CN117487346B - Wheel lining and preparation method thereof - Google Patents

Wheel lining and preparation method thereof Download PDF

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Publication number
CN117487346B
CN117487346B CN202311270054.5A CN202311270054A CN117487346B CN 117487346 B CN117487346 B CN 117487346B CN 202311270054 A CN202311270054 A CN 202311270054A CN 117487346 B CN117487346 B CN 117487346B
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scandium
porous silicon
microspheres
parts
temperature
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CN117487346A (en
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邓樱
朱杰
李在银
黄海滨
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Ningbo Fulong Synchronous Belt Co Ltd
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Ningbo Fulong Synchronous Belt Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06Polyamides derived from polyamines and polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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Abstract

The invention relates to a wheel lining and a preparation method thereof, wherein the wheel lining comprises the following components in parts by weight: 56-72 parts of polyamide resin, 21-36 parts of modified polyetherimide, 15-20 parts of silane activated silica micropowder, 3-7 parts of flame retardant, 2-6 parts of lubricant and 0.5-1.5 parts of antioxidant. The wheel lining material prepared by the invention has the advantages that the main material adopted by the wheel lining material is polyamide, namely nylon material, the auxiliary material is modified polyetherimide, the filler is silane activated silica micropowder, and in addition, the additives such as flame retardant, lubricant, antioxidant and the like are added.

Description

Wheel lining and preparation method thereof
Technical Field
The invention relates to the field of wheel linings, in particular to a wheel lining and a preparation method thereof.
Background
The lining plate is a special lining plate and is installed inside the head sheave of crane, etc. and has the main function of reducing friction between the head sheave and rope or steel cable and preventing the rope or steel cable from being worn and damaged. The different materials and properties directly affect the effect and service life of the crown block liner.
Materials commonly used for the crown block are cast iron, polyurethane, polyethylene, and the like. The cast iron is a common lining material for the crown block, has the characteristics of high hardness and good wear resistance, and can effectively protect the surface of the crown block from being damaged; however, cast iron has certain disadvantages such as easy generation of cracks and breakage, relatively short service life, etc. Polyurethane is a material with good wear resistance, elasticity and damping performance, can effectively reduce friction between the head sheave and a rope or a steel rope, and prolongs the service life of equipment; polyurethane gaskets are easy to age and deform under high-temperature environments, and have poor aging resistance. Polyethylene is a material with good light weight, wear resistance and chemical corrosion resistance, is suitable for some equipment with low requirements on the surface of the crown wheel, has low hardness and cannot bear excessive pressure and weight.
Besides good wear resistance and antifriction effect, the head sheave liner also needs to have the performances of compression resistance, temperature resistance, corrosion resistance and the like. The head sheave is subjected to significant pressure and wear during operation, so the cushion needs to be strong and stiff enough to support the entire system. Meanwhile, the head sheave gasket also needs to have good temperature resistance so as to adapt to the use requirements of extreme environments such as high temperature, low temperature and the like, and ensure the safe and stable operation of equipment. The material and performance of the crown block lining play a vital role in the safe operation of equipment such as a crane, and therefore, a material with high strength, good wear resistance, water resistance and strong temperature resistance is required for preparing the crown block, thereby prolonging the service life of the equipment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a wheel lining and a preparation method thereof.
The aim of the invention is realized by adopting the following technical scheme:
in a first aspect, the invention provides a wheel bushing, which comprises the following material components in parts by weight:
56-72 parts of polyamide resin, 21-36 parts of modified polyetherimide, 15-20 parts of silane activated silica micropowder, 3-7 parts of flame retardant, 2-6 parts of lubricant and 0.5-1.5 parts of antioxidant.
Preferably, the polyamide resin is PA66 (polyhexamethylene adipamide), and the brand is one of basf A3HG5 (25% glass fiber reinforced), A3HG6 (30% glass fiber reinforced), A3WG6 (30% glass fiber reinforced), and A3WG7 (35% glass fiber reinforced).
More preferably, the polyamide resin is PA66 german basf A3HG6 (30% glass fiber reinforced).
Preferably, the preparation process of the modified polyetherimide comprises the following steps:
mixing polyetherimide and N, N-dimethylacetamide in a reaction bottle, continuously stirring at 50-60 ℃ until the polyetherimide and the N, N-dimethylacetamide are dissolved, adding coated porous silicon carbide scandium microspheres, insulating and stirring for 1-3h, removing the solvent, and crushing to obtain modified polyetherimide; wherein the mass ratio of the polyetherimide to the coated porous silicon carbide scandium microsphere to the N, N-dimethylacetamide is 10:2.2-3.6:50-100.
More preferably, the polyetherimide has a density of 1.44g/cm 3, a melt flow rate of 4.2g/10min (227 ℃,6.6 kg), and a water absorption of less than or equal to 0.16% (24 h).
Preferably, the preparation method of the silane activated silica micropowder comprises the following steps:
Dispersing superfine silica powder with the particle size of 5-10 mu m in deionized water, adding a silane coupling agent KH-570, stirring for 2-6 hours at the temperature of 45-55 ℃ in a water bath, filtering to remove liquid, washing for three times, and drying in an oven at 80 ℃ to obtain silane activated silica powder; wherein the mass ratio of the superfine silica powder to the silane coupling agent to the deionized water is 1:0.1-0.3:10-30.
Preferably, the flame retardant is a phosphate flame retardant, comprising one or a combination of more of triphenyl phosphate, cresyl diphenyl phosphate and tricresyl phosphate.
