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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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910000278 bentonite Inorganic materials 0.000 title claims abstract description 39
- 239000000440 bentonite Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000004048 modification Effects 0.000 title claims abstract description 21
- 238000012986 modification Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 title claims abstract description 17
- 239000000654 additive Substances 0.000 title claims abstract description 14
- 230000000996 additive effect Effects 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 57
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 48
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229940092782 bentonite Drugs 0.000 claims abstract description 38
- 239000000725 suspension Substances 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 28
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims abstract description 27
- 239000002002 slurry Substances 0.000 claims abstract description 27
- 150000007524 organic acids Chemical class 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000015165 citric acid Nutrition 0.000 claims abstract description 16
- 239000000174 gluconic acid Substances 0.000 claims abstract description 16
- 235000012208 gluconic acid Nutrition 0.000 claims abstract description 16
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 16
- 238000007873 sieving Methods 0.000 claims abstract description 15
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000280 sodium bentonite Inorganic materials 0.000 claims abstract description 11
- 229940080314 sodium bentonite Drugs 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000007832 Na2SO4 Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000004537 pulping Methods 0.000 claims abstract description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 15
- 239000011734 sodium Substances 0.000 claims description 15
- 229910052708 sodium Inorganic materials 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 2
- 159000000001 potassium salts Chemical class 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 231100000956 nontoxicity Toxicity 0.000 abstract description 2
- 235000012216 bentonite Nutrition 0.000 description 27
- 239000000243 solution Substances 0.000 description 18
- 229910000281 calcium bentonite Inorganic materials 0.000 description 7
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 3
- 238000005341 cation exchange Methods 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paper (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
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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WO2008045077A1 (en) * | 2006-10-12 | 2008-04-17 | Kivanc Isik | Expanded nanoclays and method of producing such expanded nanoclays |
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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 |
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2020
- 2020-11-19 CN CN202011306321.6A patent/CN112374506A/en active Pending
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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 |
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Title |
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