CN113084695B - Buffering polishing pad for fine polishing of electronic display screen and production method thereof - Google Patents
Buffering polishing pad for fine polishing of electronic display screen and production method thereof Download PDFInfo
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- CN113084695B CN113084695B CN202110270650.8A CN202110270650A CN113084695B CN 113084695 B CN113084695 B CN 113084695B CN 202110270650 A CN202110270650 A CN 202110270650A CN 113084695 B CN113084695 B CN 113084695B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
- B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
- B24B37/22—Lapping pads for working plane surfaces characterised by a multi-layered structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
Abstract
The invention discloses a buffering polishing pad for fine polishing of an electronic display screen, which consists of a polishing layer and a buffer layer; the buffering polishing pad for fine polishing of the electronic display screen is prepared by the following steps: firstly, putting a polyester non-woven fabric into polyurethane impregnation liquid, taking out the polyester non-woven fabric under the extrusion of a metal roller, and removing redundant impregnation liquid on the surface to obtain the impregnated non-woven fabric; secondly, putting the soaked non-woven fabric into a water tank with 20 mass percent of N, N-dimethylformamide aqueous solution for 20min to obtain a polishing layer; and thirdly, casting the buffer layer precast liquid onto the polishing layer, gelatinizing for 10-60min at the temperature of 60-80 ℃, and curing for 5-8h in a constant temperature box at the temperature of 100-160 ℃ to obtain the buffer polishing pad for fine polishing of the electronic display screen. The surfactant prepared by the invention is beneficial to buffering the polishing pad to form a micropore structure; the introduction of the siloxane structure has stronger hydrophobicity.
Description
Technical Field
The invention belongs to the technical field of surfacing, and particularly relates to a buffering polishing pad for fine polishing of an electronic display screen and a production method thereof.
Background
The polishing pad is also called polishing leather, polishing cloth, polishing sheet and important auxiliary materials for determining the surface quality in chemical mechanical polishing, and can be divided into an abrasive polishing pad and an abrasive-free polishing pad according to whether the polishing pad contains abrasives or not; according to different materials, the polishing pad can be divided into a polyurethane polishing pad, a non-woven fabric polishing pad and a composite polishing pad; the surface structure can be roughly classified into a planar type, a mesh type, and a spiral type. The polishing pad functions to (1) deliver slurry efficiently and uniformly to different regions of the polishing pad; (2) fully performing chemical reaction after polishing; (3) maintaining the thin film of polishing solution on the surface of the polishing pad so that the chemical reaction is sufficiently performed; (4) the polishing process is kept smooth and the surface is not deformed, so that better wafer surface appearance is obtained.
Disclosure of Invention
The invention provides a buffering polishing pad for fine polishing of an electronic display screen and a production method thereof.
The technical problems to be solved by the invention are as follows:
polyesters generally have good uv stability and thermo-oxidative stability, but at the same time also have poor hydrolytic stability. The polyurethane polishing pads currently in use on the market are mainly polyether polyol systems, which, although having a certain hydrolytic stability, do not exhibit good stability in other weather resistance aspects, and are increasingly unable to meet the demands of miniaturization processes and the storage of materials.
The purpose of the invention can be realized by the following technical scheme:
a buffering polishing pad for fine polishing of an electronic display screen comprises a polishing layer and a buffer layer;
the buffering polishing pad for fine polishing of the electronic display screen is prepared by the following steps:
firstly, putting a polyester non-woven fabric into polyurethane impregnation liquid, taking out the polyester non-woven fabric under the extrusion of a metal roller, and removing redundant impregnation liquid on the surface to obtain the impregnated non-woven fabric;
secondly, putting the soaked non-woven fabric into a water tank with 20 mass percent of N, N-dimethylformamide aqueous solution for 20min to obtain a polishing layer;
and thirdly, casting the buffer layer precast liquid onto the polishing layer, then gelling for 10-60min at the temperature of 60-80 ℃, and then curing for 5-8h in a constant temperature box at the temperature of 100-160 ℃ to obtain the buffer polishing pad for fine polishing of the electronic display screen. The polishing layer and the buffer layer of the polishing pad are manufactured by a continuous casting mode, the combination of the polishing layer and the buffer layer of the polishing pad is firm, the problem that an interlayer adhesive is easily corroded by chemical of polishing liquid does not exist, and a micropore structure is generally required to be introduced into the polishing pad in order to balance the removal efficiency and the wafer defects in the polishing process.
Further, the polyurethane impregnation liquid is prepared by the following steps:
step A1, mixing the fluorine-containing polyurethane and the 1, 4-dioxane according to the mass ratio of 1: 10, then adding carbon black, finally adjusting the viscosity to be 1000-1500 centipoises by using 1, 4-dioxane, grinding for 1-2h at 50-60 ℃, and defoaming the obtained solution to obtain the polyurethane impregnation liquid, wherein the mass percent of fluorine in the fluorine-containing polyurethane is 1-10%, the fluorine-containing polyurethane has an average molecular weight of 30,000-80,000 and the hardness is 85-95 Shore A.
