CN111762793A - Purification modification process of attapulgite clay - Google Patents
Purification modification process of attapulgite clay Download PDFInfo
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Abstract
The invention discloses an attapulgite clay purification modification process, which relates to the technical field of attapulgite clay purification and comprises the following steps: step 1: pre-treating the taken materials; step 2: primary high-temperature gradient roasting activation treatment; and step 3: pulping, grinding and selecting and primary acidizing; and 4, step 4: secondary high-temperature gradient calcining and activating treatment; and 5: secondary acidification treatment: step 6: and (4) surface active treatment. Compared with the prior art, the purification and modification process is more practical and efficient, and particularly aims at attapulgite clay in the city of local Ming Dynasty, and multiple modification methods are used together, so that the purity and the adsorption performance of the treated attapulgite clay are greatly improved, and the attapulgite clay is particularly applied to the field of adsorbents.
Description
Technical Field
The invention relates to the technical field of purification of attapulgite clay, and in particular relates to a process for purifying and modifying attapulgite clay.
Background
Attapulgite clay (ATP for short) is a clay mineral mainly composed of attapulgite, and belongs to the sepiolite family in mineralogy. The attapulgite rod crystal is a natural one-dimensional inorganic nano material, and has wide raw material source and low preparation cost. Because the inside of the single crystal is of a pore channel structure, a plurality of parallel tunnel gaps are naturally formed among the nano single crystal fibers which are arranged in parallel, the volume of the gaps in the micron-level attapulgite accounts for more than 30 percent of the total volume of particles, and the inside of the micron-level attapulgite has a huge specific area, so that the attapulgite is widely used as an adsorbent, a catalyst and a carrier, a drilling mud thickener, an adhesive, a feed additive and the like. The attapulgite has a layer chain structure, high specific surface area and strong adsorbability and decolorization capacity, and can be used for preparing an adsorbent, purifying water and treating sewage. However, the attapulgite clay raw material has a large amount of impurities in the component structure, is easy to agglomerate, and has limited original adsorption performance, so the raw material needs to be purified and modified.
At present, the attapulgite obtained by mining and processing the mountain attapulgite clay ore in Yangtze town of Mingguang city is generally not very high in purity, the performances and the quality of the attapulgite are uniform, and the cooperation of local enterprises aims to improve the problems so as to promote the development and the export of local attapulgite products.
Disclosure of Invention
In order to solve the problems, the invention provides a brand-new attapulgite clay purification and modification process which is more practical and efficient than the prior purification and modification method, and particularly aims at attapulgite clay in the city of local Minggui, and a plurality of modification methods are used together, so that the purity and the adsorption property of the treated attapulgite clay are greatly improved, and the attapulgite clay is particularly applied to the field of adsorbents.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the attapulgite clay purification and modification process roughly comprises material taking pretreatment, high-temperature activation treatment, acidification treatment and surface activity treatment, and specifically comprises the following steps:
step 1: pre-treating the taken materials;
step 2: first-stage high-temperature roasting activation treatment
Carrying out gradient roasting treatment on the attapulgite obtained in the step 1 at the temperature of 120 +/-5 ℃, 150 +/-5 ℃, 180 +/-5 ℃, 210 +/-5 ℃ and 240 +/-5 ℃ for 25min, 30min, 40min, 50min and 60min respectively, and carrying out furnace air cooling after roasting;
and step 3: pulping grinding and selecting and primary acidizing treatment
Adding water into the attapulgite obtained in the step 2 to prepare slurry with the concentration of 32.5-36.5 wt%, adding a nitric acid solution with the concentration of 2.5-3.5 mol/L, mixing, wherein the mass ratio of the attapulgite to the nitric acid solution is 1:1.25, fully shearing and stirring, oscillating for 25min under the ultrasonic condition, the ultrasonic oscillation frequency is 40-50 Hz, then sieving by a 12.5-mesh sieve, standing for 6-8h, washing by clear water until the pH value is 6-7, removing upper turbid liquid after settling, drying the attapulgite slurry until the concentration is 6-8 wt%, adding a proper amount of activating component, fully mixing uniformly, and ball-milling to 50-60 meshes for later use;
and 4, step 4: two-stage high-temperature calcination activation treatment
Carrying out gradient calcination treatment on the attapulgite obtained in the step 3 at the temperature of 180 +/-10 ℃, 230 +/-10 ℃, 280 +/-10 ℃, 330 +/-10 ℃ and 380 +/-10 ℃ for 30min, 50min and 50min respectively, and carrying out furnace air cooling after calcination is finished;
and 5: secondary acidification treatment
Adding the attapulgite obtained in the step (4) into a phosphoric acid solution of 4-5 mol/L, fully stirring at the temperature of 45-55 ℃, performing ultrasonic oscillation for 25min in cooperation with the ultrasonic oscillation, wherein the ultrasonic oscillation frequency is 40-50 Hz, washing with water to be neutral after the ultrasonic oscillation is finished, filtering, drying, and performing ball milling to 200 meshes, wherein the mass ratio of the attapulgite to the phosphoric acid solution is 1: 1.5;
