CN113842011B - Mirror inlaid from front surface - Google Patents

Mirror inlaid from front surface Download PDF

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Publication number
CN113842011B
CN113842011B CN202111094060.0A CN202111094060A CN113842011B CN 113842011 B CN113842011 B CN 113842011B CN 202111094060 A CN202111094060 A CN 202111094060A CN 113842011 B CN113842011 B CN 113842011B
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mirror
poss
frame
phytic acid
component
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CN113842011A (en
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龚品忠
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Huahonghua Home Furnishing Co ltd
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Huahonghua Home Furnishing Co ltd
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    • A—HUMAN NECESSITIES
    • A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47G—HOUSEHOLD OR TABLE EQUIPMENT
    • A47G1/00—Mirrors; Picture frames or the like, e.g. provided with heating, lighting or ventilating means
    • A47G1/02—Mirrors used as equipment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2170/00—Compositions for adhesives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention discloses a mirror embedded from the front, which comprises a frame and a mirror body, wherein the front of the frame is provided with a groove, the mirror body is embedded into the groove of the frame from the front, and the back of the mirror body is bonded with the frame through an adhesive. The front surface of the frame is provided with the groove, the mirror body is placed in the groove from the front surface during installation, and then the back surface of the mirror body is bonded with the frame by using the adhesive, so that the mirror body is fixed in the frame, the edge of the mirror body is not shielded by the frame, the mirror surface is high in utilization rate and wide in visual field, and the mirror surface image acquisition and use effects are improved.

Description

Mirror inlaid from front surface
Technical Field
The invention relates to a mirror, in particular to a mirror inlaid from the front surface.
Background
The mirror in the prior art is usually arranged on the back surface of a frame and is lapped on a step surface in the frame, so that the edge part of the mirror is shielded, and the utilization rate of the mirror surface is limited, for example, the mirror with the cleaning scraper is disclosed in Chinese patent literature, and the publication No. CN208625118U of the mirror comprises a mirror body and an outer frame shell, wherein the mirror body is embedded in the outer frame shell, a driving screw rod and a polished rod are respectively arranged in two side edges of the outer frame shell, a window opening design is arranged on the outer frame shell in front of the driving screw rod and the polished rod correspondingly, a threaded sliding block is arranged on the driving screw rod, a driven sliding block is arranged on the polished rod, a soft rubber scraper is transversely arranged at the front ends of the threaded sliding block and the driven sliding block, the soft rubber scraper is arranged on the upper surface of the mirror body, and the lower edge of the soft rubber scraper is abutted against the surface of the mirror body; the lower end of the drive screw rod is connected with a drive motor, and the lower end of the polish rod is provided with a fixed seat; and a control circuit board and a power supply device are arranged in the lower frame of the outer frame shell, and a control key is arranged on the control circuit board. The mirror has the condition that part of the mirror is shielded, so that the imaging visual field is influenced, and the mirror is not beneficial to use.
Disclosure of Invention
The invention provides a mirror embedded from the front, aiming at overcoming the problems that the edge part of the mirror installed from the back of a frame can be shielded, the imaging visual field is influenced, and the use is not facilitated in the prior art, so that the front of a mirror body is not shielded by the frame, the utilization rate is high, the visual field is wide, and the mirror surface image acquisition and use effects are improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the mirror inlaid from the front comprises a frame and a mirror body, wherein the front surface of the frame is provided with a groove, the mirror body is embedded into the groove of the frame from the front surface, and the back surface of the mirror body is bonded with the frame through an adhesive.
The front surface of the frame is provided with the groove, the mirror body is placed in the groove from the front surface during installation, and then the back surface of the mirror body is bonded with the frame by using the adhesive, so that the mirror body is fixed in the frame, the edge of the mirror body is not shielded by the frame, the mirror surface is high in utilization rate and wide in visual field, and the mirror surface image acquisition and use effects are improved.
Preferably, the depth of the groove is larger than or equal to the thickness of the mirror body, so that the periphery of the mirror body can be completely positioned in the frame, the mirror body is effectively protected, and the attractiveness of the mirror is improved.
