CN117946575B - Coating material for camera lens ring and preparation method and application thereof - Google Patents
Coating material for camera lens ring and preparation method and application thereof Download PDFInfo
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- CN117946575B CN117946575B CN202410012586.7A CN202410012586A CN117946575B CN 117946575 B CN117946575 B CN 117946575B CN 202410012586 A CN202410012586 A CN 202410012586A CN 117946575 B CN117946575 B CN 117946575B
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- matting agent
- polyaspartic
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- 238000000576 coating method Methods 0.000 title claims abstract description 73
- 239000011248 coating agent Substances 0.000 title claims abstract description 72
- 239000000463 material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000006224 matting agent Substances 0.000 claims abstract description 170
- MTZQAGJQAFMTAQ-UHFFFAOYSA-N ethyl benzoate Chemical compound CCOC(=O)C1=CC=CC=C1 MTZQAGJQAFMTAQ-UHFFFAOYSA-N 0.000 claims abstract description 104
- 150000002148 esters Chemical class 0.000 claims abstract description 81
- 108010064470 polyaspartate Proteins 0.000 claims abstract description 61
- 229920000805 Polyaspartic acid Polymers 0.000 claims abstract description 46
- LDCRTTXIJACKKU-ARJAWSKDSA-N dimethyl maleate Chemical compound COC(=O)\C=C/C(=O)OC LDCRTTXIJACKKU-ARJAWSKDSA-N 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 42
- 229920000608 Polyaspartic Polymers 0.000 claims abstract description 33
- -1 mercaptosiloxane Chemical class 0.000 claims abstract description 22
- YCGLLKBCDJTRBY-UHFFFAOYSA-N but-1-ene-1,1-diamine Chemical compound CCC=C(N)N YCGLLKBCDJTRBY-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012948 isocyanate Substances 0.000 claims abstract description 13
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 13
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012986 modification Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 21
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 20
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 20
- 239000006185 dispersion Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000006845 Michael addition reaction Methods 0.000 claims description 13
- 239000006229 carbon black Substances 0.000 claims description 13
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 12
- 239000002041 carbon nanotube Substances 0.000 claims description 12
- 229910021389 graphene Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 6
- 238000005809 transesterification reaction Methods 0.000 claims description 6
- 125000003396 thiol group Chemical class [H]S* 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 125000003277 amino group Chemical group 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 150000002978 peroxides Chemical class 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 32
- 239000011347 resin Substances 0.000 abstract description 32
- 239000011159 matrix material Substances 0.000 abstract description 16
- 229920002396 Polyurea Polymers 0.000 abstract description 10
- 238000003384 imaging method Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 8
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 6
- 230000031700 light absorption Effects 0.000 abstract description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 230000008033 biological extinction Effects 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000004342 Benzoyl peroxide Substances 0.000 description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 8
- 235000019400 benzoyl peroxide Nutrition 0.000 description 8
- 239000003822 epoxy resin Substances 0.000 description 6
- 229920000647 polyepoxide Polymers 0.000 description 6
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- PUSKHXMZPOMNTQ-UHFFFAOYSA-N ethyl 2,1,3-benzoselenadiazole-5-carboxylate Chemical group CCOC(=O)C1=CC=C2N=[Se]=NC2=C1 PUSKHXMZPOMNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000006838 isophorone group Chemical group 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/02—Polyureas
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/42—Gloss-reducing agents
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/111—Anti-reflection coatings using layers comprising organic materials
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a coating material for a camera lens ring, a preparation method and application thereof, wherein the preparation method comprises the following steps: preparing ethyl benzoate modified polyaspartic ester; sequentially carrying out surface modification on the matting agent by mixed acid of concentrated sulfuric acid and concentrated nitric acid, mercaptosiloxane, diaminobutene and dimethyl maleate; uniformly mixing the surface modified matting agent and the polyaspartic ester modified by the ethyl benzoate to obtain a component A; the A component and the B component comprising isocyanate curing agent are stored independently. The polyaspartic acid ester polyurea resin obtained by the reaction of the polyaspartic acid ester and the isocyanate curing agent is used as matrix resin, polyaspartic acid ester is used for modifying the surface of the matting agent, and the coating material has excellent adhesive force, wear resistance and corrosion resistance through the adjustment of the polyaspartic acid ester structure on the surfaces of the matrix resin and the matting agent; meanwhile, the coating material has good light absorption performance, can effectively eliminate stray light, and improves the imaging effect of a camera.
Description
Technical Field
The invention relates to the field of coatings, in particular to a coating material for a camera lens ring, a preparation method and application thereof.
Background
The lens is one of the most important components of the camera, and the camera lens ring can play a role in protecting the lens and enhancing the imaging effect of the lens, and is also an important component in the camera. Firstly, the lens ring is used as a peripheral component, so that a certain degree of protection can be provided for the lens to prevent the lens from direct contact and collision; dust and dirt on the surface of the lens can be prevented from entering, and the lens is kept clean. Secondly, when light passes through the lens, the light can be disturbed by stray light, so that the imaging effect is reduced, and the probability that the light deviating from the main light beam enters the lens is reduced by shielding the non-main light beam and the scattered light beam by the lens ring, so that scattering and disturbance are reduced, and imaging is clearer.