step 6: surface active treatment
Placing the attapulgite obtained in the step (5) and the surface modifier in an organic solvent, fully and uniformly mixing to prepare a mixed solution, carrying out ultrasonic oscillation for 30min at the temperature of 80-90 ℃, wherein the ultrasonic oscillation frequency is 40-50 Hz, then standing for at least 12h, and finally filtering, washing and drying;
wherein the surface modifier is any one of dodecyl dimethyl benzyl ammonium chloride, dodecyl trimethyl ammonium chloride or octadecyl trimethyl ammonium chloride.
Further, in the step 1, the pretreatment comprises airing, rolling, crushing, magnetic separation, screening and grinding the attapulgite clay.
Further, in the step 3, the amount of the activating component is 2.0-3.5% of the mass of the attapulgite.
Preferably, in step 3, the activating component is ZnO, MnO, TiO2、Al2O3And MgO.
Further, in the step 6, the mass ratio of the attapulgite, the surface modifier and the organic solvent is 1 (0.12-0.20) to (4-6).
Preferably, in step 6, the organic solvent is toluene or 1, 2-propanediol.
The attapulgite clay purification modification process at least comprises the following beneficial effects and advantages:
the invention discovers the working procedures of purifying and modifying the attapulgite crude product according to the following steps by researching and improving the invention: the whole process consisting of material taking pretreatment → high-temperature roasting activation treatment → pulping and grinding plus primary acidification treatment → secondary high-temperature calcining activation treatment → secondary acidification treatment → surface activation treatment can better improve the purification and performance quality of the attapulgite clay; wherein the whiteness range of the obtained attapulgite competitive product is [ 86.12%, 88.40%]The purity can reach more than 99.6 percent, and the specific surface area interval is [374.3 m%2/g，386.7m2/g]The method is suitable for large-scale mass production of enterprises;
the attapulgite product obtained by the purification and modification process has strong adsorption capacity and is suitable for further processing into products such as adsorbent, desiccant, decolorant, washing assistant, binder, molecular sieve and the like;
particularly, in the improved purification and modification process, the material taking pretreatment can screen out large-particle impurities and refine attapulgite; the first-stage high-temperature roasting activation treatment and the second-stage high-temperature roasting activation treatment are alternately operated, and the roasting temperature and time are reasonably controlled in the process, and the adsorption water, the crystal water and the structural water in an octahedron in the attapulgite can be just, mildly and effectively removed by adopting a gradient high-temperature activation treatment mode, the interior of a crystal lattice and a pore structure are changed, an active center is increased, the fibrous and needle-rod-shaped groups mixed on the surface of the attapulgite become loose and porous, the pore volume and the specific surface area are increased, and the laying and laying foundation is laid for the subsequent acid washing and surface modification; in the acid leaching process, different acid solutions and acidity thereof have different influences on the structural performance of the attapulgite, the pulping milling, primary acidification treatment and secondary acidification treatment in the invention can effectively dissolve part of the octahedral structure, better dredge impurities in a loose pore channel, further increase the pore channel volume and the specific surface area of pores, reasonably control the ultrasonic intensity and time in the grinding and acid leaching processes, and utilize the cavitation of ultrasonic waves and shock waves and micro-jets formed in the solution to enable molecules to generate strong mutual collision and aggregation phenomena, the phenomena can play a good energy generating impact role on a liquid-solid phase system, and the strong shearing effect of collision can quickly disperse the mixed fibrous and needle-rod-shaped groups on the surface of the attapulgite uniformly; the process of the invention finally reasonably selects the surfactant and the dosage, well removes inorganic cations among attapulgite, enlarges the interlayer spacing, replaces organic matters to be condensed with the hydroxyl on the surface of the attapulgite, thereby chemically grafting/adsorbing organic groups on the surface of the attapulgite, thus strengthening the affinity with high polymers and enhancing the adsorption performance.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is an electron microscope (SEM) image of a dental attapulgite clay scanned after treatment in step 1 according to an embodiment;
FIG. 1 shows that the fibrous and needle-stick-shaped clusters on the surface of the attapulgite are disordered and the structural groups are densely stacked, and the pores, the pore canals and the specific surface area in the attapulgite are small;
FIG. 2 is an electron microscope (SEM) image obtained by scanning the attapulgite clay treated in step 5 in example 2 according to the specific embodiment; in fig. 2, it is shown that the surface of the attapulgite is loose and porous from the original mixed aggregation group, the fiber and needle-bar structure is greatly reduced, the flake-block structure is aggregated, and the internal pores, pore channels and specific surface area of the attapulgite are obviously increased.
