CN111470514A - Modification method of calcium bentonite - Google Patents
Modification method of calcium bentonite Download PDFInfo
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- CN111470514A CN111470514A CN202010287941.3A CN202010287941A CN111470514A CN 111470514 A CN111470514 A CN 111470514A CN 202010287941 A CN202010287941 A CN 202010287941A CN 111470514 A CN111470514 A CN 111470514A
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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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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- 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
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
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- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
Abstract
The invention discloses a modification method of calcium bentonite, which comprises the steps of purifying the calcium bentonite by a wet method, carrying out sodium modification by using a sodium treatment agent consisting of trisodium phosphate and sodium carbonate under the synergistic action of ultrasound and microwaves, and carrying out organic modification by using quaternary ammonium salt; the method specifically comprises the following steps: (1) multi-stage purification; (2) sodium modification: blending refined bentonite into slurry with the concentration of 10%, adding a sodium treatment agent with the amount of 2.5-7.5% of the mass of the refined bentonite, uniformly stirring, reacting at 70-90 ℃ for 10-15 min under the synergistic action of ultrasound and microwave, filtering, washing to be neutral by using dilute hydrochloric acid, drying at 80 ℃, and grinding to obtain sodium bentonite; the sodium reagent comprises the following components in percentage by mass: 5-10% of trisodium phosphate and the balance of sodium carbonate; (3) and (4) carrying out organic modification. The invention utilizes the synergistic means of ultrasound and microwave to improve the permeability and the interlaminar mass transfer rate of the bentonite, further accelerates the enrichment effect of a sodium catalyst and quaternary ammonium salt between bentonite layers, obviously shortens the modification time and improves the product quality.
Description
Technical Field
The invention belongs to the technical field of bentonite modification, and particularly relates to a modification method of calcium bentonite.
Background
The bentonite has montmorillonite as main component, layered silicate crystal comprising two Si-O tetrahedrons and Al-O octahedron sandwiched between the two Si-O tetrahedrons, and has high expansibility, adsorptivity, thixotropy, dispersivity, cation exchange performance, low cost and wide application in industrial fields. The mineral area of the bentonite in the Xuan city of Anhui is mainly formed by weathering of acid lava, the mineral components are mainly montmorillonite, a small amount of kaolinite, illite, mica and the like, the content of the montmorillonite is 31.82 percent at the lowest, 93.18 percent at the highest and 52.26 percent on average, and the bentonite is mostly calcium bentonite of grade III and grade II.
Compared with calcium-based soil, the sodium bentonite has large swelling capacity and high cation exchange amount, and the interlayer ions are mainly Na+The total amount of interlayer charges is not high, the cohesive force is weak, the particles are small, and the like, so that the calcium bentonite needs to be subjected to sodium modification before use to improve the performance and the use value of the calcium bentonite. The sodium modification method comprises physical, chemical, mechanical and other methods, but the existing calcium bentonite modification method generally has the problems of small cation exchange quantity, low reaction rate, long modification time, general modification effect and the like. Therefore, it is necessary to provide a rapid modification method of bentonite with high calcium ion substitution rate, which is beneficial to improving the application value and economic value of bentonite.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for modifying calcium bentonite.
