CN112661165B - High-energy grinding preparation of rare earth-loaded bentonite and preparation method thereof - Google Patents
High-energy grinding preparation of rare earth-loaded bentonite and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-energy grinding preparation method of rare earth loaded bentonite and a preparation method thereof, and relates to the technical field of preparation methods of rare earth loaded bentonite. A preparation method for preparing rare earth loaded bentonite by high-energy grinding comprises the following steps: putting the bentonite into a high-energy ball mill for grinding, and obtaining weak crystalline state bentonite after grinding; putting the weak crystalline state bentonite into a multi-rare earth solution and stirring; and after stirring, carrying out plate-and-frame filtration, then repeating the stirring operation again, filtering and washing the obtained product with a plate-and-frame filter after stirring, and drying to obtain the rare earth-loaded bentonite. The invention reduces the particle size of the bentonite through high-energy grinding, and simultaneously the crystal structure of the bentonite is also partially destroyed to form the weak crystalline state bentonite, thereby being more beneficial to the subsequent preparation of the rare earth load bentonite.
Description
Technical Field
The invention relates to the technical field of preparation methods of rare earth-loaded bentonite, in particular to a preparation method of rare earth-loaded bentonite by high-energy grinding.
Background
In recent years, in water environment pollution, a series of pollutants which are toxic and hard to degrade and have persistence and biological accumulation effects, such as halogenated hydrocarbon organic matters, industrial heavy metal wastewater, soil waste pollution and the like, are more and more focused.
The rare earth load bentonite can be used for organic synthesis catalyst to catalyze organic esterification reaction, can also be used as a green, safe and ecological risk-free water body restoration agent to fix inorganic phosphorus in surface water body and prevent water bloom. The rare earth loading of bentonite, whether as an organic synthesis catalyst or as a water treatment agent, has a decisive effect on the final properties of the material. The rare earth load bentonite is mainly obtained by ion exchange, the bentonite is crushed and then added into a high-concentration rare earth solution to be stirred, after the bentonite is stirred for a certain time, rare earth ions enter a crystal structure of the bentonite through the ion exchange effect, and then the rare earth load bentonite product can be obtained through solid-liquid separation.
The inventor of the invention finds that in the method for preparing the rare earth loaded bentonite in the prior art, the bentonite is directly stirred with the rare earth easily without treatment, the rare earth loading capacity of the bentonite is low, and the actual loading capacity of the bentonite is far lower than the theoretical loading capacity of the bentonite, so that the actual application performance of the product is poorer. Therefore, a preparation method capable of effectively increasing the loading capacity of the rare earth loaded bentonite is urgently needed.
Disclosure of Invention
In order to solve at least one problem in the background technology, the invention provides the rare earth load bentonite prepared by high-energy grinding and the preparation method thereof.
According to one aspect of the invention, a preparation method for preparing rare earth loaded bentonite by high-energy grinding comprises the following steps: placing bentonite into a high-energy ball mill, selecting a grinding medium from 3mm-8mm steel balls, grinding the bentonite to obtain weak crystalline state bentonite after grinding, wherein the filling rate of the steel balls is 10% -30%, the ball-material ratio is 20/1-10/1, and the grinding centrifugal acceleration is 5G-30G; putting the weak crystalline state bentonite into a multi-rare earth solution and stirring; and after stirring, carrying out plate-and-frame filtration, then repeating the stirring operation again, filtering and washing the obtained product with a plate-and-frame filter after stirring, and drying to obtain the rare earth-loaded bentonite.
Further optionally, the high-energy ball mill is one of a stirring mill, a planetary ball mill and a vibration mill.
Further optionally, the grinding time is 5min-10min.
Further optionally, the stirring time is 24-48 hours.
Further optionally, the bentonite is sodium bentonite, the purity of the sodium bentonite is 70% -90%, and the cation exchange capacity CEC is 0.6mmol/g-1.2mmol/g.
Further optionally, the multi-rare earth solution is one or more of lanthanum chloride, cerium chloride, yttrium chloride and europium chloride solutions.