Further, the buffer layer precast liquid is prepared by the following steps:
and step B1, mixing 4, 4 '-diphenylmethane diisocyanate and polypropylene ether glycol with the molecular weight of 1500, reacting for 2h at 70 ℃, and defoaming in vacuum to obtain a first component, wherein the dosage mass ratio of the 4, 4' -diphenylmethane diisocyanate to the polypropylene ether glycol is 1: 1;
step B2, mixing 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, polytetramethylene ether glycol with the molecular weight of 2500, an organic zinc catalyst, a surfactant, soft foam silicone oil and azobisisobutyronitrile to obtain a second component; mixing a first component and a second component according to the mass ratio of 2: 1, mixing to obtain a buffer layer precast liquid; wherein, the dosage mass ratio of the 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, the polytetramethylene ether glycol with the molecular weight of 2500, the organic zinc catalyst, the surfactant and the azobisisobutyronitrile is 15: 80: 0.1: 3: 0.1.
further, the surfactant is prepared by the following steps:
step S11, adding abietic acid into a four-neck flask, heating to 220 ℃ under the protection of nitrogen, dropwise adding acrylic acid by using a constant-pressure dropping funnel, after the dropwise adding is finished, heating to 230 ℃, reacting for 4 hours, then cooling to 170 ℃, reacting for 10-20min, then cooling to room temperature, transferring to a rotary evaporator, removing unreacted acrylic acid, and then recrystallizing with glacial acetic acid to obtain an intermediate 1;
step S12, adding the intermediate 1 into a three-neck flask, then dropwise adding epoxy chloropropane by using a constant-pressure dropping funnel, stirring for 10-15min at 90 ℃, then adding tetrabutylammonium bromide to keep the temperature unchanged, continuing to react for 3-4h, transferring the obtained reaction liquid into a rotary evaporator after the reaction is finished, concentrating the reaction liquid at 40 ℃ under reduced pressure until the volume is unchanged, and then washing the reaction liquid for three times by using deionized water to obtain an intermediate 2;
step S13, adding absolute ethyl alcohol, the intermediate 2 and a silicon-containing monomer into a three-neck flask, heating and refluxing for 3-4 hours at the temperature of 85 ℃, transferring the reaction solution into a rotary evaporator after the reaction is finished, and concentrating under reduced pressure at 40 ℃ until the volume is unchanged to obtain an intermediate 3;
and step S14, adding the intermediate 3 into a three-neck flask, then dropwise adding epoxy chloropropane, carrying out reflux reaction for 3h at the constant temperature of 90 ℃, transferring the reaction solution to a rotary evaporator after the reaction is finished, removing unreacted epoxy chloropropane, then extracting with water and petroleum ether, and finally recrystallizing with absolute ethyl alcohol to obtain the surfactant. The surfactant prepared by the invention contains a biquaternary ammonium salt structure, an ester group and a siloxane structure, and the introduction of the ester group is beneficial to the self-assembly of surfactant molecules to form various aggregates such as spherical, rod-shaped, tubular and worm-shaped micelles and vesicles, and is beneficial to the formation of a microporous structure; the introduction of the siloxane structure has stronger hydrophobicity, and is helpful to improve the service life of the buffer polishing pad.
Further, in the step S11, the mass ratio of the rosin acid to the acrylic acid is 3: 0.8 to 1; in the step S12, the dosage ratio of the intermediate 1, the epichlorohydrin to the tetrabutylammonium bromide is 3.7-4 g: 2 g: 30 mg; the dosage ratio of the absolute ethyl alcohol, the intermediate 2 and the silicon-containing monomer in the step S13 is 10 mL: 5.7 g: 4.5-5 g; in the step S14, the mass ratio of the intermediate 3 to the epichlorohydrin is 50: 1-1.8. Reacting abietic acid with acrylic acid to obtain an intermediate 1, carrying out ring-opening esterification reaction on epoxy chloropropane and the intermediate 1 to obtain an intermediate 2, reacting chlorine on the intermediate 2 with amino on a silicon-containing monomer to obtain an intermediate 3, and reacting the intermediate 3 with epoxy chloropropane to obtain the surfactant.
Further, the silicon-containing monomer is prepared by the following steps:
step S21, adding aminopropyl trimethoxy silane, hexamethyl disiloxane and tetramethyl ammonium hydroxide into a four-neck flask, heating and refluxing for 3 hours under the conditions of nitrogen protection and 100 ℃, then heating to 130 ℃, distilling at normal pressure, and continuing to react for 50-60min to obtain an intermediate a; aminopropyl trimethoxy silane and hexamethyl disiloxane are catalyzed by tetramethyl ammonium hydroxide to obtain an intermediate a.
