CN110980754B - Preparation method of natural sodium bentonite - Google Patents
Preparation method of natural sodium bentonite Download PDFInfo
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- CN110980754B CN110980754B CN201911406404.XA CN201911406404A CN110980754B CN 110980754 B CN110980754 B CN 110980754B CN 201911406404 A CN201911406404 A CN 201911406404A CN 110980754 B CN110980754 B CN 110980754B
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/44—Products obtained from layered base-exchange silicates by ion-exchange with organic compounds such as ammonium, phosphonium or sulfonium compounds or by intercalation of organic compounds, e.g. organoclay material
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- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The invention relates to a preparation method of natural sodium bentonite, and belongs to the field of deep processing of bentonite. A preparation method of natural sodium bentonite comprises the following steps: (1) Adding water into the bentonite raw material to prepare slurry, wherein the slurry concentration is 2-20 wt%, uniformly stirring and dispersing, and sieving the slurry with a 200-mesh sieve; (2) Adding acid into the sieved bentonite slurry to adjust the pH value to acidity, and stirring and dispersing uniformly; (3) Adding ammonium salt into the bentonite slurry with the adjusted pH value for pretreatment, wherein the addition amount of the ammonium salt is more than 0.8 time of the CEC of the bentonite, and stirring and dispersing uniformly; (4) Washing the slurry obtained in the step (3) by adding water, and washing the slurry by water until the pH =4.0-7.0; (5) And adding sodium salt into the slurry after water washing for sodium modification, wherein the adding amount of the sodium salt is 0.5-1.5 times of that of the bentonite CEC, and drying and crushing to obtain the sodium bentonite.
Description
Technical Field
The invention relates to a preparation method of natural sodium bentonite, and belongs to the field of deep processing of bentonite.
Technical Field
The main mineral component of bentonite is montmorillonite, which is a layered silicate mineral with a layer of aluminum oxygen octahedral sheet sandwiched between two layers of silicon oxygen tetrahedral sheet, and high valence cations in the structural unit layer are easily replaced by low valence cations, such as Si in tetrahedron 4+ Can be coated with Al 3+ Substituted, al in octahedron 3+ Can be coated with Fe 2+ 、Mg 2+ Such substitution causes permanent negative charges of different strengths between layers, and excess negative charges pass through Na as a cation adsorbed between layers to maintain the balance of self-charges + 、K + 、Ca 2+ And Mg 2+ Etc. and the cations in the interlayer region will be compensated for as long as there is a concentration of other cations in the medium higher than the concentration of cations already adsorbed between the layersThe exchange occurs to a varying extent, which is the interlayer cation exchange characteristic of montmorillonite.
The good physical and chemical properties of bentonite are greatly related to the types and the quantity of cations adsorbed between layers. The bentonite and interlayer hydrated cations are adsorbed in an electrostatic form, and the coulomb law is observed, namely, high-valence ions have more charge than low-valence ions, so that the generated electrostatic force and mutual attraction are stronger. Different exchangeable cations can make the bentonite have different hydration properties, and generally monovalent exchangeable cations have better hydration properties than divalent or trivalent exchangeable cations. This is also the interlayer adsorption of Na + The sodium bentonite has higher Ca adsorption effect 2+ The calcium-based bentonite has good expansibility and colloid property. Compared with calcium bentonite, sodium bentonite has better expansibility, cation exchange property, water dispersibility, colloid value, caking property, lubricating property and thermal stability, thereby having wider application. For different purposes, bentonite of different types is required to be selected. The mineral resources of bentonite in China are very rich and widely distributed, the total reserve is the first in the world, but calcium bentonite is taken as the main material, and natural sodium bentonite only accounts for about 10%, so that the calcium bentonite is usually subjected to sodium modification, namely, the artificial sodium bentonite.
