CN112374506A - Modification process of composite bentonite additive intermediate material - Google Patents
Modification process of composite bentonite additive intermediate material Download PDFInfo
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- CN112374506A CN112374506A CN202011306321.6A CN202011306321A CN112374506A CN 112374506 A CN112374506 A CN 112374506A CN 202011306321 A CN202011306321 A CN 202011306321A CN 112374506 A CN112374506 A CN 112374506A
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- bentonite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B33/40—Clays
Abstract
The invention discloses a modification process of a composite bentonite additive intermediate material, which comprises the following steps: 1) preparing an organic acid solution; fully dissolving organic acid in deionized water to obtain an organic acid solution; 2) fully stirring and mixing the organic acid solution and the bentonite to obtain modified slurry; 3) drying, grinding and sieving the modified slurry to obtain powdery modified bentonite; 4) adding water into the modified bentonite, stirring for pulping, adjusting the pH value of the slurry to 7.0-7.5 in the stirring process, stirring overnight, and standing to separate out an upper suspension; 5) stirring the mixture with NaOH and Na2SO4The pH value of the suspension is adjusted to 8-10 by the mixed liquid, the suspension is slowly and continuously stirred, and the pH value is adjusted to 7-8, so that sodium bentonite suspension is obtained; 6) and centrifuging the sodium bentonite suspension, drying, crushing and sieving to obtain a finished product. The invention uses oxalic acid, citric acid or gluconic acid to acidify the bentonite, and has the characteristics of no toxicity and harmlessness and environmental friendliness.
Description
Technical Field
The invention relates to the field of bentonite, and in particular relates to a modification process of a composite bentonite additive intermediate material.
Background
The bentonite has montmorillonite as main component, high expansibility, adsorptivity, thixotropy, dispersity, cation exchange property and other performance, and is widely applied to various industrial fields. Typical bentonites include calcium bentonite and sodium bentonite due to the world's calcium bentonite classificationThe cloth is far wider than sodium bentonite, so calcium bentonite is the most widely used bentonite. Compared with calcium bentonite, the sodium bentonite has large swelling capacity and high cation exchange amount because interlayer ions of the sodium bentonite 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.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a modification process of a composite bentonite additive intermediate material, so as to solve the problem of common modification effect in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a modification process of a composite bentonite additive intermediate material comprises the following steps: 1) preparing an organic acid solution; fully dissolving organic acid in deionized water to obtain an organic acid solution; 2) fully stirring and mixing the organic acid solution and the bentonite to obtain modified slurry; 3) drying, grinding and sieving the modified slurry to obtain powdery modified bentonite; 4) adding water into the modified bentonite, stirring for pulping, adjusting the pH value of the slurry to 7.0-7.5 in the stirring process, stirring overnight, and standing to separate out an upper suspension; 5) stirring the mixture with NaOH and Na2SO4The pH value of the suspension is adjusted to 8-10 by the mixed liquid, the suspension is slowly and continuously stirred, and the pH value is adjusted to 7-8, so that sodium bentonite suspension is obtained; 6) and centrifuging the sodium bentonite suspension, drying, crushing and sieving to obtain a finished product.
Further, the organic acid in the step 1) is selected from oxalic acid, citric acid or gluconic acid; the concentration of the organic acid solution is 0.4 g/L-0.7 g/L.
Further, in the step 2), the dry weight ratio of the organic acid solution to the bentonite is 5-10%, the stirring temperature is room temperature, and the stirring time is 5-7 hours.
Further, in the step 3), the drying temperature is 60-70 ℃, the moisture content after drying treatment is less than 5%, and the modified bentonite is prepared by grinding the bentonite and then sieving the ground bentonite through a 100-200-mesh standard sieve.
Further, the proportion of the modified bentonite and the water in the step 4) is 1: 15-20 parts of; the pH of the slurry is adjusted during agitation by a combination of one or more of the sodium or potassium salts of oxalic acid, citric acid, gluconic acid.
Further, the first stirring time in the step 5) is 6-10 hours; the second stirring time is 7-8 hours; after continuous stirring, the pH value is adjusted by oxalic acid, citric acid or gluconic acid.
Further, the drying temperature in the step 6) is 60-70 ℃.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, firstly, bentonite is acidified to obtain modified bentonite, and sodium bentonite is prepared from the acidified bentonite, wherein the acidified bentonite can regulate and control the impact of strong alkaline solution on the pH value of the bentonite in the sodium modification process, and meanwhile, bentonite mineral dissolution is not caused, so that the pollutant interception capability of the barrier in the environment of strong alkaline solution can be greatly improved, the time for the strong alkaline solution to puncture the barrier is prolonged, the sodium modification process condition is milder, and the sodium modification efficiency and quality are improved; the invention uses oxalic acid, citric acid or gluconic acid to acidify the bentonite, and has the characteristics of no toxicity and harmlessness and environmental friendliness.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention, and all techniques and materials that can be made based on the above teachings of the invention are within the scope of the invention.
