CN103571234B - Preparation method of modified glass beads for light reflecting film - Google Patents
Preparation method of modified glass beads for light reflecting film Download PDFInfo
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- CN103571234B CN103571234B CN201210281050.2A CN201210281050A CN103571234B CN 103571234 B CN103571234 B CN 103571234B CN 201210281050 A CN201210281050 A CN 201210281050A CN 103571234 B CN103571234 B CN 103571234B
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Abstract
The invention relates to a preparation method of modified glass beads for a light reflecting film. The preparation method comprises the following steps: modifying the glass beads by using an organic modifying agent; and then, coating organic modifying films on the surfaces of the glass beads. The glass beads are converted to be lipophilic from being hydrophilic, and therefore, the modified glass beads can form stable colloid liquor with matrix resin, and a single glass bead layer which is tightly and uniformly distributed is easily formed after coating of the colloid liquor; light reflecting performance and quality of the light reflecting film manufactured by the glass bead layer are obviously improved; meanwhile, functional groups on a coupling agent can react with the matrix resin, and the coupling agent is bonded, so that mechanical performance and weather resistance of the light reflecting film are improved; moreover, usage amount of the glass beads can be saved. Besides, the preparation method is simple in process, provided with no need of a special device, low in cost and suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of light reflecting material, particularly relate to a kind of organic modifiers that uses and the method for moditied processing is carried out to glass microballon surface.
Background technology
High refractive index glass micro pearl is just being widely used in the manufacture of tapetum lucidum, and in tapetum lucidum making processes, glass microballon energy and matrix resin form the colloid of stable and uniform, is beneficial to form individual layer and is closely uniformly distributed soot layer.In actual production, reunite because glass microballon high surface energy and surface charge performance make glass microballon produce, fold the phenomenons such as pearl, affect the performance of tapetum lucidum, cause quality to decline.Chinese patent No.200720303115.3, at glass microballon Surface coating fluoride films, makes glass microballon surface band same charge, glass microballon is evenly distributed, and be difficult to realize, and ratio defective product is low in a large amount of production.
Summary of the invention
The invention provides a kind of preparation method of tapetum lucidum modified glass microspheres, technique is simple, do not need specific installation, cost is low, be applicable to scale operation, the tapetum lucidum simultaneously using the glass microballon of modification of the present invention to make all is significantly improved in optical property, mechanical property, weather resistance and quality, and can also save the usage quantity of glass microballon.
For achieving the above object, technical scheme of the present invention is: a kind of preparation method of tapetum lucidum modified glass microspheres, use organic modifiers to glass microballon modification, after at the organically-modified film of glass microballon Surface coating one deck.
The concrete steps of preparation method of the present invention are:
1) organically-modified agent solution is prepared: the solvent first becoming organic modifiers with water and alcohol according to the proportions of 1:8-10; Then with organic acid, PH is adjusted to acidity, under fully stirring, adds the coupling agent of 5 ~ 20% until transparent, then add the tensio-active agent of 0.5 ~ 5%, finally add the membrane-forming agent of 2 ~ 10%; Be warming up to 60 ~ 90 DEG C, stir 0.5 ~ 2 hour with 500 ~ 4000 revs/min.
2) modified glass microspheres: be distributed to by glass microballon in organically-modified agent solution, at 60 ~ 90 DEG C of temperature, stirs 1 ~ 3 hour with 500 ~ 4000 revs/min.
3) the residual properties-correcting agent of removing: modified microballon mixing solutions is filtered, by the microballon hot wash after filtration, stirs 1 ~ 5 hour and filter; Washing process repeats several times, to remove unnecessary organic modifiers.
4) dry: microballon is obtained organically-modified glass microballon in less than 80 DEG C vacuum-dryings.
As the preferred embodiment of the present invention: alcohol of the present invention is generally ethanol, methyl alcohol or Virahol.