Preferably, the lubricant is one or more of liquid paraffin, octadecanoamide, ethylene bis stearamide and microcrystalline paraffin.
Preferably, the antioxidant is one or a combination of more of antioxidant 1010, antioxidant 1076 and antioxidant 1098.
Preferably, the preparation method of the coated porous silicon carbide scandium microsphere comprises the following steps:
S1, preparing porous silicon carbide scandium microspheres:
Uniformly dispersing active carbon in scandium acetate aqueous solution, then dropwise adding tetraethyl silicate, heating for reaction, drying the product, and sintering in a muffle furnace to obtain porous silicon carbide scandium microspheres;
s2, preparing active porous silicon carbide scandium microspheres:
Firstly carrying out hydroxylation treatment on the porous silicon scandium carbide microspheres by using hydrogen peroxide, then mixing the porous silicon scandium carbide microspheres with an aqueous solution of gamma-aminopropyl triethoxysilane, and heating and stirring the mixture to obtain active porous silicon scandium carbide microspheres;
S3, composite coating:
And adding the active porous silicon scandium carbide microspheres into an organic solution of pyrrole-2-formaldehyde under the protection of gas, and heating to react under the action of acetic acid to obtain the coated porous silicon scandium carbide microspheres.
Preferably, the process for preparing the porous silicon carbide scandium microsphere in the step S1 comprises the following steps:
Scandium acetate and deionized water are weighed and mixed in a reaction bottle, after being stirred uniformly, active carbon is added, hydrochloric acid is added dropwise until the pH value of the solution is 3-4, and stirring and dispersing are carried out uniformly at room temperature, so that a solution A is formed; wherein the mass ratio of scandium acetate to active carbon to deionized water is 0.22-0.44:1:20-30, and the active carbon is granular active carbon with the grain diameter of 10-20 mu m;
Dissolving tetraethyl silicate in absolute ethyl alcohol to form a solution B; wherein the mass ratio of the tetraethyl silicate to the ethanol is 1:1.5-2.5;
Gradually dripping the solution B into the solution A, controlling the dripping speed to be 30-50 drops/min, heating to 50-70 ℃ after dripping, stirring for 2-3h, and drying the reaction product in an oven to constant weight to obtain a product to be sintered; wherein the mass ratio of the solution B to the solution A is 0.35-0.55:1;
And then placing the product to be sintered in a muffle furnace, introducing inert gas as shielding gas, heating to 920-1020 ℃ at the speed of 2-6 ℃/min, preserving heat for 3-5h, and naturally cooling along with the furnace to obtain the porous silicon carbide scandium microsphere.
Preferably, the process of preparing the active porous silicon scandium carbide microsphere in S2 includes:
mixing porous silicon scandium carbide microspheres with hydrogen peroxide solution in a reaction bottle, stirring in a water bath at 65-85 ℃ for 2-5h, naturally cooling to room temperature, filtering to remove liquid, washing with water for three times, and drying to obtain hydroxylated porous silicon scandium carbide microspheres; wherein, the mass concentration of the hydrogen peroxide solution is 20% -30%, and the mass ratio of the porous silicon scandium carbide microsphere to the hydrogen peroxide solution is 1:10-20;
mixing gamma-aminopropyl triethoxysilane and deionized water, stirring for dissolving, adding hydroxylated porous silicon scandium carbide microsphere, stirring at 45-55deg.C for 5-10 hr, filtering to remove liquid, washing with water for three times, and drying to obtain active porous silicon scandium carbide microsphere; wherein the mass ratio of the hydroxylated porous silicon carbide scandium microsphere to the gamma-aminopropyl triethoxysilane to the deionized water is 1:0.2-0.4:10-20.
Preferably, the process of the composite coating of S3 includes:
Mixing pyrrole-2-formaldehyde and N, N-dimethylacetamide in a reaction bottle, introducing nitrogen as a protective gas, stirring uniformly, gradually adding active porous silicon carbide scandium microspheres, stirring uniformly again, dripping acetic acid, heating to 100-120 ℃, stirring for reaction for 10-20h, naturally cooling to room temperature, filtering to remove liquid, washing with acetone for three times, and drying in an oven to constant weight to obtain coated porous silicon carbide scandium microspheres;
wherein the mass ratio of the active porous silicon carbide scandium microspheres to the pyrrole-2-formaldehyde to the N, N-dimethylacetamide is 1:0.19-0.38:10-20.
In a second aspect, the present invention provides a method for manufacturing a wheel lining, comprising:
Mixing polyamide resin and modified polyetherimide in a mixing mill, heating to 180-200 ℃, preserving heat and mixing for 10-30min, then cooling to 160-180 ℃, adding silane activated silica micropowder, lubricant and antioxidant, preserving heat and mixing for 5-10min, then transferring into a double screw extruder, extruding and granulating to obtain a wheel lining material, and performing die forming treatment to obtain a corresponding wheel lining; wherein, the temperature interval of twin-screw extruder includes: the temperature of the first area is 200-210 ℃, the temperature of the second area is 215-235 ℃, the temperature of the third area is 235-245 ℃, the temperature of the fourth area is 240-250 ℃, the temperature of the fifth area is 235-240 ℃, the temperature of the sixth area is 225-230 ℃, the temperature of the machine head is 230-240 ℃, the diameter of the screw rod is 45-55mm, and the length-diameter ratio of the screw rod is 30-35:1.
