CN111909550A - Coating for improving cracking resistance of medicinal glass surface and preparation method and application thereof - Google Patents
Coating for improving cracking resistance of medicinal glass surface and preparation method and application thereof Download PDFInfo
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- CN111909550A CN111909550A CN202010787741.4A CN202010787741A CN111909550A CN 111909550 A CN111909550 A CN 111909550A CN 202010787741 A CN202010787741 A CN 202010787741A CN 111909550 A CN111909550 A CN 111909550A
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- 239000011521 glass Substances 0.000 title claims abstract description 60
- 238000000576 coating method Methods 0.000 title claims abstract description 41
- 239000011248 coating agent Substances 0.000 title claims abstract description 39
- 238000005336 cracking Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- 238000005507 spraying Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 13
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000003980 solgel method Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000002411 adverse Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000007373 indentation Methods 0.000 description 9
- 239000005361 soda-lime glass Substances 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- 238000007789 sealing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005524 ceramic coating Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 238000005496 tempering Methods 0.000 description 2
- 150000003606 tin compounds Chemical class 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910020442 SiO2—TiO2 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003124 biologic agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000008279 sol Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229960005486 vaccine Drugs 0.000 description 1
- -1 vaccines Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention relates to the technical field of new glass materials, and particularly discloses a coating for improving the cracking resistance of the surface of medicinal glass, and a preparation method and application thereof. The coating for improving the cracking resistance of the surface of the medicinal glass is characterized in that: the coating is prepared by taking tetraethoxysilane, ethanol, deionized water, nitric acid and aluminum nitrate as raw materials through a sol-gel method; the prepared coating solution comprises silicon dioxide and aluminum oxide. The glass coating is prepared by adopting a sol-gel method, the outer surface of the medicinal glass can be sprayed at room temperature, microcracks on the surface of the glass are effectively filled, heating and curing are not needed, energy consumption can be greatly reduced compared with the traditional glass coating material, and the economic benefit is considerable; furthermore, the glass after spraying still maintains high transparency, i.e. the coating does not adversely affect the appearance of the glass.
Description
(I) technical field
The invention relates to the technical field of new glass materials, in particular to a coating for improving the cracking resistance of the surface of medicinal glass, and a preparation method and application thereof.
(II) background of the invention
The glass industry is an important basic raw material industry, is closely related to the life and production of people, and plays an important role in national economy. The glass and the processed products thereof are widely applied to packaging, building, transportation, decoration and fitment, electronic information, solar energy utilization and other emerging industries. In particular, the medicinal glass has good chemical stability, heat-resistant stability, smoothness, transparency, easy cleaning and disinfection, good sealing performance and other physical and chemical properties, and is widely used for packaging biological agents, freeze-dried powder injections, vaccines, blood agents and other medicines.
However, glass is a brittle material, and although it has micro plasticity, its yield elongation stage is very small, and particularly when a sudden applied load is applied, the particles in the glass break apart from each other in time to make a compliant deformation flow. For medicinal glass, friction and collision inevitably occur during the production, storage and transportation of the medicinal glass. For a long time, researchers in the field of glass materials have sought to improve the mechanical properties of glass, in particular the "crack resistance".
The production process of the molded bottle medicinal glass mainly comprises two methods of blowing and pressure-blowing molding. In any molding method, microcracks inevitably exist on the surface of the glass product, and the microcracks tend to become stress concentration positions when the glass is subjected to external load, so that the actual strength of the glass is far lower than the theoretical strength of the glass. Therefore, how to control the formation of microcracks in the glass material and limit the propagation of cracks is the key to improving its mechanical properties.