Preferably, the edge of the mirror body is polished into a bevel edge; the periphery of the mirror body is polished. The invention grinds the edges around the mirror body into the bevel edges, and for the rectangular mirror body, five refraction surfaces can be obtained, and the beauty of the mirror edges is highlighted. When the lens body is embedded into the back of the frame, the periphery of the lens body is shielded by the frame and cannot be exposed, so that the edge of the lens body does not need to be processed; when the mirror body is embedded into the front side of the frame, the edge of the mirror body is exposed outside, and the periphery of the mirror body needs to be polished, so that the attractiveness of the mirror is ensured, and the phenomenon that the edge of the mirror body is easily damaged when the edge of the mirror body is too sharp to touch is avoided.
Preferably, the back surface of the frame is provided with a protective film for sealing the back surface of the frame. The back of the frame is covered by the protective film, so that moisture can be prevented from entering, the back of the mirror body is protected from being affected, and the service life of the mirror is prolonged.
Preferably, the side surface of the frame is provided with anti-skid lines. The hand-held carrying is convenient.
Preferably, the adhesive is a two-component epoxy resin adhesive, and the two-component epoxy resin adhesive comprises a component A and a component B in a mass ratio of 2-3; the component A comprises the following raw materials in parts by weight: 90-100 parts of bisphenol A epoxy resin and 3-5 parts of diluent; the component B comprises the following raw materials: 80-90 parts of phytic acid and POSS modified amine curing agent, 3-5 parts of curing accelerator and 8-10 parts of toluene.
Because the epoxy resin adhesive has the characteristics of strong adhesive force, high mechanical strength of materials, good chemical resistance, small curing shrinkage and the like, the epoxy resin adhesive is selected for bonding the lens body and the frame. However, the cured epoxy resin adhesive usually has the defects of brittleness, poor impact resistance and peeling strength, easy cracking and the like, increases the potential safety hazard that the mirror falls off from the front when being used for adhering the mirror inlaid from the front, and also influences the service life of the mirror. Meanwhile, the production method of the prior mirror generally comprises the steps of plating a layer of metal aluminum or metal silver on the surface of glass to be used as a reflecting layer, and then coating a layer of protective paint on the reflecting layer to prevent the metal layer from being chemically corroded and physically damaged; however, when the periphery of the mirror body is cut, ground, polished and the like, the protective paint near the cut part is easy to fall off and is difficult to repair, so that the metal layer around the mirror body is exposed and is easy to oxidize and discolor by air, and when the mirror body is embedded into the frame from the front side, the oxidized and blackened edge seriously influences the use attractiveness of the mirror.
Therefore, the curing agent of the epoxy resin adhesive is modified by adopting the phytic acid and the POSS, the POSS is a nano-scale cage-shaped structure compound, the internal inorganic framework consisting of Si-O endows the compound with high rigidity, heat resistance and chemical stability, and the POSS can better absorb external energy, obviously improve the toughness of the epoxy resin and improve the impact resistance and the peeling strength of the adhesive by being added into the epoxy resin. The phytic acid is a metal polydentate chelating agent, and can be added into the adhesive to effectively form a layer of protective film on the surface of an aluminum layer or a silver layer exposed on the back surface of the mirror body through chelation, so that the contact between a corrosion medium and a metal matrix is prevented, and the edge of the mirror body is prevented from being oxidized and blackened. However, because the compatibility between POSS and phytic acid and the epoxy resin matrix is poor, when the POSS and the phytic acid are directly added into the epoxy resin, the toughening and corrosion prevention effects on the adhesive are poor; according to the invention, the curing agent is modified by POSS and phytic acid, and the POSS and the phytic acid after the curing agent is mixed with the epoxy resin can be connected in the crosslinked resin matrix along with the reaction of the amine curing agent and the epoxy resin, so that the compatibility with the resin matrix is improved, and the adhesive can obtain better toughening and anticorrosion effects.
Preferably, the bisphenol a epoxy resin is epoxy resin E44 or epoxy resin E51; the diluent is selected from one or more of butyl glycidyl ether, benzyl glycidyl ether and 1, 4-butanediol diglycidyl ether; the curing accelerator is an imidazole accelerator.