The principle of the artificial sodium bentonite is that by utilizing the exchange property of cations in the interlayer domain of the bentonite, an inorganic or organic sodium salt modifier (sodium modifier for short) is added into calcium bentonite, sodium ion concentration of a medium is improved, the sodium ion enters the interlayer of the bentonite, calcium ions in the interlayer are replaced, and therefore the sodium bentonite is prepared, and the ion exchange reaction is as follows:
Ca-Bentonite+Na + →Na-Bentonite+Ca 2+
the most commonly used sodium salt is sodium carbonate from an economic point of view.
In the deep processing processes of research, development, application and the like of bentonite products, the selection of natural sodium bentonite or artificial sodium bentonite as a raw material is often involved, and the artificial sodium bentonite and the natural sodium bentonite have great difference in performances such as temperature resistance, weather resistance, stability, pH and the like:
(1) As a foundry sand binder. The artificial sodium-modified soil has poor durability, the compressive strength of the bonded molding sand is reduced by half after the bonded molding sand is used twice, and the natural sodium-based soil can be reused for more than 10 times.
(2) The temperature resistance is very different. The artificial sodium-modified soil is heated to 400 ℃, the effective montmorillonite content is reduced by 40 percent, and the effective montmorillonite content of the natural sodium-based soil is only reduced by 8 percent. The natural sodium-based soil is used for the iron ore concentrate pellet binder, and the bursting temperature of the iron ore concentrate pellet binder is 100 ℃ higher than that of the artificial sodium-modified soil.
(3) As a waterproof material, the natural sodium bentonite has good durability, while the artificial sodium bentonite has short service life.
(4) The alkalinity of natural sodium-based soil is low, the general pH is less than 10.0, the alkalinity of artificial sodium-based soil is relatively high, the general pH is more than 10.0, in the actual use process, the pH is usually required to be adjusted to be neutral or alkalescent, the stronger the alkalinity is, the more the acid consumption is, the higher the conductivity of the system is, the product quality is influenced, and in addition, the strong alkalinity also has certain influence on the compatibility and the like.
The difference is mainly caused by incomplete sodium modification and interlayer high valence cations such as Ca 2 + 、Mg 2+ 、Fe 2+ Etc. The natural sodium-based soil layers basically contain no or very little calcium and magnesium ions, and the artificial sodium-modified soil is generally calcium-based bentonite and Na 2 CO 3 The sodium ions replace calcium ions between bentonite layers to generate water-insoluble CaCO 3 The ion exchange reaction is promoted to proceed rightwards, and sodium bentonite is formed. However, due to Ca 2+ The potential is strong, and the bentonite has preferential Ca adsorption 2+ The reaction is therefore reversible and it is impossible to reach 100% sodium base, which in turn leads to inhomogeneities in the artificial sodified bentonite and to defects of incomplete sodium modification. In addition, in the process of sodium treatment, the calcium carbonate particles which are generated by the reaction and are extremely fine are enriched on the bentonite particles, the suspension dispersibility of the sodium bentonite is influenced, and the calcium carbonate has certain activity under certain conditions, such as CO 2 In the presence or at a slightly reduced pH, a reverse reaction takes placeAnd calcium ions exchange sodium ions and enter the bentonite layer again, so that the stability of the artificial sodium modified soil is poor.
In patent CN102974750A "preparation method of natural sodium-based bentonite for precision casting", soda ash and caustic soda are added into dried and pulverized bentonite ore, and sodium modification is performed by an extrusion sodium modification machine, and then drying and pulverizing are performed. The patent is basically the same as the conventional semi-dry sodium treatment mode, the bentonite is directly subjected to alkali treatment, but calcium and magnesium ions and the like between layers of the bentonite still remain in the bentonite, the defect that the artificial sodium-treated soil is incompletely or unstably subjected to sodium treatment still exists, and the artificial sodium-treated soil cannot completely replace natural sodium-based soil for use.
