CN110982479A - LED packaging conductive polyamide hot melt adhesive and preparation method thereof - Google Patents
LED packaging conductive polyamide hot melt adhesive and preparation method thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J177/00—Adhesives based on polyamides obtained by reactions forming a carboxylic amide link in the main chain; Adhesives based on derivatives of such polymers
- C09J177/06—Polyamides derived from polyamines and polycarboxylic acids
- C09J177/08—Polyamides derived from polyamines and polycarboxylic acids from polyamines and polymerised unsaturated fatty acids
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- 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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/34—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids using polymerised unsaturated fatty acids
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses an LED packaging conductive polyamide hot melt adhesive and a preparation method thereof, wherein the LED packaging conductive polyamide hot melt adhesive comprises 55-100 parts of unsaturated fatty acid dimer, 10-20 parts of ethylenediamine, 10-20 parts of hexamethylenediamine, 15-20 parts of sebacic acid, 5-12 parts of dimethyl silicone oil, 1-2 parts of alkyl modified organic siloxane, 5-12 parts of waterproof filler, 5-10 parts of conductive agent, 3-5 parts of tackifier, 1-4 parts of viscosity regulator, 2-4 parts of anti-aging agent, 3-8 parts of transparent agent and 2-5 parts of fluorescent powder. The conductive polyamide hot melt adhesive prepared by the invention has good heat resistance and heat dissipation, has waterproof and anti-permeability performance, chemical erosion resistance and abrasion resistance, has strong bonding force, and has excellent conductivity and dispersibility and stable conductivity by using the conductive mica powder as a conductive agent.
Description
Technical Field
The invention relates to the technical field of hot melt adhesive processing, in particular to an LED packaging conductive polyamide hot melt adhesive and a preparation method thereof.
Background
The polyamide hot melt adhesive takes polyamide resin as a matrix, and is linear thermoplastic resin with a plurality of repeated amide groups on a molecular main chain. Polyamide hot melt adhesives have a notable feature over other thermoplastic resins in that, when heated and cooled, both melting and solidification of the resin occur within a relatively narrow temperature range. The characteristics ensure that the polyamide hot melt adhesive can be rapidly solidified by slightly cooling after being heated, melted and coated during construction, and also has better adhesive property at the temperature close to the softening point. The hydrogen on the amide group of the polyamide resin can be combined with the electron-donating carbonyl on the other amide group chain segment to form a firm hydrogen bond, so that the melting point of the resin is increased, and the polyamide resin has good flexibility, oil resistance and cementing property, which are improved along with the increase of the molecular weight of the resin. Therefore, polyamide hot melt adhesives are widely used for LED packaging.
However, the polyamide hot melt adhesive used in the current market has the defect of water impermeability, when the product is wetted, the hot melt adhesive on the product is easy to separate, and the integral performance of the existing conductive polyamide hot melt adhesive needs to be improved.
Therefore, it is necessary to invent a conductive polyamide hot melt adhesive for LED package and a preparation method thereof to solve the above problems.
Disclosure of Invention
The invention aims to provide an LED packaging conductive polyamide hot melt adhesive and a preparation method thereof, which improve the heat resistance and the heat dissipation of the polyamide hot melt adhesive by preparing a high-softening-point polyamide resin adhesive and matching with dimethyl silicone oil, alkyl modified organosiloxane and waterproof filler for modification, simultaneously ensure that the inner structure is uniform and compact, improve the waterproof impermeability, the chemical erosion resistance and the abrasion resistance of the hot melt adhesive, improve the stability of the hot melt adhesive, prepare modified polymer latex and blend and polymerize with the modified polyamide hot melt adhesive for uniform tempering, adjust the viscosity of the colloid by using hydrophobic water-soluble polyelectrolyte and cyclohexanol, improve the cohesive force of the colloid, ensure that the conductive mica powder has excellent conductivity and dispersibility and stable conductivity, and solve the defects in the technology.
