CN103992700A - Preparation method and product of wear-resistant polymer coating with soft light sensation - Google Patents
Preparation method and product of wear-resistant polymer coating with soft light sensation Download PDFInfo
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- CN103992700A CN103992700A CN201410222534.9A CN201410222534A CN103992700A CN 103992700 A CN103992700 A CN 103992700A CN 201410222534 A CN201410222534 A CN 201410222534A CN 103992700 A CN103992700 A CN 103992700A
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Abstract
The invention discloses a preparation method of a wear-resistant polymer coating with soft light sensation. The method comprises the steps of dissolving epoxy resin A glue into a solvent A, dissolving epoxy resin B glue into a solvent B, and mixing the epoxy resin A glue and the epoxy resin B glue to obtain mixed liquid I; finally mixing the mixed liquid I with a fluorine-containing polymer emulsion, uniformly dispersing, coating on a substrate, and then performing high-temperature solidification and annealing cooling treatment to obtain the polymer coating, wherein the epoxy resin A glue is one or a mixture of more of semi-solid epoxy resin, solid epoxy resin or liquid epoxy resin; the epoxy resin B glue is an amine curing agent or an anhydride type curing agent; the fluorine-containing polymer emulsion is at least one of a polytetrafluoroethylene emulsion, a fluorinated ethylene-propylene emulsion, a perfluoroalkoxy resin emulsion and an ethylene-tetrafluoroethylene co-polymer emulsion. The wear resistance of the prepared polymer wear-resistant coating is greatly increased; the hardness shown by a pencil test is more than 6H; meanwhile, the coating is smooth in surface and excellent in water resistance, acid resistance and alkali resistance.
Description
Technical field
The present invention relates to the preparation field of coating, be specifically related to preparation method of a kind of wear-resisting, polymeric coating layer that light sensation is soft and products thereof.
Background technology
Fluorinated polymer material, as the one of macromolecular material, has the structure of many uniquenesses, thereby shows much special character.As: the polarizability that fluorine atom is lower, strong electronegativity, less van der Waals radius, very strong C-F bond energy, therefore, the material with higher fluorine content has just presented higher thermotolerance, chemical resistance, weather resistance and weathering resistance.There is not viscosity because fluorinated polymer material also has low surface energy, it is widely used as coating principal constituent in cooker, mould and plasthetics.In chemical plating, papermaking and electronic industry, fluoropolymer emulsion is because excellent corrosion resistance nature and resistance to elevated temperatures gain great popularity.In addition, rely on its extremely low frictional wear coefficient, fluoropolymer emulsion is more and more taken seriously in the development of automotive industry and machinery industry.But not resistance to hard friction becomes the more obstruction of widespread use of fluorinated polymer material, when people utilize its automatically cleaning character of not gluing and water-resisting property, can only on wear resisting property, make a concession.
Epoxy resin possesses abnormal outstanding wear resisting property and base material adhesion property, has now been widely used in machinery and building trade.But the wetting ability of epoxide group has limited epoxy resin in waterproof, development aspect water-fast.Fluoropolymer emulsion is introduced epoxy systems by the present invention, and to improving the wear resisting property of fluorinated polymer material, the while is because of the water resistance that improves epoxy resin that adds of fluorinated polymer material.
(the Qin Zonggen such as the total root of Qin, Tu Weiping, Xia Zhengbin, Deng Zhaofang, Shen Liangjun, the blending research of epoxy emulsion and fluorine-containing latex, China's coating is online) blending of epoxy resin and fluorine-containing latex is studied, first prepare fluorine-containing latex by in-situ polymerization, then this fluorine-containing latex is mixed with epoxy emulsion, after stirring, froth breaking, prepare film.Can obtain the film of different hardness by adjusting the mol ratio of epoxy hardener and epoxy resin, in the time that the mol ratio of solidifying agent and epoxy resin is 1.5:1, hardness optimal, but be only 2H; By the adjustment to fluorine-containing latex and epoxy emulsion content, film can obtain different contact angles, but maximum contact angle is also only 105 °.
Therefore, the film performance of the fluorine-containing latex on performance and the market of the film of preparing by aforesaid method is very nearly the same, and price is only 60% left and right of fluorine-containing latex, but still can not meet the requirement of its widespread use.
Summary of the invention
The preparation method who the invention provides a kind of wear-resisting, polymeric coating layer that light sensation is soft, technique is simple, and cost is low, has using value at machinery and building trade; The polymeric coating layer preparing, its wear resistance greatly increases, and the hardness that pencil test shows is greater than 6H; Coatingsurface is smooth, and color and luster is fine, water tolerance and acid-proof alkaline excellence.
The preparation method who the invention discloses a kind of wear-resisting, polymeric coating layer that light sensation is soft, step is as follows:
(1) epoxy resin A glue is dissolved in solvent orange 2 A, epoxy resin B glue is dissolved in solvent B, then both are mixed to get to mixed solution I;
Described epoxy resin A glue is one or more the mixture in semi-solid epoxy resin, solid epoxy or liquid epoxies;
Described epoxy resin B glue is amine curing agent or acid anhydride type curing agent;
The mass ratio of described epoxy resin A glue and epoxy resin B glue is 0.3～30:1;
(2) mixed solution I step (1) being obtained is mixed with fluoropolymer emulsion, is coated in substrate, then obtains described polymeric coating layer through hot setting, annealing cooling process after being uniformly dispersed;
Described fluoropolymer emulsion is at least one in ptfe emulsion, perfluoroethylene-propylene emulsion, mistake fluoroalkyl compound emulsion, ethylene tetrafluoroethylene copolymer emulsion;
The mass ratio of described fluoropolymer emulsion and mixed solution I is 2～200:1.
As preferably, described amine curing agent is at least one in quadrol, hexanediamine, diethylenetriamine, triethylene tetramine;
Described acid anhydride type curing agent is at least one in MALEIC ANHYDRIDE, pyromellitic dianhydride, Tetra hydro Phthalic anhydride.
As preferably, described solvent orange 2 A is at least one in ether, acetone, butanone; Described solvent B is at least one in DMF, dimethyl sulfoxide (DMSO), gamma-butyrolactone, N-Methyl pyrrolidone, acetone, butanone, methyl iso-butyl ketone (MIBK), ethyl acetate.
As preferably, described epoxy resin A glue is one or more in following structural formula:
Wherein, n
1～n
8be CH independently selected from 1～20, R
3, CH
2cH
3or CH (CH
3)
2.
Further preferably,
The mass ratio of described epoxy resin A glue and epoxy resin B glue is 3:1;
The mass ratio of described fluoropolymer emulsion and mixed solution I is 2～19:1.
As preferably, the condition of described hot setting is 150～300 DEG C.
As preferably, described substrate is metal base.
The invention also discloses prepare according to aforesaid method wear-resisting, polymeric coating layer that light sensation is soft.
Compared with prior art, tool of the present invention has the following advantages:
The present invention combines the wear resistance of high temperature resistant, the erosion resistance of fluoropolymer emulsion and epoxy resin, prepares a kind of wear-resistant macromolecule coating, solves the technical problem that epoxy resin high-abrasive material is not water-fast, fluorinated polymer material is not wear-resisting.For the hydrophobic angle of intrinsic, for the fluoropolymer emulsion of 90 °～110 °, though adding of epoxy resin declines its hydrophobicity, the wear resistance of coating greatly increases, and the hardness that pencil test shows is greater than 6H.Paint solidification film forming rear surface is smooth, and color and luster is fine, water tolerance and acid-proof alkaline excellence, and the preparation method of coating mixed liquid is simple in addition, and cost is low, has using value at machinery and building trade.
Embodiment
Following examples are to further elaboration of the present invention, and to better understanding the present invention, but these embodiment are not limiting the scope of the invention, still belong to protection scope of the present invention and be interpreted as that the present invention is made to some nonessential improvement.
Embodiment 1
(1) preparation of fluoropolymer emulsion-epoxy resin adhesive liquid mixed liquid
Epoxy resin A glue 4.00g is dissolved in the middle of 5.00g acetone, B glue-MALEIC ANHYDRIDE 1.33g is dissolved in 12.00g gamma-butyrolactone, after AB glue mixes, get 1.50g and mix 3.50g ptfe emulsion (Guangdong Li Kalong Science and Technology Ltd., viscosity is 750～800cst) in, the slightly mixed liquid of thickness obtained with magnetic agitation 30min, sonic oscillation 20min respectively.
Wherein, the molecular formula of epoxy resin A glue is
N
3=1～5, R is CH
3.
(2) mixed liquid is in the coating of material surface with solidify
The mixed liquid of fluoropolymer emulsion-epoxy resin adhesive liquid is coated on the aluminium material surface of sand papering, is heated to 200 DEG C and makes mixed liquid solidify that after annealing is cooling makes even, the smooth dispersion of coating.
Embodiment 2
(1) preparation of fluoropolymer emulsion-epoxy resin adhesive liquid mixed liquid
Epoxy resin A glue-dicyclopentadiene benzene phenol-type epoxy resin (Ba Ling petrochemical complex company limited) 4.00g is dissolved in the middle of 5.00g acetone, B glue-diethylenetriamine 1.33g is dissolved in 12.00g gamma-butyrolactone, after AB glue mixes, getting 1.25g mixes 3.75g and crosses fluoroalkyl compound emulsion (Shanghai Pu Chun Industrial Co., Ltd., PFAD335D), in, obtain the slightly mixed liquid of thickness with magnetic agitation 30min, sonic oscillation 20min respectively.
Wherein, the molecular formula of dicyclopentadiene benzene phenol-type epoxy resin is
n
1＝3.4。
(2) mixed liquid is in the coating of material surface with solidify
The mixed liquid of fluoropolymer emulsion-epoxy resin adhesive liquid is coated on the steel material surface of sand papering, is heated to 200 DEG C and makes mixed liquid solidify that after annealing is cooling makes even, the smooth dispersion of coating.
Embodiment 3
(1) preparation of fluoropolymer emulsion-epoxy resin adhesive liquid mixed liquid
Epoxy resin A glue-phenol-aralkyl epoxy resin 4.00g is dissolved in the middle of 5.00g acetone, B glue-quadrol 1.33g is dissolved in 12.00g gamma-butyrolactone, after AB glue mixes, get 1.00g and mix 4.00g ethylene tetrafluoroethylene copolymer emulsion (Shanghai Pu Chun Industrial Co., Ltd., F-40), in, obtain the slightly mixed liquid of thickness with magnetic agitation 30min, sonic oscillation 20min respectively.
Wherein, the molecular formula of phenol-aralkyl epoxy resin is
n
2＝3.5～33.3。
(2) mixed liquid is in the coating of material surface with solidify
The mixed liquid of fluoropolymer emulsion-epoxy resin adhesive liquid is coated on the copper sheet surface of sand papering, is heated to 200 DEG C and makes mixed liquid solidify that after annealing is cooling makes even, the smooth dispersion of coating.
Embodiment 4
(1) preparation of fluoropolymer emulsion-epoxy resin adhesive liquid mixed liquid
Epoxy resin A glue 4.00g is dissolved in the middle of 5.00g acetone, B glue-pyromellitic dianhydride 1.33g is dissolved in 12.00g gamma-butyrolactone, after AB glue mixes, get 0.75g and mix 4.25g perfluoroethylene-propylene emulsion (Shanghai Pu Chun Industrial Co., Ltd., FEPD121), in, obtain the slightly mixed liquid of thickness with magnetic agitation 30min, sonic oscillation 20min respectively.
The molecular formula of epoxy resin A glue is
(2) mixed liquid is in the coating of material surface with solidify
The mixed liquid of fluoropolymer emulsion-epoxy resin adhesive liquid is coated in the surface of stainless steel of sand papering, is heated to 200 DEG C and makes mixed liquid solidify that after annealing is cooling makes even, the smooth dispersion of coating.
Embodiment 5
(1) preparation of fluoropolymer emulsion-epoxy resin adhesive liquid mixed liquid
Epoxy resin A glue 4.00g is dissolved in the middle of 5.00g acetone, B glue-Tetra hydro Phthalic anhydride 1.33g is dissolved in 12.00g gamma-butyrolactone, after AB glue mixes, get 0.50g and mix 4.50g ethylene tetrafluoroethylene copolymer emulsion (Shanghai Pu Chun Industrial Co., Ltd., F-40), in, obtain the slightly mixed liquid of thickness with magnetic agitation 30min, sonic oscillation 20min respectively.