Detailed Description
The following examples are provided to more clearly illustrate the technical solutions of the present invention, and should not be construed as limiting the scope of the present invention.
Example 1
Step 1: pretreatment of the feed stock
Taking Jianxi Zhenyuan mountain attapulgite clay (hereinafter referred to as attapulgite), spreading the Jianxi Zhenyuan mountain attapulgite clay on a field, airing for at least 3 days (in rainy and snowy days), and grinding, crushing, magnetically separating, screening (vibrating screening) and grinding (ball milling) the attapulgite clay naturally dried to a certain degree to a particle size of less than 1mm for later use.
Step 2: first-stage high-temperature roasting activation treatment
Placing the attapulgite obtained in the step 1 in a muffle furnace, performing gradient roasting treatment for 25min, 30min, 40min, 50min and 60min respectively at the temperature of 120 +/-5 ℃, 150 +/-5 ℃, 180 +/-5 ℃, 210 +/-5 ℃ and 240 +/-5 ℃, and performing air cooling along with the furnace after roasting is finished;
and step 3: pulping grinding and selecting and primary acidizing treatment
Adding water into the attapulgite obtained in the step 2 to prepare slurry with the concentration of 32.5 wt%, adding a nitric acid solution with the concentration of 2.5mol/L, mixing, wherein the mass ratio of the attapulgite to the nitric acid solution is 1:1.25, fully shearing and stirring, oscillating for 25min under the ultrasonic condition, the ultrasonic oscillation frequency is 40Hz, then sieving by a 12.5-mesh sieve, standing for 6h, washing by clear water until the pH value is 6-7, after settling, pumping out upper-layer turbid liquid, drying the attapulgite slurry until the concentration is 6 wt%, adding a proper amount of activating component, further fully mixing uniformly and ball-milling to 50-60 meshes for later use;
based on the above, the amount of the activating component is 2.0% of the mass of the attapulgite; and the activating component is preferably MnO;
and 4, step 4: two-stage high-temperature calcination activation treatment
Placing the attapulgite obtained in the step 3 in a muffle furnace, respectively carrying out gradient calcination treatment for 30min, 50min and 50min at the temperature of 180 +/-10 ℃, 230 +/-10 ℃, 280 +/-10 ℃, 330 +/-10 ℃ and 380 +/-10 ℃, and carrying out air cooling along with the furnace after calcination is finished;
and 5: secondary acidification treatment
Adding the attapulgite obtained in the step (4) into a 4mol/L phosphoric acid solution, fully stirring at the temperature of 47 +/-2 ℃, performing ultrasonic oscillation for 25min in cooperation with the ultrasonic oscillation, wherein the ultrasonic oscillation frequency is 40Hz, washing with water to be neutral after the ultrasonic oscillation is finished, filtering, drying, and performing ball milling to 200 meshes, wherein the mass ratio of the attapulgite to the phosphoric acid solution is 1: 1.5;
step 6: surface active treatment
Putting the attapulgite obtained in the step (5) and the surface modifier into an organic solvent, fully and uniformly mixing to prepare a mixed solution, fully stirring at the temperature of 82 +/-2 ℃, performing ultrasonic oscillation for 30min (the ultrasonic oscillation frequency is 40Hz), standing for 12h, and finally filtering, washing and drying;
wherein the mass ratio of the attapulgite to the surface modifier to the organic solvent is 1:0.12: 4;
the surface modifier is preferably dodecyl dimethyl benzyl ammonium chloride;
the organic solvent is preferably toluene;
the attapulgite obtained by the purification and modification of the example has the whiteness of 87.05 percent, the purity of more than 99.73 percent and the specific surface area of 376.1m2/g。
Example 2
Step 1: pretreatment of the feed stock
Taking Jianxi Zhenyuan mountain attapulgite clay (hereinafter referred to as attapulgite), spreading the Jianxi Zhenyuan mountain attapulgite clay on a field, airing for at least 3 days (in rainy and snowy days), and grinding, crushing, magnetically separating, screening (vibrating screening) and grinding (ball milling) the attapulgite clay naturally dried to a certain degree to a particle size of less than 1mm for later use.