In order to achieve the above purpose, the invention provides the following technical scheme: an LED packaging conductive polyamide hot melt adhesive and a preparation method thereof are disclosed, wherein the hot melt adhesive comprises the following components by weight: 55-100 parts of unsaturated fatty acid dimer, 10-20 parts of ethylenediamine, 10-20 parts of hexanediamine, 15-20 parts of sebacic acid, 5-12 parts of dimethyl silicone oil, 1-2 parts of alkyl modified organosiloxane, 5-12 parts of waterproof filler, 5-10 parts of conductive agent, 3-5 parts of tackifier, 1-4 parts of viscosity regulator, 2-4 parts of anti-aging agent, 3-8 parts of transparent agent and 2-5 parts of fluorescent powder.
Preferably, the hot melt adhesive composition comprises by weight: 75-78 parts of unsaturated fatty acid dimer, 19-22 parts of ethylenediamine, 18-21 parts of hexamethylene diamine, 16-19 parts of sebacic acid, 6-9 parts of dimethyl silicone oil, 1-2 parts of alkyl modified organosiloxane, 7-10 parts of waterproof filler, 8-10 parts of conductive agent, 3-5 parts of tackifier, 2-4 parts of viscosity regulator, 2-4 parts of anti-aging agent, 4-6 parts of transparent agent and 2-5 parts of fluorescent powder.
Preferably, the waterproof filler consists of silicon micropowder and sodium bentonite, and the proportion of the silicon micropowder to the sodium bentonite is set to be 2-4: 1.
preferably, the tackifier is hydrophobic water-soluble polyelectrolyte, and the viscosity regulator is cyclohexanol.
Preferably, the conductive agent is set as conductive mica powder, and the anti-aging agent is set as polymerized rosin glycerin ester.
Preferably, the transparent agent is chloroform, and the fluorescent powder is photo-induced energy storage luminous powder.
A preparation method of an LED packaging conductive polyamide hot melt adhesive comprises the following specific operation steps:
the method comprises the following steps: preparing raw materials, and collecting unsaturated fatty acid dimer, ethylenediamine, hexanediamine, sebacic acid, simethicone, alkyl modified organic siloxane, waterproof filler, conductive agent, tackifier, viscosity regulator, anti-aging agent, transparent agent and fluorescent powder for later use;
step two: adding unsaturated fatty acid dimer, ethylenediamine, hexanediamine and sebacic acid into a high-pressure reaction kettle according to a certain proportion, heating the kettle to 230-260 ℃, keeping the pressure in the kettle at 1.5-1.8Mpa, and cooling after polycondensation reaction for 2-3h to obtain polyamide resin adhesive;
step three: adding dimethyl silicone oil, alkyl modified organic siloxane and a waterproof filler into the prepared polyamide resin adhesive, heating and uniformly stirring to prepare a modified polyamide hot melt adhesive;
step four: mixing and uniformly stirring a conductive agent, a tackifier, a viscosity regulator, an anti-aging agent, a transparent agent and fluorescent powder to prepare modified polymerization latex;
step five: mixing the modified polyamide hot melt adhesive prepared in the third step with the polyamide resin adhesive prepared in the fourth step, placing the mixture into an internal mixer, carrying out blending polymerization at the temperature of 250-280 ℃ and under the upper plug pressure of 0.6-0.8Mpa, and cooling to obtain a semi-finished product of the conductive polyamide hot melt adhesive;
step six: and (3) stirring the semi-finished product of the conductive polyamide hot melt adhesive again, performing vacuum defoaming treatment by using an ultrasonic oscillator, and filling and sealing when no obvious bubbles exist to finish the preparation of the conductive polyamide hot melt adhesive.
Preferably, the heating temperature in the third step is set to be 200-220 ℃, and the stirring time is set to be 1-2 h.
In the technical scheme, the invention provides the following technical effects and advantages:
1. the preparation method comprises the steps of preparing a high-softening-point polyamide resin adhesive, modifying the high-softening-point polyamide resin adhesive by matching with dimethyl silicone oil, alkyl modified organic siloxane and a waterproof filler, improving the heat resistance and the heat dissipation of the polyamide hot melt adhesive, enabling the texture of an inner structure to be uniform and compact, improving the waterproof and anti-permeability performance, the chemical erosion resistance and the abrasion resistance of the hot melt adhesive, improving the stability of the hot melt adhesive, preparing modified polymer latex, blending and polymerizing the modified polymer latex and the modified polyamide hot melt adhesive uniformly for tempering, adjusting the viscosity of a colloid by using hydrophobic water-soluble polyelectrolyte and cyclohexanol, improving the cohesive force of the colloid, and enabling;
2. through adding dimethyl silicone oil, silica fume and sodium bentonite, this electrically conductive polyamide hot melt adhesive material can be antistatic in high conductivity, reduce surface dust and adsorb, polymerized rosin glycerin ester can effectively prolong the life and the bonding endurance of hot melt adhesive, chloroform makes the hot melt adhesive highly transparent, the LED light of being convenient for passes through, phosphor powder absorbs LED light energy to release shimmer in the dark, the wholeness ability of electrically conductive polyamide hot melt adhesive has been improved.
