CN115011304B - Optical bonding pouring sealant and preparation method thereof - Google Patents

Optical bonding pouring sealant and preparation method thereof Download PDF

Info

Publication number
CN115011304B
CN115011304B CN202210880559.2A CN202210880559A CN115011304B CN 115011304 B CN115011304 B CN 115011304B CN 202210880559 A CN202210880559 A CN 202210880559A CN 115011304 B CN115011304 B CN 115011304B
Authority
CN
China
Prior art keywords
parts
pouring sealant
component
raw materials
optical bonding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210880559.2A
Other languages
Chinese (zh)
Other versions
CN115011304A (en
Inventor
屈裴
汪云川
孟田忠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Huizhou Huali New Material Co ltd
Original Assignee
Huizhou Huali New Material Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Huizhou Huali New Material Co ltd filed Critical Huizhou Huali New Material Co ltd
Priority to CN202210880559.2A priority Critical patent/CN115011304B/en
Publication of CN115011304A publication Critical patent/CN115011304A/en
Application granted granted Critical
Publication of CN115011304B publication Critical patent/CN115011304B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The application relates to the field of pouring sealant production, and in particular discloses an optical bonding pouring sealant and a preparation method thereof, wherein the optical bonding pouring sealant comprises the following components in percentage by weight (1-1.5): 1 and B, wherein the A comprises the following raw materials: 100 parts of base material, 5-10 parts of double-end vinyl silicone oil and 0.1-1 part of platinum catalyst; the component B comprises the following raw materials: 100 parts of base material, 7-12 parts of hydrogen-containing silicone oil, 30-45 parts of phenyl silicone oil with the mass concentration of phenyl not less than 30%, 1-5 parts of modified tackifier, 1-5 parts of modified organosilicon and 1-30 parts of high-phenyl resin; the base material comprises: 100 parts of high-phenyl resin; the preparation method of the pouring sealant comprises the following steps: mixing and stirring the raw materials of the component A and the component B, and vacuum defoaming; and uniformly stirring the prepared component A and component B to obtain the optical bonding pouring sealant. The pouring sealant can be obtained, and has high light transmittance, high refractive index, good adhesive property and high tensile strength, and the pouring sealant has excellent comprehensive performance.

