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Publication numberCN105175608 A
Publication typeApplication
Application numberCN 201510590690
Publication date23 Dec 2015
Filing date16 Sep 2015
Priority date16 Sep 2015
Also published asCN105175608B
Publication number201510590690.5, CN 105175608 A, CN 105175608A, CN 201510590690, CN-A-105175608, CN105175608 A, CN105175608A, CN201510590690, CN201510590690.5
Inventors雷海波, 崔存丽, 冯仲善, 安国成
Applicant寿光市鲁源盐化有限公司, 潍坊科技学院
Export CitationBiBTeX, EndNote, RefMan
External Links: SIPO, Espacenet
High-refractivity lens resin monomer
CN 105175608 A
Abstract
The invention belongs to the technical field of optical resin materials, and particularly relates to a high-refractivity lens resin monomer which is composed of the following components in percentage by weight: 5-15% of dibenzyl maleate, 5-15% of styrene compound, 30-60% of diallyl terephthalate, diallyl isophthalate or mixture thereof and 30-40% of bromo ether. The preparation method comprises the following steps: proportionally taking the components, uniformly mixing, adding an initiator, degassing, injecting into a mold, putting in a drying oven, carrying out programmed heating to 120 DEG C, and cooling to room temperature. The high-refractivity lens resin monomer formed by component polymerization has the advantages of higher refractivity, higher impact resistance and higher wear resistance; and the refractivity can reach 1.60 or above. The preparation method provided by the invention has the advantages of simple technique, high process controllability and repetitiveness, mild reaction conditions, no pollution and low cost.
Claims(9)  translated from Chinese
1. 一种高折射率镜片树脂单体,其特征在于,按重量百分比,所述单体由以下组分组成:马来酸二苄酯5~15%,苯乙烯类化合物5~15%,对苯二甲酸二烯丙酯或间苯二甲酸二烯丙酯或者两者的混合物30~60%,含溴醚30~40%。 A high refractive index lens resin monomer, wherein, by weight percent, of the monomer represented by the following components: maleic acid dibenzyl ester 5 to 15%, a styrene compound 5 to 15%, the mixture of diallyl isophthalate or diallyl phthalate, or both, 30 to 60%, containing 30 to 40% bromine ether.
2. 如权利要求1所述的高折射率镜片树脂单体,其特征在于,按重量百分比,所述单体由以下组分组成:马来酸二苄酯7~10%,苯乙烯类化合物7~10%,对苯二甲酸二烯丙酯或间苯二甲酸二烯丙酯或者两者的混合物45~50%,含溴醚35~40%。 Styrene-maleic dibenzyl maleate compound 7 to 10%,: 2. The high refractive index monomer lens resin as claimed in claim 1, characterized in that the percentage by weight of the monomer comprises the following components 7 to 10% of diallyl phthalate or a mixture of two or diallyl isophthalate 45 to 50%, containing 35 to 40% bromine ether.
3. 如权利要求1或2所述的高折射率镜片树脂单体,其特征在于,所述苯乙烯类化合物是苯乙烯或二乙烯基苯。 A high refractive index monomer or resin lens as claimed in claim 2, characterized in that said styrene compound is styrene or divinylbenzene.
4. 一种高折射率镜片树脂单体的制备方法,其特征在于,所述制备方法包括以下步骤: 按权利要求1所述的重量比取对苯二甲酸二烯丙酯或间苯二甲酸二烯丙酯或者两者的混合物、马来酸二苄酯、苯乙烯类化合物和含溴醚,混合搅拌均匀,加入引发剂,脱气,注模后放入烘箱,1~2h内由20C升至30C,2~5h内由30C升至70C,保温4~10h,2~5h 内由70C升至120C,保温2~6h,1~5h内由120C降至室温,即得。 4. A method of preparing high refractive index resin lens monomer, wherein the preparation method comprises the following steps: according to claim 1 wherein the weight ratio r of diallyl isophthalate or terephthalate or a mixture of both diallyl maleate, benzyl ester, styrene compounds and bromine-containing ethers, mixing evenly, the initiator is added, degassing, after injection molding oven, within 1 ~ 2h from 20 C rose to 30 C, 2 ~ 5h raised within the 30 C 70 C, heat 4 ~ 10h, within 2 ~ 5h by a 70 C rise to 120 C, heat 2 ~ 6h, 1 ~ 5h within the 120 C to room temperature, that is, too.
5. 如权利要求4所述的高折射率镜片树脂单体的制备方法,其特征在于,所述引发剂是偶氮二异丁腈或偶氮二异庚腈。 Preparation of high refractive index lens 5. The resin monomer as claimed in claim 4, characterized in that the initiator is azobisisobutyronitrile or azo two different G nitrile.
6. 如权利要求4所述的高折射率镜片树脂单体的制备方法,其特征在于,所述含溴醚按以下步骤合成:取反应物四溴双酚A和烯丙基缩水甘油醚,混合搅拌均匀,加入有机溶剂,然后混合搅拌均匀,所述有机溶剂的重量为所述反应物总重量的30~60%,再加入催化剂,所述催化剂的重量为所述反应物总重量的〇. 3~3%,于30~80C下搅拌、反应5~ 15h,反应结束后,减压蒸馏除去溶剂,用蒸馏水水洗、分液、减压蒸馏提纯产物,即得。 The method of preparing high refractive index lens 6. The resin monomer according to claim 4, characterized in that said bromine-containing ethers synthesized by the following steps: Reaction from tetrabromobisphenol A and allyl glycidyl ether, mixing evenly, adding an organic solvent, and then mixing evenly, by weight of the organic solvent is from 30 to 60% of the total weight of reactants, then adding the catalyst, the catalyst weight is total weight of the reactants billion 3 ~ 3%, followed by stirring at 30 ~ 80 C, the reaction of 5 ~ 15h, after completion of the reaction, the solvent was distilled off under reduced pressure, washed with distilled water, liquid separation, the product was purified by distillation under reduced pressure, that is, too.
7. 如权利要求6所述的高折射率镜片树脂单体的制备方法,其特征在于,所述四溴双酚A与所述烯丙基缩水甘油醚的摩尔比为1 :1~2。 The method of preparing high refractive index resin lens 7. The monomer according to claim 6, characterized in that said tetrabromobisphenol A and the allyl glycidyl ether molar ratio of 1: 1 ~ 2.
8. 如权利要求6所述的高折射率镜片树脂单体的制备方法,其特征在于,所述有机溶剂为甲醇、乙醇或异丙醇。 The method of preparing high refractive index resin lens 8. The monomers recited in claim 6, wherein said organic solvent is methanol, ethanol or isopropanol.
9. 如权利要求6所述的高折射率镜片树脂单体的制备方法,其特征在于,所述催化剂为三乙胺、三丙胺、三正丁胺、N,N-二甲基苄胺或N,N-二乙基苄胺。 The method of preparing high refractive index resin lens 9. monomers according to claim 6, characterized in that the catalyst is triethylamine, tripropylamine, tributylamine, N, N- dimethylbenzylamine or N, N- diethyl-benzylamine.
Description  translated from Chinese
一种高折射率镜片树脂单体 A high-refractive index lens resin monomer