The procedure is as follows:
and step S22, under the protection of nitrogen, adding a silicon-containing monomer and absolute ethyl alcohol into a reaction kettle, dropwise adding methyl acrylate, keeping the temperature at 25 ℃ in the dropwise adding process, detecting the reaction by using a TLC plate in the reaction process, transferring the obtained reaction solution into a rotary evaporator after the reaction is finished, and concentrating the reaction solution at 40 ℃ under reduced pressure until the volume is unchanged to obtain the silicon-containing monomer. And carrying out Michael addition on the intermediate a and methyl acrylate to prepare the silicon-containing monomer.
The procedure is as follows:
further, in the step S21, the mass ratio of the used aminopropyltrimethoxysilane, the used hexamethyldisiloxane to the used tetramethylammonium hydroxide is 26-27: 121-122: 2.01; the dosage ratio of the absolute ethyl alcohol, the intermediate a and the methyl acrylate in the step S22 is 100 mL: 10 g: 2.5-3 g.
A production method of a buffering polishing pad for fine polishing of an electronic display screen comprises the following steps:
firstly, putting a polyester non-woven fabric into polyurethane impregnation liquid, taking out the polyester non-woven fabric under the extrusion of a metal roller, and removing redundant impregnation liquid on the surface to obtain the impregnated non-woven fabric;
secondly, putting the soaked non-woven fabric into a water tank with 20 mass percent of N, N-dimethylformamide aqueous solution for 20min to obtain a polishing layer;
and thirdly, casting the buffer layer precast liquid onto the polishing layer, then gelling for 10-60min at the temperature of 60-80 ℃, and then curing for 5-8h in a constant temperature box at the temperature of 100-160 ℃ to obtain the buffer polishing pad for fine polishing of the electronic display screen.
The invention has the beneficial effects that:
the preparation process of the silicon-containing monomer comprises the following steps: under the catalytic action of tetramethylammonium hydroxide, aminopropyltrimethoxysilane and hexamethyldisiloxane are used to obtain an intermediate a; and carrying out Michael addition on the intermediate a and methyl acrylate to prepare the silicon-containing monomer. Reacting abietic acid with acrylic acid to obtain an intermediate 1, carrying out ring-opening esterification reaction on epoxy chloropropane and the intermediate 1 to obtain an intermediate 2, reacting chlorine on the intermediate 2 with amino on a silicon-containing monomer to obtain an intermediate 3, and reacting the intermediate 3 with epoxy chloropropane to obtain the surfactant.
The polishing layer and the buffer layer of the polishing pad are manufactured by a continuous casting mode, the combination of the polishing layer and the buffer layer of the polishing pad is firm, the problem that an interlayer adhesive is easily corroded by chemical of polishing liquid does not exist, and a micropore structure is generally required to be introduced into the polishing pad in order to balance the removal efficiency and the wafer defects in the polishing process. The surfactant prepared by the invention contains a biquaternary ammonium salt structure, an ester group and a siloxane structure, and the introduction of the ester group is beneficial to the self-assembly of surfactant molecules to form various aggregates such as spherical, rod-shaped, tubular and worm-shaped micelles and vesicles, and is beneficial to the formation of a microporous structure; the siloxane structure is introduced to have stronger hydrophobicity, and the strong hydrophobicity can prevent polishing liquid from being absorbed into the porous structure, thereby being beneficial to prolonging the service life of the buffering polishing pad.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Firstly, putting a polyester non-woven fabric into polyurethane impregnation liquid, taking out the polyester non-woven fabric under the extrusion of a metal roller, and removing redundant impregnation liquid on the surface to obtain the impregnated non-woven fabric;
secondly, putting the soaked non-woven fabric into a water tank with 20 mass percent of N, N-dimethylformamide aqueous solution for 20min to obtain a polishing layer;
and thirdly, casting the buffer layer precast liquid onto the polishing layer, gelatinizing for 10min at the temperature of 60 ℃, and curing for 5h in a thermostat at the temperature of 100 ℃ to obtain the buffer polishing pad for fine polishing of the electronic display screen.
The polyurethane impregnating solution is prepared by the following steps:
step A1, mixing the fluorine-containing polyurethane and the 1, 4-dioxane according to the mass ratio of 1: 10, adding carbon black, finally adjusting the viscosity to be 1000 centipoises by using 1, 4-dioxane, grinding for 1h at 50 ℃, and defoaming the obtained solution to obtain the polyurethane impregnation liquid, wherein the mass percent of fluorine in the fluorine-containing polyurethane is 1%, the fluorine-containing polyurethane has an average molecular weight of 30,000, and the hardness is 85 Shore A.
The buffer layer precast liquid is prepared by the following steps:
and step B1, mixing 4, 4 '-diphenylmethane diisocyanate and polypropylene ether glycol with the molecular weight of 1500, reacting for 2h at 70 ℃, and defoaming in vacuum to obtain a first component, wherein the dosage mass ratio of the 4, 4' -diphenylmethane diisocyanate to the polypropylene ether glycol is 1: 1;
step B2, mixing 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, polytetramethylene ether glycol with the molecular weight of 2500, an organic zinc catalyst, a surfactant, soft foam silicone oil and azobisisobutyronitrile to obtain a second component; mixing a first component and a second component according to a mass ratio of 2: 1, mixing to obtain a buffer layer precast liquid; wherein, the dosage mass ratio of the 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, the polytetramethylene ether glycol with the molecular weight of 2500, the organic zinc catalyst, the surfactant and the azobisisobutyronitrile is 15: 80: 0.1: 3: 0.1.
wherein the surfactant is prepared by the following steps:
step S11, adding abietic acid into a four-neck flask, heating to 220 ℃ under the protection of nitrogen, dropwise adding acrylic acid by using a constant-pressure dropping funnel, after the dropwise adding is finished, heating to 230 ℃, reacting for 4 hours, then cooling to 170 ℃, reacting for 10min, then cooling to room temperature, transferring to a rotary evaporator, removing unreacted acrylic acid, and then recrystallizing with glacial acetic acid to obtain an intermediate 1;
step S12, adding the intermediate 1 into a three-neck flask, then dropwise adding epoxy chloropropane by using a constant-pressure dropping funnel, stirring for 10min at 90 ℃, then adding tetrabutyl ammonium bromide to keep the temperature unchanged, continuing to react for 3h, after the reaction is finished, transferring the obtained reaction liquid into a rotary evaporator, carrying out reduced pressure concentration at 40 ℃ until the volume is unchanged, and then washing with deionized water for three times to obtain an intermediate 2;
step S13, adding absolute ethyl alcohol, the intermediate 2 and a silicon-containing monomer into a three-neck flask, heating and refluxing for 3 hours at the temperature of 85 ℃, transferring the reaction liquid into a rotary evaporator after the reaction is finished, and concentrating under reduced pressure at 40 ℃ until the volume is unchanged to obtain an intermediate 3;
and step S14, adding the intermediate 3 into a three-neck flask, then dropwise adding epoxy chloropropane, carrying out reflux reaction for 3 hours at a constant temperature of 90 ℃, transferring the reaction solution into a rotary evaporator after the reaction is finished, removing unreacted epoxy chloropropane, then extracting with water and petroleum ether, and finally recrystallizing with absolute ethyl alcohol to obtain the surfactant.
Wherein the dosage mass ratio of the abietic acid to the acrylic acid in the step S11 is 3: 0.8; in the step S12, the using amount ratio of the intermediate 1 to the epichlorohydrin to the tetrabutylammonium bromide is 3.7 g: 2 g: 30 mg; the dosage ratio of the absolute ethyl alcohol, the intermediate 2 and the silicon-containing monomer in the step S13 is 10 mL: 5.7 g: 4.5 g; in the step S14, the mass ratio of the intermediate 3 to the epichlorohydrin is 50: 1.
wherein the silicon-containing monomer is prepared by the following steps:
step S21, adding aminopropyl trimethoxy silane, hexamethyl disiloxane and tetramethyl ammonium hydroxide into a four-neck flask, heating and refluxing for 3 hours under the conditions of nitrogen protection and 100 ℃, then heating to 130 ℃, distilling at normal pressure, and continuing to react for 50min to obtain an intermediate a;
and step S22, under the protection of nitrogen, adding a silicon-containing monomer and absolute ethyl alcohol into a reaction kettle, dropwise adding methyl acrylate, keeping the temperature at 25 ℃ in the dropwise adding process, detecting the reaction by using a TLC plate in the reaction process, transferring the obtained reaction solution into a rotary evaporator after the reaction is finished, and concentrating the reaction solution at 40 ℃ under reduced pressure until the volume is unchanged to obtain the silicon-containing monomer.
Wherein, in the step S21, the mass ratio of the used aminopropyltrimethoxysilane, the used hexamethyldisiloxane to the used tetramethylammonium hydroxide is 26: 121: 2.01; the dosage ratio of the absolute ethyl alcohol, the intermediate a and the methyl acrylate in the step S22 is 100 mL: 10 g: 2.5 g.