Preferably, the preparation method of the phytic acid and POSS modified amine curing agent comprises the following steps:
(1) Adding 3-glycidyloxypropyltrimethoxysilane and aqueous solution of tetramethylammonium hydroxide into isopropanol, stirring and reacting for 5-7 h, then carrying out reduced pressure distillation to remove the isopropanol, adding toluene to dissolve the product, carrying out reflux reaction at 70-80 ℃ for 5-6 h, washing the reacted solution with saturated sodium chloride solution to be neutral, separating to obtain an organic phase, and carrying out rotary evaporation and drying to obtain epoxy group POSS;
(2) Dissolving epoxy POSS in DMF, adding ethylene glycol, stirring uniformly, adding NaOH, and stirring at 60-80 ℃ for reaction for 2-3 h; then adding triethylenetetramine, and continuing to react for 3-5 h under heat preservation; removing the solvent by rotary evaporation and drying to obtain the POSS modified amine curing agent;
(3) Dissolving POSS modified amine curing agent in dimethyl sulfoxide, adding dicyandiamide and urea, heating to 100-110 ℃ under the protection of nitrogen, then adding phytic acid aqueous solution and toluene, and stirring and reacting for 1-3 h; and precipitating the product by using absolute ethyl alcohol, washing and drying the precipitated product to obtain the phytic acid and POSS modified amine curing agent.
Firstly, through the step (1), preparing eight epoxy group POSS with epoxy groups at the top by utilizing the hydrolysis reaction of 3-glycidoxypropyltrimethoxysilane; then modifying ethylene glycol and triethylenetetramine on POSS by using the reaction of epoxy group, hydroxyl group and amino group through the step (2) to enable POSS to have hydroxyl group and amino group; and (3) performing esterification reaction on hydroxyl on the POSS and phosphate groups in the phytic acid to connect the phytic acid to the POSS, and finally obtaining the phytic acid and the POSS modified amine curing agent. After the component A and the component B are mixed, the phytic acid and POSS can be connected in a crosslinked resin matrix along with the reaction of amino and epoxy, so that the compatibility with the resin matrix is improved.
Preferably, the mass fraction of the aqueous solution of tetramethylammonium hydroxide in step (1) is 5 to 8%; the addition ratio of the 3-glycidoxypropyltrimethoxysilane to the aqueous solution of the tetramethylammonium hydroxide to the isopropanol is 90-100g.
Preferably, the mass-to-volume ratio of the epoxy POSS to the DMF in the step (2) is 1g; the mass ratio of NaOH, glycol, triethylene tetramine and epoxy POSS added is 1-3.
Preferably, the mass ratio of the POSS modified amine curing agent to the dicyandiamide to the urea in the step (3) is (10); the mass fraction of the phytic acid aqueous solution is 20-40%, and the mass ratio of the phytic acid in the phytic acid aqueous solution to the POSS modified amine curing agent is 1; the volume ratio of the phytic acid aqueous solution to the toluene is 1.
Therefore, the invention has the following beneficial effects:
(1) The mirror body is embedded into the frame from the front side, so that the front side of the mirror body is not shielded by the frame, the utilization rate is high, the visual field is wide, and the mirror image acquisition and use effects are improved;
(2) The periphery of the mirror body is polished into bevel edges, so that the five-plane refraction effect is obtained, and the attractiveness of the mirror edge is highlighted;
(3) The POSS and the phytic acid are used for modifying the epoxy resin adhesive, so that the impact resistance and the peel strength of the adhesive are improved, and the oxidation, corrosion and color change of the edge of the lens body can be effectively prevented.
Drawings
Fig. 1 is a schematic view of an exploded structure of embodiment 1 of the present invention.
Fig. 2 is a schematic structural view of a frame in embodiment 1 of the present invention.
FIG. 3 is a sectional view of example 1 of the present invention.
In the figure: 1 frame, 101 groove, 102 anti-slip texture, 2 lens body, 201 bevel edge, 3 protective film and 4 adhesive.
Detailed Description
The invention is further described with reference to the following figures and embodiments.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
as shown in fig. 1 to 3, a mirror to be mounted from the front comprises a rectangular frame 1 and a mirror body 2. The front surface of the frame is provided with a groove 101, the depth of the groove of the frame is 1.2cm, the back surface of the frame is provided with a protective film 3 for sealing the back surface of the frame, the protective film adopts kraft paper, and the periphery of the kraft paper is bonded with the back surface of the frame; the side of the frame is provided with anti-skid lines 102 which are uniformly distributed in a pit shape. The mirror body is embedded into the groove of the frame from the front side, the back side of the mirror body is bonded with the frame through an adhesive 4, the edge of the mirror body is polished into a bevel edge 201, the periphery of the mirror body is polished, and the mirror body is a commercially available aluminum mirror with the thickness of 0.7 cm.