技术领域 TECHNICAL FIELD

[0001] 本发明属于光学树脂材料技术领域,尤其涉及一种高折射率镜片树脂单体。 [0001] The present invention belongs to the technical field of optical resin material, particularly to a high refractive index lens resin monomer.

背景技术 Background technique

[0002] 近年来,光学树脂镜片在国内外眼镜市场上异军突起,尤其是高折射率光学树脂镜片更以其质地轻、强度高、不易碎、高透光率、防紫外、超薄型等特有的优势,深受弱视群体的欢迎。 [0002] In recent years, optical resin lens glasses in the domestic market sprung up everywhere, especially in high-index optical resin lenses but also for its light texture, high strength, non-friable, high transmittance, UV, and other unique ultra-thin the advantages, by amblyopia groups welcome. 通常,在镜片行业中以折射率达到1. 60以上的为高折射率,折射率达到1. 56以上的为中折射率,折射率在1. 56以下的为低折射率。 Typically, the refractive index in the lens industry to achieve 1.60 or more for a high refractive index, the refractive index of 1.56 or more was reached in the refractive index, the refractive index of 1.56 or less in a low refractive index. 有以主要成分是苯丙烯酸酯类与其它组分配制而成的化学单体制作而成的折射率为1. 56的光学树脂镜片,但其厚度较厚,且热阻性、可见光透光率性能较差,因此需要有制作高折射率树脂镜片的光学树脂单体材料。 There is a main component to benzene acrylic formulated with other components of chemical units made of optical refractive index of 1.56 resin lenses, but thicker, and thermal resistance, visible light transmittance poor performance, thus the need for the production of high refractive index resin lens optical resin monomer material.