The molecular formula of epoxy resin A glue is
(2) mixed liquid is in the coating of material surface with solidify
The mixed liquid of fluoropolymer emulsion-epoxy resin adhesive liquid is coated on the steel material surface of sand papering, is heated to 200 DEG C and makes mixed liquid solidify that after annealing is cooling makes even, the smooth dispersion of coating.
Embodiment 6
(1) preparation of fluoropolymer emulsion-epoxy resin adhesive liquid mixed liquid
Epoxy resin A glue 4.00g is dissolved in the middle of 5.00g acetone, B glue-hexanediamine 1.33g is dissolved in 12.00g gamma-butyrolactone, after AB glue mixes, get 0.25g and mix 4.75g perfluoroethylene-propylene emulsion (Shanghai Pu Chun Industrial Co., Ltd., FEPD121), in, obtain the slightly mixed liquid of thickness with magnetic agitation 30min, sonic oscillation 20min respectively.
The molecular formula of epoxy resin A glue is
(2) mixed liquid is in the coating of material surface with solidify
The mixed liquid of fluoropolymer emulsion-epoxy resin adhesive liquid is coated on the aluminium material surface of sand papering, is heated to 200 DEG C and makes mixed liquid solidify that after annealing is cooling makes even, the smooth dispersion of coating.
Comparative example 1
(1) preparation of fluoropolymer emulsion-epoxy resin adhesive liquid mixed liquid
Epoxy resin A glue 4.00g is dissolved in the middle of 5.00g acetone, and B glue MALEIC ANHYDRIDE 1.33g is dissolved in 12.00g gamma-butyrolactone, and AB glue mixes and obtains the slightly mixed liquid of thickness with magnetic agitation 30min, sonic oscillation 20min respectively afterwards.
The molecular formula of epoxy resin A glue is
N
3=1～5, R is CH
3.
(2) mixed liquid is in the coating of material surface with solidify
The mixed liquid of fluoropolymer emulsion-epoxy resin adhesive liquid is coated on the aluminium material surface of sand papering, is heated to 200 DEG C and makes mixed liquid solidify that after annealing is cooling makes even, the smooth dispersion of coating.
Comparative example 2
(1) preparation of epoxy resin adhesive liquid
Epoxy resin A glue 618#E-51 (Kunshan City, Jiangsu Province green cycle industrial and commercial bank) 4.00g is dissolved in the middle of 5.00g acetone, B glue 650 type Versamids (Kunshan City, Jiangsu Province green cycle industrial and commercial bank) 1.33g is dissolved in 12.00g gamma-butyrolactone, after AB glue mixes, get 1.50g and mix 3.50g ptfe emulsion (Guangdong Li Kalong Science and Technology Ltd., viscosity is 750～800cst) in, the slightly mixed liquid of thickness obtained with magnetic agitation 30min, sonic oscillation 20min respectively.
(2) mixed liquid is in the coating of material surface with solidify
The mixed liquid of fluoropolymer emulsion-epoxy resin adhesive liquid is coated on the steel material surface of sand papering, heat to 200 DEG C makes mixed liquid solidify that after annealing is cooling makes even, the smooth dispersion of coating.
Performance test
The wear-resistant macromolecule coating that embodiment 1～6 and comparative example 1,2 are prepared is respectively carried out following sticking power, pencil hardness and resistance to elevated temperatures test, and embodiment 1 is carried out to acid and alkali-resistance and water resistance test.
1. sticking power test
Testing standard: GB/T9286-1998 (ISO2409:1992)
Testing method: material wear-resisting by being coated with, the soft polymeric coating layer of light sensation is placed on experiment table, hand-held stroke of lattice device handle, multi-edge cutting knife, perpendicular to being coated with layer plane, cuts and draws with the gimmick of not trembleing of uniform pressure, balance and the speed of 20mm/s～50mm/s.By coating half-twist, cutting the salty multiple above operation of cutting-up with formation lattice battle array.With banister brush along the diagonal lines of lattice battle array gently backward, brush applied coating 5 times forward.Experiment completes at three different positionss of coating.The wide senior scotch tape of 3M600 for 19mm is attached on whole stroke of lattice, tears with minimum angles, see that amount that coatingsurface is sticked up by adhesive tape accounts for the per-cent of hundred lattice.Test result is in table 1.
