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CN103819976A - Coating material for diagnosis glass slide and preparation method for coating material - Google Patents

Coating material for diagnosis glass slide and preparation method for coating material Download PDF

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CN103819976A
CN103819976A CN201410074553.1A CN201410074553A CN103819976A CN 103819976 A CN103819976 A CN 103819976A CN 201410074553 A CN201410074553 A CN 201410074553A CN 103819976 A CN103819976 A CN 103819976A
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parts
coating material
diagnostic
slides
preparation
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朱鹏
沈拥军
石玉军
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Nantong University
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Abstract

本发明公开了一种诊断载玻片用涂层材料,该涂层材料的组成及按照重量份数组成为:氟碳树脂15份-20份;封闭型多异氰酸酯5份-10份;稀释剂15份-20份;固化促进剂0.1份-0.5份;助剂5份-10份;无机颜料10份-15份;纳米粉体10份-15份;微米粉体25份-30份。本发明还公开了诊断载玻片用涂层材料的制备方法:称取各组分后,采用分散机高速分散1~2小时;后加入纳米、微米粉体及无机颜料,采用三辊研磨,使涂层材料粒度达到10μm以下。本发明涂层材料用于诊断载玻片适用于丝网印刷,疏水性能优异,与载波片的附着力较好。此外成本较低而且工艺简单,能够满足各种性能要求。The invention discloses a coating material for diagnostic glass slides. The composition of the coating material is as follows: 15-20 parts of fluorocarbon resin; 5-10 parts of blocked polyisocyanate; 15 parts of diluent 0.1-0.5 parts of curing accelerator; 5-10 parts of auxiliary agent; 10-15 parts of inorganic pigment; 10-15 parts of nanometer powder; 25-30 parts of micron powder. The invention also discloses a preparation method of the coating material for diagnostic glass slides: after weighing each component, disperse at high speed for 1 to 2 hours with a disperser; then add nano, micron powder and inorganic pigment, and grind with three rolls. Make the particle size of the coating material below 10 μm. The coating material of the invention is suitable for screen printing when used for diagnostic glass slides, has excellent hydrophobicity and good adhesion to slide slides. In addition, the cost is low and the process is simple, which can meet various performance requirements.