The beneficial effects of the invention are as follows:
1. The wheel lining material prepared by the invention has the advantages that the main material adopted by the wheel lining material is polyamide, namely nylon material, the auxiliary material is modified polyetherimide, the filler is silane activated silica micropowder, and in addition, the additives such as flame retardant, lubricant, antioxidant and the like are added.
2. Although the polyamide material has relatively high strength, the polyamide material has insufficient impact resistance, poor heat resistance, relatively poor dimensional stability and the like, so that the prepared product has short service life outdoors. In the invention, the modified polyetherimide is added as an auxiliary modified material, so that the performance of impact resistance, heat resistance stability and wear resistance of the polyurethane material is greatly improved, and in addition, the flame retardance is also improved to a certain extent, the addition of the flame retardant can be reduced, and the influence of the flame retardant on the performance of the polyamide material is reduced.
3. The modified polyetherimide is prepared by compounding polyetherimide with coated porous silicon carbide scandium microspheres. The coated porous silicon scandium carbide microsphere has the structure that porous silicon scandium carbide microsphere is used as a matrix, and the surface of the matrix is coated with a layer of Schiff base compound with activity containing pyrrole groups.
4. The porous silicon scandium carbide microsphere is a porous silicon scandium carbide microsphere containing scandium element, and is prepared by compounding scandium acetate serving as a scandium source, tetraethyl silicate serving as a silicon source and active carbon, and sintering at high temperature. Compared with the silicon carbide microspheres in the market, the porous silicon carbide scandium microspheres prepared by the invention have higher strength, wear resistance and chemical stability.
5. The preparation method of the active porous silicon scandium carbide microsphere comprises the steps of carrying out hydroxylation treatment on the porous silicon scandium carbide microsphere by hydrogen peroxide, and then carrying out treatment on the porous silicon scandium carbide microsphere by aminosilane to obtain the active porous silicon scandium carbide microsphere containing rich amino groups. The purpose of the reactive treatment microspheres is to enhance the surface activity of the microspheres on the one hand and to impart certain graftable groups to the microspheres on the other hand.
6. The aldehyde group on pyrrole-2-formaldehyde is combined with the amino group on the surface of the active porous silicon scandium carbide microsphere, and amine aldehyde is condensed to obtain the Schiff base compound containing imine characteristic groups, wherein the Schiff base compound is coated on the surface of the porous microsphere and is rich in pyrrole groups. The prepared coated porous silicon scandium carbide microsphere has enhanced activity, is beneficial to crosslinking with polyetherimide, and the Schiff base compound containing pyrrole groups on the surface of the microsphere can provide a certain degree of enhancement on the performance of the polyetherimide, such as strength, flame retardance and temperature resistance, so that the performance of the polyamide resin is greatly influenced after the coated porous silicon scandium carbide microsphere is finally compounded with the polyamide resin.
Drawings
The invention will be further described with reference to the accompanying drawings, in which embodiments do not constitute any limitation of the invention, and other drawings can be obtained by one of ordinary skill in the art without inventive effort from the following drawings.
FIG. 1 is a Scanning Electron Microscope (SEM) schematic view of coated porous scandium silicon carbide microspheres prepared according to example 1 of the present invention.
Detailed Description
The technical scheme of the invention is described below through specific examples. It is to be understood that the mention of one or more method steps of the present invention does not exclude the presence of other method steps before and after the combination step or that other method steps may be interposed between these explicitly mentioned steps; it should also be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the method steps is merely a convenient tool for identifying the method steps and is not intended to limit the order of arrangement of the method steps or to limit the scope of the invention in which the invention may be practiced, as such changes or modifications in their relative relationships may be regarded as within the scope of the invention without substantial modification to the technical matter.
In order to better understand the above technical solution, exemplary embodiments of the present invention are described in more detail below. While exemplary embodiments of the invention are shown, it should be understood that the invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The invention is further described with reference to the following examples.
Example 1
The wheel lining comprises the following material components in parts by weight:
64 parts of polyamide resin, 27 parts of modified polyetherimide, 18 parts of silane activated silica micropowder, 5 parts of flame retardant, 4 parts of lubricant and 1 part of antioxidant.
The polyamide resin was PA66 german basf A3HG6 (30% glass reinforcement).
The density of the polyetherimide is 1.44g/cm 3, the melt flow rate is 4.2g/10min (227 ℃,6.6 kg), and the water absorption rate is less than or equal to 0.16% (24 h).
The flame retardant is triphenyl phosphate. The lubricant is ethylene bis stearamide. The antioxidant is antioxidant 1010.
The preparation method of the silane activated silica micropowder comprises the following steps:
Dispersing superfine silica powder with the particle size of 5-10 mu m in deionized water, adding a silane coupling agent KH-570, stirring for 4 hours at the temperature of 50 ℃ in a water bath, filtering to remove liquid, washing for three times, and drying in an oven at 80 ℃ to obtain silane activated silica powder; wherein the mass ratio of the superfine silica powder to the silane coupling agent to the deionized water is 1:0.2:20.
The preparation process of the modified polyetherimide comprises the following steps:
Mixing polyetherimide and N, N-dimethylacetamide in a reaction bottle, continuously stirring at 55 ℃ until the polyetherimide and the N, N-dimethylacetamide are dissolved, adding coated porous silicon carbide scandium microspheres, insulating and stirring for 2 hours, removing the solvent, and crushing the mixture into particles of 300+/-50 mu m to obtain modified polyetherimide; wherein the mass ratio of the polyetherimide to the coated porous silicon carbide scandium microsphere to the N, N-dimethylacetamide is 10:2.8:75.