Grade classification:
ISO grade: 0 grade
Cut edge is completely smooth, and none lattice comes off.
ISO grade: 1 grade
There is a little disbonding in the intersection of otch, can not obviously be greater than 5% but cross cut area is influenced.
ISO grade: 2 grades
At otch infall and/or have coating shedding along notching edge, affected cross cut area is obviously greater than 5%, but can not obviously be greater than 15%.
ISO grade: 3 grades
Coating partly or entirely comes off with large fragment along cut edge, and/or partly or entirely peels off on grid different sites, and affected cross cut area is obviously greater than 15%, but can not obviously be greater than 35%.
ISO grade: 4 grades
Along cut edge, large fragment peels off coating, and/or some grid parts or all occur coming off, and affected cross cut area is obviously greater than 35%, but can not obviously be greater than 65%.
ISO grade: 5 grades
The degree of peeling off exceedes 4 grades.
Test result is in table 1.
2. pencil hardness test
Testing standard: GB/T6739-2006 (ISO15184:1998)
Testing method: experiment comprises each one of 6H, 5H, 4H, 3H, 2H, H, HB, B, 2B, 3B, 4B, 5B and 6B pencil with Chinese board advanced drawing pencil.The rod part of pruning, pen core is the cylindric about 3mm that exposes.Place No. 400 sand paper at experiment table, vertically hold pencil, keep 90 ° of front and back mobile lead pencils on sand paper with sand paper, pencil-lead tip is polished.Mobile lead pencil is until pen core becomes a smooth smooth circular cross section, and edge is without chip and breach (all repeating this step before using pencil) at every turn.Hand-held pencil tilts approximately 45 °, with not degree of breaking into of pen core, in coating, push 1cm left and right towards the direction of leaving experimenter with uniform, about 1cm/s speed, the pencil of same label repeats five roads, all chips of cleaning pencil-lead on coatingsurface with Great Wall board advanced drawing rubber, show so that cut is more apparent.
Coating scratches: Wu road scratches in experiment, and if any the two Dao Huo bis-above scratch primer coatings in road, the pencil of using last position hardness label instead carries out same experiment, is scratched the pencil below two roads until find out coating, writes down the hardness label of this pencil.
Coating scratch: Wu road scratches in experiment, abrades above primer coating if any two Dao Huo bis-roads, uses the pencil of last position hardness label instead and tests equally, is scratched the pencil below two roads until find out coating, writes down the hardness label of this pencil.
Coating hardness is judged:
Coating scratches: for mutually contiguous two pencils of hardness label, find out coating and scratched after two roads or above and pencil less than two roads, the pencil hardness using the pencil hardness less than two roads as coating.
Coating scratch: for hardness label contiguous two pencils mutually, find out coating and be scratched after two roads or above and pencil less than two roads, the pencil hardness using the pencil hardness less than two roads as coating.
3, resistance to elevated temperatures test
Coating prepared by embodiment and comparative example is placed on intelligent temperature controller, and it is 300 DEG C that Heating temperature is set, and heats up gradually, observes coating and is not destroyed, and top temperature wrinkling, that the catabiosis such as come off can bear does not appear in coatingsurface.
Pencil hardness, sticking power and the high temperature resistant test result of coating are in table 1.
Table 1
4. water tolerance and acid-proof alkaline test
Sulfuric acid, 6.0mol/L hydrochloric acid, 6.1mol/L sodium hydroxide and distilled water that wear-resisting, the soft fluoropolymer emulsion-epoxy resin adhesive liquid of light sensation coating prepared by embodiment 1 is placed in respectively 3.7mol/L soak 48h.Test result shows, that prepared by the present invention is wear-resisting, the immersion of the resistance to tap water of light sensation soft fluoropolymer emulsion-epoxy resin adhesive liquid coating, sulfuric acid, hydrochloric acid and sodium hydroxide corrosion that can resisting high-concentration, and coatingsurface is excellent.
