CN104629500B - The preparation method of eyeglass hardening liquid - Google Patents
The preparation method of eyeglass hardening liquid Download PDFInfo
- Publication number
- CN104629500B CN104629500B CN201510041012.3A CN201510041012A CN104629500B CN 104629500 B CN104629500 B CN 104629500B CN 201510041012 A CN201510041012 A CN 201510041012A CN 104629500 B CN104629500 B CN 104629500B
- Authority
- CN
- China
- Prior art keywords
- solution
- hardening liquid
- eyeglass
- preparation
- methanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention is a kind of preparation method of eyeglass hardening liquid, is comprised the following steps that：20 27wt% Ludox and 1 2wt% acetic acid are mixed to get after aqueous premix in proportion and add 4 5.5wt% methanol the first solution of formation, continue to stir until pH value is 4~5；19.8 20wt% propyl trimethoxy silicanes and 10 15wt% MTMSs are added into the first solution, lasting stirring forms the second solution；7 8wt% ethylene glycol ethyl ethers, 9 12wt% methanol, 18 25wt% aluminium acetylacetonates, the blue pigment of 0.1 0.4wt% auxiliary agents and 0.1 0.4wt% are put into the second solution in order, and solution, which is stirred, to be filtered out solid impurity and obtain hardening liquid finished product after 1 1.5 hours；The hardening liquid, which is plated in after eyeglass, can ensure the not yellow side of eyeglass, without lathe work and wear-resisting.
Description
Technical field
The present invention relates to a kind of preparation method of eyeglass hardening liquid, belong to optical device processing technique field.
Background technology
Since being born from resin lens, how manufacturer always allows the performances of light, saturating resin lens if being pursued
Further get a promotion, but the quality of high-quality eyeglass is not only determined by lens materials, its surface coating also functions to heavy to closing
The effect wanted, the film layer of lens surface is also being continuously updated the replacement, now in the domestic market mainly using refractive index 1.46
Silica coating materials, configures organosilicon hardening liquid, and eyeglass carries out vacuum ion membrane plating again after stiffened is handled, main plating oxidation
Zirconium, silica, aluminum fluoride etc., it is first in the chip base of eyeglass so that France is according to regarding brilliant (crizal) composite membrane of the brill of road company as an example
First plate the wear-resistant film with organosilicon；Then IPC technology is used, is carried out with Ions Bombardment pre- before coated with antireflection film
Cleaning；The vacuum for carrying out double-layer reflection reducing coating layer using materials such as the zirconium dioxides (ZrO2) of high rigidity after cleaning is coated with；Finally
The teleblem with 110 contact angle is plated again.The VG films of Shanghai Tag Heuer S. A. also use to enter using ion beam bombardment technology
Prerinse before row coated with antireflection film.France plate this (TITUS) stiffened according to another coating process regarding road company in Supreme Being
Both organic substrate is contained in liquid, again containing the inorganic ultrafine particulate of element silicon is included, using immersion plated film work；But above-mentioned eyeglass according to
It is old to exist：The easily yellow side of lens surface, lens surface has lathe work, and the easy film of lens surface splits, and lens surface easily scratches not wear-resisting, pole
Big influence product qualification rate.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of eyeglass hardening liquid, and what it was produced adds
Hard liquid, which is plated in after eyeglass, can ensure the not yellow side of eyeglass, without lathe work and wear-resisting.
The present invention solves the technical scheme of above technical problem：A kind of preparation method of eyeglass hardening liquid, its feature exists
In comprising the following steps that：
（1）20-27wt% Ludox and 1-2wt% acetic acid are mixed in proportion, obtain adding 4- after aqueous premix
5.5wt% methanol the first solution of formation, has the crystalline solid of white on wall during charging, mainly methanol reacts with Ludox and generated
Thing, which is insoluble in have in methanol, and reaction, a little to generate heat, general 1~2 DEG C of heating；First solution continues to stir the PH until solution
It is worth to be standby after between 4~5；
（2）If can double mixing speed if, by 19.8-20wt% propyl trimethoxy silicanes and 10-15wt%
The first solution added after MTMS is well mixed under stirring, mixture needs uniform speed slow to add when feeding
Enter, main cause is that propyl trimethoxy silicane can produce heat in addition with the reaction of moisture in reactor；Lasting stirring
Form the second solution and detect the index of refraction of its solution, when x: th detects what obtained index of refraction n1 and (x+1)th time detection were obtained
When relation between index of refraction n2 is 0≤n1-n2≤1, step reaction terminates；
（3）7-8wt% ethylene glycol ethyl ethers, 9-12wt% methanol, 18-25wt% aluminium acetylacetonates, 0.1-0.4wt% auxiliary agents and
0.1-0.4wt% indigo plant pigment is put into the second solution in order, and solution filters out solid impurity after stirring 1-1.5 hours and obtains stiffened
Liquid finished product.