发明内容 SUMMARY

[0003] 本发明的目的之一在于:针对现有技术存在的不足,提供一种折射率高、抗冲击能力强的高折射率镜片树脂单体。 [0003] It is an object of the present invention is: for deficiency of the prior art, providing high having a refractive index, strong shock resistance of the high refractive index lens resin monomer.

[0004] 为解决上述技术问题,本发明的技术方案是: [0004] In order to solve the above problems, the present invention is a technical solution:

[0005] -种高折射率镜片树脂单体,按重量百分比,所述单体由以下组分组成:马来酸二苄酯5~15%,苯乙烯类化合物5~15%,对苯二甲酸二烯丙酯或间苯二甲酸二烯丙酯或者两者的混合物30~60 %,含溴醚30~40 %。 [0005] - a high refractive index lens resin monomer species, by weight percent, of the monomer represented by the following components: maleic acid dibenzyl ester 5 to 15%, a styrene compound 5 to 15%, of terephthalic diallyl phthalate, or a mixture of both formic acid or diallyl between 30 to 60%, containing 30 to 40% bromine ether.

[0006] 其中,含溴醚的结构式如下: [0006] wherein the bromine-containing ether structural formula as follows:

[0007] [0007]

Figure CN105175608AD00031

[0008] 其化学名称为2, 2-双(4-(3-烯丙氧基-2-羟丙氧基)3, 5-二溴苯基)丙烷,英文名称为2, 2_bis (4-(3-(allyloxy)-2_hydroxypropoxy) _3, 5-dibromophenyl) propane。 [0008] Its chemical name is 2,2-bis (4- (3-allyloxy-2-hydroxypropoxy) 3,5-dibromophenyl) propane, the English name for 2, 2_bis (4- (3- (allyloxy) -2_hydroxypropoxy) _3, 5-dibromophenyl) propane.

[0009] 作为一种改进,按重量百分比,所述单体由以下组分组成:马来酸二苄酯7~ 10%,苯乙烯类化合物7~10%,对苯二甲酸二烯丙酯或间苯二甲酸二烯丙酯或者两者的混合物45~50 %,含溴醚35~40 %。 [0009] As a modification, by weight percent, of the monomer represented by the following components: maleic acid dibenzyl ester 7 to 10%, a styrene compound 7 to 10% of diallyl phthalate Room or propyl phthalate or a mixture of both the diene 45 to 50%, containing 35 to 40% bromine ether.

[0010] 作为进一步地改进,所述苯乙烯类化合物是苯乙烯或二乙烯基苯。 [0010] As a further improvement, the styrenic compound is styrene or divinylbenzene.

[0011] 本发明的目的之二在于:提供一种成本较低,工艺简单的高折射率镜片树脂单体的制备方法。 [0011] Another object of the present invention is that the two: to provide a method for preparing a low-cost, simple process high refractive index lens resin monomers.

[0012] 为解决上述技术问题,本发明的技术方案是: [0012] In order to solve the above problems, the present invention is a technical solution:

[0013] -种高折射率镜片树脂单体的制备方法,所述制备方法包括以下步骤:按权利要求1所述的重量比取对苯二甲酸二烯丙酯或间苯二甲酸二烯丙酯或者两者的混合物、马来酸二苄酯、苯乙烯类化合物和含溴醚,混合搅拌均匀,加入引发剂,脱气,注模后放入烘箱, 1~2h内由20C升至30C,2~5h内由30C升至70C,保温4~10h,2~5h内由70C升至120C,保温2~6h,1~5h内由120C降至室温,即得。 [0013] - kind of a high refractive index resin lens production method of a monomer, the process comprising the steps of: according to claim 1 wherein the weight ratio r of isophthalate or diallyl phthalate diallyloxydiphenylsulfone ester or a mixture of both, maleic acid benzyl ester, styrene compounds and bromine-containing ethers, mixing evenly, the initiator is added, degassing, after injection molding oven, within 1 ~ 2h increased from 20 C to 30 C, within 2 ~ 5h raised to 30 C by a 70 C, heat 4 ~ 10h, the 2 ~ 5h raised to 70 C by the 120 C, heat 2 ~ 6h, the 1 ~ 5h 120 by the C to room temperature, that is, too.

[0014] 优选的,所述引发剂是偶氮二异丁腈或偶氮二异庚腈。 [0014] Preferably, the initiator is azobisisobutyronitrile or azo two different G nitrile.

