CN111454567A - Preparation method for producing polyurethane imitation marble decorative material by using industrial saponified waste residue - Google Patents
Preparation method for producing polyurethane imitation marble decorative material by using industrial saponified waste residue Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3802—Low-molecular-weight compounds having heteroatoms other than oxygen having halogens
- C08G18/3814—Polyamines
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to a preparation method for preparing a polyurethane imitation marble decorative material by using industrial saponification waste residues, wherein high-molecular polyol is polyester polyol or polyether polyol, isocyanate, a chain extender is 3,3 '-dichloro-4, 4' -diaminodiphenylmethane, and a filler is industrial saponification waste residues. The manufacturing steps are as follows: (1) preparing a prepolymer; (2) preparing a chain extender component; (3) blending and molding at normal temperature; (4) and (5) post-curing process. The polyurethane elastomer is used as a main raw material of the marble-like decorative material, has the characteristic of difficult fracture, and solves the defects of easy crushing, difficult transportation and the like of the existing ceramic tile; meanwhile, the industrial saponification waste residue is utilized, and the industrial saponification waste residue can be added more under the condition of the same destructive power, so that the cost is saved, and the environmental protection is facilitated; the invention is poured at normal temperature, namely, the prepolymer component and the chain extender component are mixed and injected at normal temperature, thereby saving energy and reducing environmental pollution.
Description
Technical Field
The invention relates to a polyurethane imitation marble decorative material product made of industrial saponified waste residues and a preparation method thereof, belonging to the technical field of building decorative materials.
Background
The polyurethane marble-like material is rarely applied to the field of architectural decoration as a ceramic tile, and is mainly prepared by adding talcum powder serving as a filler into polyurethane resin, wherein the adding amount of the talcum powder is less, and the production cost is higher. The application amount of the ceramic tiles in the building field is large, the ceramic tiles are formed by sintering a large amount of clay, quartz sand and other natural resources at high temperature, fossil fuels such as coal and the like need to be consumed, the environment is polluted, and the ceramic tiles are easy to break and difficult to transport.
The industrial saponified waste residue is used as waste residue for producing the epoxypropane by chemical enterprises, so that the development of the enterprises is restricted, and the environment is also influenced. The utilization of industrial saponification waste residue is a problem to be solved urgently. The industrial saponified waste residue contains CaO and SiO2、MgO、Al2O3And the like, the components are complicated, the compatibility of the filler as a polyurethane imitation marble material in polyurethane resin is not ideal, and the filler is more difficult than adding talcum powder as a filler.
Disclosure of Invention
The invention provides a method for preparing a polyurethane marble-like decorative material by using industrial saponified waste residues, aiming at solving the problems of small addition amount of talcum powder filler and high cost of the existing polyurethane marble-like material, and the method is light in weight and easy to transport, and simultaneously utilizes the industrial saponified waste residues, thereby saving resources and reducing environmental pollution.
The technical scheme of the invention is as follows:
a preparation method for preparing a polyurethane marble-imitated decorative material by using industrial saponified waste residues comprises the following steps:
step (1) preparation of prepolymer:
heating the high molecular polyol with the molecular weight of 1000-;
step (2) preparation of chain extender components:
drying and grinding the filler to 200-600 meshes, heating the polymer polyol with the molecular weight of 1000-5000-;
the filler is industrial saponified waste residue;
the surface treating agent is 3-glycidol ether oxygen propyl trimethoxy silane surface treating agent;
and (3) normal-temperature blending and forming:
uniformly mixing the prepolymer prepared in the step (1) and the chain extender prepared in the step (2) at normal temperature according to the mass ratio of 100 (340-460) to obtain a mixed material;
quickly injecting the prepared mixed material into a mold, closing the mold, curing for 30-60 min in a normal-temperature environment, and demolding to obtain a casting-molded parison;
and (4) post-curing process:
and (4) placing the casting-molded parison prepared in the step (3) in an oven at 80 ℃ and then curing for 24 hours.
In the above technical solution, the polymer polyol in step (1) is polyester polyol or polyether polyol, the polyester polyol is polyester polyol with a functionality of 2, and the polyether polyol is polyether polyol with a functionality of 2-3.
In the above technical scheme, the isocyanate in step (1) is polyphenyl polymethylene isocyanate or modified diphenylmethane diisocyanate.
In the above technical scheme, the polymer polyol in step (2) is polyether polyol with functionality of 2-3.
In the technical scheme, the gel catalyst in the step (2) is dibutyltin dilaurate or stannous octoate.
The invention has the beneficial effects that:
the process of the invention comprises the reaction of hydroxyl in the high polymer polyol and isocyanate group in isocyanate to generate carbamate, wherein the high polymer polyol provides a soft segment phase, the isocyanate provides a hard segment phase, and the soft segment phase and the hard segment phase are orderly arranged. Meanwhile, the industrial saponified waste residue is utilized, so that the cost is saved, and the environmental protection is facilitated; the polyurethane prepolymer of the invention reacts at a temperature close to normal temperature (70-80 ℃), and the prepolymer component and the chain extender component can be mixed and injected at normal temperature, thereby saving energy and reducing environmental pollution. The addition of the surface treating agent can increase the addition amount of the industrial soaping slag by 5 percent under the condition of the same destructive power. The imitation marble material of the invention has light weight and the density of the imitation marble material is 1.4 to 1.6g/cm3The density of the common ceramic tile is 1.0-3.0g/cm3。
The main properties of the conventional tiles are compared with those of the imitation marble material in table 1.