A modification process of a composite bentonite additive intermediate material comprises the following steps:
1) preparing an organic acid solution; the organic acid is selected from oxalic acid, citric acid or gluconic acid; fully dissolving organic acid in deionized water to obtain an organic acid solution with the concentration of 0.4-0.7 g/L;
2) and fully stirring and mixing the organic acid solution and the bentonite to obtain modified slurry, wherein the dry weight ratio of the organic acid solution to the bentonite is 5-10%, the stirring temperature is room temperature, and the stirring time is 5-7 hours.
3) Drying and grinding the modified slurry to obtain powdery modified bentonite; and (3) drying the modified slurry in an oven at the temperature of 60-70 ℃ until the moisture content is less than 5%, grinding the slurry, and screening the ground slurry through a 100-200-mesh standard sieve to obtain the modified bentonite.
4) Adding water into the modified bentonite, stirring and pulping, wherein the ratio of the modified bentonite to the water is 1: 15-20, adjusting the pH value of the slurry to 7.0-7.5 in the stirring process, then continuing stirring overnight, standing for one day, and separating out an upper suspension; the pH value of the slurry is adjusted by an alkaline agent selected from one or more of sodium salt or potassium salt of oxalic acid, citric acid and gluconic acid;
5) stirring with NaOH and Na2SO4The pH value of the suspension is adjusted to 8-10 by the mixed liquid, and the suspension is slowly and continuously stirred for 6-10 hours; then, regulating the pH value to 7-8 by using oxalic acid, citric acid or gluconic acid, keeping the state of weak base, and continuously stirring for 7-8 hours; sodium treatment of the modified bentonite is completed;
6) centrifuging, drying, crushing and sieving the suspension after sodium modification to obtain a finished product; the drying temperature is 60-70 ℃.
Example 1
1) Fully dissolving citric acid in deionized water to obtain a citric acid solution with the concentration of 0.5 g/L;
2) and fully stirring and mixing the citric acid solution and the bentonite to obtain modified slurry, wherein the dry weight ratio of the citric acid solution to the bentonite is 10%, the stirring temperature is room temperature, and the stirring time is 6 hours.
3) Drying and grinding the modified slurry to obtain powdery modified bentonite, drying at the temperature of 60-70 ℃ until the moisture content is less than 5%, and sieving the ground modified bentonite through a 100-200-mesh standard sieve;
4) adding water into the modified bentonite, stirring and pulping, wherein the ratio of the modified bentonite to the water is 1: 17, adjusting the pH value of the slurry to 7.0-7.5 by sodium citrate in the stirring process, then continuously stirring overnight, standing for one day, and separating out an upper suspension;
5) stirring with NaOH and Na2SO4The pH value of the suspension is adjusted to 8-10 by the mixed liquid, and the suspension is slowly and continuously stirred for 10 hours; then, regulating the pH value to 7-8 by using citric acid, keeping the state of weak base, and continuously stirring for 7-8 hours; sodium treatment of the modified bentonite is completed;
6) centrifuging, drying, crushing and sieving the suspension after sodium modification to obtain a finished product; the drying temperature was 70 ℃.
Example 2
1) Fully dissolving oxalic acid in deionized water to obtain an oxalic acid solution with the concentration of 0.7 g/L;
2) fully stirring and mixing the oxalic acid solution and the bentonite to obtain modified slurry, wherein the dry weight ratio of the oxalic acid solution to the bentonite is 5%, the stirring temperature is room temperature, and the stirring time is 7 hours.
3) Drying and grinding the modified slurry to obtain powdery modified bentonite, drying at the temperature of 60-70 ℃ until the moisture content is less than 5%, and sieving the ground modified bentonite through a 100-200-mesh standard sieve;
4) adding water into the modified bentonite, stirring and pulping, wherein the ratio of the modified bentonite to the water is 1: 15, adjusting the pH value of the slurry to 7.0-7.5 by potassium oxalate in the stirring process, then continuously stirring overnight, standing for one day, and separating out an upper suspension;
5) stirring with NaOH and Na2SO4The pH value of the suspension is adjusted to 8-10 by the mixed liquid, and the suspension is slowly and continuously stirred for 6 hours; then, regulating the pH value to 7-8 by using oxalic acid, keeping the weak base state, and continuously stirring for 7-8 hours; sodium treatment of the modified bentonite is completed;
6) centrifuging, drying, crushing and sieving the suspension after sodium modification to obtain a finished product; the drying temperature was 65 ℃.
Example 3
1) Fully dissolving gluconic acid in deionized water to obtain a gluconic acid solution with the concentration of 0.4 g/L;
2) and fully stirring and mixing the gluconic acid solution and the bentonite to obtain modified slurry, wherein the dry weight ratio of the gluconic acid to the bentonite is 7%, the stirring temperature is room temperature, and the stirring time is 5 hours.