[0015] 作为一种改进,所述含溴醚按以下步骤合成:取反应物四溴双酚A和烯丙基缩水甘油醚,加入有机溶剂,然后混合搅拌均匀,所述有机溶剂的重量为所述反应物总重量的30~60%,再加入催化剂,所述催化剂的重量为所述反应物总重量的0. 3~3%,于30~ 80C下搅拌、反应5~15h,反应结束后,减压蒸馏除去溶剂,用蒸馏水水洗、分液、减压蒸馏提纯产物,即得。 [0015] As a modification, the bromine-containing ethers synthesized by following these steps: Take the reactants and tetrabromobisphenol A allyl ether, adding an organic solvent, and then mixing evenly, the weight of the organic solvent is the reaction of 30 to 60% by weight of the total composition, and then adding the catalyst, the weight of the catalyst is 0.3 to 3% by weight of the total composition of the reaction mixture was stirred at 30 ~ 80 C, the reaction of 5 ~ 15h, after completion of the reaction, the solvent was distilled off under reduced pressure, washed with distilled water, liquid separation, the product was purified by distillation under reduced pressure, that is, too.

[0016] 含溴醚的合成过程如下: [0016] Brominated ether synthesis process is as follows:

[0017] [0017]

Figure CN105175608AD00041

[0018] 作为一种改进,所述四溴双酚A与所述烯丙基缩水甘油醚的摩尔比为1:1~2。 [0018] As a modification, the tetrabromobisphenol A of the allyl glycidyl ether with a molar ratio of 1: 1 ~ 2.

[0019] 优选的,所述有机溶剂为甲醇、乙醇或异丙醇。 [0019] Preferably, the organic solvent is methanol, ethanol or isopropanol.

[0020] 优选的,所述催化剂为三乙胺、三丙胺、三正丁胺、N,N_二甲基苄胺或N,N_二乙基节胺。 [0020] Preferably, the catalyst is triethylamine, tripropylamine, tributylamine, N, N_-dimethylbenzylamine or N, N_ section diethylamine.

[0021] 由于采用了上述技术方案,本发明的有益效果是: [0021] As a result of the technical proposal, the beneficial effects of the present invention are:

[0022] 本发明提供的高折射率镜片树脂单体,组分中引入含溴醚,有效地提高了单体的折射率,组分中引进的马来酸二苄酯、苯乙烯类化合物和苯二甲酸二烯丙酯类化合物,各组分聚合后形成的单体,具有更高的折射率和更强的抗冲击性及耐磨性,其折射率可达1. 60 以上。 [0022] The high refractive index lens resin monomer of the present invention provides a component introducing bromine-containing ethers, effectively improve the refractive index of the monomer component introduced maleic acid benzyl ester, styrene compounds and diallyl phthalate compound, monomer components formed after polymerization, having a higher refractive index and a stronger impact and abrasion resistance, a refractive index of up to 1.60 or more. 本发明提供的制备方法,其工艺简单,过程的可控性和重复性好,反应条件温和,无污染,成本低,制得的产品折射率高,抗冲击性能好。 Preparation method of the present invention provides a process is simple, controllable and reproducible process, mild reaction conditions, pollution, low cost, high refractive index prepared product, good impact resistance.

具体实施方式 detailed description

[0023] 为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。 [0023] In order to make the objects, technical solutions and advantages of the present invention will become apparent from, the following examples of the present invention will be described in further detail. 应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。 It should be understood that the specific embodiments described herein are merely used to explain the present invention and are not intended to limit the present invention.

[0024] 实施例一 [0024] Example a

[0025] -种高折射率镜片树脂单体,按重量百分比,所述单体由以下组分组成:马来酸二苄酯5 %,苯乙烯类化合物15 %,对苯二甲酸二烯丙酯类化合物50 %,含溴醚30 %;其中,苯乙烯类化合物为苯乙烯。 [0025] - a high refractive index lens resin monomer species, by weight percent, of the monomer represented by the following components: 5% maleic acid benzyl ester, 15% styrene compound, terephthalic Diallylamino esters 50%, 30% ether bromine; wherein the styrenic compound is styrene.

[0026] 实施例二 [0026] Second Embodiment

[0027] -种高折射率镜片树脂单体,按重量百分比,所述单体由以下组分组成:马来酸二苄酯10%,苯乙烯类化合物10%,间苯二甲酸二烯丙酯类化合物40%,含溴醚40%;其中, 苯乙烯类化合物为二乙烯基苯。 [0027] - a high refractive index lens resin monomer species, by weight percent, of the monomer represented by the following components: 10% maleic acid benzyl ester, 10% styrene compound, isophthalic acid Diallylamino 40% ester compounds, bromine-containing ether 40%; wherein the compound is styrene divinylbenzene.