In order to make the camera lens ring effectively protect the lens and reduce the interference of stray light on imaging, a coating material with high light absorption is generally coated on the surface of the lens ring in the prior art. For example, the publication number CN101497763a of the "a two-component matting coating for optical use and a method for producing the same" disclosed in the chinese patent literature is composed of a two component a, b, wherein the component a includes polyurethane modified epoxy resin (20% -60%), phenolic epoxy resin (10% -30%), high pigment carbon black (1% -5%), high light absorption nanomaterial (1% -5%), additive (1% -10%), matting agent (1% -4%), mixed anti-aging agent (0.5% -2%), diluent (0% -40%), and the component b includes epoxy curing agent (70% -90%), silane coupling agent (0% -3%), diluent (10% -30%).
The extinction coating for the camera lens in the prior art generally adopts epoxy resin as a matrix material, but the epoxy resin has poor corrosion resistance, poor coating adhesive force and wear resistance, and can lead to shorter service life of the camera lens; moreover, the extinction performance of the extinction coating in the prior art is generally insufficient, which is not beneficial to eliminating stray light of a camera lens ring.
Disclosure of Invention
The invention aims to overcome the problems of the coating material for the camera lens in the prior art, and provides the coating material for the camera lens, a preparation method and application thereof, wherein polyaspartic acid ester polyurea resin obtained by the reaction of polyaspartic acid ester and isocyanate curing agent is used as matrix resin, polyaspartic acid ester is used for modifying the surface of a flatting agent, and the coating material has excellent adhesive force, wear resistance and corrosion resistance by adjusting the structures of the polyaspartic acid ester on the matrix resin and the surface of the flatting agent, so that the service life of the camera lens is prolonged; meanwhile, the coating material has good light absorption performance, can effectively eliminate stray light, and improves the imaging effect of a camera.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a coating material for a camera rim, comprising the steps of:
(1) Preparation of ethyl benzoate modified polyaspartic esters: firstly, carrying out Michael addition reaction on dimethyl maleate and isophorone diamine to obtain polyaspartic acid ester; then, carrying out transesterification on ethyl benzoate and polyaspartic ester to obtain ethyl benzoate modified polyaspartic ester;
(2) Surface modifying the matting agent: sequentially reacting mixed acid of concentrated sulfuric acid and concentrated nitric acid, mercaptosiloxane, diaminobutene and dimethyl maleate with a matting agent to obtain a surface modified matting agent; the matting agent comprises graphene, carbon nanotubes and carbon black;
(3) Uniformly mixing the surface modified matting agent and the polyaspartic ester modified by the ethyl benzoate to obtain a component A;
(4) And (3) independently storing the component A and the component B comprising the isocyanate curing agent to obtain the coating material for the camera lens.
Compared with the epoxy resin adopted by the traditional matting paint, the polyaspartate polyurea resin has better adhesive force, wear resistance and corrosion resistance, and is beneficial to prolonging the service life of a camera lens ring. The traditional polyaspartic acid ester is generally prepared by using dialkyl maleate and diprimary amine through Michael addition reaction, isophorone diamine with rigid groups is selected to react with dimethyl maleate, polyaspartic acid ester polyurea resin with rigid groups in a main chain can be obtained, ethyl benzoate is further adopted to modify the polyaspartic acid ester polyurea resin, and the rigid groups are also introduced into side chains of the polyurea resin, so that the wear resistance, scratch resistance and mechanical property of a coating material can be further improved, and the service life of a camera lens ring is prolonged.
Meanwhile, in order to enable the coating material to have good extinction performance and improve the capability of the camera lens ring in eliminating stray light, the extinction agent comprising graphene, carbon nano tubes and carbon black is added into the coating material, and can effectively absorb visible light and eliminate the influence of the stray light on the imaging effect of a camera. In addition, the surface of the matting agent is modified, the surface of the matting agent is treated by concentrated sulfuric acid and concentrated nitric acid, and hydroxyl is introduced to the surface of the matting agent; then, the hydroxylated matting agent reacts with mercaptosiloxane, and mercapto is introduced to the surface of the matting agent; then introducing amino groups on the surface of the matting agent through click chemical reaction of the sulfhydrylation matting agent and diaminobutene; finally, through the Michael addition reaction of the aminated matting agent and the dimethyl maleate, polyaspartic acid ester is bonded on the surface of the matting agent through chemical bonds, and on one hand, the connection of the polyaspartic acid ester can promote the dispersibility of the matting agent in matrix resin, and avoid the influence of aggregation of the matting agent on the mechanical property and the light absorption property of the coating; on the other hand, the polyaspartate obtained by adopting the reaction of diaminobutene and dimethyl maleate has larger flexibility of molecular chains and smaller steric hindrance compared with matrix resin through adjusting the molecular structure of polyaspartate on the surface of the matting agent, so that the resin on the surface of the matting agent and the matrix resin have different curing rates and curing shrinkage rates, the non-uniformity of the cured coating is improved, and a defect structure is generated in the coating; meanwhile, the graphene, the carbon nano tube and the carbon black with different dimensions and forms are used as the matting agent together, so that the formation of a defect structure is facilitated in the curing process; the generation of the defect structure can greatly increase the reflection path of incident light, further reduce the reflectivity of the coating to visible light and improve the capability of the coating to eliminate stray light.