Disclosure of Invention
The invention aims to provide a preparation method of natural sodium bentonite, which solves the problems of low reserve of natural sodium bentonite, insufficient sodium conversion and poor stability of conventional artificial sodium bentonite, and thus the use is limited.
In order to achieve the purpose, the technical scheme is as follows:
a preparation method of natural sodium bentonite comprises the following steps:
(1) Adding water into the bentonite raw material to prepare slurry, wherein the slurry concentration is 2-20 wt%, uniformly stirring and dispersing, and sieving the slurry with a 200-mesh sieve;
(2) Adding acid into the screened bentonite slurry to adjust the pH value to acidity, and stirring and dispersing the bentonite slurry uniformly;
(3) Adding ammonium salt into the bentonite slurry with the adjusted pH value for pretreatment, wherein the addition amount of the ammonium salt is more than 0.8 time of the CEC of the bentonite, and stirring and dispersing uniformly;
(4) Washing the slurry obtained in the step (3) by adding water, and washing the slurry by water until the pH is =4.0-7.0;
(5) And adding sodium salt into the slurry after water washing for sodium modification, wherein the adding amount of the sodium salt is 0.5-1.5 times of that of the bentonite CEC, and drying and crushing to obtain the sodium bentonite.
According to the scheme, the bentonite raw material in the step (1) can be any one of calcium bentonite, magnesium bentonite, hydrogen bentonite, aluminum bentonite, lithium bentonite and mixed bentonite.
According to the scheme, the montmorillonite content of the bentonite raw material in the step (1) is more than 50%, preferably more than 70%, and most preferably more than 90%.
According to the above scheme, the pH value in the step (2) is adjusted to be acidic, and the pH value is less than 5, preferably less than 4, and most preferably less than 3.
According to the scheme, the ammonium salt in the step (3) can be any one or a mixture of more of ammonium chloride, ammonium sulfate, ammonium nitrate, ammonium acetate, ammonium fluoride and ammonium bromide.
According to the scheme, the adding amount of the ammonium salt in the step (3) is more than 0.8 time of the CEC of the bentonite, preferably more than 1.2 times of the CEC of the bentonite, and most preferably more than 1.5 times of the CEC of the bentonite.
According to the scheme, the sodium salt in the step (5) can be one or more of sodium carbonate, sodium bicarbonate, sodium sulfite, sodium acetate, sodium silicate, sodium phosphate, sodium hydroxide, sodium fluoride, sodium citrate, sodium polyphosphate, sodium hexametaphosphate, sodium pyrophosphate and sodium polyacrylate, and is preferably an alkaline sodium salt, and most preferably sodium carbonate.
Firstly, adding acid to adjust the pH of bentonite slurry to be acidic, firstly, removing carbonate impurities contained in the bentonite raw material to improve the purity of the bentonite, secondly, converting calcium, magnesium and the like in the bentonite into soluble ions to be washed and removed, and avoiding cations from slowly entering between montmorillonite layers in the process of long-term storage of the subsequently formed sodium bentonite, so as to reduce the quality of the sodium bentonite and influence the weather resistance and stability of the bentonite; pretreating bentonite with ammonium salt to obtain bentonite layer exchangeable cations such as Ca 2+ 、Mg 2+ 、Fe 2+ The plasma is completely replaced and enters the bentonite slurry, and the bentonite raw material is transformed into ammonium-based soil; washing with water to remove the impurity ions, adding sodium salt for sodium treatment, replacing ammonium ions with sodium ions to enter bentonite layers, and adding NH 4 + Conversion to NH under basic conditions 3 Volatilization also promotes the ion exchange reaction, and the finally prepared sodium bentonite interlayer basically only contains sodium ions and does not contain other exchangeable Ca 2+ 、Mg 2+ 、Fe 2+ And the components of the cations are consistent with those of the natural sodium bentonite.