[0028] 实施例三 [0028] Third Embodiment

[0029] -种高折射率镜片树脂单体,按重量百分比,所述单体由以下组分组成:马来酸二苄酯15%,苯乙烯类化合物5%,对苯二甲酸二烯丙酯和间苯二甲酸二烯丙酯的混合物45%,含溴醚35%;其中,苯乙烯类化合物为苯乙烯,所述混合物中对苯二甲酸二烯丙酯和间苯二甲酸二烯丙酯按任意比例混合。 [0029] - a high refractive index lens resin monomer species, by weight percent, of the monomer represented by the following components: 15% maleic acid benzyl ester, a styrene compound 5%, of terephthalic acid Diallylamino a mixture of ester and diallyl isophthalate 45%, 35% of the bromine-containing ether; wherein the styrene compound is styrene, the mixture of diallyl phthalate and isophthalate diene propyl arbitrary mixing ratio.

[0030] 实施例四 [0030] Fourth Embodiment

[0031] -种高折射率镜片树脂单体,按重量百分比,所述单体由以下组分组成:马来酸二苄酯15%,苯乙烯类化合物15%,间苯二甲酸二烯丙酯类化合物30%,含溴醚40%;其中, 苯乙烯类化合物为苯乙烯。 [0031] - a high refractive index lens resin monomer species, by weight percent, of the monomer represented by the following components: 15% maleic acid benzyl ester, 15% styrene compound, isophthalic acid Diallylamino esters 30%, 40% ether bromine; wherein the styrenic compound is styrene.

[0032] 实施例五 [0032] Embodiment 5

[0033] -种高折射率镜片树脂单体,按重量百分比,所述单体由以下组分组成:马来酸二苄酯7 %,苯乙烯类化合物13 %,对苯二甲酸二烯丙酯60 %,含溴醚30 %;其中,苯乙烯类化合物为二乙烯基苯。 [0033] - a high refractive index lens resin monomer species, by weight percent, of the monomer represented by the following components: maleic acid benzyl ester 7%, 13% styrene compound, terephthalic Diallylamino ester 60%, 30% ether bromine; wherein the compound is styrene divinylbenzene.

[0034] 实施例六 [0034] Sixth Embodiment

[0035] -种高折射率镜片树脂单体,按重量百分比,所述单体由以下组分组成:马来酸二苄酯13 %,苯乙烯类化合物7 %,对苯二甲酸二烯丙酯30 %,含溴醚40 %;其中,苯乙烯类化合物为苯乙烯。 [0035] - a high refractive index lens resin monomer species, by weight percent, of the monomer represented by the following components: maleic acid dibenzyl ester 13%, 7% styrene compound, terephthalic Diallylamino ester 30%, 40% ether bromine; wherein the styrenic compound is styrene.

[0036] 实施例七 [0036] Seventh Embodiment

[0037] -种高折射率镜片树脂单体的制备方法,所述制备方法包括以下步骤: [0037] - kind of a high refractive index resin lens production method of a monomer, the process comprising the steps of:

[0038] (1)含溴醚的合成:取反应物四溴双酚A 271. 9g和烯丙基缩水甘油醚85. 6g,加入到置有搅拌桨的四口瓶中,加入有机溶剂甲醇,然后混合搅拌均匀,有机溶剂的重量为反应物总重量的30%,再加入催化剂三乙胺,催化剂的重量为反应物总重量的0. 3%,于30C下搅拌、反应5h,反应结束后,减压蒸馏除去溶剂,用蒸馏水水洗、分液、减压蒸馏提纯产物,即得; [0038] (1) Synthesis of bromine-containing ethers: Reaction from tetrabromobisphenol A 271. 9g and allyl ether 85. 6g, added to a set with a stirring paddle four flask, an organic solvent such as methanol then well mixed, the weight of the organic solvent is 30% of the total weight of the reactants, the catalyst was added triethylamine weight of the catalyst was 0.3% of the total weight of the reaction mixture was stirred at 30 C, the reaction 5H, after completion of the reaction, the solvent was distilled off under reduced pressure, washed with distilled water, liquid separation, the product was purified by distillation under reduced pressure, to obtain;