TABLE 1 comparison of the main properties of ordinary tiles and imitation marble materials
Detailed Description
The first embodiment is as follows: heating polyether triol with the molecular weight of 5000 and the functionality of 3 to 120 ℃ for dehydration for 2h, cooling, adding polyphenyl polymethylene isocyanate (PAPI) to react for 2h in a reaction kettle at the temperature of 70-80 ℃ to generate polyurethane prepolymer with the NCO of 25%; drying and grinding filler industrial saponified waste residues to 200-600 meshes, heating polyether diol with the molecular weight of 2000 and the functionality of 2 to 120 ℃ for dehydration for later use, taking 107 g of dehydrated polyether diol and 54 g of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane (MOCA), melting the MOCA in the polyether diol at 100 ℃, adding 261 g of dried and ground industrial saponified waste residues, adding 0.8 g of dibutyltin dilaurate and 7.8 g of 3-glycidylethoxypropyltrimethoxysilane (KH560), and uniformly mixing to obtain a chain extender component; and uniformly mixing 100 g of polyurethane prepolymer and 431 g of chain extender component at normal temperature, pouring into a mold, closing the mold, curing at normal temperature for 30min, demolding, placing in an oven at 80 ℃ and curing for 24h to obtain the polyurethane marble-like product.
The indexes of the product obtained after post-curing are as follows: the thickness is less than 7.5mm, the average value of the failure strength is not less than 1000N, the water absorption rate is not more than 0.5 percent, and the breaking strength is not less than 15 MPa.
Example two: heating polyether triol with the molecular weight of 3000 and the functionality of 3 to 120 ℃ for dehydration for 2h, cooling, adding modified diphenylmethane diisocyanate (Hensman 2412) to react for 1h in a reaction kettle at the temperature of 70-80 ℃ to generate a polyurethane prepolymer with the NCO being 20%; drying and grinding industrial saponified waste residues of a filler to 200-600 meshes, heating polyether diol with the molecular weight of 2000 and the functionality of 2 to 120 ℃ for dehydration for later use, taking 91 g of dehydrated polyether diol and 43 g of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane (MOCA), melting the MOCA in the polyether diol at 100 ℃, adding 234 g of dried and ground industrial saponified waste residues, 0.7 g of stannous octoate and 7.3 g of 3-glycidoxy propyl trimethoxy silane (KH560), and uniformly mixing to obtain the chain extender component. And uniformly mixing 100 g of polyurethane prepolymer and 376 g of chain extender component at normal temperature, pouring into a mold, closing the mold, curing at normal temperature for 60min, demolding, placing in an oven at 80 ℃ and curing for 24h to obtain the polyurethane marble-like product.
The indexes of the product obtained after post-curing are as follows: the thickness is less than 7.5mm, the average value of the failure strength is not less than 1000N, the water absorption rate is not more than 0.5 percent, and the breaking strength is not less than 15 MPa.
Example three: heating polyether diol with the molecular weight of 1000 and the functionality of 2 to 120 ℃ for dehydration for 2h, cooling, adding polyphenyl polymethylene isocyanate (PAPI) to react for 2h in a reaction kettle at the temperature of 70-80 ℃ to generate a polyurethane prepolymer with the NCO being 15%; drying and grinding industrial saponified waste residues of a filler to 200-600 meshes, heating polyether triol with molecular weight of 3000 and functionality of 3 to 120 ℃ for dehydration for later use, taking 80 g of dehydrated polyether triol and 36 g of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane (MOCA), melting the MOCA in the polyether triol at 100 ℃, and adding 216 g of dried and ground industrial saponified waste residues, 0.6 g of stannous octoate and 6.5 g of 3-glycidyl ether oxypropyltrimethoxysilane (KH560) and uniformly mixing to serve as a chain extender component. And uniformly mixing 100 g of polyurethane prepolymer and 340 g of chain extender component at normal temperature, pouring into a mold, closing the mold, curing at normal temperature for 45min, demolding, placing in an oven at 80 ℃ and curing for 24h to obtain the polyurethane marble-like product.
The indexes of the product obtained after post-curing are as follows: the thickness is less than 7.5mm, the average value of the failure strength is not less than 1000N, the water absorption rate is not more than 0.5 percent, and the breaking strength is not less than 15 MPa.
