A method of manufacturing optical products

 

(57) Abstract:

Usage: in industry in the manufacture of optical elements, lenses, diffraction gratings, the replication of hologram, as well as in other industries in the manufacture of two - and multi-layer glass. The inventive method of manufacturing optical products is placed between at least two surfaces, one of which is optically transparent, methacrylic oligomer with subsequent curing. As methacrylic oligomer use the product of condensation of polynuclear alcohols with diisocyanate, anhydrides of dibasic acids and glycidylmethacrylate. Mixed with the oligomer used acrylic and vinyl monomers, photoinitiator, adhesion promoters. 5 C. p. F.-ly, 7 PL.

The invention relates to methods of manufacturing optical products and can be used in industry in the manufacture of optical elements, lenses, diffraction gratings, duplicating holograms, optical disks, as well as in other industries in the manufacture of two - and multi-layer glass.

There is a method of replicating optical discs by placing between photoinitiator, followed by curing by UV radiation.

However, when using this method in the manufacturing process reversible optical disc, which uses a high temperature under application of magneto-optical recording media, polymer, relevanssi composite materials increased requirements for heat resistance. The composition used in this way does not satisfy both these requirements, and the requirements of the largest determining the quality of the reproduction information of the index of birefringence of the microrelief (not more than 40 nm/mm).

Closest to the invention is a method of manufacturing optical products by placing between at least two surfaces, at least one of which is optically transparent, photopolymerizable composition, and then curing by UV radiation. In the specified method is used photopolymerizable composition containing oligoelement (OA) the product of the interaction of hydroxyethylmethacrylate with diisocyanate, acrylic monomers and photoinitiator. This method provides satisfactory (0.5 to 10.0 nm/mm), the values of the birefringence.

However, this method not allowed donosti polymer relevanssi layers.

The purpose of this invention is to improve the heat resistance utverzhdenii composition, while maintaining the required optical characteristics.

The aim is achieved in that in the method of manufacturing optical products by placing between at least two surfaces, at least one of which is optically transparent, unsaturated hydroxyacrylates ether with subsequent curing, as unsaturated hydroxyacrylates ether is used, the compound of General formula I:

[CH2= C(CH3)-C(O)O-CH2CH(OH)CH2-OC(OR1-C(O)OR2OC(O)-NH R3(I) where R1= ; -CH=CH-

R2=-CH-CH(CH3)- CHC(O)CH2)n-C(O)OCH2CH2O

R3= CH n 5-86.

Preferably, hydroxyarylalkyl oligoether formula I is used in conjunction with a vinyl monomer, chosen from a number of N-vinyl pyrrolidone, styrene, vinyl acetate or mixtures thereof, and the monomer or mixture of monomers used in the amount of 5-25 wt.h. on 100 wt.h. the compounds of formula I.

It is preferable that the composition was added acrylic monomer selected from a range of methyl methacrylate, butelgui in the number of 40-400 wt.h. on 100 wt.h. the compounds of formula I.

Active diluents necessary to regulate the rheological properties of the composition.

In all the above cases, the curing is carried out by ionizing radiation, for example radiation from a source WITH aabout60. This can be obtained two - or multi-layer products (duplex, triplex and so on).

The curing can be conducted and UV radiation. To do this, the composition further added photoinitiator selected from the range: 2,2-dimethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenyl - propane-1-he, ethers, benzoin, benzophenone, michler ketone, dialkoxybenzene or their mixtures, which are used in an amount of 0.1 to 15.0 wt.h. on 100 wt.h. the compounds I. thus the composition may have the following composition, wt.h. The compound of formula I 100

Acrylic monomer or a mixture of 0.1 to 15.0

Photoinitiator or a mixture of 0.1 to 15.0

In addition, photoinitiator or their mixture can be introduced into the composition containing compound I, an acrylic monomer or mixture of vinyl monomers or their mixture, and the composition may have the following composition, wt.h. The compound of formula I 100