The technical scheme of the invention is summarized as follows:
a modification method of calcium bentonite comprises the following steps: after the calcium bentonite is purified by a wet method, under the synergistic action of ultrasound and microwave, firstly, a sodium treatment agent consisting of trisodium phosphate and sodium carbonate is used for carrying out sodium treatment modification, and then quaternary ammonium salt is used for carrying out organic modification; the method specifically comprises the following steps:
(1) multi-stage purification: crushing raw ore soil of calcium bentonite to 100 meshes, dispersing the crushed raw ore soil in deionized water to prepare slurry with the concentration of 10%, stirring for 2 hours, standing for 0.5 hour, removing coarse slag, repeatedly cleaning for 3 times, standing for settling overnight, taking out an upper suspension, filtering, naturally drying to obtain primary purified soil, and repeating the processes of dispersing, settling and purifying until the upper suspension is not turbid to obtain refined bentonite;
(2) sodium modification: preparing refined bentonite into slurry with the concentration of 10% by using deionized water, adding a sodium agent, controlling the using amount of the sodium agent to be 2.5-7.5% of the mass of the refined bentonite, uniformly stirring, reacting for 10-15 min at 70-90 ℃ under the synergistic effect of ultrasound and microwave, filtering, washing to be neutral by using dilute hydrochloric acid, drying at 80 ℃, and grinding to obtain sodium bentonite;
the sodium reagent comprises the following components in percentage by mass: 5-10% of trisodium phosphate and the balance of sodium carbonate;
(3) organic modification: dropwise adding 5-8% of quaternary ammonium salt water solution with the same mass into the obtained sodium bentonite, stirring until the sodium bentonite is fully swelled, reacting for 15-20 min at 70-90 ℃ under the synergistic effect of ultrasound and microwave, drying, and grinding to obtain modified bentonite;
in the step (2) and the step (3), the ultrasonic frequency is 35KHz, the power is 400W, and the microwave power is 500W.
Preferably, the quaternary ammonium salt aqueous solution comprises the following components in percentage by mass: 5-8% of hexadecyl trimethyl ammonium bromide or octadecyl trimethyl ammonium bromide, and the balance of water.
The invention has the beneficial effects that:
1. the invention carries out sodium modification on calcium bentonite by using the sodium modifier prepared from trisodium phosphate and sodium carbonate for the first time, obviously improves the replacement rate of sodium ions between bentonite layers, improves the sodium modification quality, has stronger exchange and adsorption effects on calcium ions compared with the traditional sodium modifier, and realizes the complete exchange of calcium ions on the surface of the bentonite and between the bentonite layers.
2. The method utilizes a synergistic means of ultrasound and microwave to improve the permeability and the interlaminar mass transfer rate of the bentonite, improve the contact probability of the modifier and the bentonite, further accelerate the enrichment effect of the sodiumizing agent and the quaternary ammonium salt between the layers of the bentonite, obviously shorten the modification time compared with the traditional modification method, complete the modification reaction within 20min, and improve the product quality.
Drawings
FIG. 1 is a flow chart of a method for modifying calcium bentonite according to the invention;
FIG. 2 is an XRD (X-ray diffraction) pattern of calcium bentonite modified by sodium treatment with different sodium treatment agents in example 1 and comparative examples 1-2 in FIG. 2;
FIG. 3 is FTIR analysis spectra of calcium bentonite sodium-modified by different sodium-modifying agents in example 1 and comparative examples 1-2;
FIG. 4 is a particle size distribution diagram of the sodium modified calcium bentonite of example 1;
FIG. 5 is an XRD spectrum of the organically modified sodium bentonite of examples 1-2;
FIG. 6 is an FTIR spectrum of organically modified sodium-based samples of examples 1-3.
Note: FIG. 2 and FIG. 3 are views showing (a) sodium chloride of comparative example 1, (b) sodium carbonate of comparative example 2, and (c) trisodium phosphate 5% + sodium carbonate 95% of example 1;
in fig. 5 and 6, (a) shows example 1: 5% hexadecyltrimethylammonium bromide, (b) represents example 2: 5% Octadecyltrimethylammonium bromide, (c) represents example 3: 8% Octadecyltrimethylammonium bromide (FIG. 5 without curve (c)).