Therefore, the coating material prepared by the invention has excellent adhesive force, wear resistance and corrosion resistance, and is beneficial to prolonging the service life of the camera lens ring; meanwhile, the coating material has good extinction performance, can effectively eliminate stray light, and improves the imaging effect of a camera.
Preferably, in the step (1), the molar ratio of the dimethyl maleate to the isophorone diamine in the Michael addition reaction is 2-2.2:1; the molar ratio of the ethyl benzoate to the polyaspartic ester is 3.5-4.5:1 when the transesterification reaction is carried out.
Preferably, the reaction conditions for the Michael addition reaction of dimethyl maleate and isophorone diamine in step (1) are: under the protection of nitrogen, adding dimethyl maleate into isophorone diamine, and reacting for 12-24 hours at 65-75 ℃ to obtain the polyaspartic acid ester.
Preferably, the reaction conditions for transesterification of polyaspartate with ethyl benzoate in step (1) are: adding polyaspartic acid ester and ethyl benzoate into an organic solvent for dissolution, adding a sodium methoxide catalyst, reacting for 4-6 hours at 125-135 ℃, and removing the solvent to obtain the ethyl benzoate modified polyaspartic acid ester.
Preferably, when the surface of the matting agent is modified in the step (2), firstly, a mixed acid of concentrated sulfuric acid and concentrated nitric acid is used for reacting with the matting agent to obtain a hydroxylated matting agent;
Then, the hydroxylated matting agent reacts with mercaptosiloxane to obtain the mercapto matting agent; the mass ratio of the hydroxylated matting agent to the mercaptosiloxane is 1-2:1;
Then, the sulfamized matting agent is obtained through click chemistry reaction of the sulfhydrylized matting agent and diaminobutene; the mass ratio of the sulfhydrylation flatting agent to the diaminobutene is 3-5:1;
Finally, the surface modified matting agent is obtained through Michael addition reaction of the aminated matting agent and dimethyl maleate; the mass ratio of the aminated matting agent to the dimethyl maleate is 3-5:1.
Preferably, when the mixed acid of concentrated sulfuric acid and concentrated nitric acid is used for the reaction with the matting agent in the step (2), the reaction conditions are as follows: the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 3-5:1, the mass volume ratio of the matting agent to the mixed acid is 1 g:50-100 mL, the reaction time is 3-5 h, and the product is washed to be neutral after the reaction;
The conditions for the reaction of the hydroxylated matting agent with the mercaptosiloxane are: dispersing the hydroxylated matting agent in deionized water to obtain a dispersion liquid, wherein the mass volume ratio of the hydroxylated matting agent to the deionized water is 1 g:200-300 mL; adding ethanol solution of mercaptosiloxane with the mass concentration of 30-40% into the dispersion liquid, stirring and reacting for 8-12 h at 50-60 ℃, and washing the product to obtain the mercapto matting agent;
the click chemistry reaction conditions of the sulfhydrylation flatting agent and the diaminobutene are as follows: dispersing a sulfhydrylation flatting agent in an organic solvent, adding diaminobutene and a peroxide initiator, reacting for 12-24 hours at 80-100 ℃, and washing a product to obtain the aminated flatting agent;
The Michael addition reaction conditions of the aminated matting agent and dimethyl maleate are: dispersing the aminated matting agent in an organic solvent, then dropwise adding dimethyl maleate under the protection of nitrogen, reacting for 12-24 hours at 65-75 ℃, and washing the product to obtain the surface modified matting agent.
Preferably, the mass ratio of graphene, carbon nanotubes and carbon black in the matting agent is 2-4:1-3:1.
Preferably, in the step (3), 5 to 8 parts by weight of the surface-modified matting agent and 90 to 100 parts by weight of the ethyl benzoate-modified polyaspartate are uniformly mixed to obtain the component A.
In a second aspect, the invention provides a coating material for a camera lens ring, which is prepared by the preparation method, wherein the mass ratio of the component A to the component B is 10:5-8 when the coating material is used.
In a third aspect, the present invention provides an application of a coating material for a camera lens ring manufactured by the manufacturing method in the camera lens ring.
Therefore, the invention has the following beneficial effects:
(1) Compared with the epoxy resin adopted by the traditional extinction coating, the polyaspartate polyurea resin is adopted as the matrix resin of the coating material, has better adhesive force, wear resistance and corrosion resistance, and is beneficial to prolonging the service life of the camera lens;
(2) When preparing matrix resin, isophorone diamine with rigid groups is selected to react with dimethyl maleate to obtain polyaspartate polyurea resin with rigid groups in the main chain, ethyl benzoate is further adopted to modify the polyaspartate polyurea resin, and the rigid groups are also introduced into the side chains of the polyurea resin, so that the wear resistance, scratch resistance and mechanical properties of the coating material can be further improved;
(3) Polyaspartic acid ester is bonded on the surface of the matting agent through chemical bonds, and the resin on the surface of the matting agent and the matrix resin can have different curing rates and curing shrinkage rates through adjusting the molecular structure of the polyaspartic acid ester on the surface of the matting agent, so that a defect structure is generated in the coating, the reflection path of incident light can be greatly increased, the reflectivity of the coating to visible light is reduced, and the capability of the coating to eliminate stray light is improved.