Example four: heating polyester dihydric alcohol with the molecular weight of 2000 and the functionality of 2 to 120 ℃ for dehydration for 2h, cooling, adding polyphenyl polymethylene isocyanate (PAPI) to react for 2h in a reaction kettle at the temperature of 70-80 ℃ to generate a polyurethane prepolymer with the NCO being 20%; drying and grinding industrial saponified waste residues of a filler to 200-600 meshes, heating polyether triol with molecular weight of 5000 and functionality of 3 to 120 ℃ for dehydration for later use, taking 129 g of dehydrated polyether triol and 43 g of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane (MOCA), melting the MOCA in the polyether triol at 100 ℃, and adding 272 g of dried and ground industrial saponified waste residues, 0.8 g of dibutyltin dilaurate and 10.8 g of 3-glycidoxypropyltrimethoxysilane (KH560) to be uniformly mixed to serve as a chain extender component. And uniformly mixing 100 g of polyurethane prepolymer and 456 g of chain extender component at normal temperature, pouring into a mold, closing the mold, curing at normal temperature for 30min, demolding, placing in an oven at 80 ℃ and curing for 24h to obtain the polyurethane marble-like product.
The indexes of the product obtained after post-curing are as follows: the thickness is less than 7.5mm, the average value of the failure strength is not less than 1000N, the water absorption rate is not more than 0.5 percent, and the breaking strength is not less than 15 MPa.
Comparative example one: heating polyether triol with the molecular weight of 5000 and the functionality of 3 to 120 ℃ for dehydration for 2h, cooling, adding polyphenyl polymethylene isocyanate (PAPI) to react for 2h in a reaction kettle at the temperature of 70-80 ℃ to generate polyurethane prepolymer with the NCO of 25%; drying and grinding filler industrial saponified waste residues to 200-600 meshes, heating polyether diol with the molecular weight of 2000 and the functionality of 2 to 120 ℃ for dehydration for later use, melting 107 g of dehydrated polyether diol and 54 g of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane (MOCA) in 100 ℃ polyether diol, adding 213 g of dried and ground industrial saponified waste residues, and adding 0.6 g of dibutyltin dilaurate to be uniformly mixed to serve as a chain extender component. And uniformly mixing 100 g of polyurethane prepolymer and 293 g of chain extender component at normal temperature, pouring into a mold, closing the mold, curing at normal temperature for 30min, demolding, placing in an oven at 80 ℃ and curing for 24h to obtain the polyurethane marble-like product.
The indexes of the product obtained after post-curing are as follows: the thickness is less than 7.5mm, the average value of the failure strength is not less than 1000N, the water absorption rate is not more than 0.5 percent, and the breaking strength is not less than 15 MPa.
Claims (7)
1. A preparation method for preparing a polyurethane marble-like decorative material by using industrial saponified waste residues is characterized by comprising the following steps: the method comprises the following steps:
step (1) preparation of prepolymer:
heating the high molecular polyol with the molecular weight of 1000-;
step (2) preparation of chain extender components:
drying and grinding the filler to 200-600 meshes, heating the polymer polyol with the molecular weight of 1000-5000-;
the filler is industrial saponified waste residue;
the surface treating agent is 3-glycidol ether oxygen propyl trimethoxy silane surface treating agent;
and (3) normal-temperature blending and forming:
uniformly mixing the prepolymer prepared in the step (1) and the chain extender prepared in the step (2) at normal temperature according to the mass ratio of 100: 340-460 to obtain a mixed material;
injecting the prepared mixed material into a mold, closing the mold, curing for 30-60 min in a normal-temperature environment, and demolding to obtain a casting-molded parison;
and (4) post-curing process:
and (4) placing the casting-molded parison prepared in the step (3) in an oven at 80 ℃ and then curing for 24 hours to obtain the polyurethane imitation marble decorative material product.
2. The method for preparing the polyurethane imitation marble decorating material from the industrial saponified waste residue as claimed in claim 1, wherein the method comprises the following steps: the high molecular polyol in the step (1) is polyester polyol or polyether polyol.
3. The method for preparing the polyurethane imitation marble decorating material from the industrial saponified waste residue as claimed in claim 2, wherein the method comprises the following steps: the polyester polyol is polyester polyol with the functionality of 2.
4. The method for preparing the polyurethane imitation marble decorating material from the industrial saponified waste residue as claimed in claim 2, wherein the method comprises the following steps: the polyether polyol is polyether polyol with the functionality of 2-3.
5. The method for preparing the polyurethane imitation marble decorating material from the industrial saponified waste residue as claimed in claim 1, wherein the method comprises the following steps: the isocyanate in the step (1) is polyphenyl polymethylene isocyanate or modified diphenylmethane diisocyanate.
6. The method for preparing the polyurethane imitation marble decorating material from the industrial saponified waste residue as claimed in claim 1, wherein the method comprises the following steps: the high molecular polyol in the step (2) is polyether polyol with the functionality of 2-3.
7. The method for preparing the polyurethane imitation marble decorating material from the industrial saponified waste residue as claimed in claim 1, wherein the method comprises the following steps: and (3) the gel catalyst in the step (2) is dibutyltin dilaurate or stannous octoate.
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| CN113831492A (en) * | 2021-09-18 | 2021-12-24 | 北京九州一轨环境科技股份有限公司 | Preparation method of polyurethane elastomer for steel rail energy dissipation part, polyurethane elastomer and energy dissipation part |
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- 2020-04-16 CN CN202010297635.8A patent/CN111454567A/en active Pending
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|---|---|---|---|---|
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