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
Example 1
(1) Taking calcium bentonite ore in Xuan city, Anhui province as a test object, weighing 200g of calcium bentonite raw ore soil, crushing the raw ore soil to 100 meshes, dispersing the crushed raw ore soil in 1800m L deionized water to prepare slurry with the concentration of 10%, stirring the slurry for 2 hours, standing the slurry for 0.5 hour, removing coarse slag, repeatedly cleaning the slurry for 3 times, standing and settling the slurry overnight, taking out upper suspension, filtering and naturally drying the suspension to obtain primary purified soil, and repeating the dispersing, settling and purifying processes until the upper suspension is not turbid to obtain refined bentonite;
(2) sodium modification, namely preparing 40g of refined bentonite into slurry with the concentration of 10% by using 360m L deionized water, adding 1.0g of sodium agent, controlling the dosage of the sodium agent to be 2.5% of the mass of the refined bentonite, uniformly stirring, reacting for 10min at 70 ℃ under the synergistic action of ultrasound with the frequency of 35KHz and the power of 400W and microwaves with the power of 500W, filtering, washing to be neutral by using dilute hydrochloric acid, drying at 80 ℃, and grinding to obtain sodium bentonite;
the sodium reagent comprises the following components in percentage by mass: 5% of trisodium phosphate and the balance of sodium carbonate;
(3) organic modification: and (2) dropwise adding 5% hexadecyl trimethyl ammonium bromide aqueous solution with the same mass into the obtained sodium bentonite, stirring until the sodium bentonite is fully swelled, reacting for 15min at 70 ℃ under the synergistic action of ultrasound with the frequency of 35KHz and the power of 400W and microwaves with the power of 500W, drying, and grinding to obtain the modified bentonite.
Example 2
(1) The same as example 1;
(2) sodium modification, namely preparing 40g of refined bentonite into slurry with the concentration of 10% by using 360m L deionized water, adding 2.0g of sodium agent, controlling the dosage of the sodium agent to be 5.0% of the mass of the refined bentonite, uniformly stirring, reacting for 15min at 80 ℃ under the synergistic action of ultrasound with the frequency of 35KHz and the power of 400W and microwaves with the power of 500W, filtering, washing to be neutral by using dilute hydrochloric acid, drying at 80 ℃, and grinding to obtain sodium bentonite;
the sodium reagent comprises the following components in percentage by mass: 7.5 percent of trisodium phosphate and the balance of sodium carbonate;
(3) organic modification: and (2) dropwise adding 5% octadecyl trimethyl ammonium bromide aqueous solution with equal mass into the obtained sodium bentonite, stirring until the sodium bentonite is fully swelled, reacting for 20min at 80 ℃ under the synergistic action of ultrasound with the frequency of 35KHz and the power of 400W and microwaves with the power of 500W, drying, and grinding to obtain the modified bentonite.
Example 3
(1) The same as example 1;
(2) sodium modification, namely preparing 40g of refined bentonite into slurry with the concentration of 10% by using 360m L deionized water, adding 3.0g of sodium agent, controlling the dosage of the sodium agent to be 5.0% of the mass of the refined bentonite, uniformly stirring, reacting for 15min at 85 ℃ under the synergistic action of ultrasound with the frequency of 35KHz and the power of 400W and microwaves with the power of 500W, filtering, washing to be neutral by using dilute hydrochloric acid, drying at 80 ℃, and grinding to obtain sodium bentonite;
the sodium reagent comprises the following components in percentage by mass: 10% of trisodium phosphate and the balance of sodium carbonate;
(3) organic modification: and (2) dropwise adding 8% octadecyl trimethyl ammonium bromide aqueous solution with equal mass into the obtained sodium bentonite, stirring until the sodium bentonite is fully swelled, reacting for 20min at 85 ℃ under the synergistic action of ultrasound with the frequency of 35KHz and the power of 400W and microwaves with the power of 500W, drying, and grinding to obtain the modified bentonite.
Comparative examples 1-2 are the same as example 1 except that: comparative example 1 uses sodium chloride as a sodium agent, and comparative example 2 uses sodium carbonate as a modifier.
