CN100580506C - Shock resistance optical resin lens and method of manufacturing same - Google Patents

Shock resistance optical resin lens and method of manufacturing same Download PDF

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Publication number
CN100580506C
CN100580506C CN200810043684A CN200810043684A CN100580506C CN 100580506 C CN100580506 C CN 100580506C CN 200810043684 A CN200810043684 A CN 200810043684A CN 200810043684 A CN200810043684 A CN 200810043684A CN 100580506 C CN100580506 C CN 100580506C
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weight percent
temperature
percent
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CN101339301A (en
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贺建友
罗有训
郑育红
张盛元
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Shanghai Conant Optics Co Ltd
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Shanghai Conant Optics Co Ltd
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Abstract

The invention relates to an impact resistance optical resin glasses and a manufacturing method thereof, which is characterized in that optical resins materials consist of materials which have A component and B component, and the weigh percentage ratio of the two components is that: A component: B component = 40-50: 60-50, wherein, the A component is prepared by bi-isocyanic acid hexyl ester with the weigh percentage ratio 44-56 percent and multivariate isocyanate-group compounds which have a benzene ring and have the weigh percentage ratio of 56-44 percent; the B component is prepared by the reaction products of pentaerythritol and 3-sulfhydryl-acrylic acid with the weigh percentage ratio 85-95 percent and tetrathio-pentaerythritol with the weigh percentage ratio 15-5 percent; a catalyst adopts double dodecyl halide stannous: R-D2Sn-R; and the addition amount of the catalyst is 0.05-0.12 percent of the total weight of the A and the B components. A computer temperature control curing oven which is provided with a quick cooling device is adopted by the invention, thus guaranteeing the optical precision and the optical quality of the glasses, well and uniformly mixing the raw materials and greatly improving the qualification rate of the glasses.

