CN106117553B - It is a kind of for improving the protective agent and preparation and application of the anti-curability of LED silver dollar part - Google Patents
It is a kind of for improving the protective agent and preparation and application of the anti-curability of LED silver dollar part Download PDFInfo
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- CN106117553B CN106117553B CN201610288402.5A CN201610288402A CN106117553B CN 106117553 B CN106117553 B CN 106117553B CN 201610288402 A CN201610288402 A CN 201610288402A CN 106117553 B CN106117553 B CN 106117553B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
-
- 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
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- 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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/173—Macromolecular compounds
Abstract
It is a kind of for improving the protective agent and preparation and application of the anti-curability of LED silver dollar part, there is the constitutional repeating unit or two kinds of mixture such as following formula:Using three-neck flask as reaction vessel, nitrogen is led in stirring, and 0.1mol diamines is added, and is dissolved with 10ml n,N-dimethylacetamide polar solvent, adds 0.1-0.15mol dianhydride, reacts at room temperature 12-18h.LED silver-based plate is placed in solution, impregnates 30s, then be placed in 0.5-1h in 30-80 DEG C of baking oven.The present invention is low in cost, does not influence that later period encapsulation process, synthesis process are simple, improves the anti-curability of silver.
Description
Technical field
The present invention provides a kind of protective agent that silver and the anti-curability of silver coating can be improved, and is applied to commemorative coin, electric appliance
The protection of original part, especially LED silver shelf layer.
Technical background
Silver has bright silvery white, good conductive, thermally conductive, reflecting power, is commonly used for making Silver Jewelry and electronics
The conducting element and LED substrate of instrument and equipment.But silver and silver coating have the shortcomings that one it is fatal, i.e., vulnerable to electric appliance original part and big
The corrosion of sulphur compound in gas and change colour, seriously affect its application.In recent years, right with the development of high-power LED illuminating device
The protection of SERS substrate require also higher and higher, common epoxy packages glue due to temperature resistance is poor, easy xanthochromia, dimensional stability not
The problems such as good, not ageing-resistant, is no longer satisfied requirement.The ageing-resistant and better organic silicon packaging glue of heat resistance increasingly obtains
To the concern and use of industry.But since organic silicon packaging glue is based on polysiloxanes, gas barrier property is poor, it cannot
Effectively prevent erosion of the gas to bottom silver-based plate.
For silver this phenomenon easy to change, the method for protecting LED SERS substrate currently there are two kinds, first, in LED
Silver-based bottom surface provides protective agent, then encapsulates the mode of silicone resin to improve the anti-sulphur ability of silver.Such as patent CN
102766871 A improve the anti-sulphur ability of LED element by applying in LED silver-based plate surface containing zinc salt or zinc complex,
Second, by the modified encapsulation resin covered on silver-colored bracket, to improve its whole crosslink density, such as patent CN 102965069
A reports the ratio by optimization organic silicon packaging glue phenyl, vinyl and vinyl MQ resin, and Lai Tigao packaging plastic is prevented
Vulcanization effect.Although first method can effectively improve the anti-sulphur ability of LED SERS substrate, but contain phosphorus member in protective agent
Element can cause environmental pollution, and second method potting resin is easily ventilative, cannot effectively obstruct hydrogen sulfide gas, also cannot
Protection LED SERS substrate well.
Summary of the invention
It is a kind of for improving the anti-curability of LED silver dollar part the purpose of the present invention is overcoming the deficiencies of the prior art and provide
Polyimide acid protective agent, improve the anti-curability of LED element from basic.
The present invention is achieved by the following technical solutions.
The present invention synthesizes a kind of polyimide acid protective agent, the polyimide acid protection using diamines, dianhydride as raw material
Agent just like following formula (1) constitutional repeating unit or two kinds of mixture, the number of the repetitive unit between 3-10000,
It is preferred that the integer between 10-2000.
Wherein, R1For aromatic hydrocarbon, R2For aliphatic hydrocarbon.
The protectant preparation method of the present invention for being used to improve the anti-curability of LED silver dollar part, as follows:
Using three-neck flask as reaction vessel, it is equipped with magnetic agitation, passes to nitrogen protection, the diamines of 0.1mol is added, with 10ml N, N- bis-
Methylacetamide polar solvent makes it dissolve, and adds the dianhydride of 0.1-0.15mol, and (such as 25 DEG C) react 12- at room temperature
18h is diluted to 50-100mg/ml with solvent, is placed in 4 DEG C of preservations.
The protectant application method of polyimide acid of the present invention, i.e. immersion-cured process: by LED silver-based plate
It is placed in liquid level of solution or less (solution did not had LED silver-based plate), impregnates 30s, then take out, the LED silver-based plate that will be impregnated
It is placed in 0.5-1h in 30-80 DEG C of baking oven, solvent is made to volatilize, is then formed a film.