Step 2: first-stage high-temperature roasting activation treatment
Placing the attapulgite obtained in the step 1 in a muffle furnace, performing gradient roasting treatment for 25min, 30min, 40min, 50min and 60min respectively at the temperature of 120 +/-5 ℃, 150 +/-5 ℃, 180 +/-5 ℃, 210 +/-5 ℃ and 240 +/-5 ℃, and performing air cooling along with the furnace after roasting is finished;
and step 3: pulping grinding and selecting and primary acidizing treatment
Adding water into the attapulgite obtained in the step 2 to prepare slurry with the concentration of 34.5 wt%, adding a nitric acid solution with the concentration of 3.0mol/L, mixing, wherein the mass ratio of the attapulgite to the nitric acid solution is 1:1.25, fully shearing and stirring, oscillating for 25min under the ultrasonic condition, the ultrasonic oscillation frequency is 40Hz, then sieving by a 12.5-mesh sieve, standing for 7h, washing by clear water until the pH value is 6-7, after settling, pumping out upper-layer turbid liquid, drying the attapulgite slurry until the concentration is 7 wt%, adding a proper amount of activating component, further fully mixing uniformly and ball-milling to 50-60 meshes for later use;
based on the above, the amount of the activating component is 2.5% of the mass of the attapulgite; and the activating component is preferably Al2O3The MgO composition comprises 1:1 of MgO by mass;
and 4, step 4: two-stage high-temperature calcination activation treatment
Placing the attapulgite obtained in the step 3 in a muffle furnace, respectively carrying out gradient calcination treatment for 30min, 50min and 50min at the temperature of 180 +/-10 ℃, 230 +/-10 ℃, 280 +/-10 ℃, 330 +/-10 ℃ and 380 +/-10 ℃, and carrying out air cooling along with the furnace after calcination is finished;
and 5: secondary acidification treatment
Adding the attapulgite obtained in the step (4) into a 4.5mol/L phosphoric acid solution, fully stirring at the temperature of 50 +/-2 ℃ and performing ultrasonic oscillation for 25min in cooperation, wherein the ultrasonic oscillation frequency is 40Hz, washing with water to be neutral after the ultrasonic oscillation is finished, filtering, drying and performing ball milling to 200 meshes, wherein the mass ratio of the attapulgite to the phosphoric acid solution is 1: 1.5;
step 6: surface active treatment
Putting the attapulgite obtained in the step (5) and the surface modifier into an organic solvent, fully and uniformly mixing to prepare a mixed solution, fully stirring at the temperature of 85 +/-2 ℃, performing ultrasonic oscillation for 30min (the ultrasonic oscillation frequency is 40Hz), standing for 12h, and finally filtering, washing and drying;
wherein the mass ratio of the attapulgite to the surface modifier to the organic solvent is 1:0.15: 5;
the surface modifier is preferably dodecyl trimethyl ammonium chloride;
the organic solvent is preferably 1, 2-propanediol;
the attapulgite obtained by the purification and modification of the embodiment has the whiteness of 88.24 percent, the purity of more than 99.87 percent and the specific surface area of 384.0m2/g。
Example 3
Step 1: pretreatment of the feed stock
Taking Jianxi Zhenyuan mountain attapulgite clay (hereinafter referred to as attapulgite), spreading the Jianxi Zhenyuan mountain attapulgite clay on a field, airing for at least 3 days (in rainy and snowy days), and grinding, crushing, magnetically separating, screening (vibrating screening) and grinding (ball milling) the attapulgite clay naturally dried to a certain degree to a particle size of less than 1mm for later use.
Step 2: first-stage high-temperature roasting activation treatment
Placing the attapulgite obtained in the step 1 in a muffle furnace, performing gradient roasting treatment for 25min, 30min, 40min, 50min and 60min respectively at the temperature of 120 +/-5 ℃, 150 +/-5 ℃, 180 +/-5 ℃, 210 +/-5 ℃ and 240 +/-5 ℃, and performing air cooling along with the furnace after roasting is finished;
and step 3: pulping grinding and selecting and primary acidizing treatment
Adding water into the attapulgite obtained in the step 2 to prepare slurry with the concentration of 36.5 wt%, adding a nitric acid solution with the concentration of 3.5mol/L, mixing, wherein the mass ratio of the attapulgite to the nitric acid solution is 1:1.25, fully shearing and stirring, oscillating for 25min under the ultrasonic condition, the ultrasonic oscillation frequency is 50Hz, then sieving by a 12.5-mesh sieve, standing for 8h, washing by clear water until the pH value is 6-7, after settling, pumping out upper-layer turbid liquid, drying the attapulgite slurry until the concentration is 8 wt%, adding a proper amount of activating component, further fully mixing uniformly and ball-milling to 50-60 meshes for later use;
based on the above, the amount of the activating component is 3.5% of the mass of the attapulgite; and the activating component is preferably TiO2。
And 4, step 4: two-stage high-temperature calcination activation treatment
Placing the attapulgite obtained in the step 3 in a muffle furnace, respectively carrying out gradient calcination treatment for 30min, 50min and 50min at the temperature of 180 +/-10 ℃, 230 +/-10 ℃, 280 +/-10 ℃, 330 +/-10 ℃ and 380 +/-10 ℃, and carrying out air cooling along with the furnace after calcination is finished;
and 5: secondary acidification treatment
Adding the attapulgite obtained in the step (4) into a 5mol/L phosphoric acid solution, fully stirring at the temperature of 53 +/-2 ℃, performing ultrasonic oscillation for 25min in cooperation with the ultrasonic oscillation, wherein the ultrasonic oscillation frequency is 50Hz, washing with water to be neutral after the ultrasonic oscillation is finished, filtering, drying, and performing ball milling to 200 meshes, wherein the mass ratio of the attapulgite to the phosphoric acid solution is 1: 1.5;
step 6: surface active treatment
Putting the attapulgite obtained in the step (5) and the surface modifier into an organic solvent, fully and uniformly mixing to prepare a mixed solution, fully stirring at the temperature of 88 +/-2 ℃, performing ultrasonic oscillation for 30min (the ultrasonic oscillation frequency is 50Hz), standing for 12h, and finally filtering, washing and drying;
wherein the mass ratio of the attapulgite to the surface modifier to the organic solvent is 1:0.2: 6;
the surface modifier is preferably octadecyl trimethyl ammonium chloride;
the organic solvent was the same as in example 2;
the attapulgite obtained by the purification and modification of the embodiment has the whiteness of 86.96 percent, the purity of more than 99.68 percent and the specific surface area of 374.5m2/g。
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A process for purifying and modifying attapulgite clay comprises pretreating attapulgite clay, activating at high temperature, acidifying, and performing surface activity treatment; the method is characterized by comprising the following steps:
step 1: taking materials for pretreatment to obtain attapulgite;
step 2: first-stage high-temperature roasting activation treatment
Carrying out gradient roasting treatment on the attapulgite obtained in the step 1 at the temperature of 120 +/-5 ℃, 150 +/-5 ℃, 180 +/-5 ℃, 210 +/-5 ℃ and 240 +/-5 ℃ for 25min, 30min, 40min, 50min and 60min respectively, and carrying out furnace air cooling after roasting;
and step 3: pulping grinding and selecting and primary acidizing treatment