[0039] (2)镜片树脂单体的制备:按实施例一所述的重量比取马来酸二苄酯、苯乙烯、对苯二甲酸二烯丙酯和含溴醚,混合搅拌均匀,加入引发剂偶氮二异丁腈,脱气,注模后放入烘箱,1~2h内由20C升至30C,2~5h内由30C升至70C,保温4~10h,2~5h内由70C升至120C,保温2~6h,1~5h内由120C降至室温,即得。 [0039] (2) Preparation of the lens resin monomers: a weight ratio as described in Example taken maleate, benzyl acetate, styrene, diallyl phthalate and bromine-containing ethers, mixing evenly, addition of the initiator azobisisobutyronitrile, degassing, after injection molding oven, within 1 ~ 2h raised by the 20 C 30 C, within 2 ~ 5h by a 30 C rise to 70 C, heat 4 ~ 10h, within 2 ~ 5h by a 70 C rise to 120 C, heat 2 ~ 6h, within 1 ~ 5h by the 120 C to room temperature, that is, too.

[0040] 实施例八 [0040] the eighth embodiment

[0041] -种高折射率镜片树脂单体的制备方法,所述制备方法包括以下步骤: [0041] - kind of a high refractive index resin lens production method of a monomer, the process comprising the steps of:

[0042] (1)含溴醚的合成:取反应物四溴双酚A271. 9g和烯丙基缩水甘油醚114. 0g,加入到置有搅拌桨的四口瓶中,加入有机溶剂乙醇,然后混合搅拌均匀,有机溶剂的重量为反应物总重量的60%,再加入催化剂三丙胺,催化剂的重量为反应物总重量的3%,于80C下搅拌、反应15h,反应结束后,减压蒸馏除去溶剂,用蒸馏水水洗、分液、减压蒸馏提纯产物,SP 得; [0042] (1) Synthesis of bromine-containing ether: Take reactant tetrabromobisphenol A271 9g and allyl ether 114. 0g, was added to a stirring paddle set of four bottles, adding an organic solvent ethanol. then well mixed, the weight of the organic solvent is 60% of total weight of reactants, and then the catalyst is added tripropylamine, by weight of the catalyst was 3% by total weight of reactants stirred at 80 C, the reaction 15H, after the reaction, The solvent was removed by distillation under reduced pressure, washed with distilled water, liquid separation, the product was purified by distillation under reduced pressure, SP obtained;

[0043](2)镜片树脂单体的制备:按实施例二所述的重量比取马来酸二苄酯、二乙烯基苯、间苯二甲酸二烯丙酯和含溴醚,混合搅拌均匀,加入引发剂偶氮二异庚腈,脱气,注模后放入烘箱,1~2h内由20C升至30C,2~5h内由30C升至70C,保温4~10h,2~5h 内由70C升至120C,保温2~6h,1~5h内由120C降至室温,即得。 [0043] (2) Preparation of resin monomer lens: by weight of titanium as described in Example than take benzyl ester maleate, divinylbenzene, diallyl isophthalate and bromine-containing ethers, mixing homogenous, initiator azobisisobutyronitrile G nitrile, degassing, after injection molding oven, within 1 ~ 2h by a 20 C rise to 30 C, within 2 ~ 5h by a 30 C rise to 70 C, heat 4 ~ 10h, within 2 ~ 5h by a 70 C rise to 120 C, heat 2 ~ 6h, within 1 ~ 5h by the 120 C to room temperature, that is, too.

[0044] 实施例九 [0044] embodiment Example 9

[0045] -种高折射率镜片树脂单体的制备方法,所述制备方法包括以下步骤: [0045] - kind of a high refractive index resin lens production method of a monomer, the process comprising the steps of:

[0046] (1)含溴醚的合成:取反应物四溴双酚A271. 9g和烯丙基缩水甘油醚52. 6g,加入到置有搅拌桨的四口瓶中,然后加入有机溶剂异丙醇,混合搅拌均匀,有机溶剂的重量为反应物总重量的40%,再加入催化剂三正丁胺,催化剂的重量为反应物总重量的1 %,于50C 下搅拌、反应7h,反应结束后,减压蒸馏除去溶剂,用蒸馏水水洗、分液、减压蒸馏提纯产物, 即得; [0046] (1) Synthesis of bromine-containing ether: Take reactant tetrabromobisphenol A271 9g and allyl ether 52. 6g, added to a set of four with a stirring paddle bottle, and then adding an organic solvent different. propanol, mixing evenly, by weight of the organic solvent is 40% of the total weight of the reactants, the catalyst was added n-butylamine, weight of the catalyst 1% by weight of the reactants, and stirred at at 50 C, the reaction 7H, after completion of the reaction, the solvent was distilled off under reduced pressure, washed with distilled water, liquid separation, the product was purified by distillation under reduced pressure, to obtain;