The adhesive is a two-component epoxy resin adhesive and comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 2.5; the component A comprises the following raw materials in parts by weight: 95 parts of an epoxy resin E51,4 parts of a diluent 1, 4-butanediol diglycidyl ether; the component B comprises the following raw materials: 85 parts of phytic acid and POSS modified amine curing agent, 4 parts of dimethyl imidazole and 9 parts of toluene.
The preparation method of the phytic acid and POSS modified amine curing agent comprises the following steps:
(1) Adding 3-glycidoxypropyltrimethoxysilane and 6wt% of aqueous solution of tetramethylammonium hydroxide into isopropanol, wherein the addition ratio of the 3-glycidoxypropyltrimethoxysilane to the aqueous solution of the tetramethylammonium hydroxide to the isopropanol is 9540g; stirring for reacting for 6 hours, then carrying out reduced pressure distillation to remove isopropanol, then adding toluene to dissolve the product, carrying out reflux reaction at 75 ℃ for 5.5 hours, washing the reacted solution with a saturated sodium chloride solution to be neutral, separating to obtain an organic phase, and carrying out rotary evaporation and drying to obtain epoxy group POSS;
(2) Dissolving epoxy POSS in DMF, wherein the mass-volume ratio of the epoxy POSS to the DMF is 1g; adding ethylene glycol, stirring uniformly, adding NaOH, and stirring at 70 ℃ for reaction for 2.5 hours; then adding triethylenetetramine, and continuing to perform heat preservation reaction for 4 hours, wherein the mass ratio of the added NaOH, ethylene glycol, triethylenetetramine to epoxy group POSS is 2.8; removing the solvent by rotary evaporation and drying to obtain the POSS modified amine curing agent;
(3) Dissolving a POSS modified amine curing agent in dimethyl sulfoxide, and adding dicyandiamide and urea, wherein the mass ratio of the POSS modified amine curing agent to the dicyandiamide to the urea is (10); heating to 105 ℃ under the protection of nitrogen, and then adding 30wt% of phytic acid aqueous solution and toluene, wherein the mass ratio of the phytic acid in the phytic acid aqueous solution to the POSS modified amine curing agent is 1; the volume ratio of the phytic acid aqueous solution to the toluene is 1; and precipitating the product by using absolute ethyl alcohol, washing and drying the precipitated product to obtain the phytic acid and POSS modified amine curing agent.
When the mirror is installed, the mirror body is cut, edge grinding is carried out by a numerical control edge grinding machine, polishing is carried out, the component A and the component B of the double-component epoxy resin adhesive are mixed in proportion and then coated on the periphery of the back of the mirror body, then the mirror body is placed into the groove in the front of the frame from the front, finally kraft paper is pasted to the back of the frame, and curing is carried out for 12 hours at the temperature of 80 ℃.
Example 2:
the mirror structure and mounting method in example 2 were the same as in example 1; the used double-component epoxy resin adhesive comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 2; the component A comprises the following raw materials in parts by weight: 90 parts of epoxy resin E51,3 parts of diluent 1, 4-butanediol diglycidyl ether; the component B comprises the following raw materials: 80 parts of phytic acid and POSS modified amine curing agent, 3 parts of dimethyl imidazole and 8 parts of toluene.