FIG. 2 is XRD patterns of calcium bentonite sodium modified by different sodium modifiers of example 1 and comparative examples 1-2, wherein (a) sodium chloride of comparative example 1, (b) sodium carbonate of comparative example 2, (c) trisodium phosphate 5% + sodium carbonate 95% of example 1: as can be seen from fig. 2, after sodium modification is performed on purified bentonite in example 1 and comparative examples 1 to 2, sodium ions replace calcium ions as main interlayer components, but the modification effect of example 1 is more obvious than that of comparative examples 1 to 2, and it is proved that trisodium phosphate has a synergistic effect on the sodium modification effect of sodium carbonate.
FIG. 3 is FTIR analysis spectra of calcium bentonite sodium modified with different sodium modifiers of example 1 and comparative examples 1-2, wherein (a) sodium chloride of comparative example 1, (b) sodium carbonate of comparative example 2, (c) trisodium phosphate 5% + sodium carbonate 95% of example 1: as can be seen from FIG. 3, the length of the groove is 1568cm-1An absorption peak of carbonate ions of 1034cm appears-1The expansion and contraction vibration absorption peak of nearby Si-O-Si becomes broad after sodium modification and is split into 1025cm-1And 1085cm-1A bimodal absorption band at 3625cm-1The peak value of (A) is the stretching vibration of OH in montmorillonite, and the peak value is 1642cm-1Bending vibration of interlayer water is 1046cm-1Form a strong absorption band, which is the stretching vibration of Si-O-Si, 796cm-1Bending vibration for Si-O-Al, 520cm-1Is the stretching vibration of Si-O-Al, which are typical bands of silicate and are sodium-basedThe typical characteristics of bentonite are that after sodium treatment, the hydration of sodium ions is weaker than that of calcium, magnesium and aluminum ions, so that hydrogen bonds formed between the surface of the bentonite and water are weakened, the absorption of Si-O and Si-O-Si is enhanced and split into double peaks, and compared with calcium bentonite before treatment, other characteristic absorption peaks are not changed, which indicates that the structure of the bentonite is not changed by sodium treatment.
FIG. 4 is a particle size distribution diagram of the sodium modified calcium bentonite of example 1, and Table 1 shows the particle size distribution diagrams of the sodium modified calcium bentonite of different sodium modifiers of example 1 and comparative examples 1-2:
TABLE 1
As can be seen from table 1 and fig. 4, the particle size distribution of example 1 and comparative examples 1 to 2 did not change much, but the effect of example 1 on the small particle size of the sodium-modified soil was most significant, and it was confirmed that trisodium phosphate had a synergistic effect on the sodium modification effect of sodium carbonate.
FIG. 5 shows XRD patterns of organically modified sodium bentonite according to examples 1-2, wherein (a) in example 1: 5% cetyltrimethylammonium bromide, (b) example 2: 5% octadecyl trimethyl ammonium bromide: as can be seen from FIG. 5, the diffraction peaks after organic modification all shifted to small angles, and the d001 value increased, indicating that the quaternary ammonium salt modifier (cetyl trimethyl ammonium bromide or stearyl trimethyl ammonium bromide) was inserted between the bentonite layers.