Description

Optical bonding pouring sealant and preparation method thereof
Technical Field
The application relates to the field of pouring sealant production, in particular to an optical bonding pouring sealant and a preparation method thereof.
Background
The optical bonding pouring sealant is a thermosetting polymer insulating material which is cured into excellent performance under normal temperature or heating condition, can be used for pouring and sealing electronic components such as LED lamp strips, and has the functions of bonding, sealing and coating protection.
Before solidification, the optical bonding pouring sealant exists in a liquid shape, and an operator fills the liquid optical bonding pouring sealant on the electronic component with the adhesive through a glue filling machine, so that the optical bonding pouring sealant has the functions of water resistance, moisture resistance, vibration resistance, insulation and heat conduction on the electronic component after solidification.
However, the conventional optical adhesive pouring sealant still has problems in terms of light transmittance, refractive index, adhesive performance with glass substrates, PC substrates and PMMA substrates, tensile strength and the like.
Disclosure of Invention
In order to solve the problems of the prior optical bonding pouring sealant in terms of light transmittance, refractive index, bonding performance with glass substrates, PC substrates and PMMA substrates, tensile strength and the like. The application provides an optical bonding pouring sealant and a preparation method thereof.
The optical bonding pouring sealant and the preparation method thereof provided by the application adopt the following technical scheme:
in a first aspect, the present application provides an optical bonding pouring sealant, which adopts the following technical scheme:
the optical bonding pouring sealant comprises the following components in percentage by weight (1-1.5): a component A and a component B of the composition 1,
the component A comprises the following raw materials in parts by weight: 100 parts of base material, 5-10 parts of double-end vinyl silicone oil and 0.1-1 part of platinum catalyst;
the component B comprises the following raw materials in parts by weight: 100 parts of base material, 7-12 parts of hydrogen-containing silicone oil, 30-45 parts of phenyl silicone oil with the mass concentration of phenyl not less than 30%, 1-5 parts of modified tackifier, 1-5 parts of modified organosilicon and 1-30 parts of high-phenyl resin; the base material comprises the following components in parts by weight: 100 parts of high-phenyl resin;
the preparation raw materials of the high-phenyl resin comprise the following components in parts by weight: 2-3 parts of phenyl triethoxysilane, 5-7 parts of diphenyl dimethoxy silane and 3-6 parts of tetraphenyl dimethyl disiloxane; the preparation of the high-phenyl resin comprises the following steps: heating the raw materials for preparing the high-phenyl resin in an oil bath at 55-60 ℃, and condensing and refluxing under the stirring condition to prepare the high-phenyl resin.
The preparation raw materials of the modified tackifier comprise the following components in parts by weight: 15-20 parts of diphenyl silicon glycol, 8-10 parts of epoxy silane, 8-10 parts of ester silane, 1-3 parts of boric acid ester, 20-35 parts of toluene and 0.2-0.5 part of catalyst; the preparation of the modified tackifier comprises the following steps: uniformly stirring the weighed preparation raw materials of the modified tackifier at 25-60 ℃ and reacting for 4-14 h, continuously removing toluene at the vacuum degree of 0.05-0.098 MPa and the temperature of 60-140 ℃ and reacting for 2-6 h to obtain the modified tackifier;
the modified organic silicon comprises the following components in parts by weight: 1 to 4 parts of 1, 3-divinyl-1, 3-tetramethyl-disiloxane, 3 to 5 parts of trimethylolpropane triester, 0.1 to 0.3 part of 2, 2-dimethylolpropionic acid, 20 to 30 parts of tetrahydrofuran, 1 to 3 parts of terbium nitrate, 1 to 3 parts of europium nitrate, 0.3 to 0.5 part of samarium nitrate and 0.3 to 0.5 part of dysprosium nitrate; the preparation of the modified organic silicon comprises the following steps: and uniformly stirring the weighed components of the modified organic silicon under an ultraviolet lamp to obtain the modified organic silicon.
Experimental results show that the optical bonding pouring sealant has the light transmittance reaching 98 percent, the refractive index reaching 1.53, good bonding performance with glass substrates, PC substrates and PMMA substrates, and the tensile strength reaching 3mpa, namely the optical bonding pouring sealant has excellent comprehensive performance.
In terms of light transmittance of the pouring sealant, the modified organic silicon is added into the component B of the optical bonding pouring sealant, so that the light transmittance of the optical bonding pouring sealant can be improved, and the analysis is probably due to the fact that 1, 3-divinyl-1, 3-tetramethyl-disiloxane, trimethylolpropane triester, 2-dimethylolpropionic acid and tetrahydrofuran in the modified organic silicon react to form an organic silicon polymer, and the organic silicon polymer is subjected to coordination reaction with rare earth ions in terbium nitrate, europium nitrate, samarium nitrate and dysprosium nitrate to prepare the modified organic silicon with high light transmittance, so that the light transmittance of the optical bonding pouring sealant is improved.
In the aspect of refractive index of the pouring sealant, phenyl silicone oil with the mass concentration of phenyl not less than 30% is added into the component B of the optical bonding pouring sealant, so that the refractive index of the optical bonding pouring sealant can be improved, and the analysis is probably due to the fact that the phenyl is a high-refractive-index group, and the high refractive index of the optical bonding pouring sealant can be realized by adding the phenyl silicone oil.
In the aspect of the adhesive property of the pouring sealant, the modified tackifier is added into the component B of the optical adhesive pouring sealant, so that the adhesive property of the optical adhesive pouring sealant to a glass substrate, a PC substrate and a PMMA substrate can be improved, and the analysis is probably because the modified tackifier can improve the compatibility of the pouring sealant with the glass substrate, the PC substrate and the PMMA substrate respectively, and when in adhesion, the molecular motion on the interface of the pouring sealant and the substrate enables the pouring sealant to mutually permeate with the substrate, so that the adhesive property of the optical adhesive pouring sealant is improved.
