithium ion exchanged reaction 3 times, then suction filtration, distilled water washing are to detect (adopting silver nitrate to detect) without chlorion, then 60 ℃ of oven dry, be crushed to below 100 orders, obtain lithium bentonite;
2) lithium bentonite joins in the tetramethyl ammonium chloride solution that 500 mL concentration are 6 mmol/L, under 60 ℃ of heating conditions, stir 6 hours, by tetramethylammonium cation and part lithium ion exchanged, then suction filtration, distilled water washing are to detect (adopting silver nitrate to detect) without chlorion, 60 ℃ of oven dry again, be crushed to below 100 orders, obtain the organobentonite of preliminary treatment;
3) preliminary organobentonite is heated 12 hours at 180 ℃, make lithium ion enter bentonitic lamellar structure, obtain organobentonite.
embodiment 2:
1) by cation exchange capacity, be that the bentonite in powder of 1.06 mmol/g is broken to below 100 orders, getting 10 g, to put into 700 mL concentration be in the lithium chloride solution of 40 mmol/L, under 60 ℃ of heating conditions, stir 6 hours, carry out after lithium ion exchanged, suction filtration, then gained filter residue is continued to add the lithium chloride solution with amount, repeat lithium ion exchanged reaction 3 times, then suction filtration, distilled water washing are to detect (adopting silver nitrate to detect) without chlorion, then 80 ℃ of oven dry, be crushed to below 100 orders, obtain lithium bentonite;
2) lithium bentonite joins in the trimethyl benzyl ammonia chloride solution that 500 mL concentration are 5 mmol/L, under 40 ℃ of heating conditions, stir 7 hours, by trimethyl benzyl ammonium cation and part lithium ion exchanged, then suction filtration, distilled water washing are to detect (adopting silver nitrate to detect) without chlorion, 50 ℃ of oven dry again, be crushed to below 100 orders, obtain the organobentonite of preliminary treatment;
3) preliminary organobentonite is heated 12 hours at 180 ℃, make lithium ion enter bentonitic lamellar structure, obtain organobentonite.
embodiment 3:
1) by cation exchange capacity, be that the bentonite in powder of 1.06 mmol/g is broken to below 100 orders, getting 10 g, to put into 500 mL concentration be in the lithium chloride solution of 30 mmol/L, under 60 ℃ of heating conditions, stir 4 hours, carry out after lithium ion exchanged, suction filtration, then gained filter residue is continued to add the lithium chloride solution with amount, repeat lithium ion exchanged reaction 3 times, then suction filtration, distilled water washing are to detect (adopting silver nitrate to detect) without chlorion, then 60 ℃ of oven dry, be crushed to below 100 orders, obtain lithium bentonite;
2) lithium bentonite joins in the trimethyl benzyl ammonia chloride solution that 1000 mL concentration are 4 mmol/L, under 80 ℃ of heating conditions, stir 5 hours, by trimethyl benzyl ammonium cation and part lithium ion exchanged, then suction filtration, distilled water washing are to detect (adopting silver nitrate to detect) without chlorion, 80 ℃ of oven dry again, be crushed to below 100 orders, obtain the organobentonite of preliminary treatment;
3) preliminary organobentonite is heated 12 hours at 150 ℃, make lithium ion enter bentonitic lamellar structure, obtain organobentonite.
Below the organobentonite of preparing in embodiment is made to further Performance Detection.
the absorption property of organobentonite p-nitrophenyl
It is in the nitrobenzene solution of 100 mg/L that the organobentonite 0.1g that gets embodiment 1 preparation joins 20 mL concentration, and centrifugation after absorption 4h, detects supernatant concentration, calculates corresponding adsorbance, adsorption coefficient.
Get 0.1g tradition subtracts electric charge organobentonite and carries out same experiment in contrast simultaneously, wherein, tradition subtracts electric charge method for preparing organobentonite, first bentonite is carried out to lithium ion exchanged, then 160 ℃ of heating of high temperature make lithium ion enter lamellar structure in 12 hours, finally with tetramethyl ammonium, be fully swapped out bentonite interlamination region lithium ion, obtain traditional electric charge organobentonite that subtracts, detailed method of operating can be referring to Komadel, P., Madejova, J., Bujdak, J., 2005. Preparation and properties of reduced-charge smectites:a review. Clays Clay Miner. 53, 313 – 334.
Absorption result demonstration, the organobentonite p-nitrophenyl adsorbance of embodiment 1 preparation is 11.6 mg/g, adsorption coefficient is 278 L/kg; And tradition subtracts electric charge organobentonite adsorbance, be 6.2 mg/g, adsorption coefficient is 92 L/kg, and the relatively traditional organobentonite of bentonite adsorption coefficient prepared by the present invention has improved 3 times.
bentonite X-ray diffractogram
Organobentonite prepared by embodiment 1 and tradition subtract electric charge organobentonite and carry out X-ray diffraction (XRD) sign, and its XRD characterization result as shown in Figure 1.