The preparation method of the phytic acid and POSS modified amine curing agent comprises the following steps:
(1) Adding 3-glycidoxypropyltrimethoxysilane and a 5wt% aqueous solution of tetramethylammonium hydroxide into isopropanol, wherein the addition ratio of the 3-glycidoxypropyltrimethoxysilane to the aqueous solution of the tetramethylammonium hydroxide to the isopropanol is 9045g; stirring for reacting for 5h, then carrying out reduced pressure distillation to remove isopropanol, adding toluene to dissolve the product, carrying out reflux reaction at 70 ℃ for 6h, washing the reacted solution with a saturated sodium chloride solution to neutrality, separating to obtain an organic phase, and carrying out rotary evaporation and drying to obtain epoxy group POSS;
(2) Dissolving epoxy POSS in DMF, wherein the mass-to-volume ratio of epoxy POSS to DMF is 1g; adding ethylene glycol, stirring uniformly, adding NaOH, and stirring at 60 ℃ for reaction for 3 hours; then adding triethylenetetramine, and continuing to perform heat preservation reaction for 5 hours, wherein the mass ratio of the added NaOH, ethylene glycol, triethylenetetramine to epoxy group POSS is 1.5; removing the solvent by rotary evaporation and drying to obtain the POSS modified amine curing agent;
(3) Dissolving a POSS modified amine curing agent in dimethyl sulfoxide, and adding dicyandiamide and urea, wherein the mass ratio of the POSS modified amine curing agent to the dicyandiamide to the urea is 10.3; heating to 100 ℃ under the protection of nitrogen, and then adding 20wt% of phytic acid aqueous solution and toluene, wherein the mass ratio of the phytic acid in the phytic acid aqueous solution to the POSS modified amine curing agent is 1; the volume ratio of the phytic acid aqueous solution to the toluene is 1; and precipitating the product by using absolute ethyl alcohol, washing and drying the precipitated product to obtain the phytic acid and POSS modified amine curing agent.
Example 3:
the mirror structure and mounting method in example 3 are the same as in example 1; the used two-component epoxy resin adhesive comprises a component A and a component B in a mass ratio of 3; the component A comprises the following raw materials in parts by weight: 100 parts of epoxy resin E51,5 parts of diluent 1, 4-butanediol diglycidyl ether; the component B comprises the following raw materials: 90 parts of phytic acid and POSS modified amine curing agent, 5 parts of dimethyl imidazole and 10 parts of toluene.
The preparation method of the phytic acid and POSS modified amine curing agent comprises the following steps:
(1) Adding 3-glycidoxypropyltrimethoxysilane and 8wt% of aqueous solution of tetramethyl ammonium hydroxide into isopropanol, wherein the addition ratio of the 3-glycidoxypropyltrimethoxysilane to the aqueous solution of the tetramethyl ammonium hydroxide to the isopropanol is 10035g; stirring for reacting for 6h, then carrying out reduced pressure distillation to remove isopropanol, adding toluene to dissolve the product, carrying out reflux reaction for 5h at 80 ℃, washing the reacted solution to be neutral by using a saturated sodium chloride solution, separating to obtain an organic phase, and carrying out rotary evaporation and drying to obtain epoxy group POSS;
(2) Dissolving epoxy POSS in DMF, wherein the mass-to-volume ratio of epoxy POSS to DMF is 1g; adding ethylene glycol, stirring uniformly, adding NaOH, and stirring at 80 ℃ for reaction for 2 hours; then adding triethylenetetramine, and continuing to perform heat preservation reaction for 3h, wherein the mass ratio of the added NaOH, ethylene glycol, triethylenetetramine to epoxy group POSS is 3; removing the solvent by rotary evaporation and drying to obtain the POSS modified amine curing agent;
(3) Dissolving a POSS modified amine curing agent in dimethyl sulfoxide, and adding dicyandiamide and urea, wherein the mass ratio of the POSS modified amine curing agent to the dicyandiamide to the urea is 10.5; heating to 110 ℃ under the protection of nitrogen, and then adding 40wt% of phytic acid aqueous solution and toluene, wherein the mass ratio of the phytic acid in the phytic acid aqueous solution to the POSS modified amine curing agent is 1; the volume ratio of the phytic acid aqueous solution to the toluene is 1; and precipitating the product by using absolute ethyl alcohol, washing and drying the precipitated product to obtain the phytic acid and POSS modified amine curing agent.
Comparative example 1 (no POSS and phytic acid added):
the mirror structure and mounting method in comparative example 1 were the same as in example 1; the used two-component epoxy resin adhesive comprises a component A and a component B in a mass ratio of 2.5; the component A comprises the following raw materials in parts by weight: 95 parts of an epoxy resin E51,4 parts of a diluent 1, 4-butanediol diglycidyl ether; the component B comprises the following raw materials: 30 parts of triethylenetetramine, 4 parts of dimethylimidazole and 9 parts of toluene.