The currently common glass surface strengthening process includes: physical reinforcement (tempering), chemical reinforcement (ion exchange), coating method reinforcement, and the like. Wherein, the physical tempering is more suitable for plate glass, and the homogenization of stress distribution is difficult to realize for products with complex shapes (such as bottle glass); the ion exchange time of the molten salt method is long, the method is not suitable for mass production lines, the variability of molten salt components is not beneficial to quality control, and the problem of environmental pollution of waste liquid exists; the implementation process of the spraying process is relatively simple, and continuous online operation is easy to realize. For example: the hot end spraying agent mainly adopts organic tin compound or inorganic tin compound, namely: between the bottle making machine and the annealing furnace, the glass bottle can still in a glowing state is subjected to surface spraying treatment by adopting a nozzle or atomizing equipment, which is helpful for improving the hardness and the impact strength of glass, but the volatilization of organic matters also has certain pollution to the environment. In addition, in order to improve the surface lubricity and brightness of the glass product, so-called "cold-end spraying agents" are generally sprayed, wherein the cold-end spraying agent is mainly aqueous polymer solution or polymer emulsion, the spraying temperature of the cold-end spraying agent is about 100 ℃, and the defects such as stripes and the like are generated when the temperature is lower than 90 ℃.
The sol-gel method for preparing nano particles has the advantages of simple process, low temperature and the like, and has important application in many fields in recent years, and a plurality of related patents are obtained, such as: a process for preparing antioxidizing composite coating on the surface of carbon fibres (ZL 201510429877.7) discloses an Al-type composite coating on the surface of carbon fibres2O3-SiO2-TiO2An anti-oxidation composite coating; the composite ceramic coating preparation method (ZL 200810159025.0) discloses a method for preparing composite ceramic powder by a sol-gel method; a preparation and sealing process of a high-temperature resistant sealing agent (application No. 200910063903.3) discloses a ceramic coating, which comprises the following steps: al with mica flakes, whisker silicon or hexagonal boron nitride as filler2O3-SiO2And (3) a sol hole sealing agent. The above patents require either high temperature heating or fillers during application, resulting in higher costs.
To date, there has been no report of glass coatings with good crack resistance that can be used for pharmaceutical glasses and cured at room temperature without the need for heating.
Disclosure of the invention
The invention provides a coating which is applied at room temperature and does not need heating curing and is used for improving the cracking resistance of the surface of medicinal glass, and a preparation method and application thereof, aiming at overcoming the defects of the prior art.
The invention is realized by the following technical scheme:
a coating for improving the cracking resistance of a pharmaceutical glass surface, characterized in that: the coating is prepared by taking tetraethoxysilane, ethanol, deionized water, nitric acid and aluminum nitrate as raw materials through a sol-gel method; the prepared coating solution comprises silicon dioxide and aluminum oxide.
The coating is prepared by a sol-gel method, the process is simple, the cost is relatively low, and the existence of silicon dioxide and aluminum oxide ensures that the coating has the characteristics of strong chemical bonding property with the cross section of a glass substrate and ageing resistance.
The preparation method of the coating for improving the cracking resistance of the surface of the medicinal glass comprises the following steps:
(1) mixing ethyl orthosilicate, ethanol, deionized water and nitric acid at room temperature to obtain a mixed solution;
(2) stirring the mixed solution at 60 ℃ for 3 hours, and cooling to room temperature;
(3) and at room temperature, dropwise adding 1.5M aluminum nitrate solution into the mixed solution, and continuously stirring for 2 hours to obtain the solution for the glass coating.
Preferably, in the step (1), the molar ratio of the ethyl orthosilicate, the ethanol, the deionized water and the nitric acid is 1: 4.2-4.7: 2.2-2.8: 0.03-0.05; further preferred is a molar ratio of 1:4.5:2.5: 0.04.
preferably, in the step (3), the aluminum nitrate solution is added in an amount such that the molar ratio of silicon dioxide to aluminum oxide is 9.5-8: 1; further preferred is a molar ratio of 9: 1.
the application of the coating comprises the following steps:
the medicinal glass bottle conveyed by the caterpillar band is discharged from the annealing kiln and exposed in the air, and when the temperature is reduced to below 30 ℃, the coating solution is sprayed on the glass on line by a spraying pump, wherein the spraying thickness is 50-300 nanometers.
Preferably, the coating thickness is 60 to 200 nm, more preferably 60 to 150 nm.
The glass coating is prepared by adopting a sol-gel method, the outer surface of the medicinal glass can be sprayed at room temperature, microcracks on the surface of the glass are effectively filled, heating and curing are not needed, energy consumption can be greatly reduced compared with the traditional glass coating material, and the economic benefit is considerable; furthermore, the glass after spraying still maintains high transparency, i.e. the coating does not adversely affect the appearance of the glass.
(IV) description of the drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a graph of the Vickers hardness indentation of uncoated soda-lime-silica glass for pharmaceutical use held at a load of 0.2 kg for 15 seconds;
FIG. 2 is a graph of the Vickers hardness indentation of a coated thickness of a soda-lime-silica glass for pharmaceutical use of example 3 held at a load of 0.2 kg for 15 seconds.
(V) detailed description of the preferred embodiments
A coating for improving the resistance of a glass surface to cracking in accordance with the present invention is further illustrated by the following specific examples, of which example 3 is the preferred example.
Example 1:
according to the molar ratio of each component, namely: tetraethoxysilane (TEOS): ethanol: deionized water: nitric acid =1: 4.3:2.2:0.03, and the four liquids are mixed uniformly at room temperature in sequence; then stirring the mixed solution at 60 ℃ for 3 hours, and cooling to room temperature; and (3) dropwise adding an aluminum nitrate solution with the molar concentration of 1.5M into the solution at room temperature according to the proportion (the molar ratio of silicon dioxide to aluminum oxide is 9.5: 1), and continuously stirring for 2 hours to obtain a solution for the glass coating for later use.
The soda-lime-silica medical glass bottle transported by the crawler passes through an annealing kiln and is exposed in the air, and when the temperature is reduced to room temperature, the solution is sprayed on the outer surface of the glass, and the spraying thickness is 50 nanometers. The sprayed soda-lime-silica glass for medical use did not develop crack propagation at the tip of the indentation after being held under a load of 0.2 kg for 15 seconds.
Example 2:
the difference between this example and example 1 is the molar ratio of the components, namely: tetraethoxysilane (TEOS): ethanol: deionized water: nitric acid =1: 4.6:2.6: 0.04; and the molar ratio of silicon dioxide to aluminum oxide is 8: 1; the spray thickness was 300 nm.
The sprayed soda-lime-silica glass for medical use did not develop crack propagation at the tip of the indentation after being held under a load of 0.2 kg for 15 seconds.
Example 3:
the difference between this example and example 1 is the molar ratio of the components, namely: tetraethoxysilane (TEOS): ethanol: deionized water: nitric acid =1:4.5:2.5: 0.04; and the molar ratio of silicon dioxide to aluminum oxide is 9: 1; the spray thickness was 60 nm.
The sprayed soda-lime-silica glass for medical use did not develop crack propagation at the tip of the indentation after being held under a load of 0.2 kg for 15 seconds.
As shown in the attached figures 1 and 2, compared with the uncoated glass, the sprayed glass has no phenomenon of crack propagation at the tip of an indentation under the action of load, and only the crack of the coating occurs, namely the crack of the glass surface is inhibited by the existence of the coating.
Example 4:
the difference between this example and example 1 is the molar ratio of the components, namely: tetraethoxysilane (TEOS): ethanol: deionized water: nitric acid =1:4.7:2.3: 0.03; and the molar ratio of silicon dioxide to aluminum oxide is 9.2: 1; the spray thickness was 150 nm.
The sprayed soda-lime-silica glass for medical use did not develop crack propagation at the tip of the indentation after being held under a load of 0.2 kg for 15 seconds.
Example 5:
the difference between this example and example 1 is the molar ratio of the components, namely: tetraethoxysilane (TEOS): ethanol: deionized water: nitric acid =1: 4.3:2.7: 0.04; and the molar ratio of silicon dioxide to aluminum oxide is 8.9: 1; the spray thickness was 150 nm.
The sprayed soda-lime-silica glass for medical use did not develop crack propagation at the tip of the indentation after being held under a load of 0.2 kg for 15 seconds.