The organobentonite of embodiment 1 preparation has more sharp-pointed diffraction maximum as can be seen from Figure 1, and crystal formation is better, and layer structure is more regular, show its relatively tradition subtract electric charge organobentonite and there is better layer structure.
bentonite nitrogen adsorption-desorption characterizes
Getting the organobentonite of embodiment 1 preparation and tradition subtracts electric charge organobentonite and carries out nitrogen adsorption-desorption and characterize experiment, first 100 ℃ of vacuum outgas 12h, then absorption nitrogen.As shown in Figure 2, organobentonite prepared by two kinds of methods has all kept laminar hole structure to characterization result, but the organobentonite of embodiment 1 preparation has better nitrogen adsorption ability.
bentonite specific area detects
Adopt BET method, organobentonite prepared by embodiment 1 and tradition subtract electric charge organobentonite and carry out specific area detection, testing result demonstration, and the organobentonite specific area of embodiment 1 preparation is 234.6 m
2/ g is almost that conventional method makes organobentonite specific area (131.7 m
2/ g) 2 times.
bentonite absorption property prepared by variable concentrations organic cation
1) according to method described in example 1, be prepared into lithium bentonite;
2) 5g lithium bentonite is joined in the tetramethyl ammonium chloride solution of 500 mL variable concentrations, the consumption of guaranteeing tetramethyl ammonium is respectively 5%, 10%, 20% and 40% of bentonite cation exchange capacity, under 60 ℃ of heating conditions, stir suction filtration after 6 hours, distilled water washing to detecting (silver nitrate detection) without chlorion, then 60 ℃ of oven dry, be crushed to below 100 orders, obtain preliminary organobentonite;
3) preliminary organobentonite is heated 12 hours at 200 ℃, obtain serial organobentonite;
4) gained series organobentonite is carried out to the detection of the absorption property of nitrobenzene.
Testing result shows, the consumption of tetramethyl ammonium (TMA) is respectively four kinds of organobentonite p-nitrophenyl adsorbances that 5%, 10%, 20% and 40% of bentonite cation exchange capacity prepares and is respectively 10.5 mg/g, 15.3 mg/g, 12.2 mg/g and 10.9 mg/g.Prepared organobentonite shows the variation tendency of absorption property first increases and then decreases with the increase of TMA exchange capacity, and wherein TMA exchange capacity is that the organobentonite absorption property of bentonite cation exchange capacity 10% is best, is 15.3 mg/g.
Claims (6)
1. a high absorption property method for preparing organobentonite, is characterized in that: comprise the following steps:
1) add in lithium salt solution after bentonite is ground, carry out lithium ion exchanged, then dry, pulverize acquisition lithium bentonite;
2) by adding organic cation solution in lithium bentonite, carry out organic cation exchange, then dry, pulverize the organobentonite that obtains preliminary treatment;
3) organobentonite of preliminary treatment is heated to 10～20h at 150～180 ℃, make lithium ion enter bentonitic lamellar structure, make organobentonite.
2. a kind of high absorption property method for preparing organobentonite according to claim 1, it is characterized in that: the detailed process of step 1) is: by adding mole in bentonite, be the lithium salts of 1～3 times of bentonite cation exchange capacity, quality is the water of 40～60 times of bentonites, mix, under 40～80 ℃ of heating conditions, stir 4～6h and carry out cation exchange reaction, then suction filtration, lithium salts and the water of isodose will be added in filter residue again, repeated exchanged process 2～4 times, then suction filtration, distilled water washes clean, 50～80 ℃ of oven dry, be crushed to 100 orders and obtain below lithium bentonite.
3. a kind of high absorption property method for preparing organobentonite according to claim 1 and 2, is characterized in that: described lithium salts is selected from lithium chloride and lithium nitrate.
4. a kind of high absorption property method for preparing organobentonite according to claim 1, it is characterized in that: step 2) detailed process be: by adding mole in lithium bentonite, be that organic cation and the quality of bentonite cation exchange capacity 5～40% is the water of 50～100 times of bentonites, mix, under 40～80 ℃ of heating conditions, stir 5～7h and carry out organic cation exchange reaction, then suction filtration, 50～80 ℃ of oven dry of distilled water washes clean, are crushed to the organobentonite that 100 orders obtain preliminary treatment below.
5. according to a kind of high absorption property method for preparing organobentonite described in claim 1 or 4, it is characterized in that: described organic cation chemical structural formula is
, R wherein
1～R
4independently be selected from alkyl, phenyl, the benzyl of C1～C3.
6. a kind of high absorption property method for preparing organobentonite according to claim 5, is characterized in that: described in
be selected from tetramethylammonium cation, trimethyl benzyl ammonium cation.
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Cited By (5)
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| CN103962093A (en) * | 2014-05-22 | 2014-08-06 | 常州大学 | Synthesis method of bentonite loaded iron carbonyl adsorbent |
| CN107285326A (en) * | 2017-08-23 | 2017-10-24 | 重庆索利特涂料有限公司 | A kind of organobentonite of energy-conserving and environment-protective and preparation method thereof |
| CN109248650A (en) * | 2018-09-26 | 2019-01-22 | 芜湖市鹏磊新材料有限公司 | A kind of bentonite processing method increasing organic matter absorption property |
| CN111250037A (en) * | 2020-01-19 | 2020-06-09 | 招商局生态环保科技有限公司 | Preparation method of bentonite for soil remediation |
| CN114837014A (en) * | 2022-03-30 | 2022-08-02 | 哈工大机器人集团(杭州湾)国际创新研究院 | Preparation method of clay compound for carbonless copy paper |
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Cited By (5)
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| CN103962093A (en) * | 2014-05-22 | 2014-08-06 | 常州大学 | Synthesis method of bentonite loaded iron carbonyl adsorbent |
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| CN111250037A (en) * | 2020-01-19 | 2020-06-09 | 招商局生态环保科技有限公司 | Preparation method of bentonite for soil remediation |
| CN114837014A (en) * | 2022-03-30 | 2022-08-02 | 哈工大机器人集团(杭州湾)国际创新研究院 | Preparation method of clay compound for carbonless copy paper |
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Application publication date: 20140319 |