3) Drying and grinding the modified slurry to obtain powdery modified bentonite, drying at the temperature of 60-70 ℃ until the moisture content is less than 5%, and sieving the ground modified bentonite through a 100-200-mesh standard sieve;
4) adding water into the modified bentonite, stirring and pulping, wherein the ratio of the modified bentonite to the water is 1: 20, adjusting the pH value of the slurry to 7.0-7.5 by sodium gluconate in the stirring process, then continuously stirring overnight, standing for one day, and separating out an upper suspension;
5) stirring with NaOH and Na2SO4The pH value of the suspension is adjusted to 8-10 by the mixed liquid, and the suspension is slowly and continuously stirred for 8 hours; then regulating the pH value to 7-8 by using gluconic acid, keeping the weak base state, and continuously stirring for 7-8 hours; sodium treatment of the modified bentonite is completed;
6) centrifuging, drying, crushing and sieving the suspension after sodium modification to obtain a finished product; the drying temperature was 60 ℃.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
Claims (7)
1. A modification process of a composite bentonite additive intermediate material is characterized by comprising the following steps: 1) preparing an organic acid solution; fully dissolving organic acid in deionized water to obtain an organic acid solution; 2) fully stirring and mixing the organic acid solution and the bentonite to obtain modified slurry; 3) drying, grinding and sieving the modified slurry to obtain powdery modified bentonite; 4) adding water into the modified bentonite, stirring for pulping, adjusting the pH value of the slurry to 7.0-7.5 in the stirring process, stirring overnight, standing, and separatingAn upper suspension; 5) stirring the mixture with NaOH and Na2SO4The pH value of the suspension is adjusted to 8-10 by the mixed liquid, the suspension is slowly and continuously stirred, and the pH value is adjusted to 7-8, so that sodium bentonite suspension is obtained; 6) and centrifuging the sodium bentonite suspension, drying, crushing and sieving to obtain a finished product.
2. The process for modifying the intermediate material of the composite bentonite additive according to claim 1, wherein the organic acid in the step 1) is selected from oxalic acid, citric acid or gluconic acid; the concentration of the organic acid solution is 0.4 g/L-0.7 g/L.
3. The process for modifying the intermediate material of the composite bentonite additive according to claim 1, wherein the dry weight ratio of the organic acid solution to the bentonite in the step 2) is 5-10%, the stirring temperature is room temperature, and the stirring time is 5-7 hours.
4. The process for modifying the intermediate material of the composite bentonite additive according to claim 1, wherein the drying temperature in the step 3) is 60-70 ℃, the moisture content after drying treatment is less than 5%, and the modified bentonite is prepared by grinding the intermediate material and sieving the ground intermediate material through a standard sieve of 100-200 meshes.
5. The process for modifying the intermediate material of the composite bentonite additive according to claim 1, wherein the ratio of the modified bentonite to the water in the step 4) is 1: 15-20 parts of; the pH of the slurry is adjusted during agitation by a combination of one or more of the sodium or potassium salts of oxalic acid, citric acid, gluconic acid.
6. The process for modifying the intermediate material of the composite bentonite additive according to claim 1, wherein the first stirring time in the step 5) is 6-10 hours; the second stirring time is 7-8 hours; after continuous stirring, the pH value is adjusted by oxalic acid, citric acid or gluconic acid.
7. The process for modifying the intermediate material of the composite bentonite additive according to claim 1, wherein the drying temperature in the step 6) is 60-70 ℃.
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| WO2012174678A1 (en) * | 2011-06-23 | 2012-12-27 | 山东大展纳米材料有限公司 | Layered clay catalytic material and intercalation method thereof |
| CN110182819A (en) * | 2019-05-08 | 2019-08-30 | 东南大学 | A kind of modified alta-mud and its method of modifying and application |
| CN110980754A (en) * | 2019-12-31 | 2020-04-10 | 湖北三鼎科技有限公司 | Preparation method of natural sodium bentonite |
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| WO2008045077A1 (en) * | 2006-10-12 | 2008-04-17 | Kivanc Isik | Expanded nanoclays and method of producing such expanded nanoclays |
| CN102259881A (en) * | 2011-06-20 | 2011-11-30 | 浙江丰虹新材料股份有限公司 | Method for preparing high-viscosity organic bentonite by virtue of calcium-based bentonite |
| WO2012174678A1 (en) * | 2011-06-23 | 2012-12-27 | 山东大展纳米材料有限公司 | Layered clay catalytic material and intercalation method thereof |
| CN110182819A (en) * | 2019-05-08 | 2019-08-30 | 东南大学 | A kind of modified alta-mud and its method of modifying and application |
| CN110980754A (en) * | 2019-12-31 | 2020-04-10 | 湖北三鼎科技有限公司 | Preparation method of natural sodium bentonite |
| CN111573685A (en) * | 2020-06-03 | 2020-08-25 | 湖南师范大学 | Method for preparing organobentonite from calcium-based bentonite raw soil in efficient and environment-friendly manner |
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