An SEM (scanning electron microscope) diagram of the coated porous silicon carbide scandium microsphere is shown in fig. 1, and the preparation method comprises the following steps:
S1, preparing porous silicon carbide scandium microspheres:
Scandium acetate and deionized water are weighed and mixed in a reaction bottle, after being stirred uniformly, active carbon is added, hydrochloric acid is added dropwise until the pH value of the solution is 3-4, and stirring and dispersing are carried out uniformly at room temperature, so that a solution A is formed; wherein the mass ratio of scandium acetate to active carbon to deionized water is 0.33:1:25, and the active carbon is granular active carbon with the particle size of 10-20 mu m; dissolving tetraethyl silicate in absolute ethyl alcohol to form a solution B; wherein the mass ratio of the tetraethyl silicate to the ethanol is 1:2; gradually dripping the solution B into the solution A, controlling the dripping speed to be 30-50 drops/min, heating to 60 ℃ after dripping, stirring for 2.5h, and drying the reaction product in an oven to constant weight to obtain a product to be sintered; wherein the mass ratio of the solution B to the solution A is 0.45:1; and then placing the product to be sintered in a muffle furnace, introducing inert gas as shielding gas, heating to 960 ℃ at the speed of 4 ℃/min, preserving heat for 4 hours, and naturally cooling along with the furnace to obtain the porous silicon carbide scandium microspheres.
S2, preparing active porous silicon carbide scandium microspheres:
mixing porous silicon scandium carbide microspheres with hydrogen peroxide solution in a reaction bottle, stirring in a water bath at 75 ℃ for 3 hours, naturally cooling to room temperature, filtering to remove liquid, washing with water for three times, and drying to obtain hydroxylated porous silicon scandium carbide microspheres; wherein the mass concentration of the hydrogen peroxide solution is 25%, and the mass ratio of the porous silicon carbide scandium microspheres to the hydrogen peroxide solution is 1:15;
Mixing and stirring gamma-aminopropyl triethoxysilane and deionized water for dissolution, adding hydroxylated porous silicon carbide scandium microspheres, stirring at 50 ℃ for 8 hours, filtering to remove liquid, washing with water for three times, and drying to obtain active porous silicon carbide scandium microspheres; wherein the mass ratio of the hydroxylated porous silicon carbide scandium microsphere, the gamma-aminopropyl triethoxysilane and the deionized water is 1:0.3:15.
S3, composite coating:
Mixing pyrrole-2-formaldehyde and N, N-dimethylacetamide in a reaction bottle, introducing nitrogen as a shielding gas, stirring uniformly, gradually adding active porous silicon carbide scandium microspheres, stirring uniformly again, dripping acetic acid, heating to 110 ℃, stirring for reaction for 15 hours, naturally cooling to room temperature, filtering to remove liquid, washing with acetone for three times, and drying in an oven to constant weight to obtain coated porous silicon carbide scandium microspheres; wherein the mass ratio of the active porous silicon carbide scandium microspheres to the pyrrole-2-formaldehyde to the N, N-dimethylacetamide is 1:0.28:15.
The preparation method of the wheel lining material comprises the following steps:
Mixing polyamide resin and modified polyetherimide in a mixing mill, heating to 190 ℃, preserving heat and mixing for 20min, then cooling to 170 ℃, adding silane activated silica micropowder, a lubricant and an antioxidant, preserving heat and mixing for 8min, transferring into a double-screw extruder, extruding and granulating to obtain a wheel lining material, and performing mold forming treatment to obtain a corresponding wheel lining; wherein, the temperature interval of twin-screw extruder includes: the temperature of the first region is 205 ℃, the temperature of the second region is 225 ℃, the temperature of the third region is 240 ℃, the temperature of the fourth region is 245 ℃, the temperature of the fifth region is 235 ℃, the temperature of the sixth region is 225 ℃, the temperature of the machine head is 235 ℃, the diameter of the screw rod is 50mm, and the length-diameter ratio of the screw rod is 30:1.
Example 2
The wheel lining comprises the following material components in parts by weight:
56 parts of polyamide resin, 36 parts of modified polyetherimide, 15 parts of silane activated silica micropowder, 3 parts of flame retardant, 6 parts of lubricant and 0.5 part of antioxidant.
The polyamide resin is PA66 (polyhexamethylene adipamide) with the brand name of Basoff A3HG5 (25% glass fiber reinforcement).
The preparation process of the modified polyetherimide comprises the following steps:
Mixing polyetherimide and N, N-dimethylacetamide in a reaction bottle, continuously stirring at 50 ℃ until the polyetherimide and the N, N-dimethylacetamide are dissolved, adding coated porous silicon carbide scandium microspheres, insulating and stirring for 1h, removing the solvent, and crushing to obtain modified polyetherimide; wherein the mass ratio of the polyetherimide to the coated porous silicon carbide scandium microsphere to the N, N-dimethylacetamide is 10:2.2:50.
The density of the polyetherimide is 1.44g/cm 3, the melt flow rate is 4.2g/10min (227 ℃,6.6 kg), and the water absorption rate is less than or equal to 0.16% (24 h).