Preferably following a, b, c, d, the four kind of structure of heretofore described Kapton.
As shown in formula (1), containing-NH- and-COOH-, free carboxyl and amino and silver key in a manner of chemical bond in structure
Close, be formed by polyimides sorrel tightly be attached to silver surface, due to silver surface formed polyimides sorrel it is unusual
Densification can prevent gas from contacting with LED SERS substrate, to fundamentally improve the anti-curability of silver.It selects suitable molten
Agent, the infiltration convenient for polyimide acid to substrate, is bonded it preferably with SERS substrate, and curing schedule makes polyimides form friendship
Join reticular structure, plays a protective role.This method is low in cost, not influence later period encapsulation process, synthesis process simple, subsequent makes
With easy to operate, and belong to environmentally friendly product.
Detailed description of the invention
Fig. 1 is red ink permeability test result of the present invention.
Specific embodiment
The present invention will be described further by following embodiment.
As described above, the present invention forms fine and close polyimide acid macromolecule membrane using diamines and dianhydride, and utilize trip
From carboxyl and amino be bonded in a manner of chemical bond with silver, enhance the adhesive force of film, to improve protectant stability.Film
Itself has fabulous compactness, has effectively obstructed hydrogen sulfide gas and has contacted with silver, to achieve the effect that silver-colored anti-vulcanization.
Below by specific example is combined, the present invention will be further described, but not thereby limiting the invention.
Material therefor of the present invention can be obtained in no specified otherwise by public commercial source.Meanwhile with
LED element used in lower example, be it is common commercially available, specially treated further is not being done to silver surface using preceding, generally
Size is not limited and required.
One, the preparation of anti-silver tarnish solution.
Embodiment 1.
The preparation of anti-silver tarnish solution is equipped with magnetic agitation using three-neck flask as reaction vessel, passes to nitrogen protection, quasi-
4,4 '-diaminodiphenyl ether 0.2g of diamines really is weighed, n,N-dimethylacetamide 10ml is then added, after diamines dissolution, is claimed
It takes 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydride (BTDA) 0.3g of dianhydride to be added in three-necked bottle, 12h is reacted at 25 DEG C, then by it in 4
It is saved at DEG C stand-by.
Above-mentioned solution 1ml is taken, 8.0mlN is added, N- dimethyl acetamide shakes up, is named as A1, take A11ml is added
9mlN, N- dimethyl acetamide, shake up, and are named as A2, take A21ml, is added 9mlN, and N- dimethyl acetamide shakes up, is named as
A3.Three LED silver dollar parts are taken to immerse above-mentioned three kinds of solution respectively, solution did not had LED SERS substrate, and was then slowly withdrawn, no
Solution can be made to overflow the groove of LED element, it is then solidified into 0.8h in 50 DEG C of baking ovens.
Embodiment 2.
The preparation of anti-silver tarnish solution is equipped with magnetic agitation using three-neck flask as reaction vessel, passes to nitrogen protection, quasi-
Diamines is really weighed, then n,N-Dimethylformamide 10ml is added in 4,4 '-diaminodiphenyl ether 0.2g, after diamines dissolution, claim
Take dianhydride, pyromellitic acid anhydride 0.2g is added in three-necked bottle, and 14h is reacted at 25 DEG C, then it is saved at 4 DEG C to
With.
Above-mentioned solution 1ml is taken, 6mlN is added, dinethylformamide shakes up, and is named as B.LED silver dollar part is taken to immerse
Solution is stated, solution did not had LED SERS substrate, and was then slowly withdrawn, and solution can not be made to overflow the groove of LED element, then will
It solidifies 1h in 60 DEG C of baking ovens.
Embodiment 3.
The preparation of anti-silver tarnish solution is equipped with magnetic agitation using three-neck flask as reaction vessel, passes to nitrogen protection, quasi-
Diamines is really weighed, then n,N-dimethylacetamide 10ml is added in 4,4 '-diaminodiphenyl ether 0.2g, after diamines dissolution, claim
Dianhydride is taken, 4,4- oxygen diphthalic anhydrides 0.3g are added in three-necked bottle, 15h is reacted at 25 DEG C, then protects it at 4 DEG C
It deposits stand-by.
Above-mentioned solution 1ml is taken, 8.0mlN is added, N- dimethyl acetamide shakes up, is named as C, and LED silver dollar part is taken to immerse
Above-mentioned solution, solution did not had LED SERS substrate, were then slowly withdrawn, and solution can not be made to overflow the groove of LED element, then
It is solidified into 1h in 40 DEG C of baking ovens.
Embodiment 4.
The preparation of anti-silver tarnish solution is equipped with magnetic agitation using three-neck flask as reaction vessel, passes to nitrogen protection, quasi-
Diamines is really weighed, then n,N-Dimethylformamide 10ml is added in 4,4 '-diaminodiphenyl ether 0.2g, after diamines dissolution, claim
Take dianhydride, pyromellitic acid anhydride 0.2g is added in three-necked bottle, and 14h is reacted at 25 DEG C, then it is saved at 4 DEG C to
With.
Above-mentioned solution 1ml is taken, 6mlN is added, dinethylformamide shakes up, and is named as D, and LED silver dollar part is taken to immerse
Solution is stated, solution did not had LED SERS substrate, and was then slowly withdrawn, and solution can not be made to overflow the groove of LED element, then will
It solidifies 1h in 60 DEG C of baking ovens.
Embodiment 5.
The preparation of anti-silver tarnish solution is equipped with magnetic agitation using three-neck flask as reaction vessel, passes to nitrogen protection, quasi-
Diamines is really weighed, then n,N-dimethylacetamide 10ml is added in p-phenylenediamine 0.1g, after diamines dissolution, weigh dianhydride,
Pyromellitic dianhydride 0.2g is added in three-necked bottle, and 13h is reacted at 25 DEG C, then saves it at 4 DEG C stand-by.
Above-mentioned solution 1ml is taken, 4mlN is added, N- dimethyl acetamide shakes up, is named as E, and LED silver dollar part is taken to immerse
Solution is stated, solution did not had LED SERS substrate, and was then slowly withdrawn, and solution can not be made to overflow the groove of LED element, then will
It solidifies 1h in 60 DEG C of baking ovens.
Embodiment 6.
The preparation of anti-silver tarnish solution is equipped with magnetic agitation using three-neck flask as reaction vessel, passes to nitrogen protection, quasi-
Diamines is really weighed, then n,N-dimethylacetamide 10ml is added in 4,4 '-diaminodiphenyl ether 0.2g, after diamines dissolution, claim
Dianhydride is taken, hexafluorodianhydride (6FDA) 0.45g is added in three-necked bottle, and 14h is reacted at 25 DEG C, then saves it at 4 DEG C stand-by.
Above-mentioned solution 1ml is taken, 10.5mlN is added, N- dimethyl acetamide shakes up, is named as F, and LED silver dollar part is taken to immerse
Above-mentioned solution, solution did not had LED SERS substrate, were then slowly withdrawn, and solution can not be made to overflow the groove of LED element, then
It is solidified into 1h in 60 DEG C of baking ovens.
Two, anti-curability.
The processed LED silver dollar part A of 6 solution of examples detailed above 1- example will be used1,A2,A3, B, C, D, E, F are untreated
LED silver dollar part G, is respectively packaged it with packaging plastic on the market, is then uniformly put into 500ml sealed glass jars, bottle
It is provided with 20g sulphur, 0.2g water takes out flowers of sulfur bottle every 2h, room temperature to be down to takes out LED silver under 100 DEG C of air-proof conditions
Element surveys light decay.The influence that concentration puts curability to LED SERS substrate has been investigated for example 1, the results showed that, concentration is bigger,
Anti- sulphur performance is better.Then the A of normal concentration is taken1It makes comparisons with other 6 groups.
Specific data see the table below:
| The light decay of sample/step by step | A1 | B | C | D | E | F | G |
| 2h | 5.3% | 5.5% | 5.7% | 5.3% | 5.8% | 6.0% | 53.0% |
| 4h | 1.5% | 1.8% | 1.7% | 1.6% | 1.7% | 1.9% | |
| 6h | 2.9% | 3.0% | 3.1% | 3.2% | 3.3% | 3.2% | |
| 8h | 0.6% | 0.7% | 0.8% | 0.8% | 1.0% | 1.1% |
Note: it is dead lamp that LED light light decay, which is higher than 50%,.
By the LED silver dollar part and untreated G in example 2-4, LED silver dollar part (packaging plastic is not added) anti-vulcanization effect
It is detected, detection method are as follows: flowers of sulfur accelerates vulcanization experiment.
Specific testing procedure is as follows: by the B in embodiment 2-4, C, D, LED silver dollar part (packaging plastic is not added) is uniformly put into
In 500mL sealed glass jars, bottle is provided with 20g sulphur, and 0.2g deionized water divides 15 points under 100 DEG C of air-proof conditions after vulcanization
Clock, 4 hours, 8 hours, 10 hours postfixed point taking-up flowers of sulfur bottles, respectively near room temperature, taking-up LED silver dollar part control cure journey
Degree, the specific situation that vulcanizes see the table below:
| Silver-based vulcanizes situation/sample | B | C | D | G |
| 15min silver-based bottom surface | It is bright | It is bright | It is bright | Whole blackening |
| 4h silver-based bottom surface | It is bright | It is bright | It is bright | |
| 8h silver-based bottom surface | It is bright | It is bright | It is bright | |
| 10h silver-based bottom surface | Corner parts blackening | Corner parts blackening | Corner parts blackening |
In order to further prove that polyimide acid film will not have an impact packaging plastic performance, we have done red ink infiltration
Experiment thoroughly, by B processed in embodiment 2-4, C, D and untreated G, LED silver dollar part (adding packaging plastic) are uniformly put into
In the stainless steel cup of 500mL equipped with red ink, thermophilic digestion.Specific test condition is as follows: 170 DEG C of red ink solution (red ink
Water: ethyl alcohol=1:1) boiling 1 hour.Impermeable situation see the table below:
| Permeability/sample | B | C | D | G |
| Red ink permeates situation | Medium infiltration | Medium infiltration | Medium infiltration | Heavy infiltration |
The result shows that polyimide acid film has effectively delayed the infiltration of red ink, the performance of packaging plastic is not influenced.
Concrete outcome is shown in attached drawing 1, and the left side is untreated LED silver dollar part, and the right is processed B element in embodiment 2, and two
A sealing.
Claims (1)
1. it is a kind of for improving protectant application method of the anti-curability of LED silver dollar part, it is characterized in that:
Protective agent is prepared, which has the constitutional repeating unit of integer between 10-2000, duplicate structural unit are as follows:
Prepare protectant process specifically: using three-neck flask as reaction vessel, it is equipped with magnetic agitation, passes to nitrogen protection, it is quasi-
Diamines is really weighed, then n,N-Dimethylformamide 10ml is added in 4,4 '-diaminodiphenyl ether 0.2g, after diamines dissolution, claim
Take dianhydride, pyromellitic acid anhydride 0.2g is added in three-necked bottle, and 14h is reacted at 25 DEG C, then it is saved at 4 DEG C to
With；Or
Using three-neck flask as reaction vessel, it is equipped with magnetic agitation, passes to nitrogen protection, accurately weighs diamines, p-phenylenediamine 0.1g,
Then n,N-dimethylacetamide 10ml is added, after diamines dissolution, weighs dianhydride, three necks are added in pyromellitic acid anhydride 0.2g
In bottle, 13h is reacted at 25 DEG C, is then saved it at 4 DEG C stand-by；Or
Using three-neck flask as reaction vessel, it is equipped with magnetic agitation, passes to nitrogen protection, accurately weighs diamines, 4,4 '-diamino two
Then n,N-dimethylacetamide 10ml is added in phenylate 0.2g, after diamines dissolution, weigh dianhydride, hexafluorodianhydride (6FDA) 0.45g is added
In three-necked bottle, 14h is reacted at 25 DEG C, is then saved it at 4 DEG C stand-by；
Protective agent is dissolved in n,N-dimethylacetamide polar solvent, is configured to solution, by LED silver-based plate be placed in liquid level of solution with
Under, 30s is impregnated, then takes out, the LED silver-based plate impregnated is placed in 0.5-1h in 30-80 DEG C of baking oven, free carboxyl and ammonia
Base is bonded in a manner of chemical bond with silver, forms the polyimides sorrel for being firmly attached to silver surface, to prevent gas and LED silver
Substrate contact.
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|---|---|---|---|
| CN201610288402.5A CN106117553B (en) | 2016-05-03 | 2016-05-03 | It is a kind of for improving the protective agent and preparation and application of the anti-curability of LED silver dollar part |
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|---|---|---|---|
| CN201610288402.5A CN106117553B (en) | 2016-05-03 | 2016-05-03 | It is a kind of for improving the protective agent and preparation and application of the anti-curability of LED silver dollar part |
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| CN106117553B true CN106117553B (en) | 2019-10-01 |
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| WO2015046304A1 (en) * | 2013-09-26 | 2015-04-02 | 宇部興産株式会社 | Polyimide binder for power storage device, electrode sheet using same, and power storage device |
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| JP5233087B2 (en) * | 2006-06-28 | 2013-07-10 | 日亜化学工業株式会社 | LIGHT EMITTING DEVICE AND ITS MANUFACTURING METHOD, PACKAGE, LIGHT EMITTING DEVICE MOUNTING BOARD |
| CN104060274A (en) * | 2010-04-22 | 2014-09-24 | 日本化药株式会社 | Silver anti-tarnishing agent, silver anti-tarnishing resin composition, silver anti-tarnishing method, and light-emitting diode using same |
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| WO2015046304A1 (en) * | 2013-09-26 | 2015-04-02 | 宇部興産株式会社 | Polyimide binder for power storage device, electrode sheet using same, and power storage device |
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