In step 1) of the present invention, described coupling agent is selected from the silane coupling agent of structural formula as shown in formula I or the titanate coupling agent of structural formula as shown in formula II,
（Ⅰ）
In formula I, X is methoxy or ethoxy, and Y is methyl or ethyl or some functional functional groups, and coupling agent and matrix resin are reacted;
formula II
In formula II, X is carboxyl, and sulfonic group is phosphate-based, phosphorous acid ester group, and R is that long-chain tangles group or aromatic base, and Y is amino or double bond.Organic acid of the present invention is oxalic acid, citric acid, tartrate or its mixing acid.
Tensio-active agent of the present invention is sodium laurylsulfonate, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, Trimethyllaurylammonium bromide, carboxymethyl cellulose, it mainly plays and soaks and reduce capillary effect, and modified membrane can be made even.
Membrane-forming agent of the present invention is ethyl cellulose, Natvosol, methylcellulose gum, Vltra tears.
The present invention is at the organically-modified film of the coated one deck of high-transparent glass bead surface, glass microballon is made to be transformed into lipophilicity from hydrophilic, therefore modified glass microballon energy and matrix resin form stable colloidal solution, in the process making tapetum lucidum, control the settling velocity of glass microballon in matrix resin, the degree of depth of glass microballon sedimentation is controlled by the time, avoid folded pearl phenomenon, therefore easily the tight equally distributed soot layer of individual layer is formed after coating, reflective function and the quality of the tapetum lucidum made of it significantly improve, function functional group energy simultaneously on coupling agent and matrix resin react, by the bonding of coupling agent, improve mechanical property and the weather resistance of tapetum lucidum, and the usage quantity of glass microballon can also be saved.
Particle size of glass microspheres scope of the present invention is 10 ~ 100 microns, and proportion is 4.5 ~ 6.0 kg/m3.
Accompanying drawing explanation
Fig. 1 is the structural representation of the modified glass microballon of the present invention.
In figure: tensio-active agent 1, glass microballon 2, film-forming resin layer 3, coupling agent 4.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, and does not limit the scope of the invention.
Embodiment 1
First the solvent of organic modifiers is mixed with 9 parts of methyl alcohol and 1 part of deionized water, then with oxalic acid, PH is adjusted to 5, under fully stirring, add the γ-methacryloxypropyl trimethoxy silane of 5% until transparent, then the sodium laurylsulfonate of 1% is added, finally add the ethyl cellulose of 3%, at 70 DEG C, stir 1 hour with 1000 revs/min.3 glass microballons are distributed in 5 parts of organically-modified agent solutions, at 60 DEG C, stir 2 hours with 500 revs/min.Filter, by the throw out hot wash after filtration, stir 1 hour, filter.Washing process repeats 2 times, to remove unnecessary organic modifiers.Final product vacuum-drying at 80 DEG C is obtained organically-modified glass microballon.
Embodiment 2
First the solvent of organic modifiers is mixed with 9 parts of methyl alcohol and 1 part of deionized water, then with oxalic acid, PH is adjusted to 5, under fully stirring, add the vinyltrimethoxy silane of 5 % until transparent, then the sodium lauryl sulphate of 0.5% is added, finally add the Natvosol of 5%, at 60 DEG C, stir 0.5 hour with 1000 revs/min.3 parts of glass microballons are distributed in 8 parts of organically-modified agent solutions, at 90 DEG C, stir 2 hours with 2000 revs/min.Filter, by the throw out hot wash after filtration, stir 1 hour, filter.Washing process repeats 2 times, to remove unnecessary organic modifiers.Final product vacuum-drying at 78 DEG C is obtained organically-modified glass microballon.
Embodiment 3
First the solvent of organic modifiers is mixed with 9.5 parts of methyl alcohol and 1 part of deionized water, then with citric acid, PH is adjusted to 4, under fully stirring, add the γ-chloropropyl triethoxysilane of 8% until transparent, then the sodium laurylsulfonate of 2% is added, finally add the Vltra tears of 10%, at 60 DEG C, stir 0.5 hour with 2000 revs/min.2 glass microballons are distributed in 6 parts of organically-modified agent solutions, at 80 DEG C, stir 1 hour with 2000 revs/min.Filter, by the throw out hot wash after filtration, stir 1 hour, filter.Washing process repeats 2 times, to remove unnecessary organic modifiers.Final product vacuum-drying at 75 DEG C is obtained organically-modified glass microballon.