In terms of the tensile strength of the pouring sealant, the high-phenyl resin is added into the component B of the optical bonding pouring sealant, so that the tensile strength of the optical bonding pouring sealant can be improved, and the analysis is probably because the high-phenyl resin forms a net structure in the pouring sealant, so that the tensile strength of the optical bonding pouring sealant can be improved.
Optionally, the catalyst is a titanate catalyst.
By adopting the technical scheme, the titanate catalyst has good catalytic effect, and the adhesion performance of the modified tackifier prepared by the catalytic reaction of the titanate catalyst is better, so that the adhesion strength of the pouring sealant with the glass substrate, the PC substrate and the PMMA substrate can be improved.
Optionally, the hydrogen content of the hydrogen-containing silicone oil is 0.2% -0.7%.
By adopting the technical scheme, when the hydrogen content of the hydrogen-containing silicone oil is 0.2% -0.7%, the hydrogen-containing silicone oil and the double-end vinyl silicone oil undergo hydrosilylation reaction, so that the refractive index effect of the optical bonding pouring sealant is improved, and the refractive index of the pouring sealant is improved.
Optionally, the vinyl content of the double-end vinyl silicone oil is 0.2-0.7%, and the viscosity is 300-10000 mpa.s.
By adopting the technical scheme, the vinyl content of the double-end vinyl silicone oil is 0.2-0.7%, the viscosity is 300-10000 mpa.s, and the double-end vinyl silicone oil and the hydrogen-containing silicone oil undergo hydrosilylation reaction, so that the refractive index of the optical bonding pouring sealant is improved.
Optionally, the component A also comprises 10-15 parts of sodium dodecyl aminopropionate, 2-5 parts of toluenesulfonic acid and 2-5 parts of solubilizer PE-g-MAH.
Experimental results show that the optical bonding pouring sealant has the problem that the adhesive is easy to crack after being cured, and the analysis of the optical bonding pouring sealant is probably due to the fact that the optical bonding pouring sealant is high in hardness after being cured, so that the pouring sealant is cracked due to high stress.
In order to improve the phenomenon that pouring sealant cracks due to larger stress, sodium dodecyl aminopropionate and a solubilizer PE-g-MAH are added into the component A of the optical bonding pouring sealant, so that the hardness of the optical bonding pouring sealant after being cured can be reduced under the condition of meeting the requirement of the hardness of the optical bonding pouring sealant, further the stress of the pouring sealant after being cured is reduced, the phenomenon that the pouring sealant after being cured cracks is reduced, and the analysis is likely because the solubilizer PE-g-MAH enables the sodium dodecyl aminopropionate and the high-phenyl resin to have certain compatibility to react to form a network structure, so that a toughness interface layer of the pouring sealant is formed, the toughness of the pouring sealant after being cured is improved, and the effect of reducing the hardness and the stress of the pouring sealant after being cured is achieved.
Experiments show that the effect of reducing the hardness and stress of the pouring sealant by adding the toluenesulfonic acid into the component A can be further enhanced, and the analysis is probably because the toluenesulfonic acid plays a role in promoting the reaction of the dodecylaminopropionic acid sodium and the high-phenyl resin, so that the formation of a ductile interface layer of the pouring sealant after curing is facilitated, the hardness and stress of the pouring sealant after curing are further reduced, and the phenomenon that the optical bonding pouring sealant is cracked after curing is lightened.
Optionally, the component A also comprises 2-5 parts of isopropanol.
In the experimental process, the simple addition of sodium dodecyl amino propionate, toluene sulfonic acid and a solubilizer PE-g-MAH can cause the reduction of the adhesive property of the optical adhesive pouring sealant, and the analysis may be that the sodium dodecyl amino propionate is shown to be a property of a certain cationic surfactant, so that when the dodecyl amino propionic acid is added into the component A to prepare the optical adhesive pouring sealant, bubbles are easy to remain in the pouring sealant, and the residual bubbles influence the adhesive property of the pouring sealant due to the presence of air, so that the pouring property of the pouring sealant is influenced.
In order to improve the phenomenon that the bonding performance of the optical bonding pouring sealant is reduced due to the sodium dodecyl aminopropionate, the toluenesulfonic acid and the solubilizer PE-g-MAH, experiments show that the bonding performance of the optical bonding pouring sealant can be improved to be higher than that of the existing pouring sealant by adding the isopropanol into the component A, and the reason is probably that the isopropanol can reduce the intermolecular tightness of the sodium dodecyl aminopropionate to achieve the effect of reducing bubbles.
In a second aspect, the present application provides a preparation method of the optical bonding pouring sealant, which adopts the following technical scheme:
the preparation of the optical bonding pouring sealant comprises the following steps:
and (3) preparing a component A: mixing and stirring the weighed raw materials of the component A, stirring the raw materials until the raw materials are uniform, and then carrying out vacuum defoaming to obtain the component A;
and (2) preparing a component B: mixing and stirring the weighed raw materials of the component B, stirring until the raw materials are uniform, and then vacuum defoaming to obtain the component B; preparing pouring sealant: and uniformly stirring the component A and the component B, and carrying out vacuum defoaming to obtain the optical bonding pouring sealant.
By adopting the technical scheme, the optical bonding pouring sealant with excellent comprehensive performance can be prepared, and has the effects of high light transmittance, high refractive index, good bonding performance with glass substrates, PC substrates and PMMA substrates and high tensile strength.
Optionally, the vacuum defoaming time in the preparation of the component A is 10-25 min.
By adopting the technical scheme, when the vacuum defoaming time in the component A is 10-25 min, the defoaming effect of the pouring sealant is optimal, the pouring sealant with less bubble content can be prepared, and the adhesive property of the pouring sealant is improved.