Detailed Description
The present invention will be described in further detail below in order to enable those skilled in the art to better understand the technical solution of the present invention.
The invention provides an LED packaging conductive polyamide hot melt adhesive and a preparation method thereof, wherein the hot melt adhesive comprises the following components in parts by weight: 75 parts of unsaturated fatty acid dimer, 19 parts of ethylenediamine, 18 parts of hexamethylenediamine, 16 parts of sebacic acid, 6 parts of dimethyl silicone oil, 1 part of alkyl modified organosiloxane, 7 parts of waterproof filler, 8 parts of conductive agent, 3 parts of tackifier, 2 parts of viscosity regulator, 2 parts of anti-aging agent, 4 parts of transparent agent and 2 parts of fluorescent powder;
the waterproof filler is composed of silicon micropowder and sodium bentonite, and the proportion of the silicon micropowder to the sodium bentonite is set to be 2: 1;
further, the tackifier is set to be hydrophobic water-soluble polyelectrolyte, and the viscosity regulator is set to be cyclohexanol;
further, the conductive agent is set as conductive mica powder, and the anti-aging agent is set as polymerized rosin glycerin ester;
further, the transparent agent is chloroform, and the fluorescent powder is photo-induced energy storage luminous powder.
A preparation method of an LED packaging conductive polyamide hot melt adhesive comprises the following specific operation steps:
the method comprises the following steps: preparing raw materials, and collecting unsaturated fatty acid dimer, ethylenediamine, hexanediamine, sebacic acid, simethicone, alkyl modified organic siloxane, waterproof filler, conductive agent, tackifier, viscosity regulator, anti-aging agent, transparent agent and fluorescent powder for later use;
step two: adding unsaturated fatty acid dimer, ethylenediamine, hexamethylenediamine and sebacic acid into a high-pressure reaction kettle according to a certain proportion, heating the kettle to 230 ℃, keeping the pressure in the kettle at 1.5Mpa, and cooling after polycondensation reaction for 2 hours to obtain polyamide resin adhesive;
step three: adding dimethyl silicone oil, alkyl modified organic siloxane and a waterproof filler into the prepared polyamide resin adhesive, heating and stirring uniformly, then heating to 200 ℃, stirring for 1h, and cooling to prepare a modified polyamide hot melt adhesive;
step four: mixing and uniformly stirring a conductive agent, a tackifier, a viscosity regulator, an anti-aging agent, a transparent agent and fluorescent powder to prepare modified polymerization latex;
step five: mixing the modified polyamide hot melt adhesive prepared in the third step with the polyamide resin adhesive prepared in the fourth step, placing the mixture into an internal mixer, performing blending polymerization at the temperature of 250 ℃ and under the upper ram pressure of 0.6Mpa, and cooling to obtain a semi-finished product of the conductive polyamide hot melt adhesive;
step six: and (3) stirring the semi-finished product of the conductive polyamide hot melt adhesive again, performing vacuum defoaming treatment by using an ultrasonic oscillator, and filling and sealing when no obvious bubbles exist to finish the preparation of the conductive polyamide hot melt adhesive.
The conductive polyamide hot melt adhesive prepared in the embodiment has the advantages of high transparency, good brightness, high surface smoothness of a hot melt adhesive solid body, uniform texture, excellent waterproof and anti-seepage performance, high heat dissipation efficiency, strong bonding force of the hot melt adhesive, aging resistance and good conductive effect, and in addition, the result of the performance detection of the prepared conductive polyamide hot melt adhesive shows that: the softening point of the hot melt adhesive solid is 184 ℃, the bonding stripping strength is 6.52N/mm, the shear strength of the hot melt adhesive solid is 6.2Mpa, the Shore hardness is 74HD, the resistivity is 106 omega cm, the conductivity is good, the overall performance is stable, the market demand can be met, and compared with the existing similar products, the hot melt adhesive has obvious performance improvement.