[0047] (2)镜片树脂单体的制备:按实施例三所述的重量比取马来酸二苄酯、苯乙烯、对苯二甲酸二烯丙酯与间苯二甲酸二烯丙酯及含溴醚,混合搅拌均匀,加入引发剂偶氮二异庚腈,脱气,注模后放入烘箱,1~2h内由20C升至30C,2~5h内由30C升至70C,保温4~10h,2~5h内由70C升至120C,保温2~6h,1~5h内由120C降至室温,即得。 (2) Preparation of [0047] monomer lens resin: weight ratio of three as described in Example from maleic acid dibenzyl ester, styrene, diallyl phthalate and diallyl isophthalate and bromine-containing ethers, mixing evenly, adding initiator azobisisobutyronitrile G nitrile, degassing, after injection molding oven, within 1 ~ 2h by a 20 C rise to 30 C, within 2 ~ 5h by the 30 C to 70 C, heat 4 ~ 10h, within 2 ~ 5h by a 70 C rise to 120 C, heat 2 ~ 6h, within 1 ~ 5h by the 120 C to room temperature, that is, too. [0048] 实施例十 [0048] the tenth embodiment

[0049] -种高折射率镜片树脂单体的制备方法,所述制备方法包括以下步骤: [0049] - kind of a high refractive index resin lens production method of a monomer, the process comprising the steps of:

[0050] (1)含溴醚的合成:取反应物四溴双酚A271. 9g和烯丙基缩水甘油醚87. 9g,加入到置有搅拌桨的四口瓶中,然后加入有机溶剂甲醇,混合搅拌均匀,有机溶剂的重量为反应物总重量的50 %,再加入催化剂N,N-二甲基苄胺,催化剂的重量为反应物总重量的2 %,于60C下搅拌、反应8h,反应结束后,减压蒸馏除去溶剂,用蒸馏水水洗、分液、减压蒸馏提纯产物,即得; [0050] (1) Synthesis of bromine-containing ether: Reaction from the tetrabromobisphenol A271 9g and allyl glycidyl ether 87. 9g, there are added to the set of four stirring blades flask, followed by addition of an organic solvent such as methanol. , mixing evenly, by weight of the organic solvent is 50% of the total weight of the reactants, the catalyst was added N, N- dimethylbenzylamine, the catalyst was 2% by weight of the total weight of the reaction mixture was stirred at at 60 C, The reaction 8h, after completion of the reaction, the solvent was distilled off under reduced pressure, washed with distilled water, liquid separation, the product was purified by distillation under reduced pressure, to obtain;

[0051] (2)镜片树脂单体的制备:按实施例四所述的重量比取马来酸二苄酯、苯乙稀、间苯二甲酸二烯丙酯和含溴醚,混合搅拌均匀,加入引发剂偶氮二异丁腈,脱气,注模后放入烘箱,1~2h内由20C升至30C,2~5h内由30C升至70C,保温4~10h,2~5h内由70C升至120C,保温2~6h,1~5h内由120C降至室温,即得。 [0051] (2) Preparation of the lens resin alone: four weight ratio as described in Example taken maleate, benzyl acetate, styrene, diallyl isophthalate and bromine-containing ethers, mixing evenly adding initiator azobisisobutyronitrile, degassing, after injection molding oven, within 1 ~ 2h by a 20 C rise to 30 C, within 2 ~ 5h by a 30 C rise to 70 C, thermal insulation 4 ~ 10h, within 2 ~ 5h by a 70 C rise to 120 C, heat 2 ~ 6h, within 1 ~ 5h by the 120 C to room temperature, that is, too.

[0052] 实施例^^一 [0052] Example ^^ a

[0053] -种高折射率镜片树脂单体的制备方法,所述制备方法包括以下步骤: [0053] - kind of a high refractive index resin lens production method of a monomer, the process comprising the steps of:

[0054] (1)含溴醚的合成:取反应物四溴双酚A271. 9g和烯丙基缩水甘油醚102. 8g,加入到置有搅拌桨的四口瓶中,然后加入有机溶剂异丁醇,混合搅拌均匀,有机溶剂的重量为反应物总重量的30%,再加入催化剂N,N-二乙基苄胺,催化剂的重量为反应物总重量的0.5%,于60C下搅拌、反应5h,反应结束后,减压蒸馏除去溶剂,用蒸馏水水洗、分液、减压蒸馏提纯产物,即得; [0054] (1) Synthesis of bromine-containing ether: Take reactants tetrabromobisphenol A271 9g and allyl ether 102. 8g, was added to a stirring paddle set of four bottles, and then added to the organic solvent is iso butanol, mixing evenly, by weight of the organic solvent is 30% of the total weight of the reactants, the catalyst was added N, N- diethyl-benzylamine, the catalyst was 0.5% by weight of the total weight of the reactants, at 60 C in stirring, the reaction 5H, after the completion of the reaction, the solvent was distilled off under reduced pressure, washed with distilled water, liquid separation, the product was purified by distillation under reduced pressure, to obtain;

[0055] (2)镜片树脂单体的制备:按实施例五所述的重量比取马来酸二苄酯、二乙烯基苯、对苯二甲酸二烯丙酯和含溴醚,混合搅拌均匀,加入引发剂偶氮二异丁腈,脱气,注模后放入烘箱,1~2h内由20C升至30C,2~5h内由30C升至70C,保温4~10h,2~5h 内由70C升至120C,保温2~6h,1~5h内由120C降至室温,即得。 [0055] (2) Preparation of a lens resin monomer: five weight ratio r as described in Example benzyl ester maleate, divinyl benzene, diallyl phthalate, and bromine-containing ethers, mixing homogenous, initiator azobisisobutyronitrile, degassing, after injection molding oven, within 1 ~ 2h by a 20 C rise to 30 C, within 2 ~ 5h by a 30 C rise to 70 C, heat 4 ~ 10h, within 2 ~ 5h by a 70 C rise to 120 C, heat 2 ~ 6h, within 1 ~ 5h by the 120 C to room temperature, that is, too.

[0056] 实施例十二 [0056] The 12 cases

[0057] -种高折射率镜片树脂单体的制备方法,所述制备方法包括以下步骤: [0057] - kind of a high refractive index resin lens production method of a monomer, the process comprising the steps of:

[0058](1)含溴醚的合成:取反应物四溴双酚A271. 9g和烯丙基缩水甘油醚68. 5g,加入到置有搅拌桨的四口瓶中,然后加入有机溶剂异丁醇,混合搅拌均匀,有机溶剂的重量为反应物总重量的360%,再加入催化剂三乙胺,催化剂的重量为反应物总重量的3%,于70C 下搅拌、反应12h,反应结束后,减压蒸馏除去溶剂,用蒸馏水水洗、分液、减压蒸馏提纯产物,即得; [0058] (1) Synthesis of bromine-containing ether: Take reactants tetrabromobisphenol A271 9g and allyl ether 68. 5g, added to a set of four with a stirring paddle bottle, and then adding an organic solvent iso butanol, mixing evenly, by weight of the organic solvent is 360% of the total weight of the reactants, the catalyst was added triethylamine weight of the catalyst was 3% of the total weight of the reactants, and stirred at 70 C, the reaction 12h, the reaction after completion, the solvent was removed by distillation under reduced pressure, washed with distilled water, liquid separation, the product was purified by distillation under reduced pressure, to obtain;

[0059] (2)镜片树脂单体的制备:按实施例六所述的重量比取马来酸二苄酯、苯乙烯、对苯二甲酸二烯丙酯和含溴醚,混合搅拌均匀,加入引发剂偶氮二异丁腈,脱气,注模后放入烘箱,1~2h内由20C升至30C,2~5h内由30C升至70C,保温4~10h,2~5h内由70C升至120C,保温2~6h,1~5h内由120C降至室温,即得。 (2) Preparation of [0059] monomer lens resin: weight ratio of six described in Example from maleic acid dibenzyl ester, styrene, diallyl phthalate, and bromine-containing ethers, mixing evenly, addition of the initiator azobisisobutyronitrile, degassing, after injection molding oven, within 1 ~ 2h raised by the 20 C 30 C, within 2 ~ 5h by a 30 C rise to 70 C, heat 4 ~ 10h, within 2 ~ 5h by a 70 C rise to 120 C, heat 2 ~ 6h, within 1 ~ 5h by the 120 C to room temperature, that is, too.

[0060] 以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。 [0060] The foregoing is only preferred embodiments of the present invention, it is not intended to limit the present invention, any modifications within the spirit and principles of the present invention made, equivalent replacement and improvement, etc., should be included in this within the scope of the invention.

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Classifications
International ClassificationC08F212/08, C08F216/12, C08F218/16, C08F212/36, C08F222/14, G02B1/04
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