Description

A kind of diagnosis coating material for glass slide and preparation method thereof
Technical field
The present invention relates to diagnose coating material for glass slide and preparation method thereof, it is specifically related to a kind ofly have the coated material of super-hydrophobic effect and be printed on slide glass, as biological, medical diagnosis analysis.
Background technology
Diagnosis slide glass is widely used in cytodiagnosis, pathology experiment, HPV detection etc., and its profile as shown in Figure 1.Visible, test agent drops in hole, and around coating has super-hydrophobic effect, thereby it is spherical that test agent is formed, and avoids the effect of reagent crossed contamination.Therefore, diagnosis slide glass coated material should have ultra-hydrophobicity, and the contact angle of coating and water should be greater than 150 °, should have good sticking power with slide glass substrate glass, the characteristics such as resistance to each alanysis solvent for use simultaneously.
Large quantity research shows, super-hydrophobic character and surperficial microtexture and lower surface can have very large associated.Super hydrophobic surface has the surface property of a lot of uniquenesses, such as: hydrophobicity, didirtresistance, automatically cleaning etc.Therefore, it has broad application prospects in life and production field.But manually preparing super hydrophobic surface is not to be easy to so.The technology of preparing now super hydrophobic surface exists many deficiencies such as the high and complex process of cost.
Chinese patent [CN200910217946.2] discloses a kind of method that adopts laser ablation and has manufactured super hydrophobic surface.First it is the laser multiple-beam interference system of building, and the then curable or degradable material of spin coating in substrate solidifies curable materials or made degradation material degraded by laser interference lithography, after developing, obtains micro structure array; Then in microstructure, carry out the modification of low-surface-energy material, and then in substrate, obtain the biomimetic colour super-hydrophobic coating that utilizes multi-beam interference photoetching technology to prepare.But this method more complicated is not easy to operate, and cost is higher.
Chinese patent [CN201010164798.5] a kind of polymer matrix composite with super hydrophobic surface and preparation method thereof of openly knowing clearly.Concrete method is: first pre-treatment is carried out in the surface of this matrix material body; Then by resin system brushing its surface and strike off; Be sprayed on resin system surface with metallic oxide nano powder again; Finally be heating and curing, and be placed in the similar solution such as stearic acid ethanolic soln and carry out self-assembly.Same also more complicated of this method, is not easy to operation.Similar patent also comprises Chinese patent [CN200710119670.5], Chinese patent [CN200710065079.6].
Chinese patent [CN200710070728.1] discloses a kind of preparation method of transparent hydrophobic coating.Adopt sol-gel method to carry out film at substrate material surface, and self-assembled modified with coatingsurface being carried out containing the material of hydrophobic chain, and gained contact angle on surface of coating is greater than 150 °.Sol-gel method mainly changes nano inorganic particle by organic precursor into through chemical reaction, but colloidal sol section storage time (being only that several minutes was to several hours).Therefore, this method is unfavorable for large-scale production.
Chinese patent [CN200810061480.7] the invention discloses a kind of preparation method of epoxy resin super-hydrophobic coat.It is characterized in that comprising the steps: the preparation of (1) coating colloidal sol, silicon-dioxide powdery is dissolved in solvent, add silane coupling agent, heated and stirred reaction, adds epoxide resin coating material, hydrophobizing agent, and stirring reaction, makes coating colloidal sol; (2) substrate material surface film, uses the method that lifts film, spin coating, curtain coating film or spraying that the colloidal sol making in step (1) is evenly applied in to substrate surface, set aside for use under room temperature after proposing; (3) process that is heating and curing, puts into baking oven by the base material of film in step (2), and the heating of rising temperature makes epoxy resin cure crosslinked, obtains epoxy resin super-hydrophobic coat after taking-up.Adopt sol-gel method to need low solid content, otherwise can cause that solid separates out.Therefore the super-hydrophobic coating material viscosity that prepared by this method is lower, only can adopt the method that lifts film, spin coating, curtain coating film or spraying to form coating; And for the coating with patterns such as circular holes, adopting silk screen printing more, it requires coated material viscosity to be greater than 10PaS.For this reason, the method that this patent proposes not can be applicable to diagnose slide glass yet.
Meanwhile, comprehensive client both at home and abroad mainly comprises the performance index of diagnosis slide glass coating: 1) can stand enzyme and microwave treatment; 2) can stand long-time storage; 3) HF of massfraction 1% soaks 15 seconds coating performances without impact; 4) HC1 of massfraction 5% soaks 30 minutes performances without impact; 5) more than reaching 5B with substrate glass sticking power.
The present invention, in meeting above-mentioned requirements, has the features such as simple, the with low cost and excellent performance of technique.In addition, the super-hydrophobic coat that the present invention makes, containing poisonous composition, is not suitable for diagnosing slide glass.Inquire about domestic and international patent and have no relevant report.
Summary of the invention
Goal of the invention: the present invention is the super-hydrophobic coating material that preparation is applicable to diagnose slide surface.Meeting outside properties requirement, there is the feature that technique is simple, effect is remarkable and with low cost simultaneously.