The preparation method of the silane activated silica micropowder comprises the following steps:
Dispersing superfine silica powder with the particle size of 5-10 mu m in deionized water, adding a silane coupling agent KH-570, stirring for 2 hours at the temperature of 45 ℃ in a water bath, filtering to remove liquid, washing for three times, and drying in an oven at 80 ℃ to obtain silane activated silica powder; wherein the mass ratio of the superfine silica powder to the silane coupling agent to the deionized water is 1:0.1:10.
The flame retardant is toluene diphenyl phosphate. The lubricant is liquid paraffin. The antioxidant 1076.
The preparation method of the coated porous silicon carbide scandium microsphere comprises the following steps:
S1, preparing porous silicon carbide scandium microspheres:
Scandium acetate and deionized water are weighed and mixed in a reaction bottle, after being stirred uniformly, active carbon is added, hydrochloric acid is added dropwise until the pH value of the solution is 3-4, and stirring and dispersing are carried out uniformly at room temperature, so that a solution A is formed; wherein the mass ratio of scandium acetate to active carbon to deionized water is 0.22:1:20, and the active carbon is granular active carbon with the particle size of 10-20 mu m; dissolving tetraethyl silicate in absolute ethyl alcohol to form a solution B; wherein the mass ratio of the tetraethyl silicate to the ethanol is 1:1.5; gradually dripping the solution B into the solution A, controlling the dripping speed to be 30-50 drops/min, heating to 50 ℃ after dripping, stirring for 2 hours, and drying the reaction product in an oven to constant weight to obtain a product to be sintered; wherein the mass ratio of the solution B to the solution A is 0.35:1; and then placing the product to be sintered in a muffle furnace, introducing inert gas as shielding gas, heating to 920 ℃ at the speed of 2 ℃/min, preserving heat for 5 hours, and naturally cooling along with the furnace to obtain the porous silicon carbide scandium microspheres.
S2, preparing active porous silicon carbide scandium microspheres:
Mixing porous silicon scandium carbide microspheres with hydrogen peroxide solution in a reaction bottle, stirring in a water bath at 65 ℃ for 2 hours, naturally cooling to room temperature, filtering to remove liquid, washing with water for three times, and drying to obtain hydroxylated porous silicon scandium carbide microspheres; wherein the mass concentration of the hydrogen peroxide solution is 20%, and the mass ratio of the porous silicon carbide scandium microspheres to the hydrogen peroxide solution is 1:10;
Mixing and stirring gamma-aminopropyl triethoxysilane and deionized water for dissolution, adding hydroxylated porous silicon carbide scandium microspheres, stirring at 45 ℃ for 5 hours, filtering to remove liquid, washing with water for three times, and drying to obtain active porous silicon carbide scandium microspheres; wherein the mass ratio of the hydroxylated porous silicon carbide scandium microsphere, the gamma-aminopropyl triethoxysilane and the deionized water is 1:0.2:10.
S3, composite coating:
Mixing pyrrole-2-formaldehyde and N, N-dimethylacetamide in a reaction bottle, introducing nitrogen as a protective gas, stirring uniformly, gradually adding active porous silicon carbide scandium microspheres, stirring uniformly again, dripping acetic acid, heating to 100 ℃, stirring for reaction for 10 hours, naturally cooling to room temperature, filtering to remove liquid, washing with acetone for three times, and drying in an oven to constant weight to obtain coated porous silicon carbide scandium microspheres; wherein the mass ratio of the active porous silicon carbide scandium microspheres to the pyrrole-2-formaldehyde to the N, N-dimethylacetamide is 1:0.19:10.
The preparation method of the wheel lining material comprises the following steps:
Mixing polyamide resin and modified polyetherimide in a mixing mill, heating to 180 ℃, preserving heat and mixing for 10min, then cooling to 160 ℃, adding silane activated silica micropowder, a lubricant and an antioxidant, preserving heat and mixing for 5min, transferring into a double-screw extruder, extruding and granulating to obtain a wheel lining material, and performing mold forming treatment to obtain a corresponding wheel lining; wherein, the temperature interval of twin-screw extruder includes: the temperature of the first area is 200 ℃, the temperature of the second area is 215 ℃, the temperature of the third area is 235 ℃, the temperature of the fourth area is 240 ℃, the temperature of the fifth area is 235 ℃, the temperature of the sixth area is 225 ℃, the temperature of the machine head is 230 ℃, the diameter of the screw rod is 45mm, and the length-diameter ratio of the screw rod is 30:1.
Example 3
The wheel lining comprises the following material components in parts by weight:
72 parts of polyamide resin, 21 parts of modified polyetherimide, 20 parts of silane activated silica micropowder, 7 parts of flame retardant, 2 parts of lubricant and 1.5 parts of antioxidant.
The polyamide resin is PA66 (polyhexamethylene adipamide) with the brand name of Basoff A3WG6 (30% glass fiber reinforcement).
The preparation process of the modified polyetherimide comprises the following steps:
Mixing polyetherimide and N, N-dimethylacetamide in a reaction bottle, continuously stirring at 60 ℃ until the polyetherimide and the N, N-dimethylacetamide are dissolved, adding coated porous silicon carbide scandium microspheres, insulating and stirring for 3 hours, removing the solvent, and crushing to obtain modified polyetherimide; wherein the mass ratio of the polyetherimide to the coated porous silicon carbide scandium microsphere to the N, N-dimethylacetamide is 10:3.6:100.
The density of the polyetherimide is 1.44g/cm 3, the melt flow rate is 4.2g/10min (227 ℃,6.6 kg), and the water absorption rate is less than or equal to 0.16% (24 h).
The preparation method of the silane activated silica micropowder comprises the following steps:
Dispersing superfine silica powder with the particle size of 5-10 mu m in deionized water, adding a silane coupling agent KH-570, stirring for 6 hours at the temperature of 55 ℃ in a water bath, filtering to remove liquid, washing for three times, and drying in an oven at 80 ℃ to obtain silane activated silica powder; wherein the mass ratio of the superfine silica powder to the silane coupling agent to the deionized water is 1:0.3:30.
The flame retardant is tricresyl phosphate. The lubricant is octadecanoamide. The antioxidant is antioxidant 1098.
The preparation method of the coated porous silicon carbide scandium microsphere comprises the following steps:
S1, preparing porous silicon carbide scandium microspheres:
Scandium acetate and deionized water are weighed and mixed in a reaction bottle, after being stirred uniformly, active carbon is added, hydrochloric acid is added dropwise until the pH value of the solution is 3-4, and stirring and dispersing are carried out uniformly at room temperature, so that a solution A is formed; wherein the mass ratio of scandium acetate to active carbon to deionized water is 0.44:1:30, and the active carbon is granular active carbon with the particle size of 10-20 mu m; dissolving tetraethyl silicate in absolute ethyl alcohol to form a solution B; wherein the mass ratio of the tetraethyl silicate to the ethanol is 1:2.5; gradually dripping the solution B into the solution A, controlling the dripping speed to be 30-50 drops/min, heating to 70 ℃ after dripping, stirring for 3 hours, and drying the reaction product in an oven to constant weight to obtain a product to be sintered; wherein the mass ratio of the solution B to the solution A is 0.55:1; and then placing the product to be sintered in a muffle furnace, introducing inert gas as shielding gas, heating to 1020 ℃ at the speed of 6 ℃/min, preserving heat for 5 hours, and naturally cooling along with the furnace to obtain the porous silicon carbide scandium microspheres.
S2, preparing active porous silicon carbide scandium microspheres:
Mixing porous silicon scandium carbide microspheres with hydrogen peroxide solution in a reaction bottle, stirring in a water bath at 85 ℃ for 5 hours, naturally cooling to room temperature, filtering to remove liquid, washing with water for three times, and drying to obtain hydroxylated porous silicon scandium carbide microspheres; wherein the mass concentration of the hydrogen peroxide solution is 30%, and the mass ratio of the porous silicon carbide scandium microspheres to the hydrogen peroxide solution is 1:20;
Mixing and stirring gamma-aminopropyl triethoxysilane and deionized water for dissolution, adding hydroxylated porous silicon carbide scandium microspheres, stirring at 55 ℃ for 10 hours, filtering to remove liquid, washing with water for three times, and drying to obtain active porous silicon carbide scandium microspheres; wherein the mass ratio of the hydroxylated porous silicon carbide scandium microsphere, the gamma-aminopropyl triethoxysilane and the deionized water is 1:0.4:20.
S3, composite coating:
Mixing pyrrole-2-formaldehyde and N, N-dimethylacetamide in a reaction bottle, introducing nitrogen as a protective gas, stirring uniformly, gradually adding active porous silicon carbide scandium microspheres, stirring uniformly again, dripping acetic acid, heating to 120 ℃, stirring for reaction for 20 hours, naturally cooling to room temperature, filtering to remove liquid, washing with acetone for three times, and drying in an oven to constant weight to obtain coated porous silicon carbide scandium microspheres; wherein the mass ratio of the active porous silicon carbide scandium microspheres to the pyrrole-2-formaldehyde to the N, N-dimethylacetamide is 1:0.38:20.
The preparation method of the wheel lining material comprises the following steps:
Mixing polyamide resin and modified polyetherimide in a mixing mill, heating to 200 ℃, preserving heat and mixing for 30min, then cooling to 180 ℃, adding silane activated silica micropowder, a lubricant and an antioxidant, preserving heat and mixing for 10min, transferring into a double-screw extruder, extruding and granulating to obtain a wheel lining material, and performing mold forming treatment to obtain a corresponding wheel lining; wherein, the temperature interval of twin-screw extruder includes: the temperature of the first area is 210 ℃, the temperature of the second area is 235 ℃, the temperature of the third area is 245 ℃, the temperature of the fourth area is 250 ℃, the temperature of the fifth area is 240 ℃, the temperature of the sixth area is 230 ℃, the temperature of the machine head is 240 ℃, the diameter of the screw rod is 55mm, and the length-diameter ratio of the screw rod is 35:1.
Comparative example 1
A material for a wheel hub was prepared in the same manner as in example 1 except that the modified polyetherimide in the material was replaced with conventional polyetherimide having a density of 1.44g/cm 3, a melt flow rate of 4.2g/10min (227 ℃ C., 6.6 kg) and a water absorption of not more than 0.16% (24 hours) in the composition slightly different from that in example 1.
The material components of the wheel bushing in the comparative example are calculated according to parts by weight and comprise:
64 parts of polyamide resin, 27 parts of modified polyetherimide, 18 parts of silane activated silica micropowder, 5 parts of flame retardant, 4 parts of lubricant and 1 part of antioxidant.
Comparative example 2
A material for a wheel lining is prepared by the same method as in example 1, except that the composition is slightly different from that in example 1, the preparation method of modified polyetherimide is different, and the preparation process of the modified polyetherimide comprises the following steps:
Mixing polyetherimide and N, N-dimethylacetamide in a reaction bottle, continuously stirring at 55 ℃ until the polyetherimide and the N, N-dimethylacetamide are dissolved, adding silicon carbide microspheres (commercially available), insulating and stirring for 2 hours, removing the solvent, and crushing to obtain modified polyetherimide; wherein the mass ratio of the polyetherimide to the silicon carbide microsphere to the N, N-dimethylacetamide is 10:2.8:75.
The density of the polyetherimide is 1.44g/cm 3, the melt flow rate is 4.2g/10min (227 ℃,6.6 kg), and the water absorption rate is less than or equal to 0.16% (24 h).
The material components of the wheel bushing in the comparative example are calculated according to parts by weight and comprise:
64 parts of polyamide resin, 27 parts of modified polyetherimide, 18 parts of silane activated silica micropowder, 5 parts of flame retardant, 4 parts of lubricant and 1 part of antioxidant.
Comparative example 3
A wheel lining material was prepared in the same manner as in example 1, except that the composition was slightly different from that in example 1, and the modified polyetherimide was prepared in a different manner by substituting coated porous silicon carbide scandium microspheres with silicon carbide microspheres (commercially available).
The preparation process of the modified polyetherimide comprises the following steps:
Mixing polyetherimide and N, N-dimethylacetamide in a reaction bottle, continuously stirring at 55 ℃ until the polyetherimide and the N, N-dimethylacetamide are dissolved, adding pyrrole-2-formaldehyde and silicon carbide microspheres (commercially available), insulating and stirring for 2 hours, removing the solvent, and crushing to obtain modified polyetherimide; wherein the mass ratio of the polyetherimide to the pyrrole-2-formaldehyde to the silicon carbide microspheres to the N, N-dimethylacetamide is 10:0.78:2.8:75.
The density of the polyetherimide is 1.44g/cm 3, the melt flow rate is 4.2g/10min (227 ℃,6.6 kg), and the water absorption rate is less than or equal to 0.16% (24 h).
The material components of the wheel bushing in the comparative example are calculated according to parts by weight and comprise:
64 parts of polyamide resin, 27 parts of modified polyetherimide, 18 parts of silane activated silica micropowder, 5 parts of flame retardant, 4 parts of lubricant and 1 part of antioxidant.
Comparative example 4
The preparation method of the wheel lining material is the same as that of the example 1, the difference is that the component is slightly different from that of the example 1, the preparation method of the modified polyetherimide is different, and the coated porous silicon carbide scandium microsphere is replaced by a coated silicon carbide microsphere.
The preparation process of the modified polyetherimide comprises the following steps:
Mixing polyetherimide and N, N-dimethylacetamide in a reaction bottle, continuously stirring at 55 ℃ until the polyetherimide and the N, N-dimethylacetamide are dissolved, adding pyrrole-2-formaldehyde and coated silicon carbide microspheres, insulating and stirring for 2 hours, removing the solvent, and crushing to obtain modified polyetherimide; wherein the mass ratio of the polyetherimide to the pyrrole-2-formaldehyde to the coated silicon carbide microsphere to the N, N-dimethylacetamide is 10:0.78:2.8:75.
The density of the polyetherimide is 1.44g/cm 3, the melt flow rate is 4.2g/10min (227 ℃,6.6 kg), and the water absorption rate is less than or equal to 0.16% (24 h).
The preparation method of the coated silicon carbide microsphere comprises the following steps:
S1, preparing active silicon carbide microspheres:
Mixing silicon carbide microspheres (commercially available) with hydrogen peroxide solution in a reaction bottle, stirring in a water bath at 75 ℃ for 3 hours, naturally cooling to room temperature, filtering to remove liquid, washing with water for three times, and drying to obtain hydroxylated silicon carbide microspheres; wherein the mass concentration of the hydrogen peroxide solution is 25%, and the mass ratio of the silicon carbide microspheres to the hydrogen peroxide solution is 1:15;
Mixing gamma-aminopropyl triethoxysilane and deionized water, stirring for dissolving, adding hydroxylated silicon carbide microspheres, stirring at 50deg.C for 8 hr, filtering to remove liquid, washing with water for three times, and drying to obtain active silicon carbide microspheres; wherein the mass ratio of the hydroxylated silicon carbide microsphere, the gamma-aminopropyl triethoxysilane and the deionized water is 1:0.3:15.
S2, composite coating:
Mixing pyrrole-2-formaldehyde and N, N-dimethylacetamide in a reaction bottle, introducing nitrogen as a protective gas, stirring uniformly, gradually adding active silicon carbide microspheres, stirring uniformly again, dripping acetic acid, heating to 110 ℃, stirring for reaction for 15 hours, naturally cooling to room temperature, filtering to remove liquid, washing with acetone for three times, and drying in an oven to constant weight to obtain coated silicon carbide microspheres; wherein the mass ratio of the active silicon carbide microspheres to the pyrrole-2-formaldehyde to the N, N-dimethylacetamide is 1:0.28:15.
The material components of the wheel bushing in the comparative example are calculated according to parts by weight and comprise:
64 parts of polyamide resin, 27 parts of modified polyetherimide, 18 parts of silane activated silica micropowder, 5 parts of flame retardant, 4 parts of lubricant and 1 part of antioxidant.
Experimental example
The material properties of the wheel linings prepared in example 1 and comparative examples 1 to 4 were examined in relation.
The detecting content comprises the following steps: strength (tensile strength), toughness (notched impact strength), abrasion resistance (wear resistance), high and low temperature resistance, and flame retardancy (oxygen index).
Wherein, the detection of the tensile strength refers to GBT1040.5-2008 determination of plastic tensile property;
The detection of the notch impact strength refers to the determination of the impact property of a GB/T1043.1-2008 plastic simple support beam;
The detection of the abrasion loss is referred to GB/T3960-2016 plastic sliding friction abrasion test method, the temperature is 23+/-5 ℃, the humidity is 50+/-5%, the load is 196N, the time is 2h, and the rotation is 200 r/min;
the high temperature resistance is the temperature at which the deformation of the detection material reaches 0.01% at the corresponding temperature, and the low temperature resistance is the temperature at which the brittle failure of the detection material occurs at the corresponding temperature.
The oxygen index is measured by an oxygen index instrument with reference to the standard GB/T2406-93 test method for testing the burning performance of plastics oxygen index method.
The detection results are shown in the following table:
TABLE 1 Material Performance test results for different wheel linings
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms should not be understood as necessarily being directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Further, one skilled in the art can engage and combine the different embodiments or examples described in this specification.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (8)

1. The wheel lining is characterized by comprising the following material components in parts by weight:
56-72 parts of polyamide resin, 21-36 parts of modified polyetherimide, 15-20 parts of silane activated silica micropowder, 3-7 parts of flame retardant, 2-6 parts of lubricant and 0.5-1.5 parts of antioxidant;
The preparation process of the modified polyetherimide comprises the following steps:
mixing polyetherimide and N, N-dimethylacetamide in a reaction bottle, continuously stirring at 50-60 ℃ until the polyetherimide and the N, N-dimethylacetamide are dissolved, adding coated porous silicon carbide scandium microspheres, insulating and stirring for 1-3h, removing the solvent, and crushing to obtain modified polyetherimide; wherein the mass ratio of the polyetherimide to the coated porous silicon carbide scandium microsphere to the N, N-dimethylacetamide is 10:2.2-3.6:50-100;
The preparation method of the coated porous silicon carbide scandium microsphere comprises the following steps:
S1, preparing porous silicon carbide scandium microspheres:
Uniformly dispersing active carbon in scandium acetate aqueous solution, then dropwise adding tetraethyl silicate, heating for reaction, drying the product, and sintering in a muffle furnace to obtain porous silicon carbide scandium microspheres;
s2, preparing active porous silicon carbide scandium microspheres:
Firstly carrying out hydroxylation treatment on the porous silicon scandium carbide microspheres by using hydrogen peroxide, then mixing the porous silicon scandium carbide microspheres with an aqueous solution of gamma-aminopropyl triethoxysilane, and heating and stirring the mixture to obtain active porous silicon scandium carbide microspheres;
S3, composite coating:
And adding the active porous silicon scandium carbide microspheres into an organic solution of pyrrole-2-formaldehyde under the protection of gas, and heating to react under the action of acetic acid to obtain the coated porous silicon scandium carbide microspheres.
2. A wheel bushing according to claim 1, wherein the polyamide resin is PA66, and is one of the german basf A3HG5, A3HG6, A3WG 7.
3. The wheel bushing of claim 1, wherein the method of preparing the silane activated silica fume comprises:
Dispersing superfine silica powder with the particle size of 5-10 mu m in deionized water, adding a silane coupling agent KH-570, stirring for 2-6 hours at the temperature of 45-55 ℃ in a water bath, filtering to remove liquid, washing for three times, and drying in an oven at 80 ℃ to obtain silane activated silica powder; wherein the mass ratio of the superfine silica powder to the silane coupling agent to the deionized water is 1:0.1-0.3:10-30.
4. A wheel bushing as in claim 1, wherein the flame retardant is a phosphate flame retardant comprising one or more combinations of triphenyl phosphate, cresyl diphenyl phosphate, tricresyl phosphate.
5. A wheel bushing according to claim 1, wherein the lubricant is one or more of liquid paraffin, octadecanoamide, ethylenebisstearamide, microcrystalline paraffin.
6. The wheel bushing of claim 1, wherein the antioxidant is one or a combination of antioxidants 1010, 1076, 1098.
7. A method of making a wheel bushing as defined in claim 1, comprising:
Mixing polyamide resin and modified polyetherimide in a mixing mill, heating to 180-200 ℃, preserving heat and mixing for 10-30min, then cooling to 160-180 ℃, adding silane activated silica powder, a lubricant and an antioxidant, preserving heat and mixing for 5-10min, then transferring into a double screw extruder, extruding and granulating to obtain a wheel lining material, and performing die forming treatment to obtain a corresponding wheel lining.
8. The method of claim 7, wherein the temperature interval of the twin screw extruder comprises: the temperature of the first area is 200-210 ℃, the temperature of the second area is 215-235 ℃, the temperature of the third area is 235-245 ℃, the temperature of the fourth area is 240-250 ℃, the temperature of the fifth area is 235-240 ℃, the temperature of the sixth area is 225-230 ℃, the temperature of the machine head is 230-240 ℃, the diameter of the screw rod is 45-55mm, and the length-diameter ratio of the screw rod is 30-35:1.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104379651A (en) * 2012-05-24 2015-02-25 沙特基础创新塑料Ip私人有限责任公司 Improved flame retardant polymer compositions

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