Detailed Description
The invention is further described below in connection with the following detailed description.
In the present invention, all raw materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
General examples:
a coating material for a camera lens ring comprises a component A and a component B in a mass ratio of 10:5-8; the component A comprises 90-100 parts of polyaspartic ester modified by ethyl benzoate and 5-8 parts of matting agent modified by surface by weight; the component B comprises isocyanate curing agent;
The preparation method of the coating material for the camera lens ring comprises the following steps:
(1) Preparation of ethyl benzoate modified polyaspartic esters: dropwise adding dimethyl maleate into isophorone diamine under the protection of nitrogen and continuous stirring, and reacting for 12-24 hours at 65-75 ℃ to obtain polyaspartic acid ester, wherein the molar ratio of the dimethyl maleate to isophorone diamine is 2-2.2:1; adding polyaspartic acid ester and ethyl benzoate into an organic solvent according to a molar ratio of 1:3.5-4.5, stirring and dissolving, adding a sodium methoxide catalyst, wherein the adding amount of sodium methoxide is 0.05-0.1% of the total mass of polyaspartic acid ester and ethyl benzoate, reacting for 4-6 hours at 125-135 ℃, and removing the solvent to obtain the ethyl benzoate modified polyaspartic acid ester; (2) preparing a surface-modified matting agent:
A) Mixing graphene, carbon nano tubes and carbon black according to a mass ratio of 2-4:1-3:1 to obtain a matting agent; adding a matting agent into mixed acid of concentrated sulfuric acid and concentrated nitric acid with the volume ratio of 3-5:1, wherein the mass volume ratio of the matting agent to the mixed acid is 1 g:50-100 mL, carrying out ultrasonic treatment for 3-5 h, and washing the treated product to be neutral by deionized water to obtain a hydroxylated matting agent;
B) Dispersing the hydroxylated matting agent in deionized water to obtain a dispersion liquid, wherein the mass volume ratio of the hydroxylated matting agent to the deionized water is 1 g:200-300 mL; adding ethanol solution of mercaptosiloxane with the mass concentration of 30-40% into the dispersion liquid, enabling the mass ratio of the added hydroxylated matting agent to the mercaptosiloxane to be 1-2:1, stirring and reacting for 8-12 h at 50-60 ℃, and washing the product to obtain the mercaptolated matting agent;
C) Dispersing a sulfhydrylation flatting agent in DMF, adding diaminobutene and benzoyl peroxide initiator, wherein the mass ratio of the sulfhydrylation flatting agent to the diaminobutene is 3-5:1, the mass of benzoyl peroxide is 0.03-0.1% of the mass of the sulfhydrylation flatting agent, and after reacting for 12-24 hours at 80-100 ℃, washing the product to obtain the aminated flatting agent;
D) Dispersing an aminated matting agent in DMF (dimethyl formamide), dropwise adding dimethyl maleate under the protection of nitrogen and continuous stirring, reacting for 12-24 hours at the temperature of 65-75 ℃ with the mass ratio of the aminated matting agent to the dimethyl maleate being 3-5:1, and washing the product to obtain the surface modified matting agent;
(3) Uniformly mixing the surface modified matting agent and the polyaspartic ester modified by the ethyl benzoate according to a proportion to obtain a component A;
(4) And (3) independently storing the component A and the component B to obtain the coating material for the camera lens.
Example 1:
A coating material for a camera lens ring comprises a component A and a component B in a mass ratio of 10:7; the component A comprises 95 parts of polyaspartic ester modified by ethyl benzoate and 5 parts of matting agent modified by surface by weight; the component B is isocyanate curing agent N3800 (Kogyo);
The preparation method of the coating material for the camera lens ring comprises the following steps:
(1) Preparation of ethyl benzoate modified polyaspartic esters: dropwise adding dimethyl maleate into isophorone diamine under the protection of nitrogen and continuous stirring, and reacting for 18 hours at 70 ℃ with the molar ratio of the dimethyl maleate to isophorone diamine being 2.1:1 to obtain polyaspartic acid ester; adding polyaspartic acid ester and ethyl benzoate into toluene according to a molar ratio of 1:4, stirring and dissolving, adding a sodium methoxide catalyst, wherein the adding amount of sodium methoxide is 0.1% of the total mass of polyaspartic acid ester and ethyl benzoate, reacting for 5 hours at 130 ℃, and removing the solvent under reduced pressure to obtain the ethyl benzoate modified polyaspartic acid ester;
(2) Preparing a surface modified matting agent:
a) Mixing graphene, carbon nanotubes and carbon black according to a mass ratio of 3:2:1 to obtain a matting agent; adding a matting agent into mixed acid of concentrated sulfuric acid and concentrated nitric acid with the volume ratio of 4:1, wherein the mass volume ratio of the matting agent to the mixed acid is 1g:80mL, carrying out ultrasonic treatment for 4 hours, and washing the treated product to be neutral by deionized water to obtain a hydroxylated matting agent;
B) Dispersing the hydroxylated matting agent in deionized water to obtain a dispersion liquid, wherein the mass-volume ratio of the hydroxylated matting agent to the deionized water is 1g:250mL; adding 35% by mass of ethanol solution of mercaptosiloxane into the dispersion liquid, stirring and reacting for 10 hours at 55 ℃ with the mass ratio of the added hydroxylated matting agent to the mercaptosiloxane being 1.5:1, and washing the product with deionized water to obtain the mercaptolated matting agent;
C) Dispersing a sulfhydrylation flatting agent in DMF, adding diaminobutene and benzoyl peroxide initiator, wherein the mass ratio of the sulfhydrylation flatting agent to the diaminobutene is 4:1, the mass of benzoyl peroxide is 0.05% of the mass of the sulfhydrylation flatting agent, reacting for 18 hours at 90 ℃, and washing the product with ethanol to obtain the aminated flatting agent;
D) Dispersing an aminated matting agent in DMF (dimethyl formamide), dropwise adding dimethyl maleate under the protection of nitrogen and continuous stirring, reacting for 18 hours at 70 ℃ with the mass ratio of the aminated matting agent to the dimethyl maleate being 4:1, and washing the product with ethanol to obtain the surface modified matting agent;
(3) Uniformly mixing the surface modified matting agent and the polyaspartic ester modified by the ethyl benzoate according to a proportion to obtain a component A;
(4) And (3) independently storing the component A and the component B to obtain the coating material for the camera lens.
