CN106582595A - Preparation method for blue TiO2 catalyst - Google Patents
Preparation method for blue TiO2 catalyst Download PDFInfo
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- CN106582595A CN106582595A CN201611234135.XA CN201611234135A CN106582595A CN 106582595 A CN106582595 A CN 106582595A CN 201611234135 A CN201611234135 A CN 201611234135A CN 106582595 A CN106582595 A CN 106582595A
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- blue
- tio
- catalyst
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- ticl
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910003074 TiCl4 Inorganic materials 0.000 claims abstract description 18
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine Substances NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000036571 hydration Effects 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 14
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 210000001124 body fluid Anatomy 0.000 abstract description 6
- 239000010839 body fluid Substances 0.000 abstract description 6
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 2
- 230000004298 light response Effects 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- IDIJOAIHTRIPRC-UHFFFAOYSA-J hexaaluminum;sodium;2,2,4,4,6,6,8,8,10,10,12,12-dodecaoxido-1,3,5,7,9,11-hexaoxa-2,4,6,8,10,12-hexasilacyclododecane;iron(2+);triborate;tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Fe+2].[Fe+2].[Fe+2].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-][Si]1([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O[Si]([O-])([O-])O1 IDIJOAIHTRIPRC-UHFFFAOYSA-J 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910000246 schorl Inorganic materials 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention provides a preparation method for a blue TiO2 catalyst. The preparation method for the blue TiO2 catalyst comprises the following steps that TiCl4 and hydrazine hydrate are mixed according to the molar ratio of 1: (5-10), and a TiCl4-hydrazine complex is obtained; deionized water is added into the complex according to the mass ratio of the TiCl4 and water of 1:15-30, and a TiO2 precursor body fluid is obtained; and the obtained precursor body fluid is put into a hydrothermal reactor and reacted for 16-24 hours at the temperature of 170-220 DEG C, and then, after suction filtration, washing and drying, the blue TiO2 catalyst is obtained. Through the preparation method for the blue TiO2 catalyst, the obtained blue TiO2 catalyst has a good ultraviolet-visual light response and a good photocatalytic wastewater dye degradation property under ultraviolet-visual light. A methyl orange solution of 20 mg/L can be completely degraded by blue TiO2 powder within 25 minutes, and the photocatalytic effect of the blue TiO2 powder is better than that of white TiO2.
Description
Technical field
The invention belongs to chemical field, is related to a kind of catalyst, a kind of specifically blue TiO2The preparation of catalyst
Method.
Background technology
TiO2Photocatalysis technology as a kind of " green technology " and " environmentally-friendly technique ", with it is simple to operate, react bar
The advantages of part gentle non-secondary pollution, be one of research direction that 21 century catalysis subject receives much concern, in the industry of water process
Change and have in sizable application huge potentiality and wide application prospect, wherein nano titanium oxide P25 has been realized in industry
Metaplasia is produced.But, with regard to TiO2For, there are two problems to govern its performance all the time, one is TiO2Energy gap it is wider,
For 3.2eV, this causes its photoresponse scope narrower, can only absorb ultraviolet light of the sunshine medium wavelength less than 380nm, and this is only
Account for the 4%-6% for being irradiated to earthbound solar energy ray;Two is that photo-generated carrier is easily combined again, causes photo-quantum efficiency very low.
Therefore, solve the problems, such as that two above is present TiO2In the focus and emphasis of photocatalysis field research.General T iO2Powder outward appearance is led to
It is often white, affected larger by the two factors above.More preferably to solve the problems, such as both the above, non-white color system TiO2Research
Increasingly receive publicity.Blue TiO2It is the TiO after specially treated2, this TiO2Black appearance be by absorbing wavelength
Moved to visible region from ultraviolet region and caused.Blue TiO2It is right to also achieve while remaining to ultraviolet light response
The response of visible ray, and can effectively suppress being combined again for photo-generated carrier, show stronger photo-catalysis capability.
With titanium trichloride as raw material in patent CN103553124A, the chlorination of balance conjugate pair four of certain mol proportion is added
Titanium, and using sodium fluoride as stabilizer, blue titanium dioxide nano particle is gone out by solvent structure.But this method institute
Need raw material many, temperature is high, the time is long.Red schorl phase titanium dioxide is mixed with deionized water in patent CN103482698A, so
Obtain blue titanium dioxide under the irradiation of Ultra-Violet Laser instrument afterwards.Although this method raw material is less, equipment needed thereby is more
Harshness, is unfavorable for large-scale production.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of blue TiO2Raw powder's production technology,
Described this blue TiO2Raw powder's production technology will solve preparation blueness TiO of the prior art2The method technique of powder is answered
Miscellaneous, condition is harsh, is unfavorable for the technical problem of large-scale industrial production.
The invention provides a kind of blue TiO2The preparation method of catalyst, comprises the steps:
1) TiCl is weighed respectively4And hydrazine hydrate, described TiCl4It is 1 with the mol ratio of hydrazine hydrate:5-10, by TiCl4And hydration
Hydrazine mixes, and obtains TiCl4- hydrazine complex;
2) deionized water is weighed, described deionized water and TiCl4Mass ratio be 1:15-30, deionized water is added above-mentioned
TiCl4In-hydrazine complex, TiO is obtained2Precursor liquid;
3) by above-mentioned TiO2Precursor liquid be fitted in water heating kettle, at 170-220 DEG C, after reaction 16-24h, suction filtration, wash
Wash, be dried acquisition blueness TiO2Catalyst.
Further, in step 3)In, washed using ethanol.
The present invention adopts one kettle way, the coordination and reduction by hydrazine hydrate, through simple hydro-thermal process, it is not required to
The high-temperature process in later stage is wanted, one-step synthesis has the blue TiO of Anatase under the conditions of relatively mild2Catalyst.According to this
TiO prepared by the method for invention2Powder outward appearance is blueness, and epigranular, soilless sticking has good photocatalysis under daylight light irradiation
Effect.Such blue TiO2Powder, can be degradable by the methyl orange solution of 20mg/L in 30min.
The present invention is compared with prior art, and its technological progress is significant.The blueness obtained using the method for the present invention
TiO2Catalyst has preferable ultraviolet-visible photoresponse, contaminates with preferable wastewater by photocatalysis under ultraviolet-visible light
The performance of material.Such blue TiO2Powder, most soon can be degradable by the methyl orange solution of 20mg/L in 25min.The present invention
Preparation method process is simple, without the need for special material and equipment.The blue TiO of acquisition2Catalyst powder epigranular, soilless sticking,
Stable performance, yield is high, the whiter TiO of photocatalysis effect2More preferably.
Description of the drawings:
Fig. 1 is blue TiO prepared by embodiment 1-42The XRD of catalyst.
Specific embodiment
With reference to embodiment and relevant chart, the present invention will be described in detail, but the invention is not restricted to real
Example:
Embodiment 1
1) by TiCl4With hydrazine hydrate according to mol ratio be 1:8 ratio mixing, obtains TiCl4- hydrazine complex;
2) according to mass ratio TiCl4:Water=1:20, deionized water is added in above-mentioned (1) in complex, obtain TiO2Forerunner
Body fluid;
3) by 2)Gained precursor liquid is fitted in water heating kettle, at 180 DEG C, after reaction 20h, and suction filtration, ethanol washing, dry acquisition
Blue TiO2Catalyst.
XRD spectra test is carried out to gained sample using German Brooker D8 Advance, as a result such as Fig. 1.XRD spectra
With anatase TiO2Standard card it is consistent, illustrate in embodiment 1, using the blue anatase TiO of one-step synthesis method2;From diffraction
The generation width at peak, it can be seen that the crystallite dimension of sample is less.
The preparation-obtained blue TiO of the present embodiment2Powder, the ratio with mass ratio as 0.1g/100mL is added to
In the methyl orange solution of 20mg/L, under ultraviolet-visible light, methyl orange solution is degradable finishing in 30min.
Embodiment 2
1) by TiCl4With hydrazine hydrate according to mol ratio be 1:10 ratio mixing, obtains TiCl4- hydrazine complex;
2) according to mass ratio TiCl4:Water=1:25, deionized water is added in above-mentioned (1) in complex, obtain the forerunner of TiO2
Body fluid;
3) by 2)Gained precursor liquid is fitted in water heating kettle, at 220 DEG C, after reaction 16h, and suction filtration, ethanol washing, dry acquisition
Blue TiO2Catalyst.
XRD spectra test is carried out to gained sample using German Brooker D8 Advance, as a result such as Fig. 1.XRD spectra
With anatase TiO2Standard card it is consistent, illustrate in example 2, using the blue anatase TiO of one-step synthesis method2;From diffraction
The generation width at peak, it can be seen that the crystallite dimension of sample is less.
The preparation-obtained blue TiO of the present embodiment2Powder, the ratio with mass ratio as 0.1g/100mL is added to
In the methyl orange solution of 20mg/L, under ultraviolet-visible light, methyl orange solution is degradable finishing in 25min.
Embodiment 3
1) by TiCl4With hydrazine hydrate according to mol ratio be 1:8 ratio mixing, obtains TiCl4- hydrazine complex;
2) according to mass ratio TiCl4:Water=1:15, deionized water is added in above-mentioned (1) in complex, obtain the forerunner of TiO2
Body fluid;
3) will(2)Gained precursor liquid is fitted in water heating kettle, and at 220 DEG C, after reaction 16h, suction filtration, ethanol washing, drying are obtained
Obtain blue TiO2Catalyst.
XRD spectra test is carried out to gained sample using German Brooker D8 Advance, as a result such as Fig. 1.XRD spectra
With anatase TiO2Standard card it is consistent, illustrate in embodiment 3, using the blue anatase TiO of one-step synthesis method2;From diffraction
The generation width at peak, it can be seen that the crystallite dimension of sample is less.
