CN113322009A - Process method for preparing optical transparent UV adhesive - Google Patents
Process method for preparing optical transparent UV adhesive Download PDFInfo
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- CN113322009A CN113322009A CN202110828887.3A CN202110828887A CN113322009A CN 113322009 A CN113322009 A CN 113322009A CN 202110828887 A CN202110828887 A CN 202110828887A CN 113322009 A CN113322009 A CN 113322009A
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- C—CHEMISTRY; METALLURGY
- 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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- C—CHEMISTRY; METALLURGY
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a process method for preparing an optical transparent UV adhesive, which comprises the following steps of weighing 100 parts of alicyclic epoxy resin and 10-25 parts of diisocyanate, putting the alicyclic epoxy resin and 10-25 parts of diisocyanate into a mixing tank, uniformly stirring to obtain a prepolymer, weighing organic antimony and calcium stearate with certain mass, uniformly mixing by a stirrer, putting the organic antimony and calcium stearate into a screw extruder for extrusion granulation, carrying out ventilation cooling for 1-2 hours under a dark condition to obtain stable auxiliary agent particles, weighing 5 parts of coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stable auxiliary agent particles and 10 parts of active diluent, putting the mixture into the prepolymer, uniformly stirring in the mixing tank, heating to 80 ℃, and obtaining a mixture in a molten state. According to the invention, two silane coupling agents are mixed to serve as the coupling agent, so that the adhesion of the finished UV adhesive can be improved, and organic antimony and calcium stearate serve as stabilizing agents, so that the stability and heat resistance can be improved, the adhesion is prevented from being reduced due to heating, and the safety and the practicability are improved.
Description
Technical Field
The invention relates to the technical field of UV adhesives, in particular to a process method for preparing an optical transparent UV adhesive.
Background
The adhesive is a substance with good adhesive property. The UV adhesive is used for connecting objects by surface adhesion through adhesion and cohesion, and is characterized in that a photoinitiator (or photosensitizer) is added into a specially-formulated resin, and after high-intensity ultraviolet light in an Ultraviolet (UV) light curing device is absorbed, active free radicals or ionic groups are generated, so that polymerization, crosslinking and grafting reactions are initiated, and the resin (UV coating, ink, adhesive and the like) is converted from liquid to solid within seconds (unequal), wherein the change process is called 'UV curing'.
In the optical field, when fixing an optical element using a UV adhesive, the UV adhesive is required to be transparent, the UV adhesive cannot have any bubbles and yellowing, and a good adhesion is required.
Based on the existing UV adhesive production technology, the produced UV adhesive has generally yellow surface and poor thermal stability, and after the optical element operates for a long time, the UV adhesive is easily heated, so that the adhesive force is reduced.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a process method for preparing an optical transparent UV adhesive.
The invention provides a process method for preparing an optical transparent UV adhesive, which comprises the following steps:
s1: weighing 100 parts of alicyclic epoxy resin and 10-25 parts of diisocyanate, and putting the alicyclic epoxy resin and the diisocyanate into a mixing tank to be uniformly stirred to obtain a prepolymer;
s2: weighing organic antimony and calcium stearate with certain mass, uniformly mixing by a stirrer, putting into a screw extruder for extrusion granulation, and ventilating and cooling for 1-2h under a light-tight condition to obtain stable auxiliary agent particles;
s3: weighing 5 parts of coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of reactive diluent, putting the coupling agent, the thixotropic agent, the stabilizing additive particles and the reactive diluent into a prepolymer, uniformly stirring the mixture in a mixing tank, and heating the mixture to 80 ℃ to obtain a molten mixture;
s4: and (3) putting the mixture in the molten state into a light-resistant container, putting the container into a centrifuge, performing centrifugal defoaming for 1-2h, and standing for 24h to obtain the adhesive.
Preferably, the mass ratio of the organic antimony to the calcium stearate in the S2 is 3:2, and the heating temperature of the screw extruder is 120 ℃.