Example 2:
A coating material for a camera lens ring comprises a component A and a component B in a mass ratio of 10:7; the component A comprises 90 parts of polyaspartic ester modified by ethyl benzoate and 5 parts of matting agent modified by surface by weight; the component B is isocyanate curing agent N3800 (Kogyo);
The preparation method of the coating material for the camera lens ring comprises the following steps:
(1) Preparation of ethyl benzoate modified polyaspartic esters: dropwise adding dimethyl maleate into isophorone diamine under the protection of nitrogen and continuous stirring, and reacting for 24 hours at 65 ℃ with the molar ratio of the dimethyl maleate to isophorone diamine being 2:1 to obtain polyaspartic acid ester; adding polyaspartic acid ester and ethyl benzoate into toluene according to a molar ratio of 1:3.5, stirring and dissolving, adding a sodium methoxide catalyst, wherein the adding amount of sodium methoxide is 0.05% of the total mass of polyaspartic acid ester and ethyl benzoate, reacting for 4 hours at 135 ℃, and removing the solvent under reduced pressure to obtain the ethyl benzoate modified polyaspartic acid ester;
(2) Preparing a surface modified matting agent:
A) Mixing graphene, carbon nanotubes and carbon black according to a mass ratio of 4:3:1 to obtain a matting agent; adding a matting agent into mixed acid of concentrated sulfuric acid and concentrated nitric acid with the volume ratio of 3:1, wherein the mass volume ratio of the matting agent to the mixed acid is 1g:50mL, carrying out ultrasonic treatment for 5 hours, and washing the treated product to be neutral by deionized water to obtain a hydroxylated matting agent;
b) Dispersing the hydroxylated matting agent in deionized water to obtain a dispersion liquid, wherein the mass-volume ratio of the hydroxylated matting agent to the deionized water is 1 g/200 mL; adding an ethanol solution of mercaptosiloxane with the mass concentration of 30% into the dispersion liquid, enabling the mass ratio of the added hydroxylated matting agent to the mercaptosiloxane to be 1:1, stirring and reacting for 12 hours at 50 ℃, and washing the product with deionized water to obtain the mercaptolated matting agent;
C) Dispersing a sulfhydrylation flatting agent in DMF, adding diaminobutene and benzoyl peroxide initiator, wherein the mass ratio of the sulfhydrylation flatting agent to the diaminobutene is 3:1, the mass of benzoyl peroxide is 0.05% of the mass of the sulfhydrylation flatting agent, reacting for 24 hours at 80 ℃, and washing the product with ethanol to obtain the aminated flatting agent;
d) Dispersing an aminated matting agent in DMF (dimethyl formamide), dropwise adding dimethyl maleate under the protection of nitrogen and continuous stirring, reacting for 24 hours at the temperature of 65 ℃ with the mass ratio of the aminated matting agent to the dimethyl maleate being 3:1, and washing the product with ethanol to obtain the surface modified matting agent;
(3) Uniformly mixing the surface modified matting agent and the polyaspartic ester modified by the ethyl benzoate according to a proportion to obtain a component A;
(4) And (3) independently storing the component A and the component B to obtain the coating material for the camera lens.