Acrylic monomer or a mixture of 40-400

The vinyl monomer ropolitan contain an adhesion promoter, selected from a number Methacrylonitrile - LAN, methacryloyloxyethyl, vinyl, mercaptoethane or their mixture in the following ratio, wt.h: Compound of formula I 100 Acrylic monomer or a mixture of 40-400 Vinyl monomer or a mixture of 5-25 Photoinitiator or a mixture of 0.1-15.0 adhesion Promoter or a mixture of 1.0 to 15.0

In the case of UV curing may receive duplex glass, when, after the stage of curing one of the surfaces is removed from the cured layer. It is also possible the manufacture of laminated products by consecutive application of the composition and its cured between two surfaces, at least one of which is optically transparent.

P R I m e R s 1-9. Synthesis of acrylic oligomer of formula I.

In a reaction flask is charged with 2000 g (2 mol) of polytetramethylene with a molecular weight of 1000, previously dried under vacuum by heating to a moisture content of not higher than 0.03 wt. Include the mixer, when mixing the injected catalyst dibutyltindilaurate in the amount of 0.02% (by weight of the reactants). Then 2-3 reception load 174 g (1 mol) toluylenediisocyanate brand T-65/35, observing that the temperature of the reaction mixture /SUP>C for 1 h, take a sample and analyze the content of isocyanate groups, which must match the calculated value.

The second stage of the synthesis is the acylation received orlandiana 196 h(2 mol) of maleic anhydride. The reaction is carried out at a temperature of 100-105aboutIn the presence of 0.1% (by weight of reactants) of potassium acetate catalyst, which was previously introduced into the reaction mixture in the form of a solution in ethanol. The reaction of the lead within 3 hours, take a sample and analyze for acid number, which must match the calculated value.

The third stage of the synthesis consists in processing oligomerisation acid 284 hours (2 mol) of glycidylmethacrylate, the Reaction is carried out at 95-100aboutC for 7-8 hours, then take a sample and analyze for acid number, which must not exceed 10 m Koh/g

Physico-chemical characteristics of the acrylic oligomer and other oligomers of General formula I are given in table.1.

P R I m e R s 10-18. By known techniques produce an optical disk by applying between the glass disc is the original and the glass of the compounds of formula I followed by radiation from a source WITH aabout60tx2">

As shown, the proposed method can improve the heat resistance of the composition of the prototype when saving measure birefringence.

P R I m e R s 20-27. A method of manufacturing optical products is the same as in examples 10-19, only the compound of formula I (example 2, table.1) is placed between the glass disc is the original and the glass together with the acrylic monomer or a mixture of acrylic monomers.

Formulations of the compositions and their properties are given in table.3.

As follows from the table. 3, the introduction of acrylic monomers can increase the heat resistance of the formed polymers. In addition, significantly improves the rheological properties of the compositions.

P R I m e R s 28-34. A method of manufacturing optical products is the same as in examples 20-27, only the composition of 100 wt.h. the compounds of formula I (example 2, table.1) 100 wt.h. acrylic monomer (MMA) is placed between the glass disc is the original and the glass together with a vinyl monomer or mixture of vinyl monomers.

Formulations of the compositions and their properties are given in table.4.

As follows from the table.4, the introduction of vinyl monomers will increase thermal stability of polymers.

P R I m e R s 35-42. The way the radiation of LUF-80-04 with an intensity of 100 W/m2in the region of wavelengths of 320-380 nm. The exposure time of 5-20 minutes Using a composition of 100 wt.h. compounds of formula I (example 2, table.1) 100 wt.h. MMA together with photoinitiator or a mixture of photoinitiators. Formulations of the compositions and their properties are given in table.5.

As follows from the data table.5, the introduction of photoinitiator allows the use of UV-radiation sources and, accordingly, to reduce the time of curing of the compositions.

P R I m e R s 43-50. Match the examples 35-42 with additional introduction into the composition of 15 wt.h. styrene. Properties are given in table.6.