Further optionally, the concentration of the multi-rare earth solution is 0.5mol/L-2mol/L.
Further optionally, the plate-and-frame filter adopts a plate-and-frame filter press with a back flush.
According to another aspect of the invention, the high-energy grinding method for preparing the rare earth-loaded bentonite is characterized in that the high-energy grinding method for preparing the rare earth-loaded bentonite mainly comprises the following steps: a main active ingredient, an impurity ingredient and an auxiliary ingredient; the main active component is rare earth accounting for 1-10% of the total weight, the impurity component is one or more selected from quartz, calcite, feldspar and mica accounting for 5-25% of the total weight, and the auxiliary component is bentonite accounting for 70-90% of the total weight.
Further optionally, the use of the rare earth-loaded bentonite for organic synthesis catalysts or water treatment agents.
The invention has the beneficial effects that:
1. the invention reduces the particle size of the bentonite through high-energy grinding, and simultaneously the crystal structure of the bentonite is also partially destroyed to form the weak crystalline state bentonite, thereby being more beneficial to the subsequent preparation of the rare earth load bentonite.
2. According to the invention, the layered structure of the crystalline state bentonite is changed, namely, relative slippage and activation are generated under the action of high-energy ball milling, so that the exchangeability of interlayer cations is greatly improved, rare earth ions can be exchanged in a rare earth solution to the maximum degree to enter the interlayer of the bentonite, the rare earth loading capacity is very close to the theoretical maximum rare earth loading capacity of the bentonite, and the loading capacity of the rare earth loaded bentonite is improved.
Drawings
FIG. 1 shows a flow chart of a method for preparing rare earth-loaded bentonite by high-energy grinding in an embodiment of the invention.
Detailed Description
The contents of the present invention will now be discussed with reference to several exemplary embodiments. It is to be understood that these examples are discussed only to enable those of ordinary skill in the art to better understand and thus implement the teachings of the present invention, and are not meant to imply any limitations on the scope of the invention.
As used herein, the term "include" and its variants are to be read as open-ended terms meaning "including, but not limited to. The term "based on" is to be read as "based, at least in part, on". The terms "one embodiment" and "an embodiment" are to be read as "at least one embodiment". The term "another embodiment" is to be read as "at least one other embodiment".
Example 1:
according to one embodiment of the invention, the preparation method of the rare earth loaded bentonite for organic synthesis comprises the following steps:
(1) 100 kg of sodium bentonite (with cation exchange capacity CEC1 mmol/G) is placed in a planetary ball mill, a 5mm steel ball is preferably selected as a grinding medium in the embodiment, the filling rate of the steel ball is 20%, the ball-material ratio is 20/1, the grinding centrifugal acceleration is 30G, and the grinding time is 5min;
(2) And (3) putting the ground sodium bentonite into a 0.5M lanthanum chloride rare earth solution, stirring the sodium bentonite with a liquid-solid ratio of 25/1, precipitating and extracting a supernatant after stirring the sodium bentonite for 24 hours, adding the 0.5M lanthanum chloride rare earth solution until the liquid-solid ratio is 25/1, and stirring the mixture for 24 hours again.
(3) After stirring, performing filter pressing and backwashing by using a plate and frame filter press with backwashing reset to obtain a rare earth loaded bentonite wet material;
(4) Drying at 100 deg.C for 12h, and crushing to obtain rare earth-loaded bentonite for organic synthesis.
In this example, the use performance of the rare earth-loaded bentonite prepared by the method for preparing rare earth-loaded bentonite for organic synthesis is embodied by organic catalytic esterification, which is detailed in table 1:
table 1: example 1: organic catalytic esterification reaction
Example 2:
according to one embodiment of the invention, the preparation method of the rare earth loaded bentonite for water treatment comprises the following steps:
(1) 30 kg of sodium bentonite (with cation exchange capacity CEC 1.2 mmol/G) is placed in a stirring mill, a grinding medium in the embodiment preferably adopts a 3mm steel ball, the filling rate of the steel ball is 30%, the ball-material ratio is 20/1, the grinding centrifugal acceleration is 5G, and the grinding time is 20min;
(2) And (2) putting the ground sodium bentonite into a multi-rare earth solution (0.5M lanthanum chloride, 0.5M cerium chloride and 0.5M yttrium chloride) for stirring, wherein the liquid-solid ratio is 25/1, precipitating and extracting supernatant after stirring is completed for 24 hours, adding the multi-rare earth solution (0.5M lanthanum chloride, 0.5M cerium chloride and 0.5M yttrium chloride) until the liquid-solid ratio is 25/1, and stirring for 24 hours again.