Adding water into the attapulgite obtained in the step 2 to prepare slurry with the concentration of 32.5-36.5 wt%, adding a nitric acid solution with the concentration of 2.5-3.5 mol/L, mixing, wherein the mass ratio of the attapulgite to the nitric acid solution is 1:1.25, fully shearing and stirring, oscillating for 25min under the ultrasonic condition, the ultrasonic oscillation frequency is 40-50 Hz, then sieving by a 12.5-mesh sieve, standing for 6-8h, washing by clear water until the pH value is 6-7, removing upper turbid liquid after settling, drying the attapulgite slurry until the concentration is 6-8 wt%, adding a proper amount of activating component, fully mixing uniformly, and ball-milling to 50-60 meshes for later use;
and 4, step 4: two-stage high-temperature calcination activation treatment
Carrying out gradient calcination treatment on the attapulgite obtained in the step 3 at the temperature of 180 +/-10 ℃, 230 +/-10 ℃, 280 +/-10 ℃, 330 +/-10 ℃ and 380 +/-10 ℃ for 30min, 50min and 50min respectively, and carrying out furnace air cooling after calcination is finished;
and 5: secondary acidification treatment
Adding the attapulgite obtained in the step (4) into a phosphoric acid solution of 4-5 mol/L, fully stirring at the temperature of 45-55 ℃ and performing ultrasonic oscillation for 25min in cooperation, wherein the ultrasonic oscillation frequency is 40-50 Hz, washing with water to be neutral after the ultrasonic oscillation is finished, filtering, drying, and performing ball milling to 200 meshes, wherein the mass ratio of the attapulgite to the phosphoric acid solution is 1: 1.5;
step 6: surface active treatment
Placing the attapulgite obtained in the step (5) and the surface modifier in an organic solvent, fully and uniformly mixing to prepare a mixed solution, carrying out ultrasonic oscillation for 30min at the temperature of 80-90 ℃, wherein the ultrasonic oscillation frequency is 40-50 Hz, then standing for at least 12h, and finally filtering, washing and drying;
the surface modifier is any one of dodecyl dimethyl benzyl ammonium chloride, dodecyl trimethyl ammonium chloride or octadecyl trimethyl ammonium chloride.
2. The attapulgite clay purification and modification process of claim 1, wherein the pretreatment comprises air drying, rolling, crushing, magnetic separation, sieving and grinding the attapulgite clay in step 1.
3. The attapulgite clay purification and modification process of claim 1, wherein in the step 3, the amount of the activating component is 2.0-3.5% of the mass of the attapulgite clay.
4. The process for purifying and modifying attapulgite clay according to claim 1, wherein in step 3, the activating components are ZnO, MnO and TiO2、Al2O3And MgO.
5. The attapulgite clay purification and modification process of claim 4, wherein in the step 3, the activating component is Al2O3And MgO in a mass ratio of 1:1.
6. The attapulgite clay purification and modification process of claim 1, wherein in the step 6, the mass ratio of the attapulgite clay, the surface modifier and the organic solvent is 1 (0.12-0.20) to (4-6).
7. The process of claim 6, wherein in step 6, the mass ratio of the attapulgite, the surface modifier and the organic solvent is 1:0.15: 5.
8. The process for purifying and modifying attapulgite clay according to claim 1, wherein in step 6, the organic solvent is preferably toluene or 1, 2-propanediol.
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| CN112523372A (en) * | 2020-11-24 | 2021-03-19 | 兰州理工大学白银新材料研究院 | Method for manufacturing inorganic core material for outer wall vacuum insulation panel |
| CN113415897A (en) * | 2021-06-02 | 2021-09-21 | 南京公诚节能新材料研究院有限公司 | Technical method of ecological culture medium based on attapulgite |
| CN114684829A (en) * | 2022-03-21 | 2022-07-01 | 淮阴工学院 | Method for quickly converting white variegated mixed-dimension attapulgite into white variegated mixed-dimension attapulgite |
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2020
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112523372A (en) * | 2020-11-24 | 2021-03-19 | 兰州理工大学白银新材料研究院 | Method for manufacturing inorganic core material for outer wall vacuum insulation panel |
| CN113415897A (en) * | 2021-06-02 | 2021-09-21 | 南京公诚节能新材料研究院有限公司 | Technical method of ecological culture medium based on attapulgite |
| CN114684829A (en) * | 2022-03-21 | 2022-07-01 | 淮阴工学院 | Method for quickly converting white variegated mixed-dimension attapulgite into white variegated mixed-dimension attapulgite |
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