Preferably, the coupling agents in the S3 are gamma- (2, 3-glycidoxy) propyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane, the mass percentage is 1:1, the photoinitiators are hydroxycyclohexyl phenyl ketone and alpha-dimethoxy-alpha-phenyl acetophenone, the thixotropic agent is polyamide wax, and the reactive diluent is trimethylolpropane triglycidyl ether.
Preferably, the photoinitiator in S3 is weighed in a dark environment at normal temperature, and is temporarily stored in a dark container.
Preferably, the rotation speed of the centrifuge in the S4 is 5000-10000r/min, and the interior of the centrifuge is protected from light.
Preferably, the optical power of the UV curing box in S5 is 20mW/cm2。
The invention has the beneficial effects that:
according to the invention, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane are mixed as a coupling agent, so that the adhesion of a finished product of the UV adhesive can be improved, organic antimony and calcium stearate are used as stabilizers, the stability and heat resistance of the finished product of the UV adhesive can be improved, the adhesion reduction caused by heating of the finished product of the UV adhesive is prevented, and the safety and the practicability are improved.
Detailed Description
Embodiment 1, a process for preparing an optically transparent UV adhesive, comprising the steps of:
s1: weighing 100 parts of alicyclic epoxy resin and 10 parts of diisocyanate, and putting the alicyclic epoxy resin and the diisocyanate into a mixing tank to be uniformly stirred to obtain a prepolymer;
s2: weighing organic antimony and calcium stearate with certain mass, uniformly mixing the organic antimony and the calcium stearate by a stirrer, putting the mixture into a screw extruder for extrusion granulation, and carrying out ventilation cooling for 1-2 hours in a dark condition to obtain stable auxiliary agent particles, wherein the mass ratio of the organic antimony to the calcium stearate in S2 is 3:2, and the heating temperature of the screw extruder is 120 ℃;
s3: weighing 5 parts of coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of active diluent, putting the coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of active diluent into a prepolymer, uniformly stirring the mixture in a mixing tank, heating the mixture to 80 ℃ to obtain a molten mixture, wherein the coupling agent in S3 is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane in a mass percentage of 1:1, the photoinitiator is hydroxy cyclohexyl phenyl ketone and alpha-dimethoxy-alpha-phenyl acetophenone, the thixotropic agent is polyamide wax, the active diluent is trimethylolpropane triglycidyl ether, and the photoinitiator in S3 is weighed in a light-proof environment at normal temperature and is temporarily stored in a container;
s4: placing the mixture in the molten state into a light-proof container, placing the container into a centrifuge, performing centrifugal defoaming for 1-2h, and standing for 24h to obtain a UV adhesive liquid, wherein the rotation speed of the centrifuge in S4 is 5000-10000r/min, and the interior of the centrifuge is in a light-proof environment;
s5: putting the UV adhesive glue solution into a UV curing box, and irradiating for 2-3h to obtain a finished UV adhesive product, wherein the light power of the UV curing box in the S5 is 20mW/cm2。
Embodiment 2, a process for preparing an optically transparent UV adhesive, comprising the steps of:
s1: weighing 100 parts of alicyclic epoxy resin and 15 parts of diisocyanate, and putting the alicyclic epoxy resin and the diisocyanate into a mixing tank to be uniformly stirred to obtain a prepolymer;
s2: weighing organic antimony and calcium stearate with certain mass, uniformly mixing the organic antimony and the calcium stearate by a stirrer, putting the mixture into a screw extruder for extrusion granulation, and carrying out ventilation cooling for 1-2 hours in a dark condition to obtain stable auxiliary agent particles, wherein the mass ratio of the organic antimony to the calcium stearate in S2 is 3:2, and the heating temperature of the screw extruder is 120 ℃;
s3: weighing 5 parts of coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of active diluent, putting the coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of active diluent into a prepolymer, uniformly stirring the mixture in a mixing tank, heating the mixture to 80 ℃ to obtain a molten mixture, wherein the coupling agent in S3 is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane in a mass percentage of 1:1, the photoinitiator is hydroxy cyclohexyl phenyl ketone and alpha-dimethoxy-alpha-phenyl acetophenone, the thixotropic agent is polyamide wax, the active diluent is trimethylolpropane triglycidyl ether, and the photoinitiator in S3 is weighed in a light-proof environment at normal temperature and is temporarily stored in a container;
s4: placing the mixture in the molten state into a light-proof container, placing the container into a centrifuge, performing centrifugal defoaming for 1-2h, and standing for 24h to obtain a UV adhesive liquid, wherein the rotation speed of the centrifuge in S4 is 5000-10000r/min, and the interior of the centrifuge is in a light-proof environment;
s5: putting the UV adhesive glue solution into a UV curing box, and irradiating for 2-3h to obtain a finished UV adhesive product, wherein the light power of the UV curing box in the S5 is 20mW/cm2。
Embodiment 3, a process for preparing an optically transparent UV adhesive, comprising the steps of:
s1: weighing 100 parts of alicyclic epoxy resin and 20 parts of diisocyanate, and putting the alicyclic epoxy resin and the diisocyanate into a mixing tank to be uniformly stirred to obtain a prepolymer;
s2: weighing organic antimony and calcium stearate with certain mass, uniformly mixing the organic antimony and the calcium stearate by a stirrer, putting the mixture into a screw extruder for extrusion granulation, and carrying out ventilation cooling for 1-2 hours in a dark condition to obtain stable auxiliary agent particles, wherein the mass ratio of the organic antimony to the calcium stearate in S2 is 3:2, and the heating temperature of the screw extruder is 120 ℃;
s3: weighing 5 parts of coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of active diluent, putting the coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of active diluent into a prepolymer, uniformly stirring the mixture in a mixing tank, heating the mixture to 80 ℃ to obtain a molten mixture, wherein the coupling agent in S3 is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane in a mass percentage of 1:1, the photoinitiator is hydroxy cyclohexyl phenyl ketone and alpha-dimethoxy-alpha-phenyl acetophenone, the thixotropic agent is polyamide wax, the active diluent is trimethylolpropane triglycidyl ether, and the photoinitiator in S3 is weighed in a light-proof environment at normal temperature and is temporarily stored in a container;
s4: placing the mixture in the molten state into a light-proof container, placing the container into a centrifuge, performing centrifugal defoaming for 1-2h, and standing for 24h to obtain a UV adhesive liquid, wherein the rotation speed of the centrifuge in S4 is 5000-10000r/min, and the interior of the centrifuge is in a light-proof environment;
s5: putting the UV adhesive glue solution into a UV curing box, and irradiating for 2-3h to obtain a finished UV adhesive product, wherein the light power of the UV curing box in the S5 is 20mW/cm2。
Embodiment 4, a process for preparing an optically transparent UV adhesive, comprising the steps of:
s1: weighing 100 parts of alicyclic epoxy resin and 25 parts of diisocyanate, and putting the alicyclic epoxy resin and the diisocyanate into a mixing tank to be uniformly stirred to obtain a prepolymer;
s2: weighing organic antimony and calcium stearate with certain mass, uniformly mixing the organic antimony and the calcium stearate by a stirrer, putting the mixture into a screw extruder for extrusion granulation, and carrying out ventilation cooling for 1-2 hours in a dark condition to obtain stable auxiliary agent particles, wherein the mass ratio of the organic antimony to the calcium stearate in S2 is 3:2, and the heating temperature of the screw extruder is 120 ℃;
s3: weighing 5 parts of coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of active diluent, putting the coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of active diluent into a prepolymer, uniformly stirring the mixture in a mixing tank, heating the mixture to 80 ℃ to obtain a molten mixture, wherein the coupling agent in S3 is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane in a mass percentage of 1:1, the photoinitiator is hydroxy cyclohexyl phenyl ketone and alpha-dimethoxy-alpha-phenyl acetophenone, the thixotropic agent is polyamide wax, the active diluent is trimethylolpropane triglycidyl ether, and the photoinitiator in S3 is weighed in a light-proof environment at normal temperature and is temporarily stored in a container;
s4: placing the mixture in the molten state into a light-proof container, placing the container into a centrifuge, performing centrifugal defoaming for 1-2h, and standing for 24h to obtain a UV adhesive liquid, wherein the rotation speed of the centrifuge in S4 is 5000-10000r/min, and the interior of the centrifuge is in a light-proof environment;
s5: putting the UV adhesive liquid into a UV curing box, irradiating for 2-3h to obtain a finished UV adhesive product, and performing UV curing in S5The optical power of the box is 20mW/cm2。
And (3) performance testing:
uniformly coating a UV adhesive liquid solution on two optical elements to be assembled by using a cotton swab, curing the optical elements by using a UV curing box, recording curing time, uniformly coating the UV adhesive liquid solution on a glass slide by using the cotton swab, and observing the surface condition of the UV adhesive by using a microscope.
The results are shown in table 1:
TABLE 1
As can be seen from the above table, example 3 is the most preferred embodiment of the present invention.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention by equivalent replacement or change according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (6)
1. A process method for preparing an optical transparent UV adhesive is characterized by comprising the following steps:
s1: weighing 100 parts of alicyclic epoxy resin and 10-25 parts of diisocyanate, and putting the alicyclic epoxy resin and the diisocyanate into a mixing tank to be uniformly stirred to obtain a prepolymer;
s2: weighing organic antimony and calcium stearate with certain mass, uniformly mixing by a stirrer, putting into a screw extruder for extrusion granulation, and ventilating and cooling for 1-2h under a light-tight condition to obtain stable auxiliary agent particles;
s3: weighing 5 parts of coupling agent, 10 parts of photoinitiator, 5 parts of thixotropic agent, 5 parts of stabilizing additive particles and 10 parts of reactive diluent, putting the coupling agent, the thixotropic agent, the stabilizing additive particles and the reactive diluent into a prepolymer, uniformly stirring the mixture in a mixing tank, and heating the mixture to 80 ℃ to obtain a molten mixture;
s4: putting the mixture in the molten state into a light-resistant container, putting the container into a centrifuge, performing centrifugal deaeration for 1-2h, and standing for 24h to obtain a UV adhesive liquid;
s5: and (4) putting the UV adhesive liquid into a UV curing box, and irradiating for 2-3h to obtain a finished UV adhesive product.
2. The process for preparing optically transparent UV adhesive according to claim 1, wherein the mass ratio of organic antimony to calcium stearate in S2 is 3:2, and the heating temperature of the screw extruder is 120 ℃.
3. The process for preparing an optically transparent UV adhesive according to claim 1, wherein the coupling agents in S3 are γ - (2, 3-glycidoxy) propyl trimethoxy silane and γ -methacryloxypropyl trimethoxy silane, the mass percentage is 1:1, the photoinitiators are hydroxycyclohexyl phenyl ketone and α -dimethoxy- α -phenyl acetophenone, the thixotropic agent is polyamide wax, and the reactive diluent is trimethylolpropane triglycidyl ether.
4. The process for preparing optically transparent UV adhesive according to claim 1, wherein the photoinitiator in S3 is weighed in a dark environment at room temperature, and is stored in a dark container for a short time.
5. The process of claim 1, wherein the rotation speed of the centrifuge in S4 is 5000-10000r/min, and the interior of the centrifuge is protected from light.
6. The process for preparing optically transparent UV adhesive according to claim 1, wherein the optical power of the UV curing box in S5 is 20mW/cm2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110828887.3A CN113322009A (en) | 2021-07-22 | 2021-07-22 | Process method for preparing optical transparent UV adhesive |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110828887.3A CN113322009A (en) | 2021-07-22 | 2021-07-22 | Process method for preparing optical transparent UV adhesive |
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| CN113322009A true CN113322009A (en) | 2021-08-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114379180A (en) * | 2021-12-29 | 2022-04-22 | 和盛包装科技(海宁)股份有限公司 | Composite packaging film with bacteria barrier protection function and preparation method thereof |
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Application publication date: 20210831 |