Compared with the prior art, the invention has the following beneficial effects:
(1) Adding acid to adjust the pH of the bentonite slurry to acidity, removing carbonate impurities, converting insoluble calcium magnesium iron salt and the like into soluble ions, and washing to remove the soluble ions, thereby improving the purity of the bentonite to a certain extent;
(2) The invention carries out sodium treatment on the basis of ammonium base soil which is washed by water to have pH =4.0-7.0, and can obtain sodium bentonite with lower pH, the alkalinity is consistent with that of natural sodium bentonite, and the application range is wide.
(3) Ca influencing the performance of the sodium bentonite is removed 2+ 、Mg 2+ 、Fe 2+ The exchangeable cations and the impurities such as carbonate avoid the occurrence of reversible reaction and the problem of incomplete sodium treatment. The components are consistent with natural sodium bentonite, and the natural sodium bentonite can be replaced by the natural sodium bentonite in performance.
Description of the figures
FIG. 1: example 1 calcium bentonite raw material XRD
FIG. 2: EXAMPLE 1 preparation of sodium bentonite XRD
FIG. 3: example 2 calcium bentonite raw material XRD
FIG. 4: EXAMPLE 2 preparation of sodium bentonite XRD
FIG. 5: example 3 calcium bentonite raw material XRD
FIG. 6: EXAMPLE 3 preparation of sodium bentonite XRD
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
(1) Adding water into calcium bentonite with the purity of 65 percent to prepare slurry with the concentration of 20 weight percent, stirring and dispersing uniformly, and sieving the slurry with a 200-mesh sieve;
(2) Adding acid into the sieved bentonite slurry to adjust the pH value to 4.8, and stirring and dispersing uniformly;
(3) Adding ammonium sulfate into the bentonite slurry with the adjusted pH value for pretreatment, wherein the addition amount of the ammonium sulfate is 0.9 time of that of the bentonite CEC, and stirring and dispersing uniformly;
(4) Washing the slurry obtained in the step (3) by adding water, and washing the slurry by water until the pH is =6.5;
(5) And adding sodium bicarbonate into the slurry after washing for sodium modification, wherein the addition amount of sodium salt is 0.8 time of the CEC of the bentonite, drying and crushing to obtain the sodium bentonite.
Example 2
(1) Adding water into calcium bentonite with the purity of 94 percent to prepare slurry with the concentration of 10 weight percent, stirring and dispersing uniformly, and sieving the slurry with a 200-mesh sieve;
(2) Adding acid into the sieved bentonite slurry to adjust the pH value to 2.7, and stirring and dispersing uniformly;
(3) Adding ammonium chloride into the bentonite slurry with the adjusted pH value for pretreatment, wherein the addition amount of ammonium salt is 2.0 times of that of the bentonite CEC, and stirring and dispersing uniformly;
(4) Washing the slurry obtained in the step (3) by adding water, and washing the slurry by water until the pH is =5.1;
(5) And adding sodium carbonate into the washed slurry for sodium modification, wherein the addition amount of the sodium salt is 1.0 time of that of the bentonite CEC, and drying and crushing to obtain the sodium bentonite.
Example 3
(1) Adding water into calcium bentonite with the purity of 85% to prepare slurry with the concentration of 5wt%, stirring and dispersing uniformly, and sieving the slurry with a 200-mesh sieve;
(2) Adding acid into the sieved bentonite slurry to adjust the pH value to 3.5, and stirring and dispersing uniformly;
(3) Adding ammonium nitrate into the bentonite slurry with the adjusted pH value for pretreatment, wherein the addition of the ammonium salt is 1.2 times of that of the bentonite CEC, and stirring and dispersing uniformly;
(4) Washing the slurry obtained in the step (3) by adding water, and washing the slurry by water until the pH is =4.3;
(5) And adding sodium acetate into the slurry after washing for sodium modification, wherein the addition amount of sodium salt is 1.5 times of that of the bentonite CEC, drying and crushing to obtain the sodium bentonite.