Comparative example 1 is compared with embodiment 1 discovery, though it is very nearly the same with coating prepared by the present invention not add the epoxy resin adhesive liquid coating hardness of fluoropolymer emulsion, but wear-resisting, the soft fluoropolymer emulsion-epoxy resin adhesive liquid of the light sensation coating prepared by the inventive method, demonstrate excellent water-acid resistance performance, high temperature resistant and light sensation good colour, preparation technology is simple, and cost is low, has potential commercial value in wear-resisting industry.Same, the coating of preparing with general epoxy resin in comparative example 2, resistance to elevated temperatures and light sensation color and luster are all not good enough.
Claims (8)
1. a preparation method for the polymeric coating layer that wear-resisting, light sensation is soft, is characterized in that, step is as follows:
(1) epoxy resin A glue is dissolved in solvent orange 2 A, epoxy resin B glue is dissolved in solvent B, then both are mixed to get to mixed solution I;
Described epoxy resin A glue is one or more the mixture in semi-solid epoxy resin, solid epoxy or liquid epoxies;
Described epoxy resin B glue is amine curing agent or acid anhydride type curing agent;
The mass ratio of described epoxy resin A glue and epoxy resin B glue is 0.3～30:1;
(2) mixed solution I step (1) being obtained is mixed with fluoropolymer emulsion, is coated in substrate, then obtains described polymeric coating layer through hot setting, annealing cooling process after being uniformly dispersed;
Described fluoropolymer emulsion is at least one in ptfe emulsion, perfluoroethylene-propylene emulsion, mistake fluoroalkyl compound emulsion, ethylene tetrafluoroethylene copolymer emulsion;
The mass ratio of described fluoropolymer emulsion and mixed solution I is 2～200:1.
2. preparation method according to claim 1, is characterized in that, described amine curing agent is at least one in quadrol, hexanediamine, diethylenetriamine, triethylene tetramine;
Described acid anhydride type curing agent is at least one in MALEIC ANHYDRIDE, pyromellitic dianhydride, Tetra hydro Phthalic anhydride.
3. preparation method according to claim 1, is characterized in that, described solvent orange 2 A is at least one in ether, acetone, butanone;
Described solvent B is at least one in DMF, dimethyl sulfoxide (DMSO), gamma-butyrolactone, N-Methyl pyrrolidone, acetone, butanone, methyl iso-butyl ketone (MIBK), ethyl acetate.
4. according to the preparation method described in the arbitrary claim of claim 1～3, it is characterized in that, described epoxy resin A glue is one or more in following structural formula:
Wherein, n
1～n
8be CH independently selected from 1～100, R
3, CH
2cH
3or CH (CH
3)
2.
5. preparation method according to claim 4, is characterized in that, the mass ratio of described epoxy resin A glue and epoxy resin B glue is 3:1;
The mass ratio of described fluoropolymer emulsion and mixed solution I is 2～19:1.
6. preparation method according to claim 1, is characterized in that, the condition of described hot setting is 150～300 DEG C.
7. preparation method according to claim 1, is characterized in that, described substrate is metal base.
8. wear-resisting, the polymeric coating layer that light sensation is soft obtaining according to the preparation method described in the arbitrary claim of claim 1～7.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110898255A (en) * | 2019-12-06 | 2020-03-24 | 上海康宁医疗用品有限公司 | Method for manufacturing expanded polytetrafluoroethylene facial implant with coated surface |
| CN113582555A (en) * | 2021-08-24 | 2021-11-02 | 上海交通大学 | Preparation method of transparent self-cleaning coating for optical sensor glass window |
| CN115725053A (en) * | 2022-11-24 | 2023-03-03 | 深圳市郎搏万先进材料有限公司 | Epoxy resin composition, reinforced fiber prepreg and reinforced fiber composite material |
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| CN110898255A (en) * | 2019-12-06 | 2020-03-24 | 上海康宁医疗用品有限公司 | Method for manufacturing expanded polytetrafluoroethylene facial implant with coated surface |
| CN113582555A (en) * | 2021-08-24 | 2021-11-02 | 上海交通大学 | Preparation method of transparent self-cleaning coating for optical sensor glass window |
| CN115725053A (en) * | 2022-11-24 | 2023-03-03 | 深圳市郎搏万先进材料有限公司 | Epoxy resin composition, reinforced fiber prepreg and reinforced fiber composite material |
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