The technical scheme that further limits of the present invention as：
Further, whole preparation process is carried out under nitrogen atmosphere, and the reaction temperature of whole preparation process is controlled in 20-
25℃。
Further, in step 1, premixed solution need to continue to stir to be no less than after 5min to add methanol, and methanol is added
Speed be adjusted according to the temperature change for forming the first solution, to ensure the temperature T1 and premixed solution of the first solution
Relation between temperature T2, which is maintained, can react heat production after 1 DEG C≤T1- T2≤2 DEG C, Ludox and methanol mixing and generate white
Crystalline solid, so needing slow heating；In step 2, propyl trimethoxy silicane and MM mixed solution need to be slowly added into step
In rapid 1 the first solution formed, to ensure the relation between the temperature T3 for the second solution to be formed and the temperature T1 of the first solution
2 DEG C≤T3-T1≤4 DEG C are maintained, the main cause being slowly added into is propyl trimethoxy silicane meeting and reactor in addition
Interior reaction of moisture, produces heat；In step 3, add after aluminium acetylacetonate, stirring adds auxiliary agent after being no less than 60min
With blue pigment.
Further, hardening liquid finished product need to be stored in 0 DEG C -5 DEG C.
Further, the viscosity 5.5-7.5 of hardening liquid finished product, proportion 1.0-1.1, pH value 4.0-6.0, solid content 35%-
50% 。
Further, auxiliary agent is that enlightening is high by 440.
Further, step 1 needs to carry out nitrogen gas washing, and at least one times any newly adding to reaction environment before starting
It is both needed to carry out a nitrogen gas washing, plus the air valve that begins to rehearse during nitrogen after a kind of material.
In a word, eyeglass meets following index after using hardening liquid stiffened eyeglass disclosed by the invention：1st, thicknesses of layers reaches
＞ 2.5um；2nd, product hardness（Wearability）GB10810.5-2012 is met, the hardness of the actual product can be controlled in haze value
≤0.3%；3rd, the product after processing（Refractive index≤1.560）Close to without lathe work；4th, stiffening layer adhesive force meets GB10810.4-
Film adhesion requirement in 2012；5th, thermocycling meets the thermocycling requirement in GB10810.4-2012；6th, film
Layer yellowing-resistant is higher than industry level；7th, lens surface and edge are saturating, bright.
Embodiment
Embodiment
A kind of preparation method of eyeglass hardening liquid, whole preparation process is carried out under nitrogen atmosphere, and is added newly
It is both needed to carry out a nitrogen gas washing after any material, the reaction temperature of whole preparation process is controlled at 20-25 DEG C, specific step
It is rapid as follows：
Step（1）, a nitrogen gas washing first is carried out to reactor, by 20-27wt% Ludox and 1-2wt% acetic acid in proportion
It is well mixed, aqueous premix is obtained, rear to add 4-5.5wt% methanol the first solution of formation, premixed solution need to continue to stir many
In adding methanol after 5min, the speed that methanol is added is adjusted according to the temperature change for forming the first solution, to ensure
Relation between the temperature T1 of first solution and the temperature T2 of premixed solution maintains 1 DEG C≤T1- T2≤2 DEG C；First solution after
Continuous stirring is standby after being between 4~5 up to the pH value of solution；
Step（2）, 19.8-20wt% propyl trimethoxy silicanes and 10-15wt% MTMSs are mixed equal
The mixed solution of the first solution added after even under stirring, propyl trimethoxy silicane and MTMS need to delay
It is slow to add in the first solution of step 1 formation, with ensure the second solution to be formed temperature T3 and the first solution temperature T1 it
Between relation maintain 2 DEG C≤T3-T1≤4 DEG C；The second solution that lasting stirring is formed and the index of refraction for detecting its solution, when the
, should when detecting the relation between the index of refraction n2 that obtained index of refraction n1 and (x+1)th time detection are obtained for x times for 0≤n1-n2≤1
Step reaction terminates；
Step（3）, high 440 and of 7-8% ethylene glycol ethyl ethers, 9-12% methanol, 18-25% aluminium acetylacetonates, 0.1-0.4% enlightening
0.1-0.4% indigo plant pigment is put into the solution of step 2 formation in order, is added after aluminium acetylacetonate, stirring is no less than after 60min
Add enlightening high 440 and blue pigment；Solution is filtrated to get hardening liquid finished product after stirring 1-1.5 hours；
Step（4）, hardening liquid finished product need to be stored in 0 DEG C -5 DEG C, viscosity 5.5-7.5, the proportion 1.0- of hardening liquid finished product
1.1st, pH value 4.0-6.0, solid content 35%-50%.