FIG. 6 is an FTIR analysis spectrum of organically modified sodium based fibers of examples 1-3 (a) example 1: 5% cetyltrimethylammonium bromide, (b) example 2: 5% octadecyl trimethyl ammonium bromide, (c) example 3: 8% octadecyl trimethyl ammonium bromide: as can be seen from FIG. 6, at 2936cm-1Occurrence of CH2Strong absorption peak of 2851cm-1CH appears3Peak of vibration of 1489cm-1Has C-N telescopic vibration absorption, and the bands are organic group (-CH) of quaternary ammonium salt modifier (cetyl trimethyl ammonium bromide or octadecyl trimethyl ammonium bromide)2、-CH3C-N) demonstrates the quaternary ammonium salt modifier (hexadecyl)Trimethyl ammonium bromide or octadecyl trimethyl ammonium bromide) has entered the structure of bentonite, and replaces exchangeable cations between layers of bentonite at 1095cm-1The asymmetric vibration peak of the silicate mineral Si-O-Si with the layered structure appears, the peak shape is obviously widened, and the fact that the quaternary ammonium salt modifier partially enters between layers of bentonite is proved to enlarge the layered structure, so that the infrared spectrum peak is widened.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (2)
1. A modification method of calcium bentonite is characterized in that after the calcium bentonite is purified by a wet method, under the synergistic effect of ultrasound and microwave, a sodium treatment agent consisting of trisodium phosphate and sodium carbonate is firstly used for carrying out sodium treatment modification, and then quaternary ammonium salt is used for carrying out organic modification; the method specifically comprises the following steps:
(1) multi-stage purification: crushing raw ore soil of calcium bentonite to 100 meshes, dispersing the crushed raw ore soil in deionized water to prepare slurry with the concentration of 10%, stirring for 2 hours, standing for 0.5 hour, removing coarse slag, repeatedly cleaning for 3 times, standing for settling overnight, taking out an upper suspension, filtering, naturally drying to obtain primary purified soil, and repeating the processes of dispersing, settling and purifying until the upper suspension is not turbid to obtain refined bentonite;
(2) sodium modification: preparing refined bentonite into slurry with the concentration of 10% by using deionized water, adding a sodium agent, controlling the using amount of the sodium agent to be 2.5-7.5% of the mass of the refined bentonite, uniformly stirring, reacting for 10-15 min at 70-90 ℃ under the synergistic effect of ultrasound and microwave, filtering, washing to be neutral by using dilute hydrochloric acid, drying at 80 ℃, and grinding to obtain sodium bentonite;
the sodium reagent comprises the following components in percentage by mass: 5-10% of trisodium phosphate and the balance of sodium carbonate;
(3) organic modification: dropwise adding 5-8% of quaternary ammonium salt water solution with the same mass into the obtained sodium bentonite, stirring until the sodium bentonite is fully swelled, reacting for 15-20 min at 70-90 ℃ under the synergistic effect of ultrasound and microwave, drying, and grinding to obtain modified bentonite;
in the step (2) and the step (3), the ultrasonic frequency is 35KHz, the power is 400W, and the microwave power is 500W.
2. The method for modifying calcium bentonite according to claim 1, wherein the quaternary ammonium salt aqueous solution comprises the following components in percentage by mass: 5-8% of hexadecyl trimethyl ammonium bromide or octadecyl trimethyl ammonium bromide, and the balance of water.
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Cited By (4)
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| CN112694094A (en) * | 2021-03-02 | 2021-04-23 | 辽宁石油化工大学 | Method for preparing sodium bentonite by using sodium fluoride through semidry method under assistance of microwaves |
| CN113321222A (en) * | 2021-05-27 | 2021-08-31 | 建平天正矿业有限公司 | Neutral sodium treatment and decoloration bleaching combined processing technology and application of low-whiteness calcium-based bentonite |
| CN113620305A (en) * | 2021-08-25 | 2021-11-09 | 苏州欧亦博工业科技有限公司 | Preparation process of sodium modified bentonite |
| CN113754388A (en) * | 2021-09-10 | 2021-12-07 | 中铁上海工程局集团市政环保工程有限公司 | Bentonite modified aluminate inorganic anti-corrosion mortar for pipe network restoration and preparation method thereof |
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| CN113620305A (en) * | 2021-08-25 | 2021-11-09 | 苏州欧亦博工业科技有限公司 | Preparation process of sodium modified bentonite |
| CN113754388A (en) * | 2021-09-10 | 2021-12-07 | 中铁上海工程局集团市政环保工程有限公司 | Bentonite modified aluminate inorganic anti-corrosion mortar for pipe network restoration and preparation method thereof |
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