In summary, the application has the following beneficial effects:
1. the optical bonding pouring sealant has the light transmittance reaching 98 percent, the refractive index reaching 1.53, good bonding performance with glass substrates, PC substrates and PMMA substrates and the tensile strength reaching 3mpa, and can be prepared into the optical bonding pouring sealant with excellent comprehensive performance.
2. According to the application, the sodium dodecyl aminopropionate, the toluenesulfonic acid and the solubilizer PE-g-MAH are added into the component A of the optical bonding pouring sealant, so that the hardness of the optical bonding pouring sealant after curing is reduced under the condition of meeting the requirement on the hardness of the optical bonding pouring sealant, the stress of the pouring sealant after curing is further reduced, the low-stress optical bonding pouring sealant is prepared, and the phenomenon that the optical bonding pouring sealant is cracked after curing is reduced;
3. the addition of isopropanol further improves the adhesive property of the optical adhesive pouring sealant added with sodium dodecyl aminopropionate, toluene sulfonic acid and solubilizer PE-g-MAH.
Detailed Description
The present application will be described in further detail below.
Introduction of raw materials
Table 1 raw materials for preparing optical adhesive pouring sealant
Examples
Example 1:
the optical bonding pouring sealant is characterized by comprising the following components in percentage by weight: a component A and a component B of the composition 1,
the component A comprises the following raw materials in parts by weight: 100kg of base material, 10kg of double-end vinyl silicone oil and 0.1kg of platinum catalyst; the component B comprises the following raw materials in parts by weight: 100kg of base material, 12kg of hydrogen-containing silicone oil, 30kg of phenyl silicone oil with the mass concentration of phenyl group being more than or equal to 30%, 5kg of modified tackifier, 1kg of modified organosilicon and 30kg of high-phenyl resin;
the base material comprises the following components in parts by weight: 100kg of high-phenyl resin;
the preparation raw materials of the high-phenyl resin comprise the following components in parts by weight: 2kg of phenyltriethoxysilane, 7kg of diphenyldimethoxysilane and 3kg of tetraphenyldimethyl disiloxane; the preparation of the high-phenyl resin comprises the following steps: the raw materials for preparing the high-phenyl resin are heated in an oil bath at 55 ℃ and condensed and refluxed under stirring to prepare the high-phenyl resin.
The preparation raw materials of the modified tackifier comprise the following components in parts by weight: 20kg of diphenyl silanediol, 8kg of epoxy silane, 10kg of ester silane, 1kg of boric acid ester, 35kg of toluene and 0.2kg of barium hydroxide monohydrate catalyst; the preparation of the modified tackifier comprises the following steps: uniformly stirring the weighed preparation raw materials of the modified tackifier at 50 ℃ and reacting for 10 hours, continuously removing toluene at the vacuum degree of 0.075MPa and the temperature of 110 ℃, and reacting for 4 hours to obtain the modified tackifier;
the modified organic silicon comprises the following components in parts by weight: 4kg of 1, 3-divinyl-1, 3-tetramethyl-disiloxane, 3kg of trimethylolpropane triester, 0.3kg of 2, 2-dimethylolpropionic acid, 20kg of tetrahydrofuran, 3kg of terbium nitrate, 1kg of europium nitrate, 0.5kg of samarium nitrate and 0.3kg of dysprosium nitrate; the preparation of the modified organic silicon comprises the following steps: and uniformly stirring the weighed components of the modified organic silicon under an ultraviolet lamp to obtain the modified organic silicon.
The preparation method of the optical bonding pouring sealant comprises the following steps:
and (3) preparing a component A: mixing and stirring the weighed raw materials of the component A, and carrying out vacuum defoaming for 8min after stirring until the raw materials are uniform to obtain the component A;
and (2) preparing a component B: mixing and stirring the weighed raw materials of the component B, stirring until the raw materials are uniform, and then vacuum defoaming to obtain the component B; preparing pouring sealant: and uniformly stirring the component A and the component B, and carrying out vacuum defoaming to obtain the optical bonding pouring sealant.
Example 2:
the optical bonding pouring sealant is characterized by comprising the following components in percentage by weight: a component A and a component B of the composition 1,
the component A comprises the following raw materials in parts by weight: 100kg of base material, 5kg of double-end vinyl silicone oil and 1kg of platinum catalyst; the component B comprises the following raw materials in parts by weight: 100kg of base material, 7kg of hydrogen-containing silicone oil, 45kg of phenyl silicone oil with the mass concentration of phenyl group being more than or equal to 30%, 1kg of modified tackifier, 5kg of modified organosilicon and 1kg of high-phenyl resin;
the base material comprises the following components in parts by weight: 100kg of high-phenyl resin;
the preparation raw materials of the high-phenyl resin comprise the following components in parts by weight: 3kg of phenyltriethoxysilane, 5kg of diphenyldimethoxysilane and 6kg of tetraphenyldimethyl disiloxane; the preparation of the high-phenyl resin comprises the following steps: the raw materials for preparing the high-phenyl resin are heated in an oil bath at 55 ℃ and condensed and refluxed under stirring to prepare the high-phenyl resin.
The preparation raw materials of the modified tackifier comprise the following components in parts by weight: 15kg of diphenyl silanediol, 10kg of epoxy silane, 8kg of ester silane, 3kg of boric acid ester, 20kg of toluene and 0.5kg of barium hydroxide monohydrate catalyst; the preparation of the modified tackifier comprises the following steps: uniformly stirring the weighed preparation raw materials of the modified tackifier at 50 ℃ and reacting for 10 hours, continuously removing toluene at the vacuum degree of 0.075MPa and the temperature of 110 ℃, and reacting for 4 hours to obtain the modified tackifier;
the modified organic silicon comprises the following components in parts by weight: 1kg of 1, 3-divinyl-1, 3-tetramethyl-disiloxane, 5kg of trimethylolpropane triester, 0.1kg of 2, 2-dimethylolpropionic acid, 30kg of tetrahydrofuran, 1kg of terbium nitrate, 3kg of europium nitrate, 0.3kg of samarium nitrate and 0.5kg of dysprosium nitrate; the preparation of the modified organic silicon comprises the following steps: and uniformly stirring the weighed components of the modified organic silicon under an ultraviolet lamp to obtain the modified organic silicon.