Embodiment 4
First the solvent of organic modifiers is mixed with 8.8 parts of methyl alcohol and 1 part of deionized water, then with oxalic acid, PH is adjusted to 5, under fully stirring, add the titanate coupling agent TC-F of 5 % until transparent, then the sodium laurylsulfonate of 2% is added, finally add the ethyl cellulose of 10%, at 60 DEG C, stir 0.5 hour with 3000 revs/min.5 parts of glass microballons are distributed in 10 parts of organically-modified agent solutions, at 90 DEG C, stir 1 hour with 4000 revs/min.Filter, by the throw out hot wash after filtration, stir 1 hour, filter.Washing process repeats 3 times, to remove unnecessary organic modifiers.Final product vacuum-drying at 80 DEG C is obtained organically-modified glass microballon.
Embodiment 5
First 8.5 parts of methyl alcohol and 1 part of deionized water are mixed with the solvent of organic modifiers, then with oxalic acid, PH is adjusted to 3, under fully stirring, add the titanate coupling agent TC-27 of 5 % until transparent, then the palmityl trimethyl ammonium chloride of 3% is added, finally add the methylcellulose gum of 6%, at 80 DEG C, stir 1 hour with 3500 revs/min.2 parts of glass microballons are distributed in 5 parts of organically-modified agent solutions, at 70 DEG C, stir 1 hour with 3000 revs/min.Filter, by the throw out hot wash after filtration, stir 2 hours, filter.Washing process repeats 4 times, to remove unnecessary organic modifiers.Final product vacuum-drying at 76 DEG C is obtained organically-modified glass microballon.
Embodiment 6
First 9.2 parts of ethanol and 1 part of deionized water are mixed with the solvent of organic modifiers, then with tartrate, PH is adjusted to 2, under fully stirring, add the titanate coupling agent TC-114 of 5 % until transparent, then the sodium laurylsulfonate of 3% is added, finally add the ethyl cellulose of 6%, at 60 DEG C, stir 2 hours with 2000 revs/min.5 parts of glass microballons are distributed in 10 parts of organically-modified agent solutions, at 90 DEG C, stir 2 hours with 3000 revs/min.Filter, by the throw out hot wash after filtration, stir 2 hours, filter.Washing process repeats 3 times, to remove unnecessary organic modifiers.Final product vacuum-drying at 80 DEG C is obtained organically-modified glass microballon.
Claims (6)
1. a preparation method for tapetum lucidum modified glass microspheres, is characterized in that: use organic modifiers to glass microballon modification, and at the organically-modified film of glass microballon Surface coating one deck, carry out as follows:
1) organically-modified agent solution is prepared: the solvent first becoming organic modifiers with water and alcohol according to the proportions of 1:8-10; Then with organic acid, pH is adjusted to acidity, under fully stirring, adds the coupling agent of 5 ~ 20% until transparent, then add the tensio-active agent of 0.5 ~ 5%, finally add the membrane-forming agent of 2 ~ 10%; Be warming up to 60 ~ 90 DEG C, stir 0.5 ~ 2 hour with 500 ~ 4000 revs/min;
2) modified glass microspheres: be distributed to by glass microballon in organically-modified agent solution, at 60 ~ 90 DEG C of temperature, stirs 1 ~ 3 hour with 500 ~ 4000 revs/min;
3) the residual properties-correcting agent of removing: modified microballon mixing solutions is filtered, by the microballon hot wash after filtration, stirs 1 ~ 5 hour and filter; Washing process repeats several times, to remove unnecessary organic modifiers;
4) dry: microballon is obtained organically-modified glass microballon in less than 80 DEG C vacuum-dryings.
2. preparation method according to claim 1, is characterized in that: alcohol described in step 1) is ethanol, methyl alcohol or Virahol.
3. preparation method according to claim 1, is characterized in that: coupling agent described in step 1) is selected from the silane coupling agent of structural formula as shown in formula I or the titanate coupling agent of structural formula as shown in formula II,
In formula I, X is methoxy or ethoxy, and Y is methyl or ethyl or some functional functional groups, and coupling agent and matrix resin are reacted;
In formula II, X is carboxyl, and sulfonic group is phosphate-based, phosphorous acid ester group, and R is that long-chain tangles group or aromatic base, and Y is amino or double bond.
4. preparation method according to claim 1, is characterized in that: the organic acid described in step 1) is oxalic acid, citric acid, tartrate or its mixing acid.
5. preparation method according to claim 1, is characterized in that: tensio-active agent described in step 1) is sodium laurylsulfonate, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, Trimethyllaurylammonium bromide or carboxymethyl cellulose.
6. preparation method according to claim 1, is characterized in that: the membrane-forming agent described in step 1) is ethyl cellulose, Natvosol, methylcellulose gum or Vltra tears.
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| CN105925102B (en) * | 2016-05-11 | 2018-07-06 | 山东赛德丽新材料股份有限公司 | A kind of lacquer for blending glass microballoon and preparation method thereof |
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| CN107311469A (en) * | 2017-07-18 | 2017-11-03 | 合肥鼎亮光学科技有限公司 | A kind of antistatic process technique of reflective membrane glass microballoon |
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| CN107879639B (en) * | 2017-11-02 | 2020-08-04 | 江西盛汇光学科技协同创新有限公司 | Method and device for improving performance of glass beads |
| CN110157347B (en) * | 2019-05-05 | 2021-05-11 | 浙江夜光明光电科技股份有限公司 | High-strength reflective film and preparation method thereof |
| CN111446330B (en) * | 2020-03-31 | 2022-07-29 | 江苏辉伦太阳能科技有限公司 | Light-reflecting film layer positioned on surface of float glass and preparation method thereof |
| CN111472234B (en) * | 2020-04-14 | 2022-01-04 | 江苏国奥众联体育产业有限公司 | Reflective artificial turf |
| CN113500838B (en) * | 2021-07-20 | 2022-11-15 | 常州市日月反光材料有限公司 | High-strength self-cleaning reflective film and preparation method thereof |
| CN114045099B (en) * | 2021-11-15 | 2022-09-23 | 上海市建筑科学研究院有限公司 | Environment-friendly two-component marking paint and preparation method, use method and application thereof |
| CN114805890B (en) * | 2022-05-07 | 2023-09-29 | 泉州三维反光材料科技有限公司 | High-elasticity PVC reflective film and preparation method thereof |
| CN116515190B (en) * | 2023-05-29 | 2024-03-08 | 重庆维斯顿实业有限公司 | Ageing-resistant low-migration polyethylene pipe and preparation method thereof |
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|---|---|---|---|---|
| CN1473780A (en) * | 2003-08-11 | 2004-02-11 | 金坛市金鹏汽车配件有限公司 | Method for modifying and strengthening glass beads and modifying and strengthening furnace thereof |
| CN101284712A (en) * | 2007-04-09 | 2008-10-15 | 單岩崑 | Glass microballoon with dual-layer function membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1473780A (en) * | 2003-08-11 | 2004-02-11 | 金坛市金鹏汽车配件有限公司 | Method for modifying and strengthening glass beads and modifying and strengthening furnace thereof |
| CN101284712A (en) * | 2007-04-09 | 2008-10-15 | 單岩崑 | Glass microballoon with dual-layer function membrane |
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Address after: 213144 Jiangsu province Changzhou City Zhonglou District Zou Yue Yang Road, No. 8 Patentee after: Changzhou Hua R Sheng Reflective Material Co., Ltd. Address before: 213144 Jiangsu Province, Changzhou city Wujin District Industrial Park District Zou Zou Quzhen Yue Yang Road No. 8 Patentee before: Changzhou Hua R Sheng Reflective Material Co., Ltd. |