(3) After stirring, performing filter pressing and backwashing by using a plate and frame type filter press with backwashing resetting to obtain a rare earth-loaded bentonite wet material;
(4) Drying at 100 deg.C for 12 hr, and crushing to obtain bentonite loaded with rare earth for water treatment.
Example 3:
according to one embodiment of the invention, the preparation method of the rare earth loaded bentonite for water treatment comprises the following steps:
(1) 20 kilograms of sodium bentonite (with cation exchange capacity CEC1 mmol/G) is placed in a vibration mill, a grinding medium is preferably 8mm steel balls in the embodiment, the filling rate of the steel balls is 20%, the ball-material ratio is 10/1, the grinding centrifugal acceleration is 10G, and the grinding time is 15min;
(2) And (2) putting the ground sodium bentonite into a multi-rare earth solution (0.5M neodymium chloride, 0.5M cerium chloride and 0.5M praseodymium chloride) and stirring, wherein the liquid-solid ratio is 20/1, precipitating and extracting a supernatant after stirring for 48 hours, adding the multi-rare earth solution (0.5M neodymium chloride, 0.5M cerium chloride and 0.5M praseodymium chloride) until the liquid-solid ratio is 20/1, and stirring for 48 hours again.
(3) After stirring, performing filter pressing and backwashing by using a plate and frame filter press with backwashing reset to obtain a rare earth loaded bentonite wet material;
(4) Drying at 100 deg.C for 12h, and crushing to obtain rare earth-loaded bentonite for water treatment.
Example 4
According to one embodiment of the invention, the preparation method of the rare earth loaded bentonite for water treatment comprises the following steps:
(1) 50 kg of sodium bentonite (with cation exchange capacity CEC1.1 mmol/G) is placed in a planetary ball mill, a grinding medium in the embodiment preferably adopts a 3mm steel ball, the filling rate of the steel ball is 20%, the ball-material ratio is 20/1, the grinding centrifugal acceleration is 20G, and the grinding time is 10min;
(2) And (3) putting the ground sodium bentonite into a multi-rare earth solution (2M lanthanum chloride and 2M cerium chloride) for stirring, wherein the liquid-solid ratio is 25/1, precipitating and extracting supernatant after stirring is completed for 24 hours, adding the multi-rare earth solution (2M lanthanum chloride and 2M cerium chloride) until the liquid-solid ratio is 25/1, and stirring for 24 hours again.
(3) After stirring, performing filter pressing and backwashing by using a plate and frame type filter press with backwashing resetting to obtain a rare earth-loaded bentonite wet material;
(4) Drying at 100 deg.C for 12 hr, and crushing to obtain bentonite loaded with rare earth for organic synthesis.
Example 5
According to one embodiment of the invention, the preparation method of the rare earth loaded bentonite for water treatment comprises the following steps:
(1) 50 kg of sodium bentonite (with cation exchange capacity CEC1.1 mmol/G) is placed in a stirring mill, a grinding medium in the embodiment preferably adopts a 3mm steel ball, the filling rate of the steel ball is 10%, the ball-material ratio is 10/1, the grinding centrifugal acceleration is 30G, and the grinding time is 20min;
(2) And (3) putting the ground sodium bentonite into a multi-rare earth solution (2M lanthanum chloride and 2M cerium chloride) for stirring, wherein the liquid-solid ratio is 25/1, precipitating and extracting supernatant after stirring is completed for 24 hours, adding the multi-rare earth solution (2M lanthanum chloride and 2M cerium chloride) until the liquid-solid ratio is 25/1, and stirring for 24 hours again.
