CN111229157A - Preparation method of inorganic polymer modified bentonite adsorption material - Google Patents
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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Abstract
The invention provides a preparation method of an inorganic polymer modified bentonite adsorption material, which comprises the steps of adding bentonite and a sodium treatment agent into water for uniform mixing to obtain bentonite suspension, adding an inorganic polymer solution into the bentonite suspension, reacting to obtain a first mixed solution, adding water glass, silica sol and nano-silica into the first mixed solution, stirring and centrifuging in a constant-temperature water bath environment to obtain a first composition, vacuum drying the first composition to obtain an inorganic polymer modified bentonite adsorption material, wherein the inorganic polymer enhances the adsorption capacity of the modified bentonite on pollutants, the water glass, the silica sol and the nano-silica are continuously polymerized between the bentonite layers to generate a nano-zeolite porous substance, the adsorption capacity of the modified bentonite to pollutants is further improved, and the modified bentonite has good practicability.
Description
Technical Field
The invention relates to the technical field of pollution control, in particular to a preparation method of an inorganic polymer modified bentonite adsorption material.
Background
At present, in the wastewater treatment technology, the adsorption method is the most common method, which removes or recovers pollutants in wastewater by adding an adsorption material with a high specific surface area and a compact pore structure, has the advantages of small investment, simple and convenient operation, low energy consumption, multiple pollutant adsorption types and the like, and is widely applied to the treatment of industrial and urban domestic wastewater. The common adsorbing materials comprise polymer resin, activated carbon, zeolite, bentonite and the like, but the common adsorbing materials have some defects in the application process, for example, the activated carbon and the zeolite are expensive as adsorbing materials, the synthesis process of the polymer resin is complex, and the bentonite has poor pollutant adsorption capacity.
China contains abundant bentonite resources, and the reserves of the bentonite resources are the first in the world, so that the bentonite adopted as an adsorption material is a wastewater treatment material with great development prospects. However, how to further improve the pollutant adsorption capacity becomes a hot point of concern in water quality purification and wastewater treatment.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of an inorganic polymer modified bentonite adsorption material which is simple in preparation process and has strong pollutant removal capacity.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one general aspect, the present invention provides a method for preparing an inorganic polymer modified bentonite adsorption material, comprising the steps of:
adding bentonite and a sodium treatment agent into water, and uniformly mixing to obtain a bentonite suspension;
adding an inorganic polymer solution into the bentonite suspension, and reacting to obtain a first mixed solution;
adding water glass, silica sol and nano-silica into the first mixed solution, stirring in a constant-temperature water bath environment, and centrifuging to obtain a first compound;
and drying the first composition in vacuum to obtain the inorganic polymer modified bentonite adsorbing material.
Optionally, the bentonite comprises calcium bentonite.
Optionally, the sodium treatment agent comprises one or more of sodium carbonate, sodium sulfate, sodium nitrate, and sodium silicate.
Optionally, the inorganic polymer comprises one or more of polyaluminium chloride, polyaluminium sulfate, polyferric chloride and polyaluminium hydroxyferrite.
Optionally, the water glass, the silica sol and the nano-silica are 6-10 parts of the water glass, 5-20 parts of the silica sol and 10-20 parts of the nano-silica in parts by weight
Optionally, the bentonite and the sodium treatment agent are added into water and uniformly mixed to obtain the bentonite suspension, which specifically comprises the following steps:
simultaneously adding bentonite and a sodium treatment agent into water to obtain turbid liquid;
stirring the turbid solution to uniformly mix the bentonite and the sodium treatment agent;
filtering out the particulate matters with the particle size of more than 0.1mm in the turbid liquid to obtain the bentonite suspension.
Optionally, adding the inorganic polymer solution to the bentonite suspension, and reacting to obtain a first mixed solution specifically includes:
dropwise adding an inorganic polymer solution into the bentonite suspension;
ultrasonically dispersing bentonite suspension added with inorganic polymer solution;
and obtaining a first mixed solution after the reaction is finished.