Example 6:
the difference between this example and example 1 is the molar ratio of the components, namely: tetraethoxysilane (TEOS): ethanol: deionized water: nitric acid =1: 4.2:2.8: 0.05; and the molar ratio of silicon dioxide to aluminum oxide is 8.4: 1; the spray thickness was 150 nm.
The sprayed soda-lime-silica glass for medical use did not develop crack propagation at the tip of the indentation after being held under a load of 0.2 kg for 15 seconds.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (9)
1. A coating for improving the cracking resistance of the surface of medicinal glass is characterized in that: the coating is prepared by taking tetraethoxysilane, ethanol, deionized water, nitric acid and aluminum nitrate as raw materials through a sol-gel method; the prepared coating solution comprises silicon dioxide and aluminum oxide.
2. The method of claim 1, wherein the method comprises the steps of: (1) mixing ethyl orthosilicate, ethanol, deionized water and nitric acid at room temperature to obtain a mixed solution; (2) stirring the mixed solution at 60 ℃ for 3 hours, and cooling to room temperature; (3) and at room temperature, dropwise adding 1.5M aluminum nitrate solution into the mixed solution, and continuously stirring for 2 hours to obtain the solution for the glass coating.
3. The method of claim 2, wherein: in the step (1), the molar ratio of ethyl orthosilicate, ethanol, deionized water and nitric acid is 1: 4.2-4.7: 2.2-2.8: 0.03-0.05.
4. The method of claim 2, wherein: in the step (3), the adding amount of the aluminum nitrate solution is that the mol ratio of the silicon dioxide to the aluminum oxide is 9.5-8: 1.
5. the production method according to claim 3, characterized in that: the molar ratio of the ethyl orthosilicate to the ethanol to the deionized water to the nitric acid is 1:4.5:2.5: 0.04.
6. the method of claim 4, wherein: the mole ratio of the silicon dioxide to the aluminum oxide is 9: 1.
7. use of a coating for improving the resistance of a pharmaceutical glass surface to cracking according to claim 1, characterized in that: the medicinal glass bottle conveyed by the caterpillar band is discharged from the annealing kiln and exposed in the air, and when the temperature is reduced to below 30 ℃, the coating solution is sprayed on the glass on line by a spraying pump, wherein the spraying thickness is 50-300 nanometers.
8. Use according to claim 7, wherein the coating thickness is 60-200 nm.
9. Use according to claim 8, characterized in that: the thickness of the coating is 60-150 nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010787741.4A CN111909550A (en) | 2020-08-07 | 2020-08-07 | Coating for improving cracking resistance of medicinal glass surface and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010787741.4A CN111909550A (en) | 2020-08-07 | 2020-08-07 | Coating for improving cracking resistance of medicinal glass surface and preparation method and application thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654348A (en) * | 2009-09-08 | 2010-02-24 | 武汉理工大学 | Preparation of high-temperature resistant hole sealing agent and hole sealing technique |
| CN107841164A (en) * | 2017-10-30 | 2018-03-27 | 上海艾谡新材料有限公司 | A kind of antireflective coated solution and preparation method and the production method of photovoltaic glass |
| CN108892979A (en) * | 2018-06-19 | 2018-11-27 | 张文霞 | One kind is for environment friendly heat resistant refractory coating and preparation method thereof |
-
2020
- 2020-08-07 CN CN202010787741.4A patent/CN111909550A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654348A (en) * | 2009-09-08 | 2010-02-24 | 武汉理工大学 | Preparation of high-temperature resistant hole sealing agent and hole sealing technique |
| CN107841164A (en) * | 2017-10-30 | 2018-03-27 | 上海艾谡新材料有限公司 | A kind of antireflective coated solution and preparation method and the production method of photovoltaic glass |
| CN108892979A (en) * | 2018-06-19 | 2018-11-27 | 张文霞 | One kind is for environment friendly heat resistant refractory coating and preparation method thereof |
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Application publication date: 20201110 |