Fig. 1 to 6 show XRD patterns of the calcium bentonite raw material used in examples 1 to 3 and the prepared sodium bentonite sample, respectively, and it can be seen from the XRD patterns that the d001 peak values of the calcium bentonite raw material are all about 1.5nm, and after the calcium bentonite raw material is treated by the method of example, the d001 diffraction peaks are all shifted to high angles, and the peak values are changed to about 1.2nm, indicating that the prepared sample is sodium bentonite.
XRF was used to test the compositions of the samples obtained in examples 1-3 and the comparative samples using 83% pure natural Na-based soil of Xinjiang as a control, and the results are shown in Table 1 below.
TABLE 1 composition test results of the example and comparative samples
As can be seen from the analysis of Table 1, the compositions of the samples of examples are substantially the same as those of the natural sodium-based soil, and the contents of interlayer exchangeable calcium ions are all low, i.e., 0.5% or less.
The pH of the example samples and the comparative samples were tested according to the method for testing pH in the national standard GB1886.63-2015 national standard for food safety of food additives bentonite, the procedure being as follows:
weighing a proper amount of sample, adding water to prepare a suspension of 20g/L, and measuring the pH of the suspension by using a pH meter.
The test results are shown in table 2 below.
Table 2 pH of the example and comparative samples
| Sample (I) | Example 1 | Example 2 | Example 3 | Control sample |
| pH | 9.32 | 9.15 | 9.26 | 9.28 |
Analysis table 2 shows that the pH of the samples in the examples is similar to that of the comparative sample, and the pH is lower than 10.0, which indicates that the sodium bentonite prepared by the method has lower alkalinity and wide application range like natural sodium bentonite.
Claims (4)
1. A preparation method of natural sodium bentonite is characterized by comprising the following steps:
(1) Adding water into the bentonite raw material to prepare slurry, wherein the slurry concentration is 2-20 wt%, uniformly stirring and dispersing, and sieving the slurry with a 200-mesh sieve;
(2) Adding acid into the screened bentonite slurry to adjust the pH value to be less than 3, and stirring and dispersing uniformly;
(3) Adding ammonium salt into the bentonite slurry with the adjusted pH value for pretreatment, wherein the addition amount of the ammonium salt is more than 1.5 times of that of the bentonite CEC, and stirring and dispersing uniformly; the ammonium salt in the step (3) is a mixture of any one or more of ammonium chloride, ammonium sulfate, ammonium nitrate, ammonium acetate, ammonium fluoride or ammonium bromide;
(4) Washing the slurry obtained in the step (3) by adding water, and washing the slurry by water until the pH =4.0-7.0;
(5) And adding sodium salt into the slurry after water washing for sodium modification, wherein the adding amount of the sodium salt is 0.5-1.5 times of that of the bentonite CEC, and drying and crushing to obtain the sodium bentonite.
2. The method for preparing natural sodium bentonite according to claim 1, wherein the method comprises the following steps: the bentonite raw material in the step (1) is any one of calcium bentonite, magnesium bentonite, hydrogen bentonite, aluminum bentonite, lithium bentonite and mixed bentonite.
3. The method for preparing natural sodium bentonite according to claim 1, wherein the method comprises the following steps: the montmorillonite content of the bentonite raw material in the step (1) is at least over 50 percent.
4. The method for preparing natural sodium bentonite according to claim 1, wherein: in the step (5), the sodium salt is one or a mixture of sodium carbonate, sodium bicarbonate, sodium sulfite, sodium acetate, sodium silicate, sodium phosphate, sodium fluoride, sodium citrate, sodium polyphosphate, sodium hexametaphosphate, sodium pyrophosphate and sodium polyacrylate.
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| CN113265296A (en) * | 2021-05-11 | 2021-08-17 | 广州明创生物科技有限公司 | Cold pressing and physical refining method of camellia oil |
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