Form 1 be course of reaction in, the weight percentage ratio of material in each embodiment（wt%）：
In addition to the implementation, the present invention can also have other embodiment.All use equivalent substitution or equivalent transformation shape
Into technical scheme, all fall within the protection domain of application claims.
Claims (7)
1. a kind of preparation method of eyeglass hardening liquid, it is characterised in that comprise the following steps that：
（1）20-27wt% Ludox and 1-2wt% acetic acid are mixed in proportion, obtain adding 4- after aqueous premix
5.5wt% methanol the first solution of formation, first solution continues to stir standby after between the pH value of solution is 4~5；
（2）Add and stir after 19.8-20wt% propyl trimethoxy silicanes and 10-15wt% MTMSs are well mixed
The first solution under state is mixed, lasting stirring forms the second solution and detects the index of refraction of its solution, when x: th detects what is obtained
When relation between the index of refraction n2 that time detection of index of refraction n1 and (x+1)th is obtained is 0≤n1-n2≤1, step reaction terminates；
（3）7-8wt% ethylene glycol ethyl ethers, 9-12wt% methanol, 18-25wt% aluminium acetylacetonates, 0.1-0.4wt% auxiliary agents and 0.1-
0.4wt% indigo plant pigment put into order in the second solution, solution stir 1-1.5 hours after filter out solid impurity obtain hardening liquid into
Product.
2. the preparation method of eyeglass hardening liquid according to claim 1, it is characterised in that：Whole preparation process is in nitrogen
Carried out under atmosphere, the reaction temperature of whole preparation process is controlled at 20-25 DEG C.
3. the preparation method of eyeglass hardening liquid according to claim 1, it is characterised in that：In step 1, premixed solution
Stirring need to be continued and entered no less than methanol, the speed that methanol is added is added after 5min according to the temperature change for forming the first solution
Row regulation, to ensure that the relation between the temperature T1 of the first solution and the temperature T2 of premixed solution maintains 1 DEG C≤T1- T2≤2
℃；In step 2, the mixed solution of propyl trimethoxy silicane and MTMS need to be slowly added into step 1 and be formed
The first solution in, to ensure that the relation between the temperature T3 for the second solution to be formed and the temperature T1 of the first solution maintains 2
℃≤T3-T1≤4℃；In step 3, add after aluminium acetylacetonate, stirring adds auxiliary agent and Lan Yan after being no less than 60min
Material.
4. the preparation method of eyeglass hardening liquid according to claim 1, it is characterised in that：The hardening liquid finished product need to be deposited
It is stored in 0 DEG C -5 DEG C.
5. the preparation method of eyeglass hardening liquid according to claim 1, it is characterised in that：The hardening liquid finished product it is viscous
Spend 5.5-7.5, proportion 1.0-1.1, pH value 4.0-6.0, solid content 35%-50%.