Example 2:
the invention provides an LED packaging conductive polyamide hot melt adhesive and a preparation method thereof, wherein the hot melt adhesive comprises the following components in parts by weight: 76 parts of unsaturated fatty acid dimer, 20 parts of ethylenediamine, 19 parts of hexamethylenediamine, 17 parts of sebacic acid, 7 parts of dimethyl silicone oil, 1.5 parts of alkyl modified organosiloxane, 8 parts of waterproof filler, 9 parts of conductive agent, 4 parts of tackifier, 3 parts of viscosity regulator, 3 parts of anti-aging agent, 5 parts of transparent agent and 3 parts of fluorescent powder;
the waterproof filler is composed of silicon micropowder and sodium bentonite, and the proportion of the silicon micropowder to the sodium bentonite is set to be 3: 1;
further, the tackifier is set to be hydrophobic water-soluble polyelectrolyte, and the viscosity regulator is set to be cyclohexanol;
further, the conductive agent is set as conductive mica powder, and the anti-aging agent is set as polymerized rosin glycerin ester;
further, the transparent agent is chloroform, and the fluorescent powder is photo-induced energy storage luminous powder.
A preparation method of an LED packaging conductive polyamide hot melt adhesive comprises the following specific operation steps:
the method comprises the following steps: preparing raw materials, and collecting unsaturated fatty acid dimer, ethylenediamine, hexanediamine, sebacic acid, simethicone, alkyl modified organic siloxane, waterproof filler, conductive agent, tackifier, viscosity regulator, anti-aging agent, transparent agent and fluorescent powder for later use;
step two: adding unsaturated fatty acid dimer, ethylenediamine, hexamethylenediamine and sebacic acid into a high-pressure reaction kettle according to a certain proportion, heating the kettle to 240 ℃, keeping the pressure in the kettle at 1.6Mpa, and cooling after polycondensation reaction for 2.5 hours to obtain polyamide resin adhesive;
step three: adding dimethyl silicone oil, alkyl modified organic siloxane and a waterproof filler into the prepared polyamide resin adhesive, heating and stirring uniformly, then heating to 210 ℃, stirring for 1h, and cooling to prepare a modified polyamide hot melt adhesive;
step four: mixing and uniformly stirring a conductive agent, a tackifier, a viscosity regulator, an anti-aging agent, a transparent agent and fluorescent powder to prepare modified polymerization latex;
step five: mixing the modified polyamide hot melt adhesive prepared in the third step with the polyamide resin adhesive prepared in the fourth step, placing the mixture into an internal mixer, performing blending polymerization at the temperature of 260 ℃ and under the upper ram pressure of 0.7Mpa, and cooling to obtain a semi-finished product of the conductive polyamide hot melt adhesive;
step six: and (3) stirring the semi-finished product of the conductive polyamide hot melt adhesive again, performing vacuum defoaming treatment by using an ultrasonic oscillator, and filling and sealing when no obvious bubbles exist to finish the preparation of the conductive polyamide hot melt adhesive.
Comparative embodiment 1, the electrically conductive polyamide hot melt adhesive transparency degree of preparing in this embodiment is high, and luminance is good, and hot melt adhesive solid surface smoothness is high, and the texture is even, possesses good waterproof and anti-seepage performance, and the radiating efficiency is high, and hot melt colloid adhesion strength is strong, and the ageing resistance is electrically conductive effectual, and in addition, to the electrically conductive polyamide hot melt adhesive performance post detection result display of preparation in this embodiment: the hot melt adhesive has the solid softening point of 185 ℃, the bonding peel strength of 6.61N/mm, the solid shear strength of 6.8Mpa, the Shore hardness of 76HD, the resistivity of 107 omega cm, good conductivity and stable overall performance, can meet the market demand, and has obvious performance improvement compared with the existing similar products.