Example 3:
A coating material for a camera lens ring comprises a component A and a component B in a mass ratio of 10:7; the component A comprises 100 parts of polyaspartic ester modified by ethyl benzoate and 8 parts of matting agent modified by surface by weight; the component B is isocyanate curing agent N3800 (Kogyo);
The preparation method of the coating material for the camera lens ring comprises the following steps:
(1) Preparation of ethyl benzoate modified polyaspartic esters: dropwise adding dimethyl maleate into isophorone diamine under the protection of nitrogen and continuous stirring, and reacting for 12 hours at 75 ℃ to obtain polyaspartic acid ester, wherein the molar ratio of the dimethyl maleate to isophorone diamine is 2.2:1; adding polyaspartic acid ester and ethyl benzoate into toluene according to a molar ratio of 1:4.5, stirring and dissolving, adding a sodium methoxide catalyst, wherein the adding amount of sodium methoxide is 0.1% of the total mass of polyaspartic acid ester and ethyl benzoate, reacting for 6 hours at 125 ℃, and removing the solvent under reduced pressure to obtain the ethyl benzoate modified polyaspartic acid ester;
(2) Preparing a surface modified matting agent:
A) Mixing graphene, carbon nanotubes and carbon black according to a mass ratio of 2:1:1 to obtain a matting agent; adding a matting agent into mixed acid of concentrated sulfuric acid and concentrated nitric acid with the volume ratio of 5:1, wherein the mass volume ratio of the matting agent to the mixed acid is 1g:100mL, carrying out ultrasonic treatment for 3 hours, and washing the treated product to be neutral by deionized water to obtain a hydroxylated matting agent;
B) Dispersing the hydroxylated matting agent in deionized water to obtain a dispersion liquid, wherein the mass-volume ratio of the hydroxylated matting agent to the deionized water is 1 g/300 mL; adding an ethanol solution of mercaptosiloxane with the mass concentration of 40% into the dispersion liquid, enabling the mass ratio of the added hydroxylated matting agent to the mercaptosiloxane to be 2:1, stirring and reacting for 8 hours at 60 ℃, and washing the product with deionized water to obtain the mercaptolated matting agent;
C) Dispersing a sulfhydrylation flatting agent in DMF, adding diaminobutene and benzoyl peroxide initiator, wherein the mass ratio of the sulfhydrylation flatting agent to the diaminobutene is 5:1, the mass of benzoyl peroxide is 0.05% of the mass of the sulfhydrylation flatting agent, reacting for 12 hours at 100 ℃, and washing the product with ethanol to obtain the aminated flatting agent;
D) Dispersing an aminated matting agent in DMF (dimethyl formamide), dropwise adding dimethyl maleate under the protection of nitrogen and continuous stirring, reacting for 12 hours at 75 ℃ with the mass ratio of the aminated matting agent to the dimethyl maleate being 5:1, and washing the product with ethanol to obtain the surface modified matting agent;
(3) Uniformly mixing the surface modified matting agent and the polyaspartic ester modified by the ethyl benzoate according to a proportion to obtain a component A;
(4) And (3) independently storing the component A and the component B to obtain the coating material for the camera lens.
Comparative example 1 (modification of polyaspartate with ethyl benzoate):
a coating material for a camera lens ring comprises a component A and a component B in a mass ratio of 10:7; the component A comprises 95 parts of polyaspartic acid ester and 5 parts of surface modified matting agent by weight; the component B is isocyanate curing agent N3800 (Kogyo); the preparation method of the coating material for the camera lens ring comprises the following steps:
(1) Preparation of polyaspartic acid ester: dropwise adding dimethyl maleate into isophorone diamine under the protection of nitrogen and continuous stirring, and reacting for 18 hours at 70 ℃ with the molar ratio of the dimethyl maleate to isophorone diamine being 2.1:1 to obtain polyaspartic acid ester;
(2) Preparing a surface modified matting agent: the procedure was the same as in example 1;
(3) Uniformly mixing the surface modified matting agent and polyaspartic ester in proportion to obtain a component A;
(4) And (3) independently storing the component A and the component B to obtain the coating material for the camera lens.
Comparative example 2 (no surface modification of matting agent):
A coating material for a camera lens ring comprises a component A and a component B in a mass ratio of 10:7; the component A comprises 95 parts of ethyl benzoate modified polyaspartic ester and 5 parts of matting agent by weight; the component B is isocyanate curing agent N3800 (Kogyo);
The preparation method of the coating material for the camera lens ring comprises the following steps:
(1) Preparation of ethyl benzoate modified polyaspartic esters: the procedure was the same as in example 1;
(2) Preparing a matting agent: mixing graphene, carbon nanotubes and carbon black according to a mass ratio of 3:2:1 to obtain a matting agent;
(3) Uniformly mixing a delustrant and ethyl benzoate modified polyaspartic ester according to a proportion to obtain a component A;
(4) And (3) independently storing the component A and the component B to obtain the coating material for the camera lens.
Comparative example 3 (matting agent surface does not bond polyaspartate):
A coating material for a camera lens ring comprises a component A and a component B in a mass ratio of 10:7; the component A comprises 90 parts of polyaspartic ester modified by ethyl benzoate and 5 parts of matting agent modified by surface by weight; the component B is isocyanate curing agent N3800 (Kogyo);
The preparation method of the coating material for the camera lens ring comprises the following steps:
(1) Preparation of ethyl benzoate modified polyaspartic esters: the procedure was the same as in example 1;
(2) Preparing a surface modified matting agent:
A) Mixing graphene, carbon nanotubes and carbon black according to a mass ratio of 4:3:1 to obtain a matting agent; adding a matting agent into mixed acid of concentrated sulfuric acid and concentrated nitric acid with the volume ratio of 3:1, wherein the mass volume ratio of the matting agent to the mixed acid is 1g:50mL, carrying out ultrasonic treatment for 5 hours, and washing the treated product to be neutral by deionized water to obtain a hydroxylated matting agent;
B) Dispersing the hydroxylated matting agent in deionized water to obtain a dispersion liquid, wherein the mass-volume ratio of the hydroxylated matting agent to the deionized water is 1 g/200 mL; adding an ethanol solution of mercaptosiloxane with the mass concentration of 30% into the dispersion liquid, enabling the mass ratio of the added hydroxylated matting agent to the mercaptosiloxane to be 1:1, stirring and reacting for 12 hours at 50 ℃, and washing the product with deionized water to obtain the surface modified matting agent;
(3) Uniformly mixing the surface modified matting agent and the polyaspartic ester modified by the ethyl benzoate according to a proportion to obtain a component A;
(4) And (3) independently storing the component A and the component B to obtain the coating material for the camera lens.