Optionally, the dropwise addition of the inorganic polymer solution to the bentonite suspension specifically comprises:
stirring the bentonite suspension;
simultaneously, the inorganic polymer solution is added dropwise to the bentonite suspension.
Optionally, the temperature of the thermostatic water bath is 60-80 ℃.
Optionally, the temperature of the upper layer of turbid liquid is dried in vacuum below 60 ℃.
According to the preparation method of the inorganic polymer modified bentonite adsorption material, provided by the invention, bentonite is subjected to sodium treatment to obtain sodium bentonite with larger interlayer spacing, and then the inorganic polymer is introduced into the sodium bentonite interlayer, so that the interlayer spacing is further increased, more pollutants can be contained in the sodium bentonite interlayer, and the adsorption capacity of the modified bentonite on the pollutants is enhanced; then adding water glass, silica sol and nano-silica, and making them and the inorganic polymer previously fed into the interlayer undergo the process of full chemical reaction under the condition of a certain temp., and continuously polymerizing between the bentonite layers to obtain nano-level zeolite porous material so as to further raise the adsorption capacity of modified bentonite for pollutant and finally obtain a bentonite adsorption material with high pollutant adsorption capacity. In addition, the preparation method of the inorganic polymer modified bentonite adsorption material has the advantages of cheap and easily-obtained raw materials, simple and convenient preparation process, low economic cost and no corrosive or toxic raw materials, and is a simple, efficient, economic and environment-friendly bentonite modification mode.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a process flow diagram of a method for preparing an inorganic polymer-modified bentonite adsorbent material according to the present invention.
Detailed Description
In order to better understand the technical solutions, the technical solutions of the present application are described in detail with specific embodiments below, and it should be understood that the specific features in the embodiments and examples of the present application are detailed descriptions of the technical solutions of the present application, but not limitations of the technical solutions of the present application, and the technical features in the embodiments and examples of the present application may be combined with each other without conflict. It should be understood that the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Example one
Fig. 1 is a flow chart of a method for preparing an inorganic polymer-modified bentonite adsorbing material according to the present invention, and as shown in fig. 1, this example provides a method for preparing an inorganic polymer-modified bentonite adsorbing material, which includes the following steps:
s01, adding the bentonite and the sodium treatment agent into water, and uniformly mixing to obtain the bentonite suspension.
In step S01 of this example, the specific steps of adding bentonite and sodium treatment agent into water and mixing them uniformly to obtain a bentonite suspension are as follows:
the bentonite is put into water, and the sodium treatment agent is added into the water at the same time, in order to ensure that the bentonite and the sodium treatment agent are fully mixed and reacted, the mixed liquid can be put into a stirrer and uniformly mixed by the stirring of the stirrer, and simultaneously the bentonite can also be crushed by the stirrer to form fine particles.
Further, standing the stirred turbid liquid for a period of time, and filtering out precipitated fine particles by using a filter screen of 0.1mm when large-particle magazines in the liquid settle to obtain the bentonite suspension liquid with the granularity of less than 0.1 mm.
It should be noted that in this embodiment, the bentonite is calcium bentonite, and the sodium treatment agent includes one or more of sodium carbonate, sodium sulfate, sodium nitrate, and sodium silicate. And after the calcium bentonite reacts with the sodium treatment agent, the calcium bentonite is subjected to sodium treatment to obtain the sodium bentonite with larger interlayer spacing.
S02, adding the inorganic polymer solution into the bentonite suspension, and reacting to obtain a first mixed solution.
In step S02 of this example, in order to allow the inorganic polymer to react with the bentonite sufficiently, it is necessary to prepare an inorganic polymer solution in advance by adding the inorganic polymer to water, uniformly stirring to dissolve the inorganic polymer sufficiently, and standing for a while to obtain an inorganic polymer solution. After the inorganic polymer solution is prepared, dropwise adding the inorganic polymer solution into the bentonite suspension, stirring while dropwise adding until the inorganic polymer solution is completely dropwise added, placing the bentonite suspension added with the inorganic polymer solution on an ultrasonic dispersion instrument, performing ultrasonic dispersion on the bentonite suspension added with the inorganic polymer solution, and obtaining a first mixed solution after the reaction is finished.
It is noted that in this embodiment, the inorganic polymer includes one or more of polyaluminium chloride, polyaluminium sulfate, polyferric chloride, and polyaluminium hydroxy iron. Inorganic polymer is introduced to enter between sodium bentonite layers, so that the interlayer spacing is further increased, more pollutants can enter the sodium bentonite layers, and the adsorption capacity of the modified bentonite to the pollutants is enhanced.
And S03, adding water glass, silica sol and nano-silica into the first mixed solution, stirring in a constant-temperature water bath environment, and centrifuging to obtain a first compound.
In step S03 of this embodiment, after the first mixed solution is obtained, water glass, silica sol, and nano-silica may be added to react with the first mixed solution, but the environment where the water glass, the silica sol, and the nano-silica react with the first mixed solution is a constant temperature water bath environment, the temperature of the constant temperature water bath is 60 to 80 ℃, and magnetic stirring is continuously performed during the water bath process, and finally the first composition is obtained by centrifugation. Adding water glass, silica sol and nano-silica, and allowing the mixture to fully chemically react with the inorganic polymer which enters the interlayer at a certain temperature, and continuously polymerizing between the bentonite layers to generate a nano-zeolite porous substance, so that the adsorption capacity of the modified bentonite to pollutants is further improved.
The weight parts of the water glass, the silica sol and the nano-silica are 6-10 parts of the water glass, 5-20 parts of the silica sol and 10-20 parts of the nano-silica.
And S04, drying the first composition in vacuum to obtain the inorganic polymer modified bentonite adsorbing material.
In step S04 of this example, after the first composition is obtained, the reaction is continued to obtain the desired composite nanomaterial, specifically, the first composition is washed with clean water several times, and then dried under vacuum in an environment of 60 ℃ or lower, and finally the inorganic polymer-modified bentonite adsorbing material is obtained. The inorganic polymer modified bentonite adsorption material has strong adsorption capacity on heavy metal ions, and can be widely applied to the environmental fields of wastewater treatment, polluted soil solidification, polluted site restoration and the like. In addition, the preparation method of the inorganic polymer modified bentonite adsorption material has the advantages of cheap and easily-obtained raw materials, simple and convenient preparation process, low economic cost and no corrosive or toxic raw materials, and is a simple, efficient, economic and environment-friendly bentonite modification mode.
Example two
In this embodiment, a preparation method of an inorganic polymer modified bentonite adsorption material is specifically provided, and includes the following steps:
s01, adding the bentonite and the sodium treatment agent into water, and uniformly mixing to obtain the bentonite suspension.
In step S01 of this example, the specific steps of adding bentonite and sodium treatment agent into water and mixing them uniformly to obtain a bentonite suspension are as follows:
putting 8 parts of bentonite into 100 parts of water, simultaneously adding 1 part of sodium treatment agent into the water, putting the mixed liquid into a stirrer, controlling the stirring speed to be 2500r/min, stirring for 10 minutes, uniformly mixing the bentonite by stirring of the stirrer, and simultaneously crushing the bentonite by the stirrer to form fine particles.
Further, standing the stirred turbid liquid for 24 hours, and filtering out precipitated fine particles by using a filter screen with the particle size of 0.1mm when large-particle magazines in the liquid settle to the bottom to obtain the bentonite suspension with the particle size of less than 0.1 mm.
It is noted that in this example, the bentonite is calcium bentonite, and the sodium reagent is 0.5 parts sodium carbonate and 0.5 parts sodium sulfate.
S02, adding the inorganic polymer solution into the bentonite suspension, and reacting to obtain a first mixed solution.
In step S02 of this example, 35 parts of an inorganic polymer was added to 100 parts of water, uniformly stirred to be sufficiently dissolved, and allowed to stand for 12 hours to obtain an inorganic polymer solution. After the inorganic polymer solution is prepared, dropwise adding the inorganic polymer solution into the bentonite suspension, stirring while dropwise adding until the inorganic polymer solution is completely dropwise added, placing the bentonite suspension added with the inorganic polymer solution on an ultrasonic dispersion instrument, performing ultrasonic dispersion on the bentonite suspension added with the inorganic polymer solution, continuing to react for 6 hours under 25KHz ultrasonic waves, and obtaining a first mixed solution after the reaction is completed.
It is noted that in this example, the inorganic polymer is 20 parts of polyaluminium chloride, 5 parts of polyaluminium sulfate, and 10 parts of polyferric sulfate.
And S03, adding water glass, silica sol and nano-silica into the first mixed solution, stirring in a constant-temperature water bath environment, and centrifuging to obtain a first compound.
In step S03 of this embodiment, after the first mixed solution is obtained, water glass, silica sol, and nano-silica may be added to react with the first mixed solution, where the environment where the water glass, the silica sol, and the nano-silica react with the first mixed solution is a constant temperature water bath environment, the temperature of the constant temperature water bath is 60 to 80 ℃, and magnetic stirring is continuously performed during the water bath process for 48 hours, and finally a first compound is obtained by centrifugation.
The weight parts of the water glass, the silica sol and the nano-silica are 7 parts of the water glass, 10 parts of the silica sol and 15 parts of the nano-silica.
And S04, drying the first composition in vacuum to obtain the inorganic polymer modified bentonite adsorbing material.
In step S04 of this example, after the first composition was obtained, the first composition was washed with clean water several times, and then vacuum-dried in an environment at 60 ℃ or lower to finally prepare an inorganic polymer-modified bentonite adsorbing material.
EXAMPLE III
As still another embodiment of the present invention, different from the previous embodiment, in step S01 of the present embodiment, 8 parts of bentonite and 0.5 part of a sodium alkalizer are used, wherein the sodium alkalizer is 0.5 part of sodium silicate; in step S02, the inorganic polymer is 30 parts and comprises 10 parts of polyaluminium chloride, 10 parts of polyferric sulfate and 10 parts of polyaluminium hydroxyferrite, and in step S03, the temperature of the thermostatic waterbath is 70 ℃, and the weight part ratio of the water glass, the silica sol and the nano-silica is 6 parts of the water glass, 8 parts of the silica sol and 10 parts of the nano-silica.
Example four
As still another example of the present invention, unlike the previous example, in step S01 of the present example, the bentonite is 7 parts, and the sodium treatment agent is 1 part, wherein the sodium treatment agent includes 0.5 parts of sodium carbonate and 0.5 parts of sodium nitrate; in step S02, the inorganic polymer is 25 parts, the inorganic polymer comprises 5 parts of polyaluminium chloride, 5 parts of polyaluminium sulfate and 15 parts of polyaluminium hydroxy iron, and in step S03, the temperature of the thermostatic waterbath is 60 ℃, and the weight part ratio of the water glass, the silica sol and the nano-silica is 10 parts of the water glass, 15 parts of the silica sol and 10 parts of the nano-silica.
The inorganic polymer modified bentonite adsorbing material prepared by taking unmodified calcium bentonite as a blank group and working examples II, III and IV is added into 80mg/L Cr (VI) solution, the mass ratio of the adsorbing material to the solution is 1: 500, and the concentration of Cr (VI) ions in the solution is tested after the solution is magnetically stirred for 24 hours.
The results of the test solutions are shown in the following table:
it can be seen from the table that after the inorganic polymer modified bentonite adsorption materials prepared in the second, third and fourth examples are added, the concentration of Cr (VI) ions in the solution is greatly reduced to 2.96mg/L, the adsorption capacity of the modified bentonite to heavy metal ions reaches 38.52mg/g, and is improved by more than 30mg/g compared with unmodified calcium bentonite, which indicates that the inorganic polymer modified bentonite adsorption material synthesized by the invention has very excellent adsorption capacity to heavy metal ions, and can be widely applied to the environmental fields of wastewater treatment, contaminated soil solidification, contaminated site remediation and the like.
In summary, the embodiment of the invention provides a preparation method of an inorganic polymer modified bentonite adsorption material, and the bentonite is firstly subjected to sodium treatment to obtain sodium bentonite with larger interlayer spacing, and then the inorganic polymer is introduced into the sodium bentonite interlayer, so that the interlayer spacing is further increased, more pollutants can be contained in the sodium bentonite interlayer, and the adsorption capacity of the modified bentonite on the pollutants is enhanced; then adding water glass, silica sol and nano-silica, and making them and the inorganic polymer previously fed into the interlayer undergo the process of full chemical reaction under the condition of a certain temp., and continuously polymerizing between the bentonite layers to obtain nano-level zeolite porous material so as to further raise the adsorption capacity of modified bentonite for pollutant and finally obtain a bentonite adsorption material with high pollutant adsorption capacity. In addition, the preparation method of the inorganic polymer modified bentonite adsorption material has the advantages of cheap and easily-obtained raw materials, simple and convenient preparation process, low economic cost and no corrosive or toxic raw materials, is a simple, efficient, economic and environment-friendly bentonite modification mode, and has good practicability.
The foregoing description has been directed to specific embodiments of this disclosure. Other embodiments are within the scope of the following claims. In some cases, the actions or steps recited in the claims may be performed in a different order than in the embodiments and still achieve desirable results. In addition, the processes depicted in the accompanying figures do not necessarily require the particular order shown, or sequential order, to achieve desirable results. In some embodiments, multitasking and parallel processing may also be possible or may be advantageous.
It should be noted that, for those skilled in the art, without departing from the principle of the present application, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present application.
Claims (10)
1. A preparation method of an inorganic polymer modified bentonite adsorption material is characterized by comprising the following steps:
adding bentonite and a sodium treatment agent into water, and uniformly mixing to obtain a bentonite suspension;
adding an inorganic polymer solution into the bentonite suspension, and reacting to obtain a first mixed solution;
adding water glass, silica sol and nano-silica into the first mixed solution, stirring in a constant-temperature water bath environment, and centrifuging to obtain a first compound;
and drying the first composition in vacuum to obtain the inorganic polymer modified bentonite adsorbing material.
2. The method of claim 1, wherein the bentonite comprises calcium bentonite.
3. The method of claim 1, wherein the sodium reagent comprises one or more of sodium carbonate, sodium sulfate, sodium nitrate, and sodium silicate.
4. The method of claim 1, wherein the inorganic polymer comprises one or more of polyaluminum chloride, polyaluminum sulfate, polyferric chloride, and polyaluminum ferric hydroxide.
5. The preparation method according to claim 1, wherein the water glass, the silica sol and the nano silica are 6 to 10 parts of the water glass, 5 to 20 parts of the silica sol and 10 to 20 parts of the nano silica in parts by weight.
6. The method of claim 1, wherein the step of adding bentonite and the sodium treatment agent to water and mixing them uniformly to obtain the bentonite suspension comprises:
simultaneously adding bentonite and a sodium treatment agent into water to obtain turbid liquid;
stirring the turbid solution to uniformly mix the bentonite and the sodium treatment agent;
filtering out particulate matters with the particle size larger than 0.1mm in the turbid liquid to obtain the bentonite suspension.
7. The method of claim 1, wherein the step of adding an inorganic polymer solution to the bentonite suspension and reacting to obtain a first mixed solution comprises:
dropwise adding the inorganic polymer solution into the bentonite suspension;
ultrasonically dispersing the bentonite suspension added to the inorganic polymer solution;
and obtaining the first mixed solution after the reaction is finished.
8. The method according to claim 7, wherein the step of adding the inorganic polymer solution dropwise to the bentonite suspension comprises:
agitating the bentonite suspension;
simultaneously, an inorganic polymer solution is added dropwise to the bentonite suspension.
9. The method according to claim 1, wherein the temperature of the thermostatic waterbath is 60 to 80 ℃.
10. The method of claim 1, wherein the upper layer of the suspension is vacuum dried at an ambient temperature of 60 ℃ or less.
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| CN112473619A (en) * | 2020-12-08 | 2021-03-12 | 句容康泰膨润土有限公司 | Efficient and environment-friendly organic-inorganic composite bentonite material |
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