The preparation method of the optical bonding pouring sealant comprises the following steps:
and (3) preparing a component A: mixing and stirring the weighed raw materials of the component A, and carrying out vacuum defoaming for 8min after stirring until the raw materials are uniform to obtain the component A;
and (2) preparing a component B: mixing and stirring the weighed raw materials of the component B, stirring until the raw materials are uniform, and then vacuum defoaming to obtain the component B; preparing pouring sealant: and uniformly stirring the component A and the component B, and carrying out vacuum defoaming to obtain the optical bonding pouring sealant.
Example 3:
the optical bonding pouring sealant is characterized by comprising the following components in percentage by weight: a component A and a component B of the composition 1,
the component A comprises the following raw materials in parts by weight: 100kg of base material, 6kg of double-end vinyl silicone oil and 0.5kg of platinum catalyst; the component B comprises the following raw materials in parts by weight: 100kg of base material, 8kg of hydrogen-containing silicone oil, 37kg of phenyl silicone oil with the mass concentration of phenyl not less than 30%, 4kg of modified tackifier, 3kg of modified organosilicon and 18kg of high-phenyl resin;
the base material comprises the following components in parts by weight: 100kg of high-phenyl resin;
the preparation raw materials of the high-phenyl resin comprise the following components in parts by weight: 2.5kg of phenyltriethoxysilane, 6kg of diphenyldimethoxysilane and 5kg of tetraphenyldimethyl disiloxane; the preparation of the high-phenyl resin comprises the following steps: the raw materials for preparing the high-phenyl resin are heated in an oil bath at 55 ℃ and condensed and refluxed under stirring to prepare the high-phenyl resin.
The preparation raw materials of the modified tackifier comprise the following components in parts by weight: 18kg of diphenyl silanediol, 9kg of epoxy silane, 9kg of ester silane, 2kg of boric acid ester, 25kg of toluene and 0.4kg of barium hydroxide monohydrate catalyst; the preparation of the modified tackifier comprises the following steps: uniformly stirring the weighed preparation raw materials of the modified tackifier at 50 ℃ and reacting for 10 hours, continuously removing toluene at the vacuum degree of 0.075MPa and the temperature of 110 ℃, and reacting for 4 hours to obtain the modified tackifier;
the modified organic silicon comprises the following components in parts by weight: 3kg of 1, 3-divinyl-1, 3-tetramethyl-disiloxane, 4kg of trimethylolpropane triester, 0.2kg of 2, 2-dimethylolpropionic acid, 25kg of tetrahydrofuran, 2kg of terbium nitrate, 2kg of europium nitrate, 0.45kg of samarium nitrate and 0.35kg of dysprosium nitrate; the preparation of the modified organic silicon comprises the following steps: and uniformly stirring the weighed components of the modified organic silicon under an ultraviolet lamp to obtain the modified organic silicon.
The preparation method of the optical bonding pouring sealant comprises the following steps:
and (3) preparing a component A: mixing and stirring the weighed raw materials of the component A, and carrying out vacuum defoaming for 8min after stirring until the raw materials are uniform to obtain the component A;
and (2) preparing a component B: mixing and stirring the weighed raw materials of the component B, stirring until the raw materials are uniform, and then vacuum defoaming to obtain the component B; preparing pouring sealant: and uniformly stirring the component A and the component B, and carrying out vacuum defoaming to obtain the optical bonding pouring sealant.
Example 4
Example 4 differs from example 3 in that the preparation of the modified silicone was carried out using an equivalent amount of titanate catalyst in place of barium hydroxide monohydrate catalyst in the B component.
Example 5
Example 5 differs from example 3 in that the A component further comprises 10kg of sodium dodecylaminopropionate, 5kg of toluene sulfonic acid, and 5kg of solubilizer PE-g-MAH 2.
Example 6
Example 6 differs from example 3 in that the A component further comprises 15kg of sodium dodecylaminopropionate, 2kg of toluene sulfonic acid, and 5kg of solubilizer PE-g-MAH.
Example 7
Example 7 differs from example 6 in that toluene sulfonic acid was not added to the a-component.
Example 8
Example 8 differs from example 6 in that it also includes 2kg of isopropanol.
Example 9
Example 9 differs from example 6 in that 5kg of isopropanol is also included.
Example 10
Example 10 differs from example 3 in that the vacuum degassing time for the preparation of the A-component in the preparation method of the optical bonding pouring sealant is 15min.
Comparative example
Comparative example 1:
comparative example 1 differs from example 3 in that: the component B is not added with a modified tackifier.
Comparative example 2:
comparative example 2 differs from example 3 in that: the component B is not added with modified organic silicon.
Comparative example 3:
comparative example 3 differs from example 3 in that: the component B adopts phenyl silicone oil with the equal mass concentration of phenyl less than or equal to 30 percent to replace phenyl silicone oil with the mass concentration of phenyl more than or equal to 30 percent.
Comparative example 4:
comparative example 4 differs from example 3 in that: 18kg of ethylene MQ silicone resin is used in the component B instead of 18kg of high phenyl resin.
Performance detection
The optical adhesive potting adhesives prepared in examples 1 to 10 and comparative examples 1 to 4 were tested for hardness, shear strength, tensile strength, light transmittance, refractive index and viscosity, and the stress after curing of the prepared optical adhesive potting adhesive was reflected in the test results of hardness, shear strength and tensile strength, with the lower the hardness, shear strength and tensile strength, the lower the stress after curing of the potting adhesive.
The test results are shown in Table 1, and the test method is as follows: hardness: shore A hardness is tested according to GB/T531-2008; shear strength: shear strength was tested according to GB/T7124-2008; tensile strength: tensile strength was tested according to GB/T7124-2008; viscosity: the optical adhesive potting adhesives prepared in examples 1 to 10 and comparative examples 1 to 4 were subjected to viscosity test using a rotational viscometer; transmittance: the optical adhesive potting adhesives prepared in examples 1 to 10 and comparative examples 1 to 4 were subjected to light transmittance test using a spectrophotometer; refractive index: the optical adhesive potting adhesives prepared in examples 1 to 10 and comparative examples 1 to 4 were subjected to direct incidence test using a prism refractometer.