Example 2
Firstly, putting a polyester non-woven fabric into polyurethane impregnation liquid, taking out the polyester non-woven fabric under the extrusion of a metal roller, and removing redundant impregnation liquid on the surface to obtain the impregnated non-woven fabric;
secondly, putting the soaked non-woven fabric into a water tank with 20 mass percent of N, N-dimethylformamide aqueous solution for 20min to obtain a polishing layer;
and thirdly, casting the buffer layer precast liquid onto the polishing layer, gelatinizing for 50min at 70 ℃, and curing for 6h in a thermostat at 130 ℃ to obtain the buffer polishing pad for fine polishing of the electronic display screen.
The polyurethane impregnating solution is prepared by the following steps:
step A1, mixing the fluorine-containing polyurethane and the 1, 4-dioxane according to the mass ratio of 1: 10, adding carbon black, finally adjusting the viscosity to be 1200 centipoises by using 1, 4-dioxane, grinding for 1.5 hours at 555 ℃, and defoaming the obtained solution to obtain a polyurethane impregnation liquid, wherein the mass percent of fluorine in the fluorine-containing polyurethane is 1-10%, the fluorine-containing polyurethane has an average molecular weight of 60,000 and the hardness is 90 Shore A.
The buffer layer precast liquid is prepared by the following steps:
and step B1, mixing 4, 4 '-diphenylmethane diisocyanate and polypropylene ether glycol with the molecular weight of 1500, reacting for 2h at 70 ℃, and defoaming in vacuum to obtain a first component, wherein the dosage mass ratio of the 4, 4' -diphenylmethane diisocyanate to the polypropylene ether glycol is 1: 1;
step B2, mixing 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, polytetramethylene ether glycol with the molecular weight of 2500, an organic zinc catalyst, a surfactant, soft foam silicone oil and azobisisobutyronitrile to obtain a second component; mixing a first component and a second component according to a mass ratio of 2: 1, mixing to obtain a buffer layer precast liquid; wherein, the dosage mass ratio of the 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, the polytetramethylene ether glycol with the molecular weight of 2500, the organic zinc catalyst, the surfactant and the azobisisobutyronitrile is 15: 80: 0.1: 3: 0.1.
wherein the surfactant is prepared by the following steps:
step S11, adding abietic acid into a four-neck flask, heating to 220 ℃ under the protection of nitrogen, dropwise adding acrylic acid by using a constant-pressure dropping funnel, after the dropwise adding is finished, heating to 230 ℃, reacting for 4 hours, then cooling to 170 ℃, reacting for 15min, then cooling to room temperature, transferring to a rotary evaporator, removing unreacted acrylic acid, and then recrystallizing with glacial acetic acid to obtain an intermediate 1;
step S12, adding the intermediate 1 into a three-neck flask, then dropwise adding epoxy chloropropane by using a constant-pressure dropping funnel, stirring for 12.5min at 90 ℃, then adding tetrabutylammonium bromide to keep the temperature unchanged, continuing to react for 3.5h, transferring the obtained reaction liquid into a rotary evaporator after the reaction is finished, concentrating the reaction liquid at 40 ℃ under reduced pressure until the volume is unchanged, and then washing the reaction liquid for three times by using deionized water to obtain an intermediate 2;
step S13, adding absolute ethyl alcohol, the intermediate 2 and a silicon-containing monomer into a three-neck flask, heating and refluxing for reaction for 3.5 hours at the temperature of 85 ℃, transferring the reaction solution into a rotary evaporator after the reaction is finished, and concentrating under reduced pressure at 40 ℃ until the volume is unchanged to obtain an intermediate 3;
and step S14, adding the intermediate 3 into a three-neck flask, then dropwise adding epoxy chloropropane, carrying out reflux reaction for 3h at the constant temperature of 90 ℃, transferring the reaction solution to a rotary evaporator after the reaction is finished, removing unreacted epoxy chloropropane, then extracting with water and petroleum ether, and finally recrystallizing with absolute ethyl alcohol to obtain the surfactant.
Wherein the dosage mass ratio of the abietic acid to the acrylic acid in the step S11 is 3: 0.9; in the step S12, the using amount ratio of the intermediate 1 to the epichlorohydrin to the tetrabutylammonium bromide is 3.8 g: 2 g: 30 mg; the dosage ratio of the absolute ethyl alcohol, the intermediate 2 and the silicon-containing monomer in the step S13 is 10 mL: 5.7 g: 4.6 g; in the step S14, the mass ratio of the intermediate 3 to the epichlorohydrin is 50: 1.6.
wherein the silicon-containing monomer is prepared by the following steps:
step S21, adding aminopropyl trimethoxy silane, hexamethyl disiloxane and tetramethyl ammonium hydroxide into a four-neck flask, heating and refluxing for 3 hours under the protection of nitrogen and at the temperature of 100 ℃, then heating to 130 ℃, distilling at normal pressure, and continuing to react for 55min to obtain an intermediate a;
and step S22, under the protection of nitrogen, adding a silicon-containing monomer and absolute ethyl alcohol into a reaction kettle, dropwise adding methyl acrylate, keeping the temperature at 25 ℃ in the dropwise adding process, detecting the reaction by using a TLC plate in the reaction process, transferring the obtained reaction solution into a rotary evaporator after the reaction is finished, and concentrating the reaction solution at 40 ℃ under reduced pressure until the volume is unchanged to obtain the silicon-containing monomer.
Wherein, in the step S21, the mass ratio of the used aminopropyltrimethoxysilane, the used hexamethyldisiloxane to the used tetramethylammonium hydroxide is 26: 121: 2.01; the dosage ratio of the absolute ethyl alcohol, the intermediate a and the methyl acrylate in the step S22 is 100 mL: 10 g: 2.8 g.
Example 3
Firstly, putting a polyester non-woven fabric into polyurethane impregnation liquid, taking out the polyester non-woven fabric under the extrusion of a metal roller, and removing redundant impregnation liquid on the surface to obtain the impregnated non-woven fabric;
secondly, putting the soaked non-woven fabric into a water tank with 20 mass percent of N, N-dimethylformamide aqueous solution for 20min to obtain a polishing layer;
and thirdly, casting the buffer layer precast liquid onto the polishing layer, gelatinizing for 60min at the temperature of 80 ℃, and curing for 8h in a thermostat at the temperature of 160 ℃ to obtain the buffer polishing pad for fine polishing of the electronic display screen.
The polyurethane impregnating solution is prepared by the following steps:
step A1, mixing the fluorine-containing polyurethane and the 1, 4-dioxane according to the mass ratio of 1: 10, adding carbon black, finally adjusting the viscosity to be 1500 centipoises by using 1, 4-dioxane, grinding for 2 hours at 60 ℃, and defoaming the obtained solution to obtain the polyurethane impregnation liquid, wherein the mass percent of fluorine in the fluorine-containing polyurethane is 10%, the fluorine-containing polyurethane has an average molecular weight of 80,000, and the hardness is 95 Shore A.
The buffer layer precast liquid is prepared by the following steps:
and step B1, mixing 4, 4 '-diphenylmethane diisocyanate and polypropylene ether glycol with the molecular weight of 1500, reacting for 2h at 70 ℃, and defoaming in vacuum to obtain a first component, wherein the dosage mass ratio of the 4, 4' -diphenylmethane diisocyanate to the polypropylene ether glycol is 1: 1;
step B2, mixing 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, polytetramethylene ether glycol with the molecular weight of 2500, an organic zinc catalyst, a surfactant, soft foam silicone oil and azobisisobutyronitrile to obtain a second component; mixing a first component and a second component according to a mass ratio of 2: 1, mixing to obtain a buffer layer precast liquid; wherein, the dosage mass ratio of the 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, the polytetramethylene ether glycol with the molecular weight of 2500, the organic zinc catalyst, the surfactant and the azobisisobutyronitrile is 15: 80: 0.1: 3: 0.1.
wherein the surfactant is prepared by the following steps:
step S11, adding abietic acid into a four-neck flask, heating to 220 ℃ under the protection of nitrogen, dropwise adding acrylic acid by using a constant-pressure dropping funnel, after the dropwise adding is finished, heating to 230 ℃, reacting for 4 hours, then cooling to 170 ℃, reacting for 20min, then cooling to room temperature, transferring to a rotary evaporator, removing unreacted acrylic acid, and then recrystallizing with glacial acetic acid to obtain an intermediate 1;
step S12, adding the intermediate 1 into a three-neck flask, then dropwise adding epoxy chloropropane by using a constant-pressure dropping funnel, stirring for 15min at 90 ℃, then adding tetrabutyl ammonium bromide to keep the temperature unchanged, continuing to react for 4h, after the reaction is finished, transferring the obtained reaction liquid into a rotary evaporator, carrying out reduced pressure concentration at 40 ℃ until the volume is unchanged, and then washing with deionized water for three times to obtain an intermediate 2;
step S13, adding absolute ethyl alcohol, the intermediate 2 and a silicon-containing monomer into a three-neck flask, heating and refluxing for 4 hours at the temperature of 85 ℃, transferring the reaction liquid into a rotary evaporator after the reaction is finished, and concentrating under reduced pressure at 40 ℃ until the volume is unchanged to obtain an intermediate 3;
and step S14, adding the intermediate 3 into a three-neck flask, then dropwise adding epoxy chloropropane, carrying out reflux reaction for 3h at the constant temperature of 90 ℃, transferring the reaction solution to a rotary evaporator after the reaction is finished, removing unreacted epoxy chloropropane, then extracting with water and petroleum ether, and finally recrystallizing with absolute ethyl alcohol to obtain the surfactant.
Wherein the dosage mass ratio of the abietic acid to the acrylic acid in the step S11 is 3: 1; in the step S12, the using amount ratio of the intermediate 1 to the epichlorohydrin to the tetrabutylammonium bromide is 4 g: 2 g: 30 mg; the dosage ratio of the absolute ethyl alcohol, the intermediate 2 and the silicon-containing monomer in the step S13 is 10 mL: 5.7 g: 5g of the total weight of the mixture; in the step S14, the mass ratio of the intermediate 3 to the epichlorohydrin is 50: 1.8.
wherein the silicon-containing monomer is prepared by the following steps:
step S21, adding aminopropyl trimethoxy silane, hexamethyl disiloxane and tetramethyl ammonium hydroxide into a four-neck flask, heating and refluxing for 3 hours under the conditions of nitrogen protection and 100 ℃, then increasing the temperature to 130 ℃, distilling at normal pressure, and continuing to react for 60min to obtain an intermediate a;
and step S22, under the protection of nitrogen, adding a silicon-containing monomer and absolute ethyl alcohol into a reaction kettle, dropwise adding methyl acrylate, keeping the temperature at 25 ℃ in the dropwise adding process, detecting the reaction by using a TLC plate in the reaction process, transferring the obtained reaction solution into a rotary evaporator after the reaction is finished, and concentrating the reaction solution at 40 ℃ under reduced pressure until the volume is unchanged to obtain the silicon-containing monomer.
Wherein, in the step S21, the mass ratio of the used aminopropyltrimethoxysilane, the used hexamethyldisiloxane to the used tetramethylammonium hydroxide is 27: 122: 2.01; the dosage ratio of the absolute ethyl alcohol, the intermediate a and the methyl acrylate in the step S22 is 100 mL: 10 g: 3g of the total weight.
Comparative example 1
The comparison example is a common electronic display screen buffer polishing pad in the market.
Service life: and fixing the buffering polishing pad on a polishing machine disc, cleaning the surface of the adsorption pad, then installing the material to be polished on the surface of the adsorption pad, polishing, and recording the service life.
The polishing pads of example 13 and comparative example were tested and the results are shown in table 1 below:
TABLE 1
| Categories | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Service life/h | 70 | 70 | 70 | 58 |
| Water absorption capacity (mg/cm)2) | 2.3 | 2.2 | 2.5 | 8.2 |
| Surface water contact Angle (°) | 98 | 95 | 98 | 85 |
| Compression recovery ratio/%) | 97 | 97 | 97 | 90 |
The screen buffering polishing pad prepared by the invention has stronger hydrophobicity, smaller water absorption capacity and longer service life.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean 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 invention. In this specification, the schematic representations of the terms used above do not necessarily refer 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.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (5)
1. A buffering polishing pad for fine polishing of an electronic display screen is characterized by comprising a polishing layer and a buffer layer;
the buffering polishing pad for fine polishing of the electronic display screen is prepared by the following steps:
firstly, putting polyester non-woven fabric into polyurethane impregnation liquid, taking out the polyester non-woven fabric under the extrusion of a metal roller, and removing redundant impregnation liquid on the surface to obtain impregnated non-woven fabric;
secondly, putting the soaked non-woven fabric into a water tank with 20 mass percent of N, N-dimethylformamide aqueous solution for 20min to obtain a polishing layer;
thirdly, casting the buffer layer precast liquid on the polishing layer, then gelling for 10-60min at the temperature of 60-80 ℃, and then curing for 5-8h in a constant temperature box at the temperature of 100-160 ℃ to obtain the buffer polishing pad for fine polishing of the electronic display screen;
the buffer layer precast liquid is prepared by the following steps:
step B1, mixing 4, 4' -diphenylmethane diisocyanate and polypropylene ether glycol, reacting for 2h at 70 ℃, and defoaming in vacuum to obtain a first component;
step B2, mixing 2, 2 ' -diamino-3, 3 ' -dichloro-4, 4 ' -divinyl diphenylmethane, polytetramethylene ether glycol with the molecular weight of 2500, an organic zinc catalyst, a surfactant, soft foam silicone oil and azobisisobutyronitrile to obtain a second component; mixing a first component and a second component according to a mass ratio of 2: 1, mixing to obtain a buffer layer precast liquid;
the surfactant is prepared by the following steps:
step S11, adding abietic acid into a four-neck flask, heating to 220 ℃ under the protection of nitrogen, dropwise adding acrylic acid by using a constant-pressure dropping funnel, after the dropwise adding is finished, heating to 230 ℃, reacting for 4 hours, then cooling to 170 ℃, reacting for 10-20min, then cooling to room temperature, transferring to a rotary evaporator, removing unreacted acrylic acid, and then recrystallizing with glacial acetic acid to obtain an intermediate 1;
step S12, adding the intermediate 1 into a three-neck flask, then dropwise adding epoxy chloropropane by using a constant-pressure dropping funnel, stirring for 10-15min at 90 ℃, then adding tetrabutylammonium bromide to keep the temperature unchanged, continuing to react for 3-4h, transferring the obtained reaction liquid into a rotary evaporator after the reaction is finished, concentrating the reaction liquid at 40 ℃ under reduced pressure until the volume is unchanged, and then washing the reaction liquid for three times by using deionized water to obtain an intermediate 2;
step S13, adding absolute ethyl alcohol, the intermediate 2 and a silicon-containing monomer into a three-neck flask, heating and refluxing for 3-4 hours at the temperature of 85 ℃, transferring the reaction solution into a rotary evaporator after the reaction is finished, and concentrating under reduced pressure at 40 ℃ until the volume is unchanged to obtain an intermediate 3;
step S14, adding the intermediate 3 into a three-neck flask, then dropwise adding epoxy chloropropane, carrying out reflux reaction for 3 hours at a constant temperature of 90 ℃, transferring the reaction liquid into a rotary evaporator after the reaction is finished, removing unreacted epoxy chloropropane, then extracting with water and petroleum ether, and finally recrystallizing with absolute ethyl alcohol to obtain a surfactant;
the silicon-containing monomer is prepared by the following steps:
step S21, adding aminopropyl trimethoxy silane, hexamethyl disiloxane and tetramethyl ammonium hydroxide into a four-neck flask, heating and refluxing for 3 hours under the conditions of nitrogen protection and 100 ℃, then heating to 130 ℃, distilling at normal pressure, and continuing to react for 50-60min to obtain an intermediate a;
and step S22, under the protection of nitrogen, adding a silicon-containing monomer and absolute ethyl alcohol into a reaction kettle, dropwise adding methyl acrylate, keeping the temperature at 25 ℃ in the dropwise adding process, detecting the reaction by using a TLC plate in the reaction process, transferring the obtained reaction solution into a rotary evaporator after the reaction is finished, and concentrating the reaction solution at 40 ℃ under reduced pressure until the volume is unchanged to obtain the silicon-containing monomer.
2. The buffer polishing pad for fine polishing of electronic display screens according to claim 1, wherein the polyurethane dipping solution is prepared by the following steps:
step A1, mixing the fluorine-containing polyurethane and the 1, 4-dioxane according to the mass ratio of 1: 10, then adding carbon black, finally adjusting the viscosity to be 1000-1500 centipoises by using 1, 4-dioxane, grinding for 1-2h at 50-60 ℃, and defoaming the obtained solution to obtain the polyurethane impregnation liquid.
3. The buffering polishing pad for fine polishing of electronic display screens according to claim 1, wherein the amount by mass ratio of the abietic acid to the acrylic acid in step S11 is 3: 0.8 to 1; in the step S12, the dosage ratio of the intermediate 1, the epichlorohydrin to the tetrabutylammonium bromide is 3.7-4 g: 2 g: 30 mg; the dosage ratio of the absolute ethyl alcohol, the intermediate 2 and the silicon-containing monomer in the step S13 is 10 mL: 5.7 g: 4.5-5 g; in the step S14, the mass ratio of the intermediate 3 to the epichlorohydrin is 50: 1-1.8.
4. The buffer polishing pad for fine polishing of electronic display screens according to claim 1, wherein the amount by mass ratio of aminopropyltrimethoxysilane, hexamethyldisiloxane and tetramethylammonium hydroxide in step S21 is 26-27: 121-122: 2.01; the dosage ratio of the absolute ethyl alcohol, the intermediate a and the methyl acrylate in the step S22 is 100 mL: 10 g: 2.5-3 g.
5. The method for producing the buffer polishing pad for the fine polishing of the electronic display screen according to claim 1, characterized by comprising the following steps:
firstly, putting a polyester non-woven fabric into polyurethane impregnation liquid, taking out the polyester non-woven fabric under the extrusion of a metal roller, and removing redundant impregnation liquid on the surface to obtain the impregnated non-woven fabric;
secondly, putting the soaked non-woven fabric into a water tank with 20 mass percent of N, N-dimethylformamide aqueous solution for 20min to obtain a polishing layer;
and thirdly, casting the buffer layer precast liquid onto the polishing layer, then gelling for 10-60min at the temperature of 60-80 ℃, and then curing for 5-8h in a constant temperature box at the temperature of 100-160 ℃ to obtain the buffer polishing pad for fine polishing of the electronic display screen.
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| KR101107043B1 (en) * | 2006-08-28 | 2012-01-25 | 도요 고무 고교 가부시키가이샤 | Polishing pad |
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