6. the preparation method of the eyeglass hardening liquid according to claim 1 or 3, it is characterised in that：The auxiliary agent is that enlightening is high
440。
7. the preparation method of the eyeglass hardening liquid according to claim 1 or 3, it is characterised in that：Before the step 1 starts
Nitrogen gas washing at least one times need to be carried out to reaction environment, and nitrogen of progress is both needed to after any material of new addition washing
Gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510041012.3A CN104629500B (en) | 2015-01-28 | 2015-01-28 | The preparation method of eyeglass hardening liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510041012.3A CN104629500B (en) | 2015-01-28 | 2015-01-28 | The preparation method of eyeglass hardening liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104629500A CN104629500A (en) | 2015-05-20 |
| CN104629500B true CN104629500B (en) | 2017-09-29 |
Family
ID=53208761
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510041012.3A Active CN104629500B (en) | 2015-01-28 | 2015-01-28 | The preparation method of eyeglass hardening liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104629500B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107936832A (en) * | 2017-11-17 | 2018-04-20 | 上海伟星光学有限公司 | High hardness spray coating liquid and its manufacture method for polyurethane lens surface |
| CN107936829B (en) * | 2017-11-17 | 2021-09-07 | 上海伟星光学有限公司 | High-refractive-index coating liquid for polyurethane lens surface and manufacturing method thereof |
| CN113461996B (en) * | 2021-07-23 | 2022-10-11 | 盈昌集团有限公司 | Acetate fibre board hardening treatment method for glasses |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004346228A (en) * | 2003-05-23 | 2004-12-09 | Mitsubishi Chemicals Corp | Active energy ray-curable composition and hard coat film |
| CN101955728A (en) * | 2009-07-17 | 2011-01-26 | 黄祥道 | Organic-inorganic hybrid wear-resistant transparent coating for reinforcing surface of optical plastics |
| CN102260455A (en) * | 2010-05-29 | 2011-11-30 | 比亚迪股份有限公司 | A coating, and an optical element comprising the coating |
| CN101967350B (en) * | 2010-11-03 | 2013-01-30 | 厦门威亮光学涂层技术有限公司 | Wear-resistant coating material without primer on polycarbonate surface and preparation method thereof |
| CN103265884A (en) * | 2013-06-06 | 2013-08-28 | 苏州禾川化工新材料科技有限公司 | Lens hardening antireflection liquid |
-
2015
- 2015-01-28 CN CN201510041012.3A patent/CN104629500B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104629500A (en) | 2015-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102272254B (en) | Coating composition, process for production of the composition, and laminte with hard coat layer | |
| CN101553743B (en) | Optical article comprising a double-layer abrasion and scratch resistant coating and method for production thereof | |
| CN101134872B (en) | Hard coating composition and plastic optical product | |
| CN103253864B (en) | Ultrawhite float glass process technology for making glass used for solar batteries | |
| CN104629500B (en) | The preparation method of eyeglass hardening liquid | |
| US11339081B2 (en) | Antimicrobial strengthened glass and preparation process thereof | |
| EP2403817A1 (en) | Slot die coating process | |
| CN105084778B (en) | A kind of green low radiation coated glass and preparation method thereof | |
| CN104020513B (en) | A kind of anti-skidding plated film resin eyeglass and preparation method thereof | |
| TW201532994A (en) | Glass plate with anti-glare function for solar cells | |
| TW201331141A (en) | Glass base plate for chemical reinforcement, and method for producing same | |
| KR20160114616A (en) | Coating composition and optical member | |
| CN107400466A (en) | A kind of production technology of ultralow medium-temperature reinforced description film | |
| CN103269991B (en) | The method of coating glass | |
| CN103253849B (en) | Ultra-thin ultrawhite float glass process technology for making glass used for solar batteries and products thereof | |
| CN108998772A (en) | A kind of compound transparent electricity conductive film and preparation method thereof | |
| US20080050601A1 (en) | Hard coating composition and plastic optical product | |
| CN106630667A (en) | An anti-glare (AG) glass processing process adopting silicon oxide sedimentation | |
| CN105295719A (en) | Wear-resistant anti-glare glass spraying liquid and anti-glare coating processing method | |
| CN107235643B (en) | Method for manufacturing high anti-reflection reinforced glass | |
| CN101003419B (en) | Gray coated glass and preparation method | |
| CN104448975A (en) | Scratch-resistant ultraviolet coating for screen protection films | |
| CN104621875B (en) | A kind of method processing Margarita | |
| CN110256710A (en) | A kind of optics wear resistant plastic lens materials that light transmittance is high | |
| CN106634357A (en) | Special interior wall coating used on glass fiber cloth and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |