CN110981254A - Coagulation accelerating early strength agent suitable for cement-based 3D printing material and preparation method thereof - Google Patents
Coagulation accelerating early strength agent suitable for cement-based 3D printing material and preparation method thereof Download PDFInfo
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- CN110981254A CN110981254A CN201911358345.3A CN201911358345A CN110981254A CN 110981254 A CN110981254 A CN 110981254A CN 201911358345 A CN201911358345 A CN 201911358345A CN 110981254 A CN110981254 A CN 110981254A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1051—Organo-metallic compounds; Organo-silicon compounds, e.g. bentone
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/08—Acids or salts thereof
- C04B22/12—Acids or salts thereof containing halogen in the anion
- C04B22/126—Fluorine compounds, e.g. silico-fluorine compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to a set accelerating early strength agent suitable for a cement-based 3D printing material and a preparation method thereof, wherein the set accelerating early strength agent comprises the following raw materials: consists of calcium fluoroaluminate and organic matter coated on the surface of the calcium fluoroaluminate. The organic matter is composed of urea-formaldehyde resin, polyoxyethylene, polyethylene glycol and a silane coupling agent. The coagulation accelerator early strength agent can control the setting time of the cement-based material and greatly improve the hourly strength.
Description
Technical Field
The invention relates to the technical field of cement-based 3D printing materials, in particular to a set accelerating early strength agent suitable for a cement-based 3D printing material and a preparation method thereof.
Background
3D printing is an emerging technology in the manufacturing industry that is rapidly developing, called "manufacturing technology of industrial revolutionary significance". The 3D printing technology is a popular name, belongs to rapid prototyping from the aspect of a prototyping method, and is essentially additive manufacturing technology. The american society for materials and testing defines the 3D printing technique as: based on the 3D model data, the process of producing the object in a layer-by-layer superposition mode opposite to the material reduction technology is adopted, materials are usually superposed layer by layer under the control of a computer, and finally, a three-dimensional model on the computer is changed into a three-dimensional object.
The 3D printing technology of the cement-based material is to extrude the cement-based material through equipment, and the material is extruded by a printer according to a preset graph and stacked layer by layer to be printed under the control of computer three-dimensional software, so that the desired building rear component is obtained. Compared with the prior art, 3D printing can realize the die-free molding of the cement-based material, and labor cost and die cost are saved. Meanwhile, the building is carried out by means of a computer and a 3D printer, so that the building speed can be greatly increased, and the building period can be shortened.
According to the technical characteristics of 3D printing, new requirements are put forward on the cement-based material. Especially in terms of setting time and hourly intensity. Controllable setting time is convenient for 3D and prints quick shaping, improves and prints efficiency. Sufficient hour strength to prevent the cement-based material from collapsing during the stacking process. GB 175-2007 general portland cement stipulates that the initial setting time of portland cement is not less than 45min, and the final setting time is not more than 390 min. The initial setting time of ordinary portland cement, portland slag cement, pozzolanic portland cement, portland fly ash cement and composite portland cement is not less than 45min, and the final setting time is not more than 600 min. The 1D compressive strength of the common Portland cement P.O42.5 cement is only 7-10 MPa, so that the requirement of 3D printing cannot be met by using the Portland cement alone. This aspect limits the application of portland cement to 3D printing technology, and also increases the manufacturing cost of 3D printing of cement-based materials.
In order to make cement-based materials suitable for 3D printing technology, the skilled person in the art has made different attempts to achieve controllable setting time and improved hourly intensity of cement-based materials, and has achieved a series of results. CN106007587 discloses 3D printing mortar, which adopts quick-hardening sulphoaluminate cement, portland cement and aluminate cement to compound to improve the hourly strength of the mortar, and adopts anhydrous lithium chloride, anhydrous calcium chloride or anhydrous calcium chloride as a coagulant. However, improper compounding of aluminate cement with portland cement can result in abnormal setting, reduced strength, and volume stability problems. The use of chloride as an accelerator also has disadvantages in the durability of the cement-based material. CN105801023 discloses a cement-based ready-mixed dry-mixed mortar for 3D printing. The early strength accelerator is adopted to shorten the setting time of concrete, improve the early strength and shorten the initial setting time of mortar by 1 hour. However, this protocol does not disclose the specific ingredients of the set accelerating early strength agent used. However, an initial setting time of 1 hour is too long for 3D printing technology, which greatly reduces the working efficiency of the 3D printer. CN104891891 discloses a 3D printing cement-based material. Sodium aluminate, sodium silicate, sodium metasilicate, calcium formate and calcium chloride are used as early strength agents, and sodium carbonate, sodium aluminate, citric acid and the like are used as pour point regulators. Adding too much sodium salt to the cement-based material increases the risk of alkali-aggregate reactions occurring, which is detrimental to the durability of the cement-based material. Patent CN105384416 discloses a two-component cement-based composite material for 3D printing and a preparation method thereof, wherein a material a and a material B are mixed in a printer and then directly extruded and stacked. Wherein the material A consists of 34 to 40 percent of sulphoaluminate cement, 0 to 6 percent of inorganic powder, 40 to 44 percent of tailing-making sand, 2.5 to 3 percent of high molecular polymer, 12 to 13.4 percent of blending water, retarder, water reducer, stabilizer, defoamer and other chemical additives, and the material B consists of 2 to 3 percent of coagulation accelerator, 3 to 4 percent of thixotropic agent, 1 to 1.5 percent of defoamer and 94 to 91.5 percent of blending water. The two-component 3D printing cement-based material is required to be rapidly extruded and molded after being mixed in the printer, the technological processes of pre-mixing, pipeline conveying and the like cannot be realized, the requirement on printing equipment is high, and the application range is limited. In addition, the setting speed is too high, so that the interlayer bonding strength is too low in the stacking process. CN106830843 discloses a cement-based composite material suitable for 3D printing rapid prototyping process. The strengthening index is prepared by grinding activated anhydrous calcium sulphoaluminate and gypsum according to a certain proportion, and the liquid coagulation accelerating component is prepared by dissolving aluminum sulfate and diethanol amine according to a certain proportion in water. However, the liquid coagulation-accelerating component is added at the extrusion port, and the cement-based material is ensured to be mixed with the liquid coagulation-accelerating component, which puts high requirements on 3D printing equipment, and the process is relatively complex.
Calcium fluoroaluminate is an early-strength mineral and has the characteristics of high hydration speed, high condensation time, high hour strength and the like. Based on the characteristics of calcium fluoroaluminate, the calcium fluoroaluminate is generally used as super early strength cement and spray cement. The calcium fluoroaluminate has the characteristics of high hydration speed and high setting time, and is not suitable to be used as a set accelerating early strength agent for 3D printing of cement-based materials.
The surface coating technique is the most common surface modification technique in which a layer of organic or inorganic substance is coated on the surface of particles by physical or chemical means. The ball milling method belongs to a physical method particle surface coating technology. The analysis of the existing literature shows that the organic surface modified calcium fluoroaluminate serving as the set accelerating early strength agent for 3D printing of the cement-based material is not reported.
Disclosure of Invention
The invention aims to provide a set accelerating early strength agent suitable for a cement-based 3D printing material and a preparation method thereof. The single use of Portland cement cannot meet the requirements of 3D printing on controllable setting time and high hourly strength of cement-based materials. The setting time and the hourly strength of the cement-based material are regulated by adding an accelerating early strength agent.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention discloses a set accelerating early strength agent suitable for a cement-based 3D printing material, which comprises the following raw materials: consists of calcium fluoroaluminate and organic matter coated on the surface of the calcium fluoroaluminate.
Further, the organic matter comprises a water-soluble organic matter, a silane coupling agent and a swelling organic matter.
Furthermore, the organic matter of the invention is composed of urea-formaldehyde resin, polyoxyethylene, polyethylene glycol and silane coupling agent.
Furthermore, the urea resin is powdery, the average molecular weight is 1-2 ten thousand, and the fineness is 40-100 meshes.
Further, the polyoxyethylene is powdery, the average molecular weight is 80-100 ten thousand, and the fineness is 40-80 meshes.
Further, the polyethylene glycol is powdery, the average molecular weight is 1-2 ten thousand, and the fineness is 40-80 meshes.
Further, the silane coupling agent is powdery, and the fineness of the silane coupling agent is 40-100 meshes.
Further, the coagulation-accelerating early strength agent comprises the following raw materials in percentage by mass: 100 parts of calcium fluoroaluminate, 30-40 parts of urea-formaldehyde resin, 24-36 parts of polyethylene oxide, 8-16 parts of polyethylene glycol and 12-18 parts of silane coupling agent.
The preparation method of the cement-based 3D printing material by using the set accelerating early strength agent comprises the following steps:
(1) weighing 30-40 parts of urea-formaldehyde resin, 24-36 parts of polyethylene oxide, 8-16 parts of polyethylene glycol and 12-18 parts of silane coupling agent according to parts by mass, and uniformly mixing and stirring in a mixer;
(2) weighing 100 parts by mass of calcium fluoroaluminate, pouring the calcium fluoroaluminate into a ball mill, pouring the uniformly stirred material obtained in the step (1) into the ball mill, starting the ball mill, and carrying out ball milling on the material, wherein the ball milling time is controlled to be 1-2 h;
(3) and sieving the ball-milled materials by a 100-mesh sieve to obtain powdery materials with the particle size of less than 100 meshes, namely the coagulation accelerating early strength agent.
The application method of the coagulation accelerator early strength agent comprises the steps of directly adding the coagulation accelerator early strength agent into a cement-based material, adding water, and uniformly stirring for later use; the coagulation accelerating early strength agent doped into the cement-based material accounts for 4-6% of the mass of the cement-based material.
After the calcium fluoroaluminate with the surface modified by the organic matter is mixed with cement mortar and water, the organic matter on the surface of the calcium fluoroaluminate is slowly dissolved, and the cement mortar has good workability in the process. After the dissolution is finished, the calcium fluoroaluminate is contacted with water to generate hydration reaction, so that the cement mortar is rapidly solidified and hardened.
Because calcium fluoroaluminate is hydrated when meeting water. The ball milling method is adopted and the organic matter is solid, so that the contact between calcium fluoroaluminate and water is avoided. The urea-formaldehyde resin swells when meeting water, polyoxyethylene and polyethylene glycol are water-soluble organic matters, and the working performance of the cement-based material can be improved when the urea-formaldehyde resin is added into the cement-based material. The silane coupling agent can enhance the coating capability of organic matters and calcium fluoroaluminate.
The invention has the beneficial effects that: 1) the coagulation accelerator early strength agent can control the initial setting time of a cement-based material to be between 20min and 30min, and the final setting time to be between 30min and 40 min. The 1.5h compressive strength is not lower than 1.5MPa, and the 3h compressive strength is not lower than 3 MPa; the 1d strength is not lower than 20 MPa. 2) The later strength is not lost, the 28-day compressive strength ratio is more than 100 percent, and the 90d compressive strength retention rate is more than 100 percent. 3) The cement-based material is convenient to use, and can be directly added into the cement-based material, added with water and uniformly stirred for later use. 4) The mixing amount is low, and the effect can be achieved by mixing 4-6% of the cement.
Detailed Description
The invention is further described with reference to specific examples.
The invention discloses a set accelerating early strength agent suitable for a cement-based 3D printing material, which comprises the following raw materials: consists of calcium fluoroaluminate and organic matter coated on the surface of the calcium fluoroaluminate.
Further, the organic matter comprises a water-soluble organic matter, a silane coupling agent and a swelling organic matter.
Furthermore, the organic matter of the invention is composed of urea-formaldehyde resin, polyoxyethylene, polyethylene glycol and silane coupling agent.
Furthermore, the urea resin is powdery, the average molecular weight is 1-2 ten thousand, and the fineness is 40-100 meshes.
Further, the polyoxyethylene is powdery, the average molecular weight is 80-100 ten thousand, and the fineness is 40-80 meshes.
Further, the polyethylene glycol is powdery, the average molecular weight is 1-2 ten thousand, and the fineness is 40-80 meshes.
Further, the silane coupling agent is powdery, and the fineness of the silane coupling agent is 40-100 meshes.
Further, the coagulation-accelerating early strength agent comprises the following raw materials in percentage by mass: 100 parts of calcium fluoroaluminate, 30-40 parts of urea-formaldehyde resin, 24-36 parts of polyethylene oxide, 8-16 parts of polyethylene glycol and 12-18 parts of silane coupling agent.
The preparation method of the cement-based 3D printing material by using the set accelerating early strength agent comprises the following steps:
(1) weighing 30-40 parts of urea-formaldehyde resin, 24-36 parts of polyethylene oxide, 8-16 parts of polyethylene glycol and 12-18 parts of silane coupling agent according to parts by mass, and uniformly mixing and stirring in a mixer;
(2) weighing 100 parts by mass of calcium fluoroaluminate, pouring the calcium fluoroaluminate into a ball mill, pouring the uniformly stirred material obtained in the step (1) into the ball mill, starting the ball mill, and carrying out ball milling on the material, wherein the ball milling time is controlled to be 1-2 h;
(3) and sieving the ball-milled materials by a 100-mesh sieve to obtain powdery materials with the particle size of less than 100 meshes, namely the coagulation accelerating early strength agent.
The application method of the coagulation accelerator early strength agent comprises the steps of directly adding the coagulation accelerator early strength agent into a cement-based material, adding water, and uniformly stirring for later use; the coagulation accelerating early strength agent doped into the cement-based material accounts for 4-6% of the mass of the cement-based material.
Example 1
(1) According to the mass parts, 40 parts of urea-formaldehyde resin with the average molecular weight of 1 ten thousand and the fineness of 40 meshes, 24 parts of polyoxyethylene with the average molecular weight of 90 ten thousand and the fineness of 80 meshes, 16 parts of polyethylene glycol with the average molecular weight of 2 ten thousand and the fineness of 60 meshes and 12 parts of silane coupling agent powder with the fineness of 100 meshes are weighed and put into a mixer to be mixed and stirred uniformly.
(2) Weighing 100 parts by mass of calcium fluoroaluminate, pouring into a ball mill, pouring the uniformly stirred material obtained in the step (1) into the ball mill, starting the ball mill, and carrying out ball milling on the material, wherein the ball milling time is controlled to be 1 h.
(3) And sieving the ball-milled materials by a 100-mesh sieve to obtain powdery materials with the particle size of less than 100 meshes, namely the coagulation accelerating early strength agent.
Example 2
(1) According to the mass parts, 35 parts of urea-formaldehyde resin with the average molecular weight of 2 ten thousand and the fineness of 100 meshes, 36 parts of polyethylene oxide with the average molecular weight of 80 ten thousand and the fineness of 40 meshes, 10 parts of polyethylene glycol with the average molecular weight of 1.5 ten thousand and the fineness of 80 meshes and 18 parts of silane coupling agent powder with the fineness of 60 meshes are weighed and put into a mixer to be mixed and stirred uniformly.
(2) Weighing 100 parts by mass of calcium fluoroaluminate, pouring into a ball mill, pouring the uniformly stirred material obtained in the step (1) into the ball mill, starting the ball mill, and carrying out ball milling on the material, wherein the ball milling time is controlled to be 2 hours.
(3) And sieving the ball-milled materials by a 100-mesh sieve to obtain powdery materials with the particle size of less than 100 meshes, namely the coagulation accelerating early strength agent.
Example 3
(1) According to the mass parts, 30 parts of urea-formaldehyde resin with the average molecular weight of 1.5 ten thousand and the fineness of 80 meshes, 30 parts of polyoxyethylene with the average molecular weight of 100 ten thousand and the fineness of 60 meshes, 8 parts of polyethylene glycol with the average molecular weight of 1 ten thousand and the fineness of 40 meshes and 16 parts of silane coupling agent powder with the fineness of 40 meshes are weighed and put into a mixer to be mixed and stirred uniformly.
(2) Weighing 100 parts by mass of calcium fluoroaluminate, pouring into a ball mill, pouring the uniformly stirred material obtained in the step (1) into the ball mill, starting the ball mill, and carrying out ball milling on the material, wherein the ball milling time is controlled to be 1.5 h.
(3) And sieving the ball-milled materials by a 100-mesh sieve to obtain powdery materials with the particle size of less than 100 meshes, namely the coagulation accelerating early strength agent.
Example 4
(1) According to the mass parts, 36 parts of urea-formaldehyde resin with the average molecular weight of 1 ten thousand and the fineness of 60 meshes, 28 parts of polyoxyethylene with the average molecular weight of 80 ten thousand and the fineness of 60 meshes, 12 parts of polyethylene glycol with the average molecular weight of 1.5 ten thousand and the fineness of 80 meshes and 18 parts of silane coupling agent powder with the fineness of 100 meshes are weighed and put into a mixer to be mixed and stirred uniformly.
(2) Weighing 100 parts by mass of calcium fluoroaluminate, pouring into a ball mill, pouring the uniformly stirred material obtained in the step (1) into the ball mill, starting the ball mill, and carrying out ball milling on the material, wherein the ball milling time is controlled to be 2 hours.
(3) And sieving the ball-milled materials by a 100-mesh sieve to obtain powdery materials with the particle size of less than 100 meshes, namely the coagulation accelerating early strength agent.
Test examples
According to published data, a 3D printing cement-based mortar is designed to be used as a test proportion for testing the set accelerating early strength agent, and the concrete materials comprise: P.O 42.5.5 parts of cement; 160 parts of fine aggregate with the maximum particle size of 4.75mm and the fineness modulus of 2.5; 0.8 part of polycarboxylic acid water reducing agent with solid content of 20 percent; 40 parts of mixing water; 0.5 part of thickening agent. The prepared set accelerating early strength agent is added into cement mortar according to 4-6% of the mass of the cement, and the setting time and the compressive strength of the mortar at each age are tested. Cement mortar without the addition of the set accelerating early strength agent is taken as a blank example. The test results are shown in table 1:
TABLE 1 mortar setting time and compressive strength
According to test results, the early strength accelerator can control the initial setting time of a cement-based material to be between 20 and 30min and the final setting time to be between 30 and 40 min. The compressive strength is not less than 1.5MPa after 1.5h, and not less than 3MPa after 3 h. The 1d strength is not lower than 20 MPa. The later strength is not lost, the 28-day compressive strength ratio is more than 100 percent, and the 90d compressive strength retention rate is more than 100 percent.