Example 3:
the invention provides an LED packaging conductive polyamide hot melt adhesive and a preparation method thereof, wherein the hot melt adhesive comprises the following components in parts by weight: 77 parts of unsaturated fatty acid dimer, 21 parts of ethylenediamine, 20 parts of hexanediamine, 18 parts of sebacic acid, 8 parts of dimethyl silicone oil, 1.5 parts of alkyl modified organosiloxane, 9 parts of waterproof filler, 9 parts of conductive agent, 4 parts of tackifier, 4 parts of viscosity regulator, 3 parts of anti-aging agent, 5 parts of transparent agent and 4 parts of fluorescent powder;
the waterproof filler is composed of silicon micropowder and sodium bentonite, and the proportion of the silicon micropowder to the sodium bentonite is set to be 4: 1;
further, the tackifier is set to be hydrophobic water-soluble polyelectrolyte, and the viscosity regulator is set to be cyclohexanol;
further, the conductive agent is set as conductive mica powder, and the anti-aging agent is set as polymerized rosin glycerin ester;
further, the transparent agent is chloroform, and the fluorescent powder is photo-induced energy storage luminous powder.
A preparation method of an LED packaging conductive polyamide hot melt adhesive comprises the following specific operation steps:
the method comprises the following steps: preparing raw materials, and collecting unsaturated fatty acid dimer, ethylenediamine, hexanediamine, sebacic acid, simethicone, alkyl modified organic siloxane, waterproof filler, conductive agent, tackifier, viscosity regulator, anti-aging agent, transparent agent and fluorescent powder for later use;
step two: adding unsaturated fatty acid dimer, ethylenediamine, hexamethylenediamine and sebacic acid into a high-pressure reaction kettle according to a certain proportion, heating the kettle to 250 ℃, keeping the pressure in the kettle at 1.7Mpa, and cooling after polycondensation reaction for 3 hours to obtain polyamide resin adhesive;
step three: adding dimethyl silicone oil, alkyl modified organic siloxane and a waterproof filler into the prepared polyamide resin adhesive, heating and stirring uniformly, then heating to 210 ℃, stirring for 1.5h, and cooling to prepare a modified polyamide hot melt adhesive;
step four: mixing and uniformly stirring a conductive agent, a tackifier, a viscosity regulator, an anti-aging agent, a transparent agent and fluorescent powder to prepare modified polymerization latex;
step five: mixing the modified polyamide hot melt adhesive prepared in the third step with the polyamide resin adhesive prepared in the fourth step, placing the mixture into an internal mixer, performing blending polymerization at the temperature of 270 ℃ and under the upper ram pressure of 0.7Mpa, and cooling to obtain a semi-finished product of the conductive polyamide hot melt adhesive;
step six: and (3) stirring the semi-finished product of the conductive polyamide hot melt adhesive again, performing vacuum defoaming treatment by using an ultrasonic oscillator, and filling and sealing when no obvious bubbles exist to finish the preparation of the conductive polyamide hot melt adhesive.
Comparative embodiment 1 and 2, the electrically conductive polyamide hot melt adhesive transparency that prepares in this embodiment is high, and the luminance is good, and hot melt adhesive solid surface smoothness is high, and the texture is even, possesses good waterproof and anti-seepage performance, and the radiating efficiency is high, and hot melt colloid adhesion is strong, and the ageing resistance is electrically conductive effectual, in addition, to the electrically conductive polyamide hot melt adhesive performance detection back result display of preparation in this embodiment: the hot melt adhesive has the solid softening point of 188 ℃, the bonding peel strength of 6.65N/mm, the solid shear strength of 7.3Mpa, the Shore hardness of 78HD, the resistivity of 104 omega cm, good conductivity and stable overall performance, can meet the market demand, and has obvious performance improvement compared with the existing similar products.
Example 4:
the invention provides an LED packaging conductive polyamide hot melt adhesive and a preparation method thereof, wherein the hot melt adhesive comprises the following components in parts by weight: 78 parts of unsaturated fatty acid dimer, 22 parts of ethylenediamine, 21 parts of hexamethylenediamine, 19 parts of sebacic acid, 9 parts of dimethyl silicone oil, 2 parts of alkyl modified organosiloxane, 10 parts of waterproof filler, 10 parts of conductive agent, 5 parts of tackifier, 4 parts of viscosity regulator, 4 parts of anti-aging agent, 6 parts of transparent agent and 5 parts of fluorescent powder;
the waterproof filler is composed of silicon micropowder and sodium bentonite, and the proportion of the silicon micropowder to the sodium bentonite is set to be 4: 1;
further, the tackifier is set to be hydrophobic water-soluble polyelectrolyte, and the viscosity regulator is set to be cyclohexanol;
further, the conductive agent is set to be conductive mica powder, and the anti-aging agent is set to be polymerized rosin glyceride;
further, the transparent agent is chloroform, and the fluorescent powder is photo-induced energy storage luminous powder.
