CN115254034A - Preparation method and adsorption application of malic acid-kaolinite nano-composite - Google Patents
Preparation method and adsorption application of malic acid-kaolinite nano-composite Download PDFInfo
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- CN115254034A CN115254034A CN202211018231.6A CN202211018231A CN115254034A CN 115254034 A CN115254034 A CN 115254034A CN 202211018231 A CN202211018231 A CN 202211018231A CN 115254034 A CN115254034 A CN 115254034A
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- 229910052622 kaolinite Inorganic materials 0.000 title claims abstract description 49
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 24
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000009830 intercalation Methods 0.000 claims abstract description 19
- 230000002687 intercalation Effects 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000001630 malic acid Substances 0.000 claims abstract description 17
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims abstract description 12
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011090 malic acid Nutrition 0.000 claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 3
- 238000003760 magnetic stirring Methods 0.000 claims 2
- 238000000643 oven drying Methods 0.000 claims 1
- 235000006408 oxalic acid Nutrition 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 238000006467 substitution reaction Methods 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 238000006386 neutralization reaction Methods 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 8
- 229940099690 malic acid Drugs 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 6
- 238000005303 weighing Methods 0.000 description 4
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 229940116298 l- malic acid Drugs 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a preparation method and adsorption application of a malic acid-kaolinite nano compound. The method comprises the steps of successfully inserting malic acid into kaolinite layers by a secondary substitution liquid phase intercalation method, calcining the kaolinite-malic acid intercalation compound, malic acid and sodium carbonate at high temperature, promoting the thermal decomposition of the malic acid among the kaolinite layers by utilizing power provided by a neutralization reaction to finally obtain a malic acid-kaolinite nano compound, and applying the washed malic acid-kaolinite nano compound to adsorption of La (III) and Y (III) solutions. According to the invention, malic acid is inserted into kaolinite layers for the first time, and the malic acid is innovatively decomposed by the kaolinite layers to obtain the malic acid-kaolinite nano composite material, so that the problems of strong hydrogen bonds and low adsorption efficiency among the kaolinite layers are solved, and the adsorption performance of the kaolinite is obviously improved.
Description
Technical Field
The invention belongs to the field of preparation and adsorption of nano kaolin compounds, and particularly relates to a preparation method and adsorption application of a malic acid-kaolinite compound.
Background
The rare earth element is widely applied to high-tech fields such as medical electronic equipment, permanent magnets, laser, petroleum cracking catalysis and the like due to unique electrical, magnetic, optical and catalytic properties of the rare earth element. But also brings great environmental pollution and health risks in the processes of mining, processing and utilizing rare earth elements. Therefore, a technique for separating and recovering rare earth elements from industrial wastewater is attracting attention. The common technologies such as solution extraction, ion exchange, coprecipitation, membrane filtration and the like have the problems of complex operation, large energy consumption, secondary pollution and the like, so that an efficient, simple, cheap and environment-friendly adsorption method is still one of the most widely applied methods.
Kaolin (chemical formula is AI) 2 O 3 ·2SiO 2 ·2H 2 O) is a 1:1 type phyllosilicate mineral, which is commonly used as an adsorbent due to its low cost, non-toxicity, and ready availability. However, natural kaolin lacks exchangeable cations due to strong hydrogen bonding between layers, and thus it is necessary to change the surface properties of kaolin by means of acid, heat, organic substances, metal ions, etc., thereby enlarging the interlayer distance and specific surface area and improving the adsorption performance. At present, no research is carried out on the preparation of the malic acid-kaolinite nano compound by combining a secondary substitution liquid phase intercalation method and a high-temperature calcination method.
Disclosure of Invention
The invention aims to provide a preparation method of a malic acid-kaolinite nano composite material, so that the adsorption performance of kaolinite is improved.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a malic acid-kaolinite nano-composite comprises the following steps:
(1) Preparation of kaolinite-dimethyl sulfoxide (Kaol-DMSO) precursor: according to the weight ratio of kaolinite: dimethyl sulfoxide: ultrapure water =5-10g:50-100mL: adding kaolinite into dimethyl sulfoxide and ultrapure water according to the mass-volume ratio of 4.5-9mL, magnetically stirring for 12-24h at 70-90 ℃, and performing suction filtration and drying to obtain the Kaol-DMSO intercalation compound.
(2) Kaolinite-malic acid (Kaol-C) 4 H 6 O 5 ) Preparing an intercalation compound: according to Kaol-DMSO precursor: malic acid solution (ethanol as solvent) =1.5-3g:50mL (1-2 mol/L), adding the Kaol-DMSO intercalation compound into malic acid solution, magnetically stirring at room temperature for 24-48h, filtering, and drying to obtain Kaol-C 4 H 6 O 5 And (3) intercalation compound.
(3) Preparation of malic acid-kaolinite nanocomposite: according to Kaol-C 4 H 6 O 5 IntercalationThe compound is as follows: malic acid (C) 4 H 6 O 5 ): sodium carbonate (Na) 2 CO 3 ) =1:1-1.5:0.8-1.2, mixing and grinding the three components for 15-30min, calcining in a muffle furnace at 300-400 ℃ for 6-8h (the heating rate is 5 ℃/min), cooling to room temperature, and washing for 2-3 times to obtain the malic acid-kaolinite nano composite. The calcination process involves the following reactions:
C 4 H 6 O 5 +Na 2 CO 3 →C 4 H 4 Na 2 O 5 +CO 2 +H 2 O
C 4 H 6 O 5 +3O2→4CO 2 +3H 2 O
the invention also provides application of the malic acid-kaolinite nano-composite prepared by the preparation method in adsorbing rare earth metals La and Y, and the specific method is as follows:
preparing La (III) and Y (III) solutions with concentration gradient of 20-500mg/L, adding the malic acid-kaolinite nano-composite into the solution for static adsorption (constant temperature water bath: 25-30 ℃), adjusting the pH =6 of the solution by using HCI of 0.1mol/L, and measuring the concentration of La (III) and Y (III) in the supernatant after adsorption equilibrium by using ICP-OES.
The method has the beneficial effects that the malic acid-kaolinite nano compound is prepared by combining a secondary substitution liquid phase intercalation method and a high-temperature calcination method, the related experimental method is simple and low in cost, the specific surface area of the obtained malic acid-kaolinite nano compound is remarkably increased, the adsorption sites are increased, and the malic acid-kaolinite nano compound has excellent adsorption performance on rare earth metals.
Drawings
Fig. 1a, 1b are XRD patterns of the kaolinite intercalation composite and the nano-kaolinite composite of example 1, respectively.
Fig. 2a and 2b are SEM images of the kaolin intercalated composite and the nano-kaolinite composite in example 1, respectively.
Fig. 3 is a BET plot of the nano-kaolinite composite according to example 1.
Fig. 4 is a graph of adsorption kinetics of the nano-kaolinite composite in example 1.
Detailed Description
The present invention will be further specifically described with reference to the following examples.
Example 1
(1) Preparation of kaolinite-dimethyl sulfoxide (Kaol-DMSO) precursor: weighing 10g of kaolinite, adding the kaolinite into 100mL of dimethyl sulfoxide and 9mL of ultrapure water, magnetically stirring for 12h at 90 ℃, and carrying out suction filtration and drying to obtain the Kaol-DMSO intercalation compound.
(2) Kaolinite-malic acid (Kaol-C) 4 H 6 O 5 ) Preparing an intercalation compound: adding 3g of Kaol-DMSO precursor prepared in the step (1) into 1mol/L malic acid solution, magnetically stirring for 24h at room temperature, filtering and drying to obtain Kaol-C 4 H 6 O 5 And (3) intercalation compound.
(3) Preparation of malic acid-kaolinite nanocomposite: weighing 1.2g of Kaol-C prepared in step (2) 4 H 6 O 5 Intercalated composite, 1.2g C 4 H 6 O 5 、0.9g Na 2 CO 3 Mixing and grinding for 15min, calcining for 8h at 400 ℃ in a muffle furnace (the heating rate is 5 ℃/min), cooling to room temperature, and washing for 2-3 times to obtain the malic acid-kaolinite nano compound.
(4) Taking 25mg of the malic acid-kaolinite nanocomposite prepared in the step (3) to perform static adsorption in 25mL of 300mg/L La (III) and Y (III) solutions (constant-temperature water bath: 30 ℃), and controlling the pH with 0.1mol/L HCI solution to be =6.
Example 2
(1) Preparation of kaolinite-dimethyl sulfoxide (Kaol-DMSO) precursor: weighing 5g of kaolinite, adding the kaolinite into 50mL of dimethyl sulfoxide and 4.5mL of ultrapure water, magnetically stirring for 24h at 80 ℃, and carrying out suction filtration and drying to obtain the Kaol-DMSO intercalation compound.
(2) Kaolinite-malic acid (Kaol-C) 4 H 6 O 5 ) Preparing an intercalation compound: adding 2g of the Kaol-DMSO precursor prepared in the step (1) into 1.5mol/L malic acid solution, magnetically stirring for 24h at room temperature, filtering and drying to obtain Kaol-C 4 H 6 O 5 And (3) intercalation compound.
(3) Preparation of malic acid-kaolinite nanocomposite: weighing 1.2g of Kaol-C prepared in step (2) 4 H 6 O 5 Intercalated composite, 1.5g C 4 H 6 O 5 、1.2g Na 2 CO 3 Mixing and grinding for 30min, calcining for 6h at 400 ℃ in a muffle furnace (the heating rate is 5 ℃/min), cooling to room temperature, and washing for 2-3 times to obtain the malic acid-kaolinite nano composite.
(4) Taking 25mg of the malic acid-kaolinite nano compound prepared in the step (3) to perform static adsorption in 25mL of 300mg/L La (III) and Y (III) solution (constant-temperature water bath: 30 ℃), and controlling the pH to be =6 by using 0.1mol/L HCI solution.
Claims (5)
1. The preparation method of the malic acid-kaolinite nano-composite is characterized by comprising the following steps:
(1) Preparation of kaolinite-dimethyl sulfoxide (Kaol-DMSO) precursor: mixing kaolinite, dimethyl sulfoxide and ultrapure water according to a certain proportion, magnetically stirring for a certain time at a proper temperature, and carrying out suction filtration and drying to obtain the Kaol-DMSO intercalation compound.
(2) Kaolinite-malic acid (Kaol-C) 4 H 6 O 5 ) Preparing an intercalation compound: mixing Kaol-DMSO precursor and malic acid solution (ethanol as solvent) at a certain ratio, magnetically stirring at room temperature for a certain time, filtering, and oven drying to obtain Kaol-C 4 H 6 O 5 And (3) intercalation compound.
(3) Preparation of malic acid-kaolinite nanocomposite: mixing Kaol-C 4 H 6 O 5 Intercalation complex, malic acid (C) 4 H 6 O 5 ) Sodium carbonate (Na) 2 CO 3 ) Mixing and grinding the materials according to a certain proportion for a proper time, putting the materials into a muffle furnace to calcine for a certain time (the heating rate is 5 ℃/min), cooling the materials to room temperature, and washing the materials for 2 to 3 times to obtain the malic acid-kaolinite nano composite. The calcination process involves the following reactions:
C 4 H 6 O 5 +Na 2 CO 3 →C 4 H 4 Na 2 O 5 +CO 2 +H 2 O
C 4 H 6 O 5 +3O2→4CO 2 +3H 2 O
(4) Preparing La (III) and Y (III) solutions with certain concentrations, adding the malic acid-kaolinite nano-composite into the solution for static adsorption, adjusting the pH of the solution by using 0.1mol/L HCI, and measuring the concentrations of the La (III) and the Y (III) in the supernatant after adsorption equilibrium by using ICP-OES.
2. The method of claim 1, wherein the malic acid-kaolinite nanocomposite comprises: in the step (1), the mass volume ratio of the kaolin, the dimethyl sulfoxide and the ultrapure water is 5-10g:50-100mL:4.5-9mL, magnetic stirring temperature of 70-90 ℃ and time of 12-24h.
3. The method of claim 1, wherein the malic acid-kaolinite nanocomposite comprises: in the step (2), the mass volume ratio of the Kaol-DMSO precursor to the malic acid solution (ethanol is used as a solvent) is 1.5-3g:50mL (1-2 mol/L) and 24-48h of magnetic stirring time.
4. The method of claim 1, wherein the malic acid-kaolinite nanocomposite comprises: kaol-C in step (3) 4 H 6 O 5 Intercalated complex, malic acid (C) 4 H 6 O 5 ) Sodium carbonate (Na) 2 CO 3 ) The mass ratio is 1:1-1.5:0.8 to 1.2, the calcining temperature is 300 to 400 ℃, and the time is 6 to 8 hours.
5. The method for preparing the oxalic acid intercalated expanded kaolin as claimed in claim 1, wherein: in the step (4), the concentration range of the La (III) and Y (III) solutions is 20-500mg/L, the temperature of the thermostatic water bath is 25-30 ℃, and the pH value of the solution is 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117462432A (en) * | 2023-12-21 | 2024-01-30 | 铂臻(广州)生物科技有限公司 | Acne-removing composition and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5672555A (en) * | 1996-02-29 | 1997-09-30 | Thiele Kaolin Company | Kaolin-potassium acetate intercalation complex and process of forming same |
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| CN113735677A (en) * | 2021-09-30 | 2021-12-03 | 江西省科学院应用化学研究所 | Method for preparing cis-pinane by catalyzing hydrogenation of alpha-pinene with L-malic acid intercalation magnalium hydrotalcite loaded ruthenium catalyst |
| CN114849654A (en) * | 2022-05-13 | 2022-08-05 | 成都理工大学 | Preparation method and adsorption application of oxalic acid intercalation expanded kaolin |
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- 2022-08-24 CN CN202211018231.6A patent/CN115254034A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| US5672555A (en) * | 1996-02-29 | 1997-09-30 | Thiele Kaolin Company | Kaolin-potassium acetate intercalation complex and process of forming same |
| CN1957948A (en) * | 2005-11-04 | 2007-05-09 | 浙江海力生制药有限公司 | Modified montmorillonite, preparation method and application |
| WO2018078378A1 (en) * | 2016-10-27 | 2018-05-03 | Oxford Pharmascience Limited | Modifier system for compositions containing layered double hydroxide |
| CN113735677A (en) * | 2021-09-30 | 2021-12-03 | 江西省科学院应用化学研究所 | Method for preparing cis-pinane by catalyzing hydrogenation of alpha-pinene with L-malic acid intercalation magnalium hydrotalcite loaded ruthenium catalyst |
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| DOU W等: "Study on the adsorption performance of La (III) and Y (III) on malic acid-kaolinite nanocomposite", MATERIALS LETTERS * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117462432A (en) * | 2023-12-21 | 2024-01-30 | 铂臻(广州)生物科技有限公司 | Acne-removing composition and preparation method thereof |
| CN117462432B (en) * | 2023-12-21 | 2024-04-02 | 铂臻(广州)生物科技有限公司 | Acne-removing composition and preparation method thereof |
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Application publication date: 20221101 |
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