The above description is only a part of specific embodiments of the present invention (since the present invention belongs to the numerical range, the embodiments are not exhaustive, and the protection scope of the present invention is defined by the numerical range of the present invention and other technical essential ranges), and the detailed contents or common general knowledge known in the schemes are not described too much. It should be noted that the above-mentioned embodiments do not limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation for those skilled in the art are within the protection scope of the present invention. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. The coagulation accelerator early strength agent is suitable for a cement-based 3D printing material and is characterized by comprising the following raw materials: consists of calcium fluoroaluminate and organic matter coated on the surface of the calcium fluoroaluminate.
2. The set accelerating early strength agent for cement-based 3D printing material as claimed in claim 1, wherein the organic substance comprises water soluble organic substance, silane coupling agent, swelling organic substance.
3. The set accelerating early strength agent for cement-based 3D printing material as claimed in claim 1, wherein the organic substance is composed of urea formaldehyde resin, polyethylene oxide, polyethylene glycol and silane coupling agent.
4. The set accelerating early strength agent applicable to the cement-based 3D printing material as claimed in claim 3, wherein the urea-formaldehyde resin is in a powder form, the average molecular weight is 1-2 ten thousand, and the fineness is 40-100 meshes.
5. The set accelerating early strength agent applicable to the cement-based 3D printing material as claimed in claim 3, wherein the polyethylene oxide is in a powder form, the average molecular weight is 80-100 ten thousand, and the fineness is 40-80 meshes.
6. The set accelerating early strength agent applicable to the cement-based 3D printing material as claimed in claim 3, wherein the polyethylene glycol is in a powder form, the average molecular weight is 1 ten thousand to 2 ten thousand, and the fineness is 40-80 meshes.
7. The set accelerating early strength agent suitable for the cement-based 3D printing material as claimed in claim 3, wherein the silane coupling agent is in a powder form, and the fineness is 40-100 meshes.
8. The set accelerating early strength agent for the cement-based 3D printing material according to claim 3, wherein the set accelerating early strength agent is prepared from the following raw materials in mass: 100 parts of calcium fluoroaluminate, 30-40 parts of urea-formaldehyde resin, 24-36 parts of polyethylene oxide, 8-16 parts of polyethylene glycol and 12-18 parts of silane coupling agent.
9. The preparation method of the early strength accelerator for cement-based 3D printing material, which is carried out by using the early strength accelerator for accelerating setting as claimed in claim 3, is characterized by comprising the following steps:
(1) weighing 30-40 parts of urea-formaldehyde resin, 24-36 parts of polyethylene oxide, 8-16 parts of polyethylene glycol and 12-18 parts of silane coupling agent according to parts by mass, and uniformly mixing and stirring in a mixer;
(2) weighing 100 parts by mass of calcium fluoroaluminate, pouring the calcium fluoroaluminate into a ball mill, pouring the uniformly stirred material obtained in the step (1) into the ball mill, starting the ball mill, and carrying out ball milling on the material, wherein the ball milling time is controlled to be 1-2 h;
(3) and sieving the ball-milled materials by a 100-mesh sieve to obtain powdery materials with the particle size of less than 100 meshes, namely the coagulation accelerating early strength agent.
10. The use method of the set accelerating early strength agent as claimed in claim 3, wherein the use method is that the set accelerating early strength agent is directly added into the cement-based material, added with water and stirred evenly for standby; the coagulation accelerating early strength agent doped into the cement-based material accounts for 4-6% of the mass of the cement-based material.
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| CN114436578A (en) * | 2022-03-04 | 2022-05-06 | 东南大学 | Controlled-release quick-setting functional particles and application thereof in 3D printing of cement-based materials |
| CN115594469A (en) * | 2022-09-14 | 2023-01-13 | 泰州职业技术学院（Cn） | Low-drying-shrinkage 3D printing concrete and preparation method thereof |
| CN116119976A (en) * | 2023-04-04 | 2023-05-16 | 石家庄市长安育才建材有限公司 | High-adsorption water reducer, preparation method thereof and concrete |
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| CN110981254B (en) | 2022-02-22 |
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