Description

A kind of shock resistance optical resin lens and manufacture method thereof
Technical field
The present invention relates to a kind of manufacturing process of optical resin lens, particularly disclose super shock resistance optical resin lens of a kind of high index of refraction and manufacture method thereof.
Background technology
The optical resin lens production industry develops rapidly in China, becomes a domestic novel industry.The high dioptrics resin lens wind fan whole nation, it has, and quality is light, compact structure, good in optical property, eyeglass is thin and performance such as uvioresistant effectively.Domestic industry starting is late, the technology starting point is low, the factory of domestic production in recent years carries out polymerization process from the high refraction of external import resin monomer and makes high dioptrics resin lens, the high dioptrics resin lens of producing belongs to acrylic (methacrylic acid) series mostly, the high dioptrics resin lens that the acrylic resin material is made, dyeability is poor, chromatic dispersion height, impact resistance are relatively poor, not as good as the high dioptrics resin lens of super shock resistance.
Summary of the invention
The objective of the invention is to address the deficiencies of the prior art, design a kind of refractive index in 1.60~1.67 shock resistance optical resin lens and manufacture method thereof.
The present invention is achieved in that a kind of manufacture method of shock resistance optical resin lens, it is characterized in that: optical resin material is the A component by the weight percent proportioning: B component=40~50: 60~50 material is made, described A component is that the multicomponent isocyanate based compound of the band phenyl ring of 44~56% two hexyl isocyanates and 56~44% is made into by the weight percent proportioning, and described B component is that 85%~95% the pentaerythrite and the Ji Wusi mercaptan of the acrylic acid resultant of reaction of 3-sulfydryl and 15%~5% are made into by the weight percent proportioning; During batch mixing, take by weighing chemical monomer A component earlier, after 22 ℃~28 ℃ room temperature lower seals stir more than 10 minutes, add catalyzer and stirred 30 minutes at 22 ℃~28 ℃ room temperature lower seals, ice-water bath is cooled to 5 ℃~15 ℃ and keep this temperature then, adds chemical monomer B component, in 5 ℃~15 ℃ following vacuum, vacuum tightness is-0.08~0.09Mpa, stirs 30~45 minutes, and stopping to stir maintenance vacuum tightness then is-0.08~0.09Mpa 10~15 minutes; Keep mixed material temperature at 5 ℃~15 ℃, the inflated with nitrogen supercharging is filtered the back by the teflon filtering membrane and is injected the mould that has got togather, and the curing oven of putting into the computing machine temperature control then solidifies; Described catalyzer adopts two alkyl tin halide: R-D 2Sn-R, wherein R is CH 3CH 2CH 2CH 2, (CH 3) 3C or CH 2=CHCH 2CH 2, D is Cl, Br or F; The addition of described catalyzer is 0.05~0.12% of A, a B component general assembly (TW); Described employing has the computing machine temperature control curing oven of fast cold heat sink, the heat curing temperature change procedure is as follows: the beginning temperature is 35 ℃, be incubated 1~3 hour, be raised to 45~50 ℃ through 3~4 hours, be raised to 65~70 ℃, be incubated 4 hours then through 3~4 hours, be raised to 75~80 ℃ through 3~4 hours again, be raised to 130~140 ℃ through 3~4 hours, be incubated 2 hours, dropped to 70 ℃ through 1 hour; After the demoulding was cleaned, eyeglass carried out regelate, and maximum temperature is controlled at 130~140 ℃, and the time is 1~2 hour.
The production stage of product of the present invention is as follows:
1, preparation mould is through intensive treatment, use the sealing-tape machine matched moulds after the assay was approved;
2, take by weighing chemical monomer, add modifier, adjuvant and initiating agent, vacuum stirring evenly back continues vacuum outgas;
3, mixed material injects the mould that has got togather, the thermosetting polymerization forming, and the demoulding is also cleaned.
The invention has the beneficial effects as follows: adopt the computing machine temperature control curing oven that has fast cold heat sink, by the computer temperature-control technology, can well move the cure profile of setting, the a large amount of heat energy that discharge when shifting macromolecular polymerization reaction in time, eliminated the interior polymeric stress in the chemical monomer polymkeric substance, the optical accuracy and the optical quality of eyeglass have been guaranteed, low temperature seal vacuum stirring technology and the inflated with nitrogen supercharging mode during batch mixing simultaneously, avoided raw material can mix well with contacting also of air, can both improve the qualification rate of eyeglass greatly, become that mirror is qualified to be reached more than 95%.
Description of drawings
Fig. 1 is the manufacture method process flow diagram of shock resistance optical resin lens of the present invention.
Embodiment
Mould is prepared: according to production requirement, clean up after preplaning the glass optical mould intensive treatment that needs, send sealing-tape machine adhesive tape matched moulds again.
With reference to the accompanying drawings, manufacturing approach craft process step of the present invention is as follows.
1, batch mixing:
Select for use refractive index be 1.60~1.67 the high dioptrics resin material of super shock resistance as the base stock of producing the high dioptrics resin lens of this super shock resistance, this raw material is divided into A, B component.The A component is that the multicomponent isocyanate based compound of the band phenyl ring of 44~56% two hexyl isocyanates and 56~44% is made into by the weight percent proportioning.The B component is that 85%~95% the pentaerythrite and the Ji Wusi mercaptan of the acrylic acid resultant of reaction of 3-sulfydryl and 15%~5% are made into by the weight percent proportioning.
Take by weighing chemical monomer A component earlier, after room temperature (22 ℃~28 ℃) lower seal stirs more than 10 minutes, adding catalyzer stirred 30 minutes at room temperature (22 ℃~28 ℃) lower seal again, ice-water bath is cooled to 5 ℃~15 ℃ and keep this temperature then, add chemical monomer B component, (vacuum tightness stirred 30~45 minutes-0.08~0.09Mpa), stopped then stirring keeping vacuum tightness to be poured after-0.08~0.09Mpa is 10~15 minutes in 5 ℃~15 ℃ following vacuum.The addition of catalyzer is 0.05~0.12% of A, a B component general assembly (TW).
2, material feeding:
Keep mixed material temperature at 5 ℃~15 ℃, the inflated with nitrogen supercharging is filtered the back by the teflon filtering membrane and is injected the mould that has got togather, and normal material feeding pressure is at 0.05~0.10Mpa, and the filtering membrane aperture is 0.3 μ m.
3, thermosetting polymerization forming:
Heat release and viscosity constantly increase fluid and become colloid and become the solid characteristics at last when reacting according to polymerizable raw material, have designed the thermosetting curve that is fit to various eyeglasses, and have adopted the computing machine temperature control curing oven that has fast cold heat sink, pass through computer temperature-control.
The beginning temperature is 35 ℃, is incubated 1~3 hour, is raised to 45~50 ℃ through 3~4 hours, be raised to 65~70 ℃ through 3~4 hours, be incubated 4 hours then, be raised to 75~80 ℃ through 3~4 hours again, be raised to 130~140 ℃ through 3~4 hours, be incubated 2 hours, dropped to 70 ℃ through 1 hour.
4, the demoulding, cleaning:
Come out of the stove at 70 ℃, through the demoulding, side cut, cleaning.
5, regelate, check:
Make product through regelate, the check finished product.
Embodiment 1:
Take by weighing chemical monomer A component 9.4Kg earlier, room temperature (22 ℃~28 ℃) lower seal stirred after 11 minutes, adding 14g dibutyl tin dichloride catalyzer stirred 30 minutes at room temperature (22 ℃~28 ℃) lower seal again, ice-water bath is cooled to 8 ℃ and keep this temperature then, add chemical monomer B component 10.6Kg, 8 ℃ of following vacuum (vacuum tightness-0.08Mpa) stirred 35 minutes, stop stir to keep vacuum tightness at-0.08Mpa after 10 minutes then, maintain the temperature at 8 ℃, it is that 0.3 μ m teflon filtering membrane filters the mould (350) that the back injection has got togather, thermosetting polymerization forming in having the computing machine temperature control curing oven of fast cold heat sink by the aperture that inflated with nitrogen is pressurized to 0.06Mpa.The solidification temperature conversion step is: the beginning temperature is 35 ℃, be incubated 2 hours, be raised to 50 ℃, be raised to 70 ℃ through 3 hours through 3 hours, be incubated 4 hours then, be raised to 80 ℃ through 3 hours again, be raised to 140 ℃, be incubated 2 hours through 3 hours, dropped to 70 ℃ through 1 hour, come out of the stove after the demoulding, side cut, cleaning are checked behind 140 ℃ of regelates, the specification product refractive index is 341 of 1.603 the high dioptrics resin lens of shock resistance.
Embodiment 2:
Take by weighing chemical monomer A component 10Kg earlier, room temperature (22 ℃~28 ℃) lower seal stirred after 10 minutes, adding 13g dibutyl tin dichloride catalyzer stirred 30 minutes at room temperature (22 ℃~28 ℃) lower seal again, ice-water bath is cooled to 6 ℃ and keep this temperature then, add chemical monomer B component 10Kg, 6 ℃ of following vacuum (vacuum tightness-0.09Mpa) stirred 40 minutes, stop stir to keep vacuum tightness at-0.09Mpa after 12 minutes then, maintain the temperature at 8 ℃, it is that 0.3 μ teflon filtering membrane filters the mould (360) that the back injection has got togather by the aperture that inflated with nitrogen is pressurized to 0.08Mpa, thermoset forming in having the computing machine temperature control curing oven of fast cold heat sink, the solidification temperature conversion step is: the beginning temperature is 35 ℃, be incubated 1 hour, be raised to 45 ℃ through 4 hours, be raised to 65 ℃ through 4 hours, be incubated 4 hours then, be raised to 75 ℃ through 3 hours again, be raised to 130 ℃ through 3 hours, be incubated 2 hours, dropped to 70 ℃ through 1 hour, come out of the stove after the demoulding, cut edge, clean, behind 130 ℃ of regelates, check, the specification product refractive index is 345 of 1.665 the high dioptrics resin lens of shock resistance.

Claims (2)

1, a kind of manufacture method of shock resistance optical resin lens, it is characterized in that: optical resin material is the A component by the weight percent proportioning: B component=40~50: 60~50 material is made, described A component is that the multicomponent isocyanate based compound of the band phenyl ring of 44~56% two hexyl isocyanates and 56~44% is made into by the weight percent proportioning, and described B component is that 85%~95% the pentaerythrite and the Ji Wusi mercaptan of the acrylic acid resultant of reaction of 3-sulfydryl and 15%~5% are made into by the weight percent proportioning; During batch mixing, take by weighing chemical monomer A component earlier, after 22 ℃~28 ℃ room temperature lower seals stir more than 10 minutes, add catalyzer and stirred 30 minutes at 22 ℃~28 ℃ room temperature lower seals, ice-water bath is cooled to 5 ℃~15 ℃ and keep this temperature then, adds chemical monomer B component, in 5 ℃~15 ℃ following vacuum, vacuum tightness is-0.08~0.09Mpa, stirs 30~45 minutes, and stopping to stir maintenance vacuum tightness then is-0.08~0.09Mpa 10~15 minutes; Keep mixed material temperature at 5 ℃~15 ℃, the inflated with nitrogen supercharging is filtered the back by the teflon filtering membrane and is injected the mould that has got togather, and the curing oven of putting into the computing machine temperature control then solidifies; Described catalyzer adopts two alkyl tin halide: R-D 2Sn-R, wherein R is CH 3CH 2CH 2CH 2, (CH 3) 3C or CH 2=CHCH 2CH 2, D is Cl, Br or F; The addition of described catalyzer is 0.05~0.12% of A, a B component general assembly (TW); Described employing has the computing machine temperature control curing oven of fast cold heat sink, the heat curing temperature change procedure is as follows: the beginning temperature is 35 ℃, be incubated 1~3 hour, be raised to 45~50 ℃ through 3~4 hours, be raised to 65~70 ℃, be incubated 4 hours then through 3~4 hours, be raised to 75~80 ℃ through 3~4 hours again, be raised to 130~140 ℃ through 3~4 hours, be incubated 2 hours, dropped to 70 ℃ through 1 hour; After the demoulding was cleaned, eyeglass carried out regelate, and maximum temperature is controlled at 130~140 ℃, and the time is 1~2 hour.
2, a kind of shock resistance optical resin lens that obtains by the described manufacture method of claim 1, it is characterized in that: optical resin material is the A component by the weight percent proportioning: B component=40~50: 60~50 material is made, described A component is that the multicomponent isocyanate based compound of the band phenyl ring of 44~56% two hexyl isocyanates and 56~44% is made into by the weight percent proportioning, and described B component is that 85%~95% the pentaerythrite and the Ji Wusi mercaptan of the acrylic acid resultant of reaction of 3-sulfydryl and 15%~5% are made into by the weight percent proportioning.
CN200810043684A 2008-08-06 2008-08-06 Shock resistance optical resin lens and method of manufacturing same Active CN100580506C (en)

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Application Number Priority Date Filing Date Title
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CN100580506C true CN100580506C (en) 2010-01-13

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Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102241095A (en) * 2010-05-12 2011-11-16 哈尔滨乐普实业发展中心 Intelligent temperature control method for curing furnace and device thereof
CN102794847B (en) * 2011-05-24 2017-08-29 Hoya株式会社 The manufacture method of thermoset composition
CN104497547A (en) * 2014-11-28 2015-04-08 李国金 High-toughness and impact-resistant resin eyeglass and preparation method thereof
CN105082416B (en) * 2015-08-20 2017-10-27 北京耀森光电设备有限公司 A kind of curing oven and apply its resin lens processing technology
CN105254907B (en) * 2015-11-30 2018-01-05 山东益丰生化环保股份有限公司 A kind of curing of polyurethane optical resin
CN105294974A (en) * 2015-11-30 2016-02-03 黄河三角洲京博化工研究院有限公司 Method for preparing polyurethane resin optical material with high impact toughness
CN106633444A (en) * 2016-12-02 2017-05-10 安徽长庚光学科技有限公司 Anti-shock breakage-proof additive for resin type camera lens

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PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Shock resistance optical resin lens and method of manufacture

Effective date of registration: 20141115

Granted publication date: 20100113

Pledgee: Bank of China Limited by Share Ltd. Shanghai Development Zone Pudong branch

Pledgor: SHANGHAI CONANT OPTICS Co.,Ltd.

Registration number: 2014310000078

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Address after: 201299 Shanghai city Pudong New Area Sichuan Road No. 555

Patentee after: Shanghai Conant's Smart Meter Technology Group Co.

Address before: 201200 Shanghai city Pudong New Area Sichuan Road No. 555

Patentee before: SHANGHAI CONANT OPTICS Co.,Ltd.

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Effective date of registration: 20171107

Address after: 201299 Shanghai city Pudong New Area Sichuan Road 555, No. 585 building 1-15

Patentee after: SHANGHAI CONANT OPTICAL Co.,Ltd.

Address before: 201299 Shanghai city Pudong New Area Sichuan Road No. 555

Patentee before: Shanghai Conant's Smart Meter Technology Group Co.

TR01 Transfer of patent right