As can be seen from the data table.6, the combination of photoinitiators with compounds of the formula I, acrylic and vinyl monomers allows you to achieve complex high reactionary ability, optical and thermal properties of the resulting compositions.

P R I m e R s 51-57. "Triplex" glass is made in the following way. Between 2 sheet polished glass thickness of 2-3 mm pour a layer thickness of 1.0 mm composition of example 45 with the addition of adhesion promoters. In the UV curing get glass that meets the requirements of GOST. The relevant data are given in table.7.

The introduction of the adhesion promoters p is R and m e R 58. Fabricate laminated glass by pouring the composition of example 53 (a compound of formula I of example 2 of the table.1 100 wt.h; methyl methacrylate 100 wt. including styrene and 15 wt.h. methacrylate-dimethyldiethoxysilane 3 wt. h; 2,2-dimethoxy-1-phenylacetophenone 0.5.h.) 0.5 mm gaps between 4 polished sheet glass with a thickness of 2.0 mm and a curing package glass-radiation from a source WITH aabout60a dose of 30 oil and gas fields. Get a sample of a laminated glass with high physical-mechanical characteristics, heat and frost.

P R I m e R 59. A sample of the composition of example 58 is applied on the glass plate 4 mm thick layer of 1.0 mm and covered by a Mylar film thickness of 70 μm or molding glass with a thickness of 2.0 mm Molding glass pre-treated with a clear. Exposure to UV light is produced through molding glass or Mylar film. After their removal get a two-ply product, which is used in the technology of "duplex" glasses.

1. A METHOD of MANUFACTURING OPTICAL PRODUCTS by placing between at least two surfaces, one of which is optically transparent, methacrylic oligomer with its subsequent curing, the de

< / BR>
< / BR>
R2= -CH2CH(CH3)-; -(CH2)4; [-C(O)-(CH2)4- C(O)-O-(CH2CH2O)2];

R3= -(CH2)6;

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n = 5 - 86.

2. The method according to p. 1, characterized in that the compound of the formula I are used together with the acrylic monomer selected from a range of methyl methacrylate, butylmethacrylate, hydroxyethylmethacrylate, isobornylacrylat, glycidylmethacrylate, or their mixture in the following ratio, wt.h.:

The compound of formula I - 100

Acrylic monomer or mixture of monomers - 40 - 400

3. The method according to p. 2, characterized in that the source composition is injected vinyl monomer, chosen from a number of vinyl pyrrolidone, styrene, vinyl acetate or a mixture thereof, in the following ratio, wt.h.:

The compound of formula I - 100

Acrylic monomer or mixture of monomers - 40 - 400

The vinyl monomer or mixture of monomers - 5 - 25

4. The method according to PP.1 and 2, characterized in that the source composition is administered photoinitiator selected from a series of 2,2-dimethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenyl-propane-1-he, ethers, benzoin, benzophenone, michler ketone, dialkoxybenzene or their mixture, in the following ratio, wt.of n of photoinitiators - of 0.1 to 15.0

5. The method according to p. 3, characterized in that the source composition is administered photoinitiator selected from a series of 2,2-dimethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenyl-propane-1-he, ethers, benzoin, benzophenone, michler ketone, dialkoxybenzene or their mixture, in the following ratio, wt.h.:

The compound of formula I - 100

Acrylic monomer or mixture of monomers - 40 - 400

The vinyl monomer or mixture of monomers - 5 - 25

Photoinitiator or a mixture of photoinitiators of 0.1 to 15.0

6. The method according to p. 5, characterized in that the source composition is administered adhesion promoter selected from a range Methacrylonitrile, methacryloyloxyethyl, vinyl, mercaptoethane or their mixture, in the following ratio, wt.h.:

The compound of formula I - 100

Acrylic monomer or mixture of monomers - 40 - 400

The vinyl monomer or mixture of monomers - 5 - 25

Photoinitiator or a mixture of photoinitiators of 0.1 to 15.0

The adhesion promoter or a mixture of promoters - 1 - 15

 

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