A preparation method of an LED packaging conductive polyamide hot melt adhesive comprises the following specific operation steps:
the method comprises the following steps: preparing raw materials, and collecting unsaturated fatty acid dimer, ethylenediamine, hexanediamine, sebacic acid, simethicone, alkyl modified organic siloxane, waterproof filler, conductive agent, tackifier, viscosity regulator, anti-aging agent, transparent agent and fluorescent powder for later use;
step two: adding unsaturated fatty acid dimer, ethylenediamine, hexamethylenediamine and sebacic acid into a high-pressure reaction kettle according to a certain proportion, heating the kettle to 260 ℃, keeping the pressure in the kettle at 1.8Mpa, and cooling after polycondensation reaction for 3 hours to obtain polyamide resin adhesive;
step three: adding dimethyl silicone oil, alkyl modified organic siloxane and a waterproof filler into the prepared polyamide resin adhesive, heating and stirring uniformly, then heating to 220 ℃, stirring for 2h, and cooling to prepare a modified polyamide hot melt adhesive;
step four: mixing and uniformly stirring a conductive agent, a tackifier, a viscosity regulator, an anti-aging agent, a transparent agent and fluorescent powder to prepare modified polymerization latex;
step five: mixing the modified polyamide hot melt adhesive prepared in the third step with the polyamide resin adhesive prepared in the fourth step, placing the mixture into an internal mixer, carrying out blending polymerization at the temperature of 280 ℃ and under the upper ram pressure of 0.8Mpa, and cooling to obtain a semi-finished product of the conductive polyamide hot melt adhesive;
step six: and (3) stirring the semi-finished product of the conductive polyamide hot melt adhesive again, performing vacuum defoaming treatment by using an ultrasonic oscillator, and filling and sealing when no obvious bubbles exist to finish the preparation of the conductive polyamide hot melt adhesive.
Comparative example 1-3, the electrically conductive polyamide hot melt adhesive transparency degree of preparing in this embodiment is high, and luminance is good, and hot melt adhesive solid surface smoothness is high, and the texture is even, possesses good waterproof and anti-seepage performance, and the radiating efficiency is high, and hot melt colloid adhesion is strong, and the ageing resistance is electrically conductive effectual, and in addition, to the electrically conductive polyamide hot melt adhesive performance post detection result of preparation in this embodiment show: the softening point of the hot melt adhesive solid is 187 ℃, the bonding peel strength is 6.59N/mm, the shear strength of the hot melt adhesive solid is 7.1Mpa, the Shore hardness is 77HD, the resistivity is 105 omega cm, the conductivity is good, the overall performance is stable, the market demand can be met, and compared with the existing similar products, the hot melt adhesive has obvious performance improvement.
The following table is obtained according to examples 1 to 4:
from the above table, it can be seen that the raw materials in example 3 are in moderate proportion, the processing temperature is moderate, the processing technology provided by this example is most suitable for the processing production of the conductive polyamide hot melt adhesive, the mechanical properties of the polyamide hot melt adhesive can be modified to be optimal, the softening point, the peel strength, the shear strength, the shore hardness and the conductivity of the polyamide hot melt adhesive are obviously improved compared with those of the similar products in the market, the production and the popularization are convenient, the quality of the product can be approved by consumers, in addition, a proper amount of sebacic acid is added to improve the softening point of the colloid, the heat resistance and the heat dissipation of the polyamide hot melt adhesive are improved by matching with the dimethyl silicone oil, the alkyl modified organic siloxane and the waterproof filler for modification, the internal structure texture is uniform and compact, the water resistance, the chemical erosion resistance and the abrasion resistance, mixing and stirring uniformly the conductive agent, the tackifier, the viscosity regulator, the anti-aging agent, the transparent agent and the fluorescent powder to prepare modified polymerization latex, the modified polymerized latex and the modified polyamide hot melt adhesive are mixed and polymerized in an internal mixer, so that the conductive polyamide hot melt adhesive is uniformly tempered, the hydrophobic water-soluble polyelectrolyte and cyclohexanol are used for adjusting the viscosity of the colloid, the adhesive force of the colloid is improved, the conductive mica powder has excellent conductivity and dispersibility, moreover, the conductive polyamide hot melt adhesive material is antistatic, dust adsorption can be reduced, polymerized rosin glyceride can effectively prolong the service life and the bonding endurance of the hot melt adhesive, chloroform enables the hot melt adhesive to be highly transparent and facilitates LED light to pass through, fluorescent powder absorbs LED light energy, and the low-light-level adhesive releases low light in the dark, improves the overall performance of the conductive polyamide hot melt adhesive, and can be used for LED packaging materials.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Therefore, the above description is illustrative in nature and should not be construed as limiting the scope of the invention, which is defined by the appended claims, and any modifications, equivalents, improvements made within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (8)
1. The utility model provides a LED encapsulates electrically conductive polyamide hot melt adhesive which characterized in that: the hot melt adhesive comprises the following components in parts by weight: 55-100 parts of unsaturated fatty acid dimer, 10-20 parts of ethylenediamine, 10-20 parts of hexamethylene diamine, 15-20 parts of sebacic acid, 5-12 parts of dimethyl silicone oil, 1-2 parts of alkyl modified organosiloxane, 5-12 parts of waterproof filler, 5-10 parts of conductive agent, 3-5 parts of tackifier, 1-4 parts of viscosity regulator, 2-4 parts of anti-aging agent, 3-8 parts of transparent agent and 2-5 parts of fluorescent powder.
2. The LED packaging conductive polyamide hot melt adhesive as claimed in claim 1, wherein: the hot melt adhesive comprises the following components in parts by weight: 75-78 parts of unsaturated fatty acid dimer, 19-22 parts of ethylenediamine, 18-21 parts of hexamethylene diamine, 16-19 parts of sebacic acid, 6-9 parts of dimethyl silicone oil, 1-2 parts of alkyl modified organosiloxane, 7-10 parts of waterproof filler, 8-10 parts of conductive agent, 3-5 parts of tackifier, 2-4 parts of viscosity regulator, 2-4 parts of anti-aging agent, 4-6 parts of transparent agent and 2-5 parts of fluorescent powder.
3. The LED packaging conductive polyamide hot melt adhesive as claimed in claim 1, wherein: the waterproof filler is composed of silicon micropowder and sodium bentonite, and the proportion of the silicon micropowder to the sodium bentonite is set to be 2-4: 1.
4. the LED packaging conductive polyamide hot melt adhesive as claimed in claim 1, wherein: the viscosity increaser is hydrophobic water-soluble polyelectrolyte, and the viscosity regulator is cyclohexanol.
5. The LED packaging conductive polyamide hot melt adhesive as claimed in claim 1, wherein: the conductive agent is set to be conductive mica powder, and the anti-aging agent is set to be polymerized rosin glyceride.
6. The LED packaging conductive polyamide hot melt adhesive as claimed in claim 1, wherein: the transparent agent is chloroform, and the fluorescent powder is photo-induced energy storage luminous powder.
7. A preparation method of an LED packaging conductive polyamide hot melt adhesive is characterized by comprising the following steps: the specific operation steps are as follows:
the method comprises the following steps: preparing raw materials, and collecting unsaturated fatty acid dimer, ethylenediamine, hexanediamine, sebacic acid, simethicone, alkyl modified organic siloxane, waterproof filler, conductive agent, tackifier, viscosity regulator, anti-aging agent, transparent agent and fluorescent powder for later use;
step two: adding unsaturated fatty acid dimer, ethylenediamine, hexamethylenediamine and sebacic acid into a high-pressure reaction kettle according to a certain proportion, heating the kettle to 230-;
step three: adding dimethyl silicone oil, alkyl modified organic siloxane and a waterproof filler into the prepared polyamide resin adhesive, heating and uniformly stirring to prepare a modified polyamide hot melt adhesive;
step four: mixing and uniformly stirring a conductive agent, a tackifier, a viscosity regulator, an anti-aging agent, a transparent agent and fluorescent powder to prepare modified polymerization latex;
step five: mixing the modified polyamide hot melt adhesive prepared in the third step with the polyamide resin adhesive prepared in the fourth step, placing the mixture into an internal mixer, performing blending polymerization at the temperature of 250-280 ℃ and under the upper plug pressure of 0.6-0.8Mpa, and cooling to obtain a semi-finished product of the conductive polyamide hot melt adhesive;
step six: and (3) stirring the semi-finished product of the conductive polyamide hot melt adhesive again, then performing vacuum defoaming treatment by using an ultrasonic oscillator, and filling and sealing when no obvious bubbles exist, thereby completing the preparation of the conductive polyamide hot melt adhesive.