(3) After stirring, performing filter pressing and backwashing by using a plate and frame filter press with backwashing reset to obtain a rare earth loaded bentonite wet material;
(4) Drying at 100 deg.C for 12 hr, and crushing to obtain bentonite loaded with rare earth for organic synthesis.
The technical solutions of examples 2 to 5 were tested by using a surface water-solidified phosphorus test to verify the service performance of the rare earth-loaded bentonite prepared in each example, which is detailed in table 2:
table 2:
Claims (5)
1. a preparation method for preparing rare earth loaded bentonite by high-energy grinding is characterized by comprising the following steps:
putting the bentonite into a high-energy ball mill for grinding, and obtaining weak crystalline state bentonite after grinding; the step of putting the bentonite into a high-energy ball mill for grinding comprises the following steps: the grinding medium is 3mm-8mm steel balls, the filling rate of the steel balls is 10% -30%, the ball-material ratio is 20/1-10/1, the grinding centrifugal acceleration is 5G-30G, and the high-energy ball mill is one of a stirring mill, a planetary ball mill and a vibration mill;
putting the weak crystalline state bentonite into a multi-rare earth solution and stirring; the multi-rare earth solution is one or more of cerium chloride, yttrium chloride and europium chloride;
after stirring, performing plate-and-frame filtration, repeating the stirring operation again, after stirring, performing plate-and-frame filtration, washing with water, and drying to obtain the rare earth-loaded bentonite;
the high-energy grinding preparation of the rare earth loaded bentonite mainly comprises the following components: a main active ingredient, an impurity ingredient and an auxiliary ingredient;
the main active component is rare earth accounting for 1-10% of the total weight, the impurity component is one or more selected from quartz, calcite, feldspar and mica accounting for 5-25% of the total weight, and the auxiliary component is bentonite accounting for 70-90% of the total weight;
the bentonite is sodium bentonite, the purity of the sodium bentonite is 70% -90%, and the cation exchange capacity CEC is 0.6mmol/g-1.2mmol/g;
the concentration of the multi-rare earth solution is 0.5-2 mol/L.
2. The method for preparing the rare earth-loaded bentonite by high-energy grinding according to claim 1, wherein the grinding time is 5min-20min.
3. The method for preparing the rare earth-loaded bentonite by high-energy grinding according to claim 1, wherein the stirring time is 24-48 hours.
4. The preparation method for preparing the rare earth-loaded bentonite through high-energy grinding according to claim 1, wherein equipment adopted by the plate-and-frame filtration is a plate-and-frame filter press with back washing.
5. The method for preparing the rare earth-loaded bentonite by the high-energy grinding, which is prepared by the preparation method according to any one of claims 1 to 4, wherein the rare earth-loaded bentonite is used for an organic synthesis catalyst or a water treatment agent.
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| CN101044862A (en) * | 2006-12-29 | 2007-10-03 | 上海师范大学 | Nanometer bentonite bactericidal materials, and its preparing method and application |
| CN100522342C (en) * | 2007-07-27 | 2009-08-05 | 浙江大学 | A preparation method of organobentonite for removing water-solubility organic pollutant |
| CN102649052A (en) * | 2012-05-21 | 2012-08-29 | 常州大学 | Preparation method of bentonite-loaded copper water treatment material |
| CN103880140A (en) * | 2012-12-21 | 2014-06-25 | 福斯洛克股份有限公司 | Slurry For Treatment Of Oxyanion Contamination In Water |
| CN103254870A (en) * | 2013-05-19 | 2013-08-21 | 郭尧 | Lanthanum-cerium oxide rear-earth polishing powder and preparation method thereof |
| CN103949239A (en) * | 2014-04-10 | 2014-07-30 | 北京工业大学 | Preparation method of rare earth element-doped ZnO loaded bentonite composite photocatalyst |
| CN103990455B (en) * | 2014-06-11 | 2015-12-30 | 常州大学 | A kind of preparation method of alta-mud load silver vanadate photochemical catalyst |
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