The technical solution used in the present invention is: a kind of diagnosis coating material for glass slide, and the composition of this coated material and consisting of according to parts by weight:
Figure BSA0000101510880000021
Figure BSA0000101510880000031
As preferably, described fluorocarbon resin is the FEVE fluorocarbon resin of fluorochemical monomer and the copolymerization of alkyl ethane and ethylene ether.
As preferably, described blocked polyisocyanate is aliphatics blocked isocyanate resin.
As preferably, described thinner is one or more mixtures of dihydric acid fat (DBE), pimelinketone, methylethylketone, toluene, dimethylbenzene.
As preferably, described auxiliary agent is fluorine containing silicone oil, preferably trifluoro propyl methyl-silicone oil, 3, two (trifluoromethyl) phenyl silicone oil of 5-.
As preferably, described nano-powder is that particle diameter is titanium dioxide or the silica dioxide granule of 10~500nm.
As preferably, described micro-powder is that particle diameter is one or several mixtures in calcium carbonate, barium sulfate and the zinc oxide of 5-30 μ m.
A preparation method who diagnoses coating material for glass slide, comprises the following steps:
(1) take and account for 15 parts of-20 parts of fluorocarbon resins of raw material gross weight, account for 5 parts of-10 parts of blocked polyisocyanates of raw material gross weight, account for 15 parts of-20 parts of thinners of raw material gross weight, account for 0.1 part of-0.5 part of promotor of raw material gross weight; Account for after 5 parts of-10 parts of auxiliary agents mixing of raw material gross weight, adopt dispersion machine high speed dispersion 60 minutes, rotating speed is 1600r/min
(2) take that to account for raw material gross weight be 10 parts of-15 parts of nano-powders, account for 25 parts of-30 parts of micro-powders of raw material weight and account for 10 parts of-15 parts of mineral dyes of raw material weight and add in compound, adopt three rollers to grind ten times, rear encapsulation is stand-by.
Beneficial effect: coated material of the present invention is used for diagnosing slide glass to be applicable to silk screen printing, hydrophobic performance excellence is better with the sticking power of wave carrier piece.In addition cost is lower and technique is simple, can meet various performance requriementss.
Product performance result is as follows:
Figure BSA0000101510880000041
Embodiment:
Specific embodiment 1
A kind of diagnosis coating material for glass slide, the composition of this coated material and consisting of according to parts by weight: 15 parts of fluorocarbon resins; 5 parts of blocked polyisocyanates; 15 parts of pimelinketone; 0.1 part of curing catalyst; 5 parts of trifluoro propyl methyl-silicone oils; 10 parts of mineral dyes; Particle diameter is 10 parts of the titanium dioxide of 10nm; Particle diameter is 25 parts, the calcium carbonate of 5 μ m.
A preparation method who diagnoses coating material for glass slide, comprises the following steps:
(1) after taking and accounting for and consist of 15 parts of fluorocarbon resins, 5 parts of blocked polyisocyanates, 15 parts of pimelinketone, 0.1 part of curing catalyst, 5 parts of trifluoro propyl methyl-silicone oils and mix according to parts by weight, adopt dispersion machine high speed dispersion 60 minutes, rotating speed is 1600r/min.
(2) take to account for and consist of according to parts by weight calcium carbonate and the 10 parts of mineral dyes that titanium dioxide that 10 parts of particle diameters are 10nm, 25 parts of particle diameters are 5 μ m and add in compound, adopt three rollers to grind ten times, rear encapsulation is stand-by.
Specific embodiment 2
A kind of diagnosis wave carrier piece coated material, the composition of this material and consisting of according to parts by weight: 20 parts of fluorocarbon resins; 10 parts of aliphatics blocked isocyanate resins; 20 parts of methylethylketones; 0.5 part of curing catalyst; 10 parts of two (trifluoromethyl) phenyl silicone oil of 3,5-; 15 parts of mineral dyes; Particle diameter is 5 parts of the silica 1s of 500nm; Particle diameter is 30 parts, the barium sulfate of 30 μ m.
A preparation method who diagnoses coating material for glass slide, comprises the following steps:
(1) take account for according to parts by weight consist of 20 parts of fluorocarbon resins, 10 parts of aliphatics blocked isocyanate resins, 20 parts of methylethylketones, 0.5 part of curing catalyst, 10 part 3, after two (trifluoromethyl) phenyl silicone oil of 5-are mixed, adopt dispersion machine high speed dispersion 60 minutes, rotating speed is 1600r/min;
(2) take to account for and consist of according to parts by weight barium sulfate and the 15 parts of mineral dyes that silicon-dioxide that 15 parts of particle diameters are 500nm, 30 parts of particle diameters are 30 μ m and add in compound, adopt three rollers to grind ten times, rear encapsulation is stand-by.
Specific embodiment 3
A kind of diagnosis coating material for glass slide, the composition of this coated material and consisting of according to parts by weight: 18 parts of the FEVE fluorocarbon resins of fluorochemical monomer and the copolymerization of alkyl ethane and ethylene ether; 7 parts of blocked polyisocyanates; 16 parts of dimethylbenzene; 0.3 part of curing catalyst; 9 parts of fluorine containing silicone oils; 13 parts of mineral dyes; Particle diameter is 12 parts of the titanium dioxide of 300nm; Particle diameter is 28 parts, the zinc oxide of 17 μ m.
A preparation method who diagnoses coating material for glass slide, comprises the following steps:
(1) after taking and accounting for and consist of 18 parts of fluorochemical monomers and mix with the FEVE fluorocarbon resin of alkyl ethane and ethylene ether copolymerization, 7 parts of blocked polyisocyanates, 16 parts of dimethylbenzene, 0.3 part of curing catalyst, 9 parts of fluorine containing silicone oils according to parts by weight, adopt dispersion machine high speed dispersion 60 minutes, rotating speed is 1600r/min;
(2) take to account for and consist of 13 parts of 12 parts of titanium dioxide that particle diameter is 300nm, 28 parts, zinc oxide that particle diameter is 17 μ m and mineral dyes according to parts by weight and add in compound, adopt three rollers to grind ten times, rear encapsulation is stand-by.

Claims (8)

1.一种诊断载波片用涂层材料,其特征在于:该材料的组成及按照重量份数组成为:1. a coating material for diagnostic slides, characterized in that: the composition of the material and become according to parts by weight:
Figure FSA0000101510870000011
Figure FSA0000101510870000011
2.根据权利要求1所述诊断载玻片用涂层材料,其特征在于:所述的氟碳树脂为含氟单体与烷基乙烷乙烯醚共聚的FEVE氟碳树脂。2 . The coating material for diagnostic slides according to claim 1 , wherein the fluorocarbon resin is FEVE fluorocarbon resin copolymerized with fluorine-containing monomers and alkyl ethane vinyl ethers. 3.根据权利要求1所述诊断载玻片用涂层材料,其特征在于:所述的封闭型多异氰酸酯为脂肪族封闭异氰酸酯树脂。3. The coating material for diagnostic slides according to claim 1, characterized in that: the blocked polyisocyanate is an aliphatic blocked isocyanate resin. 4.根据权利要求1所述诊断载玻片用涂层材料,其特征在于:所述的稀释剂为二价酸脂(DBE)、环己酮、甲乙酮、甲苯、二甲苯的一种或多种混合物。4. according to the described coating material of diagnostic slide glass of claim 1, it is characterized in that: described diluent is one or more of divalent acid ester (DBE), cyclohexanone, methyl ethyl ketone, toluene, xylene kind of mixture. 5.根据权利要求1所述诊断载玻片用涂层材料,其特征在于:所述的助剂为含氟硅油,优选三氟丙基甲基硅油、3,5-双(三氟甲基)苯基硅油。5. according to the described coating material of diagnostic slide glass of claim 1, it is characterized in that: described auxiliary agent is fluorine-containing silicone oil, preferably trifluoropropyl methyl silicone oil, 3,5-bis(trifluoromethyl) ) Phenyl silicone oil. 6.根据权利要求1所述诊断载玻片用涂层材料,其特征在于:所述的纳米粉体为颗粒直径为10~500nm的二氧化钛或二氧化硅颗粒。6 . The coating material for diagnostic glass slides according to claim 1 , wherein the nanopowder is titanium dioxide or silicon dioxide particles with a particle diameter of 10-500 nm. 7.根据权利要求1所述诊断载玻片用涂层材料,其特征在于:所述的微米粉体为颗粒直径为5-30μm的碳酸钙、硫酸钡及氧化锌中的一种或者几种混合物。7. The coating material for diagnostic glass slides according to claim 1, characterized in that: the micron powder is one or more of calcium carbonate, barium sulfate and zinc oxide with a particle diameter of 5-30 μm mixture. 8.一种诊断载玻片用涂层材料的制备方法,其特征在于:包括以下步骤:8. A method for preparing a coating material for a diagnostic slide, characterized in that: comprising the following steps: (1)称取占原料总重量15份-20份氟碳树脂、占原料总重量5份-10份封闭型多异氰酸酯、占原料总重量15份-20份稀释剂、占原料总重量0.1份-0.5份固化促进剂;占原料总重量5份-10份助剂混合后,采用分散机高速分散60分钟,转速为1600r/min;(1) Weigh 15-20 parts of fluorocarbon resin, 5-10 parts of blocked polyisocyanate, 15-20 parts of diluent, and 0.1 part of total weight of raw materials -0.5 parts of curing accelerator; account for 5 parts of the total weight of raw materials - 10 parts of additives, after mixing, use a disperser to disperse at high speed for 60 minutes at a speed of 1600r/min; (2)称取占原料总重量为10份-15份纳米粉体、占原料重量25份-30份微米粉体及占原料重量10份-15份无机颜料加入混合料中,采用三辊研磨十遍,后封装待用。(2) Weigh 10-15 parts of nano-powders, 25-30 parts of micron powders and 10-15 parts of inorganic pigments in the total weight of raw materials and add them to the mixture, and use three-roll grinding Ten times, and then packaged for use.
CN201410074553.1A 2014-02-27 2014-02-27 Coating material for diagnosis glass slide and preparation method for coating material Pending CN103819976A (en)

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CN114937874A (en) * 2022-06-06 2022-08-23 西安工程大学 A kind of preparation method of FeSiAl/Al2O3/resin composite wave absorbing coating

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