8. The preparation method of the LED packaging conductive polyamide hot melt adhesive according to claim 7, characterized in that: in the third step, the heating temperature is set to be 200-220 ℃, and the stirring time is set to be 1-2 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773776A (en) * | 2021-09-24 | 2021-12-10 | 深圳市美之电实业有限公司 | Preparation method of waterproof adhesive |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104893625A (en) * | 2015-05-27 | 2015-09-09 | 合肥卓元科技服务有限公司 | Hot melt adhesive for sealing aluminum foil and preparation method of hot melt adhesive |
| CN105934232A (en) * | 2014-02-20 | 2016-09-07 | 堺化学工业株式会社 | Aqueous dispersion of inorganic powder particles subjected to hydrophobic organic surface treatment, and cosmetic including same |
| CN107502276A (en) * | 2017-08-25 | 2017-12-22 | 安徽省鸿鑫生物科技有限公司 | A kind of LED encapsulation electrically conductive polyamide PUR and preparation method thereof |
| CN109609053A (en) * | 2018-12-19 | 2019-04-12 | 广西华纳新材料科技有限公司 | A kind of masonry work sealant nanometer calcium carbonate and preparation method thereof |
-
2019
- 2019-12-18 CN CN201911310509.5A patent/CN110982479A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105934232A (en) * | 2014-02-20 | 2016-09-07 | 堺化学工业株式会社 | Aqueous dispersion of inorganic powder particles subjected to hydrophobic organic surface treatment, and cosmetic including same |
| CN104893625A (en) * | 2015-05-27 | 2015-09-09 | 合肥卓元科技服务有限公司 | Hot melt adhesive for sealing aluminum foil and preparation method of hot melt adhesive |
| CN107502276A (en) * | 2017-08-25 | 2017-12-22 | 安徽省鸿鑫生物科技有限公司 | A kind of LED encapsulation electrically conductive polyamide PUR and preparation method thereof |
| CN109609053A (en) * | 2018-12-19 | 2019-04-12 | 广西华纳新材料科技有限公司 | A kind of masonry work sealant nanometer calcium carbonate and preparation method thereof |
Non-Patent Citations (12)
| Title |
|---|
| 刘荣贵等: "《五金交电化工建材商品实用手册》", 31 January 1997, 中国物资出版社 * |
| 司航: "《有机化工原料 第二版》", 31 January 1995, 化学工业出版社 * |
| 周玉枝等: "《惊奇化学》", 31 August 2013, 上海辞书出版社 * |
| 廖润华等: "《环境治理功能材料》", 30 April 2017, 中国建材工业出版社 * |
| 李兰亭等: "《木材加工材料学》", 31 March 1992, 东北林业大学出版社 * |
| 杨淑丽等: "《密封胶粘剂》", 30 April 2004, 中国石化出版社 * |
| 章基凯等: "《有机硅材料》", 31 October 1999, 中国物资出版社 * |
| 绳秀珍等: "《生物实验技术》", 30 September 2007, 中国海洋大学出版社 * |
| 詹益兴等: "《精细化工新产品 第4集》", 30 June 2009, 科学技术文献出版社 * |
| 郑晓宇等: "《油田化学品》", 31 January 2001, 化学工业出版社 * |
| 马一平等: "《建筑功能材料》", 31 March 2014, 同济大学出版社 * |
| 黄玉媛等: "《精细化工配方常用原料手册》", 31 March 1998, 广东科技出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773776A (en) * | 2021-09-24 | 2021-12-10 | 深圳市美之电实业有限公司 | Preparation method of waterproof adhesive |
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