Comparative example 2 (no phytic acid added):
the mirror structure and mounting method in comparative example 2 were the same as in example 1; the used two-component epoxy resin adhesive comprises a component A and a component B in a mass ratio of 2.5; the component A comprises the following raw materials in parts by weight: 95 parts of epoxy resin E51,4 parts of diluent 1, 4-butanediol diglycidyl ether; the component B comprises the following raw materials: 85 parts of POSS modified amine curing agent, 4 parts of dimethyl imidazole and 9 parts of toluene.
The preparation method of the POSS modified amine curing agent comprises the following steps:
(1) Adding 3-glycidoxypropyltrimethoxysilane and 6wt% of aqueous solution of tetramethylammonium hydroxide into isopropanol, wherein the addition ratio of the 3-glycidoxypropyltrimethoxysilane to the aqueous solution of the tetramethylammonium hydroxide to the isopropanol is 95g; stirring for reacting for 6h, then carrying out reduced pressure distillation to remove isopropanol, adding toluene to dissolve the product, carrying out reflux reaction at 75 ℃ for 5.5h, washing the reacted solution to neutrality by using a saturated sodium chloride solution, separating to obtain an organic phase, and carrying out rotary evaporation and drying to obtain epoxy group POSS;
(2) Dissolving epoxy POSS in DMF, wherein the mass-to-volume ratio of epoxy POSS to DMF is 1g; adding triethylenetetramine, stirring uniformly, adding NaOH, and stirring at 70 ℃ for reacting for 6h; the mass ratio of the added NaOH to the added triethylenetetramine to the added epoxy POSS is 2; and (4) removing the solvent by rotary evaporation and drying to obtain the POSS modified amine curing agent.
Comparative example 3 (phytic acid directly blended with curing agent):
the mirror structure and mounting method in comparative example 3 were the same as in example 1; the used two-component epoxy resin adhesive comprises a component A and a component B in a mass ratio of 2.5; the component A comprises the following raw materials in parts by weight: 95 parts of epoxy resin E51,4 parts of diluent 1, 4-butanediol diglycidyl ether; the component B comprises the following raw materials: 7 parts of phytic acid, 78 parts of POSS modified amine curing agent, 4 parts of dimethyl imidazole and 9 parts of toluene.
The preparation method of the POSS modified amine curing agent comprises the following steps:
(1) Adding 3-glycidoxypropyltrimethoxysilane and 6wt% of aqueous solution of tetramethylammonium hydroxide into isopropanol, wherein the addition ratio of the 3-glycidoxypropyltrimethoxysilane to the aqueous solution of the tetramethylammonium hydroxide to the isopropanol is 9540g; stirring for reacting for 6h, then carrying out reduced pressure distillation to remove isopropanol, adding toluene to dissolve the product, carrying out reflux reaction at 75 ℃ for 5.5h, washing the reacted solution to neutrality by using a saturated sodium chloride solution, separating to obtain an organic phase, and carrying out rotary evaporation and drying to obtain epoxy group POSS;
(2) Dissolving epoxy POSS in DMF, wherein the mass-volume ratio of the epoxy POSS to the DMF is 1g; adding triethylenetetramine, stirring uniformly, adding NaOH, and stirring at 70 ℃ for reaction for 6h; the mass ratio of the added NaOH to the added triethylenetetramine to the added epoxy POSS is 2; and (4) performing rotary evaporation to remove the solvent, and drying to obtain the POSS modified amine curing agent.
Comparative example 4 (phytic acid addition too much):
the mirror structure and mounting method in comparative example 4 were the same as in example 1; the components of the two-component epoxy resin adhesive used are also the same as those in example 1, wherein the preparation method of the phytic acid and POSS modified amine curing agent comprises the following steps:
(1) Adding 3-glycidoxypropyltrimethoxysilane and 6wt% of aqueous solution of tetramethylammonium hydroxide into isopropanol, wherein the addition ratio of the 3-glycidoxypropyltrimethoxysilane to the aqueous solution of the tetramethylammonium hydroxide to the isopropanol is 95g; stirring for reacting for 6h, then carrying out reduced pressure distillation to remove isopropanol, adding toluene to dissolve the product, carrying out reflux reaction at 75 ℃ for 5.5h, washing the reacted solution to neutrality by using a saturated sodium chloride solution, separating to obtain an organic phase, and carrying out rotary evaporation and drying to obtain epoxy group POSS;
(2) Dissolving epoxy POSS in DMF, wherein the mass-volume ratio of the epoxy POSS to the DMF is 1g; adding ethylene glycol, stirring uniformly, adding NaOH, and stirring at 70 ℃ for reaction for 2.5 hours; then adding triethylenetetramine, and continuing to perform heat preservation reaction for 4h, wherein the mass ratio of the added NaOH, ethylene glycol, triethylenetetramine to epoxy group POSS is (2); removing the solvent by rotary evaporation and drying to obtain the POSS modified amine curing agent;
(3) Dissolving a POSS modified amine curing agent in dimethyl sulfoxide, and adding dicyandiamide and urea, wherein the mass ratio of the POSS modified amine curing agent to the dicyandiamide to the urea is (10); heating to 105 ℃ under the protection of nitrogen, and then adding 30wt% of phytic acid aqueous solution and toluene, wherein the mass ratio of the phytic acid in the phytic acid aqueous solution to the POSS modified amine curing agent is 1; the volume ratio of the phytic acid aqueous solution to the toluene is 1; and precipitating the product by using absolute ethyl alcohol, washing and drying the precipitated product to obtain the phytic acid and POSS modified amine curing agent.
The two-component epoxy adhesives of the above examples and comparative examples were tested for performance according to methods in GB/T7124-2008 (rigid material vs rigid material) and GB/T7122, with the results shown in Table 1.
Table 1: and (5) testing the performance of the two-component epoxy resin binder.
Figure BDA0003268636540000081
The kraft paper layers of the mirrors prepared in the above examples and comparative examples were peeled off, and placed in a 5% NaOH aqueous solution, and heat-insulated at 25 ℃ for 12 hours, and the change of color of the aluminized layer around the mirror body was observed, and the results are shown in table 2.
Table 2: and testing the corrosion inhibition performance of the mirror.
Figure BDA0003268636540000082
As can be seen from tables 1 and 2, the two-component epoxy resin adhesive in the embodiments 1 to 3 of the present invention has high tensile shear strength and peel strength, good cohesiveness, and good firmness and safety when used for adhering and fixing the mirror body and the frame; and the aluminum layer at the edge of the mirror body can be effectively prevented from being oxidized and discolored, so that the attractiveness of the mirror is ensured.
POSS and phytic acid are not added into the adhesive in the comparative example 1 to modify the amine curing agent, the cohesiveness of the adhesive is obviously reduced compared with that in the example 1, the use risk of inlaying the mirror from the front is increased, and the aluminum layer at the edge of the mirror is easy to oxidize and corrode to change color, so that the service life of the mirror is influenced; in the comparative example 2, phytic acid is not modified on POSS, and the corrosion inhibition of the adhesive to an aluminum layer is reduced; in the comparative example 3, the phytic acid is directly added into the component B without being modified on POSS, so that the compatibility of the phytic acid and an epoxy resin matrix is poor, the bonding performance of the adhesive is reduced, and the corrosion inhibition of the adhesive on an aluminum layer is also reduced; in comparative example 4, too much phytic acid modified on POSS also causes the reduction of the bonding performance of the adhesive, probably because the steric hindrance of the phytic acid is larger, and the addition of too much phytic acid can influence the steric hindrance of the curing agent when reacting with epoxy resin, thereby reducing the bonding performance of the curing agent.

Claims (8)

1. A mirror embedded from the front is characterized by comprising a frame (1) and a mirror body (2), wherein the front of the frame is provided with a groove (101), the mirror body is embedded into the groove of the frame from the front, and the back of the mirror body is bonded with the frame through an adhesive (4);
the adhesive is a two-component epoxy resin adhesive, and the two-component epoxy resin adhesive comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 2-3; the component A comprises the following raw materials in parts by weight: 90 to 100 parts of bisphenol A type epoxy resin and 3 to 5 parts of diluent; the component B comprises the following raw materials: 80-90 parts of phytic acid and POSS modified amine curing agent, 3-5 parts of curing accelerator and 8-10 parts of toluene;
the preparation method of the phytic acid and POSS modified amine curing agent comprises the following steps:
(1) Adding an aqueous solution of 3-glycidyloxypropyltrimethoxysilane and tetramethylammonium hydroxide into isopropanol, stirring for reaction for 5 to 7 hours, distilling under reduced pressure to remove the isopropanol, adding toluene to dissolve the product, carrying out reflux reaction at 70 to 80 ℃ for 5 to 6 hours, washing the reacted solution with a saturated sodium chloride solution to neutrality, separating to obtain an organic phase, and carrying out rotary evaporation and drying to obtain epoxy group POSS;
(2) Dissolving epoxy POSS in DMF, adding ethylene glycol, stirring uniformly, adding NaOH, and reacting at 60-80 ℃ for 2-3 h; then adding triethylenetetramine, and continuing to react for 3 to 5 hours under the condition of heat preservation; removing the solvent by rotary evaporation and drying to obtain the POSS modified amine curing agent;
(3) Dissolving a POSS modified amine curing agent in dimethyl sulfoxide, adding dicyandiamide and urea, heating to 100-110 ℃ under the protection of nitrogen, adding phytic acid aqueous solution and toluene, and stirring to react for 1-3h; and precipitating the product by using absolute ethyl alcohol, washing and drying the precipitated product to obtain the phytic acid and POSS modified amine curing agent.
2. A mirror for mounting from the front as claimed in claim 1, wherein the depth of said recess is greater than or equal to the thickness of the mirror body.
3. A mirror inlaid from the front according to claim 1 or 2, wherein the edge of said mirror body is polished to a bevel edge (201); the periphery of the mirror body is polished.
4. A mirror inlaid from the front as claimed in claim 1, wherein said frame has a protective film (3) on the back surface for sealing the back surface of the frame.
5. A mirror inlaid from the front as claimed in claim 1, wherein the side of said frame is provided with anti-slip texture (102).
6. The mirror inlaid from the front face according to claim 1, wherein the mass fraction of the aqueous solution of tetramethylammonium hydroxide in step (1) is 5 to 8%; the addition ratio of the 3-glycidoxypropyltrimethoxysilane to the aqueous solution of tetramethylammonium hydroxide to the isopropanol is 90 to 100g.
7. The mirror inlaid from the front face of claim 1, wherein the mass volume ratio of the epoxy POSS to the DMF in the step (2) is 1g; the mass ratio of NaOH, ethylene glycol, triethylene tetramine and epoxy group POSS added is 1 to 3.
8. The mirror inlaid from the front surface according to claim 1, wherein the mass ratio of the POSS modified amine curing agent, dicyandiamide and urea in the step (3) is 10.3 to 0.5; the mass fraction of the phytic acid aqueous solution is 20 to 40%, and the mass ratio of the phytic acid in the phytic acid aqueous solution to the POSS modified amine curing agent is 1 to 10 to 15; the volume ratio of the phytic acid aqueous solution to the toluene is 1 to 5-10.
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NL1011470C1 (en) * 1999-03-05 2000-09-06 Innoessentials Internat B V Mirror assembly with anti-fog feature.
US7093403B2 (en) * 2003-09-16 2006-08-22 Mirrormate, Llc Frame for mounting to a premounted mirror
CN104721847A (en) * 2013-12-19 2015-06-24 西安华雍机电科技有限公司 Mirror surface clothing disinfection cabinet
CN207444533U (en) * 2017-09-08 2018-06-05 嘉兴市成泰镜业有限公司 A kind of anticorrosion mirror
CN207461661U (en) * 2017-11-23 2018-06-08 广州市天霸美容美发用品有限公司 A kind of portable hand-held mirror
CN208550776U (en) * 2018-05-07 2019-03-01 中山建御照明有限公司 A kind of OLED mirror
CN208625118U (en) * 2018-07-04 2019-03-22 程立群 A kind of mirror that band cleaning is scraped
CN209547636U (en) * 2018-12-24 2019-10-29 嘉兴市大树镜业有限公司 One kind just installing mirror
CN111772431A (en) * 2019-04-04 2020-10-16 上海睿光新材料科技有限公司 Safe mirror and preparation method thereof

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