The preparation-obtained blue TiO of the present embodiment2Powder, the ratio with mass ratio as 0.1g/100mL is added to
In the methyl orange solution of 20mg/L, under ultraviolet-visible light, methyl orange solution is degradable finishing in 25min.
Embodiment 4
1) by TiCl4With hydrazine hydrate according to mol ratio be 1:5 ratio mixing, obtains TiCl4- hydrazine complex;
2) according to mass ratio TiCl4:Water=1:20, deionized water is added in above-mentioned (1) in complex, obtain the forerunner of TiO2
Body fluid;
3) by 2)Gained precursor liquid is fitted in water heating kettle, at 220 DEG C, after reaction 20h, and suction filtration, ethanol washing, dry acquisition
Blue TiO2Catalyst.
XRD spectra test is carried out to gained sample using German Brooker D8 Advance, as a result such as Fig. 1.XRD spectra
It is consistent with the standard card of anatase tio2, illustrate in example 4, using one-step synthesis method blueness anatase TiO2;From spreading out
Penetrate the generation width at peak, it can be seen that the crystallite dimension of sample is less.
The preparation-obtained blue TiO of the present embodiment2Powder, the ratio with mass ratio as 0.1g/100mL is added to
In the methyl orange solution of 20mg/L, under ultraviolet-visible light, methyl orange solution is degradable finishing in 32min.
Claims (2)
1. a kind of blue TiO2The preparation method of catalyst, it is characterised in that comprise the steps:
1)TiCl is weighed respectively4And hydrazine hydrate, described TiCl4It is 1 with the mol ratio of hydrazine hydrate:5-10, by TiCl4And hydration
Hydrazine mixes, and obtains TiCl4- hydrazine complex;
2)Weigh deionized water, described deionized water and TiCl4Mass ratio be 1:15-30, deionized water is added above-mentioned
TiCl4In-hydrazine complex, TiO is obtained2Precursor liquid;
3)By above-mentioned TiO2Precursor liquid be fitted in water heating kettle, at 170-220 DEG C, reaction 16-24h after, suction filtration, washing,
It is dried and obtains blueness TiO2Catalyst.
2. a kind of blue TiO according to claim 12The preparation method of catalyst, it is characterised in that:
In step 3)In, washed using ethanol.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107824181A (en) * | 2017-10-26 | 2018-03-23 | 上海应用技术大学 | A kind of preparation method of visible-light photocatalyst |
CN107827152A (en) * | 2017-11-09 | 2018-03-23 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide for carbon dioxide photocatalysis synthesizing methane and preparation method thereof |
CN110526289A (en) * | 2019-07-16 | 2019-12-03 | 南京碧盾环保科技股份有限公司 | A kind of blue Anatase TiO2Nanocrystal and preparation method thereof |
CN111298788A (en) * | 2019-12-02 | 2020-06-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of silver-loaded colored one-dimensional mesoporous titanium dioxide, product and application thereof |
CN113549407A (en) * | 2021-08-18 | 2021-10-26 | 深圳市英诺美达科技有限公司 | High-performance single-sided adhesive tape |
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Cited By (11)
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---|---|---|---|---|
CN107824181A (en) * | 2017-10-26 | 2018-03-23 | 上海应用技术大学 | A kind of preparation method of visible-light photocatalyst |
CN107827152A (en) * | 2017-11-09 | 2018-03-23 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide for carbon dioxide photocatalysis synthesizing methane and preparation method thereof |
CN107827152B (en) * | 2017-11-09 | 2019-07-16 | 中国科学院上海硅酸盐研究所 | Blue titanium dioxide and preparation method thereof for carbon dioxide photocatalysis synthesizing methane |
CN110526289A (en) * | 2019-07-16 | 2019-12-03 | 南京碧盾环保科技股份有限公司 | A kind of blue Anatase TiO2Nanocrystal and preparation method thereof |
CN110526289B (en) * | 2019-07-16 | 2021-10-08 | 南京碧盾环保科技股份有限公司 | Blue anatase phase TiO2Nanocrystals and methods of making the same |
CN111298788A (en) * | 2019-12-02 | 2020-06-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of silver-loaded colored one-dimensional mesoporous titanium dioxide, product and application thereof |
CN111298788B (en) * | 2019-12-02 | 2022-07-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of silver-loaded colored one-dimensional mesoporous titanium dioxide, product and application thereof |
CN113549407A (en) * | 2021-08-18 | 2021-10-26 | 深圳市英诺美达科技有限公司 | High-performance single-sided adhesive tape |
CN113773560A (en) * | 2021-09-08 | 2021-12-10 | 广州绿徽新材料研究院有限公司 | High-strength tableware particle material capable of being completely and naturally degraded and preparation method thereof |
CN113788991A (en) * | 2021-09-08 | 2021-12-14 | 广州绿徽新材料研究院有限公司 | Biodegradable high-performance modified particle material and preparation method thereof |
CN113736146A (en) * | 2021-09-09 | 2021-12-03 | 谭卓华 | Degradable high-performance tableware material particle with ceramic texture and preparation method thereof |
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