Table 2 results of performance tests of hardness, shear strength, tensile strength and cracking conditions of the optical bonding potting adhesives prepared in examples 1 to 10 and comparative examples 1 to 4
Table 3 the results of performance tests of light transmittance, viscosity and refractive index of the optical adhesive potting adhesives prepared in examples 1 to 10 and comparative examples 1 to 4
Sample of Light transmittance (850 nm) Viscosity (mpa.s) Refractive index
Example 1 98.5% 6670 1.54
Example 2 98.7% 6620 1.55
Example 3 98.9% 6750 1.60
Example 4 96.5% 6730 1.53
Example 5 98.5% 6430 1.57
Example 6 98.7% 6360 1.54
Example 7 98.6% 6500 1.56
Example 8 98.8% 6650 1.55
Example 9 98.7% 6670 1.54
Example 10 98.6% 6840 1.53
Comparative example 1 98.5% 6100 1.55
Comparative example 2 94.5% 6630 1.54
Comparative example 3 98.7% 6650 1.31
Comparative example 4 98.5% 6640 1.57
From the test data shown in tables 2 and 3, it can be seen from comparative example 2 and examples 1 to 10 that the addition of the modified silicone to the B component of the optical adhesive potting adhesive in the present application can improve the light transmittance of the optical adhesive potting adhesive, and the analysis may be that 1, 3-divinyl-1, 3-tetramethyl-disiloxane, trimethylolpropane triester, 2-dimethylolpropionic acid and tetrahydrofuran in the modified silicone react to form a silicone polymer, and the silicone polymer undergoes a coordination reaction with rare earth ions in terbium nitrate, europium nitrate, samarium nitrate and dysprosium nitrate to prepare a modified silicone having high light transmittance, thereby improving the light transmittance of the optical adhesive potting adhesive.
As can be seen from comparative example 3 and examples 1 to 10, the application can improve the refractive index of the optical bonding pouring sealant by adding phenyl silicone oil with the mass concentration of phenyl group being more than or equal to 30% into the component B of the optical bonding pouring sealant, and the analysis is possible because the phenyl group is a group with high refractive index, and the high refractive index of the optical bonding pouring sealant can be realized by adding phenyl silicone oil.
As can be seen from comparative example 1 and examples 1 to 10, the application adds the modified tackifier to the B component of the optical bonding pouring sealant, can improve the viscosity and shear strength of the optical bonding pouring sealant, i.e. can improve the bonding performance of the pouring sealant and the glass substrate, the PC substrate and the PMMA substrate, and the analysis is probably because the modified tackifier can improve the compatibility between the pouring sealant and the glass substrate, the PC substrate and the PMMA substrate respectively, and during bonding, the molecular motion on the interface of the pouring sealant and the substrate enables the pouring sealant and the substrate to mutually permeate, so that the bonding performance of the optical bonding pouring sealant is improved.
As can be seen from comparative example 4 and examples 1 to 10, the addition of the high-phenyl resin to the B component of the optical adhesive pouring sealant according to the present application can improve the tensile strength of the optical adhesive pouring sealant, and the analysis is probably due to the fact that the high-phenyl resin forms a network structure in the pouring sealant, which can improve the tensile strength of the optical adhesive pouring sealant.
As can be seen from examples 5, 6 and examples 1 to 3, the sodium dodecyl aminopropionate and the solubilizer PE-g-MAH are added into the component a of the optical bonding pouring sealant, so that the hardness of the optical bonding pouring sealant after curing is reduced under the condition of meeting the hardness requirement of the optical bonding pouring sealant, and further, the stress of the pouring sealant after curing is reduced, so that the phenomenon that the optical bonding pouring sealant is cracked after curing is reduced, and the reason for the phenomenon is analyzed that the solubilizer PE-g-MAH enables the sodium dodecyl aminopropionate and the high phenyl resin to have certain compatibility so as to react to form a network structure, and then a toughness interface layer of the pouring sealant is formed, so that the toughness of the pouring sealant after curing is improved, and the effect of reducing the hardness and the stress of the pouring sealant after curing is achieved.
From examples 7 and examples 5 and 6, it can be seen that the effect of reducing the hardness and stress of the pouring sealant by adding toluene sulfonic acid to the component a can be further enhanced, and the analysis may be that the toluene sulfonic acid has a promoting effect on the reaction of the sodium dodecyl amino propionate and the high phenyl resin, which is beneficial to promoting the formation of a ductile interface layer after curing the pouring sealant, so as to further reduce the hardness and stress of the pouring sealant after curing and reduce the cracking phenomenon after curing the optical bonding pouring sealant.
As can be seen from examples 8 and 9 and examples 5 and 6, the viscosity of the optical adhesive pouring sealant prepared by the application is raised to a level higher than that of the existing pouring sealant, the hardness, the shear strength and the tensile strength of the pouring sealant are reduced, but the viscosity is still kept to a level higher than that of the existing pouring sealant, and the analysis is probably because sodium dodecyl amino propionate is represented as a property of a certain cationic surfactant, so that when the dodecyl amino propionic acid is added into the component a to prepare the optical adhesive pouring sealant, bubbles are easy to remain in the pouring sealant, the residual bubbles affect the adhesiveness of the pouring sealant due to the presence of air, the pouring performance of the pouring sealant is further affected, and the isopropanol can reduce the intermolecular tightness of the sodium dodecyl amino propionate to achieve the effect of reducing the bubbles.
The above-described embodiments are only illustrative of the present application and are not intended to be limiting, and modifications which would be obvious to those skilled in the art upon reading the present specification without inventive contribution to the application are intended to be included within the scope of the present application.

Claims (8)

1. The optical bonding pouring sealant is characterized by comprising the following components in percentage by weight (1-1.5): a component A and a component B of the composition 1,
the component A comprises the following raw materials in parts by weight: 100 parts of base material, 5-10 parts of double-end vinyl silicone oil and 0.1-1 part of platinum catalyst; the component A also comprises 10 to 15 parts of sodium dodecyl aminopropionate, 2 to 5 parts of toluenesulfonic acid and 2 to 5 parts of solubilizer PE-g-MAH;
the component B comprises the following raw materials in parts by weight: 100 parts of base material, 7-12 parts of hydrogen-containing silicone oil, 30-45 parts of phenyl silicone oil with the mass concentration of phenyl not less than 30%, 1-5 parts of modified tackifier, 1-5 parts of modified organosilicon and 1-30 parts of high-phenyl resin;
the base material comprises the following components in parts by weight: 100 parts of high-phenyl resin;
the preparation raw materials of the high-phenyl resin comprise the following components in parts by weight: 2-3 parts of phenyl triethoxysilane, 5-7 parts of diphenyl dimethoxy silane and 3-6 parts of tetraphenyl dimethyl disiloxane; the preparation of the high-phenyl resin comprises the following steps: heating the raw materials for preparing the high-phenyl resin in an oil bath at 55-60 ℃, and condensing and refluxing under the stirring condition to prepare the high-phenyl resin.
2. The optical bonding pouring sealant according to claim 1, wherein: the preparation raw materials of the modified tackifier comprise the following components in parts by weight: 15-20 parts of diphenyl silicon glycol, 8-10 parts of epoxy silane, 8-10 parts of ester silane, 1-3 parts of boric acid ester, 20-35 parts of toluene and 0.2-0.5 part of catalyst; the preparation of the modified tackifier comprises the following steps: uniformly stirring the weighed preparation raw materials of the modified tackifier at 25-60 ℃ and reacting for 4-14 h, continuously removing toluene at the vacuum degree of 0.05-0.098 MPa and the temperature of 60-140 ℃ and reacting for 2-6 h to obtain the modified tackifier;
the modified organic silicon comprises the following components in parts by weight: 1 to 4 parts of 1, 3-divinyl-1, 3-tetramethyl-disiloxane, 3 to 5 parts of trimethylolpropane triester, 0.1 to 0.3 part of 2, 2-dimethylolpropionic acid, 20 to 30 parts of tetrahydrofuran, 1 to 3 parts of terbium nitrate, 1 to 3 parts of europium nitrate, 0.3 to 0.5 part of samarium nitrate and 0.3 to 0.5 part of dysprosium nitrate; the preparation of the modified organic silicon comprises the following steps: and uniformly stirring the weighed components of the modified organic silicon under an ultraviolet lamp to obtain the modified organic silicon.
3. The optical bonding pouring sealant according to claim 2, wherein: the catalyst is titanate catalyst.
4. The optical bonding pouring sealant according to claim 1, wherein: the hydrogen content of the hydrogen-containing silicone oil is 0.2% -0.7%.
5. The optical bonding pouring sealant according to claim 1, wherein: the vinyl content of the double-end vinyl silicone oil is 0.2-0.7%, and the viscosity is 300-10000 mpa.s.
6. The optical bonding pouring sealant according to claim 1, wherein: the component A also comprises 2-5 parts of isopropanol.
7. The preparation method of the optical bonding pouring sealant according to any one of claims 1 to 5, wherein the preparation method of the optical bonding pouring sealant comprises the following steps:
and (3) preparing a component A: mixing and stirring the weighed raw materials of the component A, stirring the raw materials until the raw materials are uniform, and then carrying out vacuum defoaming to obtain the component A;
and (2) preparing a component B: mixing and stirring the weighed raw materials of the component B, stirring until the raw materials are uniform, and then vacuum defoaming to obtain the component B;
preparing pouring sealant: and uniformly stirring the component A and the component B, and carrying out vacuum defoaming to obtain the optical bonding pouring sealant.
8. The method for preparing the optical bonding pouring sealant according to claim 7, wherein the method comprises the following steps: the vacuum defoamation time in the preparation of the component A is 10-25 min.
CN202210880559.2A 2022-07-25 2022-07-25 Optical bonding pouring sealant and preparation method thereof Active CN115011304B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210880559.2A CN115011304B (en) 2022-07-25 2022-07-25 Optical bonding pouring sealant and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210880559.2A CN115011304B (en) 2022-07-25 2022-07-25 Optical bonding pouring sealant and preparation method thereof

Publications (2)

Publication Number Publication Date
CN115011304A CN115011304A (en) 2022-09-06
CN115011304B true CN115011304B (en) 2023-12-05

Family

ID=83080533

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210880559.2A Active CN115011304B (en) 2022-07-25 2022-07-25 Optical bonding pouring sealant and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115011304B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0593135A (en) * 1991-10-01 1993-04-16 Shin Etsu Chem Co Ltd Water-based silicone emulsion composition
CN105418831A (en) * 2015-12-22 2016-03-23 山东大学 Synthetic method for light-emitting polyacrylic material containing acrylate functional group polyhedronal oligomeric silsesquioxane rare earth complex
CN105524282A (en) * 2016-02-04 2016-04-27 华南理工大学 Organic boron silicon adhesion promoter with high refractive index as well as preparation method and application of organic boron silicon adhesion promoter
CN109337643A (en) * 2018-09-27 2019-02-15 芜湖扬展新材料科技服务有限公司 A kind of high refractive index aminomethyl phenyl LED encapsulation silastic material and preparation method thereof
CN110055027A (en) * 2019-04-30 2019-07-26 汕头市骏码凯撒有限公司 Refractive index LED encapsulation silastic material and preparation method thereof is rolled in one kind

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0593135A (en) * 1991-10-01 1993-04-16 Shin Etsu Chem Co Ltd Water-based silicone emulsion composition
CN105418831A (en) * 2015-12-22 2016-03-23 山东大学 Synthetic method for light-emitting polyacrylic material containing acrylate functional group polyhedronal oligomeric silsesquioxane rare earth complex
CN105524282A (en) * 2016-02-04 2016-04-27 华南理工大学 Organic boron silicon adhesion promoter with high refractive index as well as preparation method and application of organic boron silicon adhesion promoter
CN109337643A (en) * 2018-09-27 2019-02-15 芜湖扬展新材料科技服务有限公司 A kind of high refractive index aminomethyl phenyl LED encapsulation silastic material and preparation method thereof
CN110055027A (en) * 2019-04-30 2019-07-26 汕头市骏码凯撒有限公司 Refractive index LED encapsulation silastic material and preparation method thereof is rolled in one kind

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王正熙等.《高分子材料剖析方法与应用》.上海科学技术出版社,2009,第306页. *
王锡娇.《涂料与颜料标准应用手册.上册》.军事谊文出版社,2005,第184页. *

Also Published As

Publication number Publication date
CN115011304A (en) 2022-09-06

Similar Documents

Publication Publication Date Title
CN107286901B (en) Touch screen full-lamination frame glue and preparation method thereof
CN105001422B (en) A kind of addition-type silicon rubber tackifier and preparation method thereof and addition-type silicon rubber
CN113150737B (en) Two-component organic silicon pouring sealant and preparation method thereof
CN112080246B (en) Organic silicon pouring sealant and preparation method thereof
CN107674640B (en) Ultraviolet-curing organic silicon liquid optical adhesive composition and preparation method thereof
CN107523259B (en) Preparation of alpha-570 coupling agent modified organosilicon sealant
CN111394052B (en) Dealcoholized condensed type double-component room temperature vulcanized silicone rubber and preparation method thereof
CN112143446A (en) Bi-component silicone sealant and preparation method and application thereof
CN104558614B (en) Crosslinking agent with MQ unit, preparation method and application thereof
CN109181623B (en) Silicone sealant for fast curing photovoltaic module and preparation method thereof
CN115124974A (en) Dealcoholized organosilicon sealant and preparation method thereof
CN113956840B (en) Dealcoholized room temperature vulcanized silicone rubber sealant and preparation method thereof
CN114262600A (en) Low-water-vapor-permeability silicone sealant
CN110205084B (en) Quick-curing type organosilicon sealant
CN113684000B (en) Double-component condensed type transparent pouring sealant and preparation method thereof
CN111440323A (en) Synthesis method of alkoxy-terminated organic silicon polyether copolymer and preparation of sealant thereof
CN115011304B (en) Optical bonding pouring sealant and preparation method thereof
CN113462165A (en) Heat-conducting organic silicon pouring sealant for inverter inductor and preparation method thereof
CN109796595B (en) High-refractive-index phenolic hydroxyl-containing organic silicon tackifier and preparation method thereof
CN115772264B (en) Alkoxy-terminated polysiloxane with self-adhesive property, and preparation method and application thereof
CN112778968A (en) Organic silicon pouring sealant and preparation method thereof
CN110483783B (en) Preparation method of phenyl vinyl silicone resin
CN111944467A (en) Nuclear-grade epoxy pouring sealant, preparation method and application
KR20100130206A (en) Thermosetting organic-inorganic hybrid transparent material
CN112778965B (en) Alcohol-type silicon rubber adhesive and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant