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CN111574644A - Application of paste BPO as initiator in optical resin lens - Google Patents

Application of paste BPO as initiator in optical resin lens Download PDF

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Publication number
CN111574644A
CN111574644A CN202010480505.8A CN202010480505A CN111574644A CN 111574644 A CN111574644 A CN 111574644A CN 202010480505 A CN202010480505 A CN 202010480505A CN 111574644 A CN111574644 A CN 111574644A
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bpo
initiator
paste
optical resin
water
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CN111574644B (en
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司君华
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Wuhan Chunling Technology Co ltd
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Wuhan Chunling Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00Polymerisation catalysts
    • C08F4/28Oxygen or compounds releasing free oxygen
    • C08F4/32Organic compounds
    • C08F4/38Mixtures of peroxy-compounds
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/04Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention provides application of paste BPO as an initiator in an optical resin lens, belonging to the technical field of optical materials. BPO is purified to remove impurities, and then the purified BPO is mixed with diethylene glycol bisallyl carbonate with the same mass to prepare a paste which is used as an initiator in the preparation of optical resin lenses. The invention has the advantages of low storage condition, capability of greatly reducing the cost of the initiator and the like.

Description

Application of paste BPO as initiator in optical resin lens
Technical Field
The invention belongs to the technical field of optical materials, and relates to application of paste BPO as an initiator in an optical resin lens.
Background
A common initiator for optical resin lenses is IPP (diisopropyl peroxydicarbonate), CAS: 105-64-6. The storage temperature is usually not higher than-15 ℃. Flammable, strong oxidizers, can explode at normal ambient temperatures. Is sensitive to heat, vibration, impact and friction, and is easy to decompose and burn and explode.
In the process of using by a terminal client, the phenomena of mixture implosion and the like are often caused due to improper temperature control. Causing economic loss and equipment and personnel safety problems.
The self-accelerated decomposition temperature (SADT) of the IPP pure product is about 10 ℃, and if the temperature exceeds the SADT, ignition and explosion caused by rapid decomposition can occur. The initiator for the optical resin lens has low safety coefficient, and is easy to cause risks such as implosion, explosion and the like caused by rapid decomposition of IPP due to improper temperature control, power failure damage of refrigeration equipment and the like.
BOP cannot be used directly as an initiator for curing of optical resin lenses because: 1. pure BPO is unstable, and can undergo self-decomposition and explosion under the conditions of heat, impact and the like; 2. adding 25% of water or other inert desensitizers into industrial products to ensure that BPO peroxide is in a certain stable state; 3. the uniform degree of moisture and inert desensitizer influences the curing effect of the lens. The defects of poor curing, splintering and the like of the lens are easily caused, and a large quality problem is brought to production; 4. due to the influence of inert desensitizers and impurities, the definition of the lens is not high in the curing process, the light transmittance is seriously influenced, and the basic requirement of the lens cannot be met.
The Chinese patent (CN 200510016657.8) inquired in the prior art discloses a preparation method of a transparent high nanophase polymer optical body material. The application of BPO is also involved, but the reference to "taking BPO as an initiator" in the document refers to the production and synthesis of a resin (liquid) by taking BPO as an initiator, wherein the liquid is used for manufacturing semiconductor particles, while the scheme takes BPO as an initiator, the resin is directly manufactured into a lens (cured object), and the BPO is used as an initiator after treatment and is not directly used for the initiator.
Disclosure of Invention
The invention aims to solve the problems of the prior art and provide application of paste BPO as an initiator in optical resin lenses, and the technical problem to be solved by the invention is how to use BPO as a raw material to prepare the initiator for preparing the optical resin lenses.
The purpose of the invention can be realized by the following technical scheme: the application of paste BPO as an initiator in optical resin lenses is characterized in that BPO is purified to remove impurities, and then the purified BPO is mixed with diethylene glycol bisallyl carbonate with the same mass to prepare a paste which is used as the initiator in the preparation of the optical resin lenses.
Filling and sealing the prepared paste, and storing at-10 deg.C.
Specifically, the purification process of BPO comprises the following steps:
1) washing with absolute ethyl alcohol (AR grade) to remove part of impurities;
2) repeatedly washing the product obtained in the step 1) by pure water to remove ethanol and partial impurities;
3) carrying out suction filtration on the product obtained in the step 2) at a low temperature (below 20 ℃), and removing most of water to reduce the water mass ratio from about 25% to 5-8%;
4) and blowing the product obtained in the step 3) by low-temperature (below 20 ℃) nitrogen to remove residual water in the product, so that the mass ratio of the water is less than 0.5%.
The preparation process of the BPO paste comprises the following steps:
1) weighing a certain amount of diethylene glycol bis (allyl carbonate), stirring at a low temperature (not higher than 10 ℃), slowly adding purified BPO with the same mass as the diethylene glycol bis (allyl carbonate), and continuously stirring (the rotating speed is 1000-;
2) and filling and sealing the prepared paste, and storing in an environment with the temperature of-10 ℃.
The manufacturing process of the resin optical lens comprises the following steps:
1) weighing the required monomers according to the proportion, placing the monomers in a batching tank, and starting stirring. (ensure the temperature of the material is not higher than 35 ℃).
2) Placing a certain amount of UV powder required by monomer dissolution in a beaker, heating, dissolving and stirring uniformly, pouring into the mixing tank in the step 1), rinsing the beaker by using the monomer, pouring rinsing liquid into the mixing tank together, and stirring and mixing uniformly;
3) placing a certain amount of color-supplementing agent required by monomer dissolution in a beaker, uniformly stirring, pouring into the mixing tank in the step 1), rinsing the beaker by using the monomer, pouring rinsing liquid into the mixing tank together, and uniformly stirring and mixing;
4) accurately and quickly weighing the needed BPO initiator, pouring the BPO initiator into the mixing tank in the step 1), and stirring and mixing for 1-2 hours to fully and uniformly mix all the materials;
5) and under the condition of stirring, vacuumizing for 0.5-1 h, and controlling the vacuum degree to be 500-1000 Pa.
6) And discharging the vacuum;
7) filling, transferring the prepared materials into a clean small pouring tank, and performing pressure filtration and filling;
8) filtering out unhomogenized particles, and pouring into a mold;
9) placing the mould in a curing box, curing for 20-24 hours and forming;
10) obtaining a lens substrate through subsequent demoulding, cleaning, inspection and the like;
11) and the finished lens can be obtained by carrying out subsequent trimming, dyeing, film coating and the like on the substrate.
Compared with the prior art, the invention has the following advantages:
1. the initiator has a relatively high safety factor, and the self-accelerated decomposition temperature (SADT) of BPO (pure product) is 60 ℃. The initiator can be stored at normal temperature without explosion hazard, so that the initiator prepared by purification can be stored at normal temperature.
2. The mixed material added with BPO as an initiator is stored for 48 hours at normal temperature (20 ℃), the change of the effective oxygen content is extremely small, and the use is not influenced.
3. The use amount is as follows: the usage amount of IPP is generally 2.8-3.3%, the same curing performance of the lens is achieved, the usage amount of BPO is generally 1.25-1.75%, which is only half of the former, and the cost advantage is better.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
BPO is purified to remove impurities, and then the purified BPO is mixed with diethylene glycol bisallyl carbonate with the same mass to prepare a paste which is used as an initiator in the preparation of optical resin lenses.
The initiator for optical resin lens preparation prepared by the method has the following characteristics:
it is an initiator suitable for curing diethylene glycol bis-allyl carbonate monomer, and is a milky white paste at normal temperature.
It is a medium-temperature initiator, can be stored at normal temperature, and improves the safety coefficient.
The active oxygen content of the catalyst is between 3.28 and 3.32 percent, and 50 percent of the catalyst is diethylene glycol bis-allyl carbonate monomer.
The physical property data of the cured product initiated by the initiator under the condition of using the amount of 2.25-3.0 percent
Physical Properties of cured product
Figure RE-GDA0002566026640000041
Figure RE-GDA0002566026640000051
Storage conditions
Hermetically stored in an environment of not more than 5 ℃ (the theoretical storage temperature is much higher than this temperature, and here only enough margin is kept to improve safety); far from heat source, radiation, direct sunlight; avoiding contact with acids, bases, reducing agents, metal ions, and the like.
Curing curve
According to the practical production condition, the curing curve is finely adjusted to match with a corresponding furnace, a corresponding mold and the like. The best curing result is achieved.
Figure RE-GDA0002566026640000052
Secondly, fixation: the secondary curing is carried out for 2h at 100-105 ℃.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.

Claims (3)

1. The application of paste BPO as an initiator in optical resin lenses is characterized in that BPO is purified to remove impurities, and then the purified BPO is mixed with diethylene glycol bisallyl carbonate with the same mass to prepare a paste which is used as the initiator in the preparation of the optical resin lenses.
2. The use of the paste-like BPO as an initiator in optical resin lenses according to claim 1, wherein the purification and impurity removal process of BPO comprises the steps of:
1) washing with absolute ethyl alcohol (AR grade) to remove part of impurities;
2) repeatedly washing the product obtained in the step 1) by pure water to remove ethanol and partial impurities;
3) carrying out suction filtration on the product obtained in the step 2) at a low temperature (below 20 ℃), and removing most of water to reduce the water mass ratio from about 25% to 5-8%;
4) and blowing the product obtained in the step 3) by low-temperature (below 20 ℃) nitrogen to remove residual water in the product, so that the mass ratio of the water is less than 0.5%.
3. The use of the paste-like BPO as an initiator in optical resin lenses according to claim 2, wherein the process for preparing the BPO initiator comprises the steps of: weighing a certain amount of diethylene glycol bis allyl carbonate, stirring at a low temperature (not higher than 10 ℃) while slowly adding purified BPO with the same mass as the diethylene glycol bis allyl carbonate, and continuously stirring until the mixture is uniformly mixed to form paste.
CN202010480505.8A 2020-05-30 2020-05-30 Application of paste BPO as initiator in optical resin lens Active CN111574644B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4590248A (en) * 1982-03-29 1986-05-20 Nippon Oil And Fats Co., Ltd. Method for producing a plastic lens using tertiary alkyl peroxy allyl carbonate
CN1063447A (en) * 1991-01-17 1992-08-12 眼科研究集团国际有限公司 The method and apparatus of preparation plastic lens
CN1152273A (en) * 1995-04-28 1997-06-18 株式会社朝日光学 Method of manufacturing plastic lenses
CN105524586A (en) * 2015-12-01 2016-04-27 东兴华鸿光学科技有限公司 Making method for high-efficiency UV mixed adhesive used for polarized lenses and 3D lenses
CN107033050A (en) * 2017-05-04 2017-08-11 江苏强盛功能化学股份有限公司 A kind of contaminated BPO processing method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4590248A (en) * 1982-03-29 1986-05-20 Nippon Oil And Fats Co., Ltd. Method for producing a plastic lens using tertiary alkyl peroxy allyl carbonate
CN1063447A (en) * 1991-01-17 1992-08-12 眼科研究集团国际有限公司 The method and apparatus of preparation plastic lens
CN1152273A (en) * 1995-04-28 1997-06-18 株式会社朝日光学 Method of manufacturing plastic lenses
CN105524586A (en) * 2015-12-01 2016-04-27 东兴华鸿光学科技有限公司 Making method for high-efficiency UV mixed adhesive used for polarized lenses and 3D lenses
CN107033050A (en) * 2017-05-04 2017-08-11 江苏强盛功能化学股份有限公司 A kind of contaminated BPO processing method

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