Comparative example 4 (molecular structure of matrix resin and matting agent surface resin is the same):
a coating material for a camera lens ring comprises a component A and a component B in a mass ratio of 10:7; the component A comprises 95 parts of polyaspartic acid ester and 5 parts of surface modified matting agent by weight; the component B is isocyanate curing agent N3800 (Kogyo); the preparation method of the coating material for the camera lens ring comprises the following steps:
(1) Preparation of polyaspartic acid ester: dropwise adding dimethyl maleate into an ethanol solution of 1, 4-butanediamine under the protection of nitrogen and continuous stirring, reacting for 18 hours at 70 ℃ with the molar ratio of the dimethyl maleate to the 1, 4-butanediamine being 2.1:1, and evaporating to remove an ethanol solvent to obtain polyaspartic acid ester;
(2) Preparing a surface modified matting agent: the procedure was the same as in example 1;
(3) Uniformly mixing the surface modified matting agent and polyaspartic ester in proportion to obtain a component A;
(4) And (3) independently storing the component A and the component B to obtain the coating material for the camera lens.
The coating materials prepared in the above examples and comparative examples were mixed in proportion and then coated on an aluminum alloy substrate, and the properties of the coating were tested after curing for 24 hours, and the results are shown in table 1.
The abrasion resistance test method refers to GB/T1768-2006, and the test conditions are 1kg and 500r.
The test method of the adhesive force refers to the pulling-off method in GB/T5210-2006;
the water resistance test method is described in GB/T1733-1993;
the test method of visible light reflectance is referred to ASTM E903.
Table 1: coating performance test results.
As can be seen from table 1, the coating materials prepared by the formulation and the method in examples 1 to 3 have excellent wear resistance, adhesion and water resistance, and have low reflectivity to visible light and good extinction performance, and are helpful for improving the imaging effect of a camera when used for a camera rim.
In contrast, in comparative example 1, in which polyaspartate not modified with ethyl benzoate was used as a matrix resin, the rigid group in the side chain was absent, and the abrasion resistance of the coating was reduced as compared with that in example 1; and the difference in cure shrinkage of the matrix resin and the matting agent surface resin was reduced, resulting in a reduction in defective structure in the coating layer, and also a reduction in matting performance as compared with that in example 1.
In comparative example 2, the matting agent was not surface-modified, and the dispersibility of the matting agent in the matrix resin was reduced, and aggregation was likely to occur, resulting in a coating having reduced abrasion resistance, adhesion, water resistance, and matting performance as compared with example 1.
In comparative example 3, the surface of the matting agent was modified with only the silane coupling agent, and the surface of the matting agent was not bonded with polyaspartate, and the defective structure of the present invention could not be formed in the coating layer by the difference in curing shrinkage rate between the base resin and the matting agent surface resin, and the matting performance of the coating layer was lowered as compared with that in example 1.
The matrix resin in comparative example 4 is polyaspartate obtained by reacting dimethyl maleate with 1, 4-butanediamine, and has no rigid isophorone group in the main chain, has the same structure as polyaspartate bonded with the surface of the matting agent, has the same curing shrinkage rate as the surface resin of the matting agent, has fewer defective structures in the coating, and reduces the extinction capability of the coating compared with that in example 1, thus being unfavorable for improving the imaging effect of a camera.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The preparation method of the coating material for the camera lens ring is characterized by comprising the following steps of:
(1) Preparation of ethyl benzoate modified polyaspartic esters: firstly, carrying out Michael addition reaction on dimethyl maleate and isophorone diamine to obtain polyaspartic acid ester; then, carrying out transesterification on ethyl benzoate and polyaspartic ester to obtain ethyl benzoate modified polyaspartic ester;
(2) Surface modifying the matting agent: firstly, carrying out surface treatment on a matting agent by using concentrated sulfuric acid and concentrated nitric acid, and introducing hydroxyl groups on the surface of the matting agent; then, the hydroxylated matting agent reacts with mercaptosiloxane, and mercapto is introduced to the surface of the matting agent; then introducing amino groups on the surface of the matting agent through click chemical reaction of the sulfhydrylation matting agent and diaminobutene; finally, through Michael addition reaction of an aminated matting agent and dimethyl maleate, polyaspartic acid ester is bonded on the surface of the matting agent through chemical bonds, and a surface modified matting agent is obtained; the matting agent comprises graphene, carbon nanotubes and carbon black;
(3) Uniformly mixing the surface modified matting agent and the polyaspartic ester modified by the ethyl benzoate to obtain a component A;
(4) And (3) independently storing the component A and the component B comprising the isocyanate curing agent to obtain the coating material for the camera lens.
2. The preparation method according to claim 1, wherein in the step (1), the molar ratio of dimethyl maleate to isophorone diamine in the michael addition reaction is 2-2.2:1; the molar ratio of the ethyl benzoate to the polyaspartic ester is 3.5-4.5:1 when the transesterification reaction is carried out.
3. The process according to claim 1 or 2, wherein the reaction conditions for the michael addition reaction of dimethyl maleate with isophorone diamine in step (1) are: and adding dimethyl maleate into isophorone diamine under the protection of nitrogen, and reacting for 12-24 hours at 65-75 ℃ to obtain the polyaspartic acid ester.
4. The process according to claim 1 or 2, wherein the reaction conditions for transesterification of polyaspartate with ethyl benzoate in step (1) are: and adding polyaspartic acid ester and ethyl benzoate into an organic solvent for dissolution, adding a sodium methoxide catalyst, reacting for 4-6 hours at 125-135 ℃, and removing the solvent to obtain the ethyl benzoate modified polyaspartic acid ester.
5. The preparation method of claim 1, wherein in the step (2), when the surface modification is performed on the matting agent, mixed acid of concentrated sulfuric acid and concentrated nitric acid is firstly used for reacting with the matting agent to obtain a hydroxylated matting agent;
Then, the hydroxylated matting agent reacts with mercaptosiloxane to obtain the mercapto matting agent; the mass ratio of the hydroxylated matting agent to the mercaptosiloxane is 1-2:1;
then, the sulfamized matting agent is obtained through click chemistry reaction of the sulfhydrylized matting agent and diaminobutene; the mass ratio of the sulfhydrylation flatting agent to the diaminobutene is 3-5:1;
Finally, the surface modified matting agent is obtained through Michael addition reaction of the aminated matting agent and dimethyl maleate; the mass ratio of the aminated matting agent to the dimethyl maleate is 3-5:1.
6. The process according to claim 5, wherein in the step (2), the mixed acid of concentrated sulfuric acid and concentrated nitric acid is reacted with the matting agent under the following reaction conditions: the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 3-5:1, the mass volume ratio of the matting agent to the mixed acid is 1 g:50-100 mL, the reaction time is 3-5 h, and the product is washed to be neutral after the reaction;
The conditions for the reaction of the hydroxylated matting agent with the mercaptosiloxane are: dispersing the hydroxylated matting agent in deionized water to obtain a dispersion liquid, wherein the mass volume ratio of the hydroxylated matting agent to the deionized water is 1 g:200-300 mL; adding an ethanol solution of mercaptosiloxane with the mass concentration of 30-40% into the dispersion liquid, stirring at 50-60 ℃ for reaction for 8-12 h, and washing the product to obtain the mercaptolated matting agent;
the click chemistry reaction conditions of the sulfhydrylation flatting agent and the diaminobutene are as follows: dispersing a sulfhydrylation flatting agent in an organic solvent, adding diaminobutene and a peroxide initiator, reacting for 12-24 hours at 80-100 ℃, and washing a product to obtain the aminated flatting agent;
The Michael addition reaction conditions of the aminated matting agent and dimethyl maleate are: dispersing the aminated matting agent in an organic solvent, then dropwise adding dimethyl maleate under the protection of nitrogen, reacting for 12-24 hours at 65-75 ℃, and washing the product to obtain the surface modified matting agent.
7. The preparation method according to claim 1, 5 or 6, wherein the mass ratio of graphene, carbon nanotubes and carbon black in the matting agent is 2-4:1-3:1.
8. The preparation method of claim 1, wherein in the step (3), 5-8 parts by weight of the surface-modified matting agent and 90-100 parts by weight of the ethyl benzoate-modified polyaspartic ester are uniformly mixed to obtain the component A.
9. A coating material for a camera lens ring manufactured by the manufacturing method according to any one of claims 1 to 7, characterized in that the mass ratio of the component a to the component B is 10:5 to 8 when in use.
10. Use of a coating material for a camera lens manufactured by the manufacturing method according to any one of claims 1 to 7 in a camera lens.
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| CN1616513A (en) * | 2003-09-17 | 2005-05-18 | 拜尔材料科学有限责任公司 | Flexibilized polyaspartic esters |
| CN114716671A (en) * | 2022-04-22 | 2022-07-08 | 深圳飞扬骏研新材料股份有限公司 | Preparation method of salt-fog-resistant polyaspartic acid ester, salt-fog-resistant polyaspartic acid ester and coating |
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| US5561214A (en) * | 1995-05-18 | 1996-10-01 | Bayer Corporation | Hyperbranched polyaspartate esters and a process for their preparation |
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| CN1616513A (en) * | 2003-09-17 | 2005-05-18 | 拜尔材料科学有限责任公司 | Flexibilized polyaspartic esters |
| CN114716671A (en) * | 2022-04-22 | 2022-07-08 | 深圳飞扬骏研新材料股份有限公司 | Preparation method of salt-fog-resistant polyaspartic acid ester, salt-fog-resistant polyaspartic acid ester and coating |
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