CN115746367B - Photochromic fashion rubber boots and preparation method thereof - Google Patents
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Abstract
The invention discloses a photochromic fashion rubber boot and a preparation method thereof, belonging to the technical field of new materials. The photochromic fashion rubber boot comprises a photochromic coating sprayed on the surface of an external rubber layer, and is characterized in that the photochromic coating comprises the following raw materials in parts by weight: 90-100 parts of resin, 0.5-3 parts of antioxidant, 0.1-1 part of auxiliary antioxidant, 0.1-1 part of light stabilizer and 0.5-3 parts of photochromic agent. The photochromic coating of the photochromic fashion rubber boot takes the spiropyran compound with carboxyl as a photochromic substance, takes resin as a base material, and takes an antioxidant, an auxiliary antioxidant and a light stabilizer as auxiliary materials, so that the photochromic coating has good stability and high long-term light transparency. The photochromic fashion rubber boot has good long-term photochromic effect.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a photochromic fashion rubber boot and a preparation method thereof.
Background
With the progress and development of technology, people pay more attention to the color of clothes, shoes and caps. Most of the colors of clothes, shoes and caps are determined when leaving factories, and only cannot be changed.
Some patents such as CNN105970625A have disclosed a photochromic spinning, a fabric and a preparation method of the photochromic spinning, wherein a polyethylene composite material is prepared by utilizing the characteristics of a photochromic master batch, and the polyethylene composite material is coated on the spinning to prepare the photochromic spinning.
In the aspect of shoe caps, related patents are few, CN106967340A is a prior patent of researchers of the invention, and discloses a photochromic coating layer which is immersed or sprayed on the surface of an outer rubber layer of an integrated full rubber boot of a boot body, a sole and a heel, and a bright oil layer is immersed or sprayed after the shoes are dried by an oven, and the components of the paint for the specific photochromic coating layer are disclosed. In subsequent studies, researchers found that the photochromic coating was prone to yellowing and increased opacity during use, resulting in poor photochromic effects.
Disclosure of Invention
Aiming at the problems, the invention provides a photochromic coating with long-term use and stable performance, and the photochromic fashion rubber boot adopting the material has long-term stable photochromic property.
The invention discloses a photochromic fashion rubber boot, which comprises a photochromic coating sprayed on the surface of an external rubber layer, wherein the photochromic coating is prepared from the following components in parts by weight:
90-100 parts of resin, 0.5-3 parts of antioxidant, 0.1-1 part of auxiliary antioxidant, 0.1-1 part of light stabilizer and 0.5-3 parts of photochromic agent.
In some embodiments of the invention, the resin is a PC resin.
In some embodiments of the invention, the antioxidant is antioxidant 1010.
In some embodiments of the invention, the secondary antioxidant is a secondary antioxidant DSTP.
In some embodiments of the invention, the light stabilizer is light stabilizer UV-327.
In some embodiments of the invention, the photochromic agent includes a spiropyran compound having a carboxyl group therein.
In some embodiments of the present invention, the photochromic agent may further include a monomer of methyl methacrylate, acrylic acid, and azobisisobutyronitrile. .
In some embodiments of the present invention, the step of preparing the photochromic agent includes:
s11, dissolving a monomer of methyl methacrylate and acrylic acid in a solvent;
s12, adding azodiisobutyronitrile in a nitrogen atmosphere for reaction;
s13, adding a spiropyran compound with carboxyl, and continuing the reaction;
s14, adding deionized water, filtering and drying.
In some embodiments of the invention, in S11, the solvent is anhydrous tetrahydrofuran.
In some embodiments of the invention, in S12, the reaction is carried out at 65-75℃for 15-25h.
In some embodiments of the invention, in S13, the reaction is carried out at 65-75℃for 15-25h.
In some embodiments of the present invention, the weight ratio of the monomer of methyl methacrylate, acrylic acid, azobisisobutyronitrile and the spiropyran compound having a carboxyl group is (2-4): (2-4): (0.2-0.4): (2.5-3.5), preferably 3:3:0.3:3.
In some embodiments of the present invention, the raw materials for preparing the photochromic coating layer include the following components in parts by weight:
96.6-97.2 parts of PC resin, 1 part of antioxidant, 0.4-0.7 part of auxiliary antioxidant DSTP, 0.4-0.7 part of light stabilizer and 1 part of spiropyran compound with carboxyl.
In some embodiments of the invention, the outer rubber layer is an outer rubber layer of an integrally formed full rubber boot of a boot body, a sole and a heel.
In some embodiments of the invention, a bright oil layer outside the photochromic coating layer is also included.
The second aspect of the invention discloses a method for preparing the photochromic fashion rubber boot according to the first aspect, which comprises the following steps:
s01, preparing a photochromic agent;
s02, mixing resin, an antioxidant, an auxiliary antioxidant, a light stabilizer and a photochromic agent, and extruding and granulating by a double-screw extruder to obtain a photochromic coating master batch;
s03, spraying the photochromic coating master batch on the surface of an external rubber layer of the integrated full rubber boot of the boot body, the sole and the heel to form a photochromic coating.
And optionally, S04, spraying a bright oil layer outside the photochromic coating to obtain the photochromic fashion rubber boot.
The invention has the beneficial effects that:
the photochromic coating of the photochromic fashion rubber boot takes the spiropyran compound with carboxyl as a photochromic substance, takes resin as a base material, and takes an antioxidant, an auxiliary antioxidant and a light stabilizer as auxiliary materials, so that the photochromic coating has the advantages of high strength, good light transmittance, good stability and high long-term light transparency. The photochromic fashion rubber boot has good long-term photochromic effect.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
The PC resin is PC300-10 of Dow. The spiropyran compound with carboxyl group is prepared according to the following literature: liu Yingren preparation of spiropyran photoresponse drug carrier and its performance study [ D ]. Shanxi university, 2017. The bright oil layer is polyurethane thermoplastic elastic resin.
The examples and comparative examples are parallel runs of the same components, component contents, preparation steps, preparation parameters, unless otherwise specified.
Example 1
A photochromic fashion rubber boot comprises a boot body, a sole, a heel, a photochromic coating sprayed on the surface of an external rubber layer and a bright oil layer outside the photochromic coating.
The preparation raw materials of the photochromic coating comprise the following components in parts by weight:
97 parts of PC resin, 1 part of antioxidant 1010, 0.5 part of auxiliary antioxidant DSTP, 0.5 part of light stabilizer UV-327 and 1 part of photochromic agent.
The preparation method comprises the following steps:
(1) Preparation of photochromic agent
3 parts by weight of methyl methacrylate monomer and 3 parts by weight of acrylic acid are taken and added into anhydrous tetrahydrofuran, and the mixture is stirred uniformly. 0.3 part by weight of azodiisobutyronitrile is added in the nitrogen atmosphere, stirred, heated to 70 ℃ for reaction for 20 hours, 3 parts by weight of spiropyran compound with carboxyl is added, and the reaction is continued for 20 hours. Deionized water is added, filtered and dried.
(2) Mixing PC resin, an antioxidant, an auxiliary antioxidant, a light stabilizer and a photochromic agent, and extruding and granulating by a double-screw machine to obtain a photochromic coating master batch;
(3) Spraying the photochromic coating master batch on the surface of an external rubber layer of the integrated full rubber boot of the boot body, the sole and the heel to form a photochromic coating;
(4) And (3) spraying a bright oil layer outside the photochromic coating to obtain the photochromic fashionable rubber boot.
Example 2
A photochromic fashion rubber boot comprises a boot body, a sole, a heel, a photochromic coating sprayed on the surface of an external rubber layer and a bright oil layer outside the photochromic coating.
The preparation raw materials of the photochromic coating comprise the following components in parts by weight:
97.2 parts of PC resin, 1010 parts of antioxidant, 0.4 part of auxiliary antioxidant DSTP, 0.4 part of light stabilizer UV-327 and 1 part of photochromic agent.
The preparation method comprises the following steps:
(1) Preparation of photochromic agent
3 parts by weight of methyl methacrylate monomer and 3 parts by weight of acrylic acid are taken and added into anhydrous tetrahydrofuran, and the mixture is stirred uniformly. 0.3 part by weight of azodiisobutyronitrile is added in the nitrogen atmosphere, stirred, heated to 70 ℃ for reaction for 20 hours, 3 parts by weight of spiropyran compound with carboxyl is added, and the reaction is continued for 20 hours. Deionized water is added, filtered and dried.
(2) Mixing PC resin, an antioxidant, an auxiliary antioxidant, a light stabilizer and a photochromic agent, and extruding and granulating by a double-screw machine to obtain a photochromic coating master batch;
(3) Spraying the photochromic coating master batch on the surface of an external rubber layer of the integrated full rubber boot of the boot body, the sole and the heel to form a photochromic coating;
(4) And (3) spraying a bright oil layer outside the photochromic coating to obtain the photochromic fashionable rubber boot.
Example 3
A photochromic fashion rubber boot comprises a boot body, a sole, a heel, a photochromic coating sprayed on the surface of an external rubber layer and a bright oil layer outside the photochromic coating.
The preparation raw materials of the photochromic coating comprise the following components in parts by weight:
96.6 parts of PC resin, 1010 parts of antioxidant, 0.7 part of auxiliary antioxidant DSTP, 0.7 part of light stabilizer UV-327 and 1 part of photochromic agent.
The preparation method comprises the following steps:
(1) Preparation of photochromic agent
3 parts by weight of methyl methacrylate monomer and 3 parts by weight of acrylic acid are taken and added into anhydrous tetrahydrofuran, and the mixture is stirred uniformly. 0.3 part by weight of azodiisobutyronitrile is added in the nitrogen atmosphere, stirred, heated to 70 ℃ for reaction for 20 hours, 3 parts by weight of spiropyran compound with carboxyl is added, and the reaction is continued for 20 hours. Deionized water is added, filtered and dried.
(2) Mixing PC resin, an antioxidant, an auxiliary antioxidant, a light stabilizer and a photochromic agent, and extruding and granulating by a double-screw machine to obtain a photochromic coating master batch;
(3) Spraying the photochromic coating master batch on the surface of an external rubber layer of the integrated full rubber boot of the boot body, the sole and the heel to form a photochromic coating;
(4) And (3) spraying a bright oil layer outside the photochromic coating to obtain the photochromic fashionable rubber boot.
Example 4
A photochromic fashion rubber boot comprises a boot body, a sole, a heel, a photochromic coating sprayed on the surface of an external rubber layer and a bright oil layer outside the photochromic coating.
The preparation raw materials of the photochromic coating comprise the following components in parts by weight:
97 parts of PC resin, 1 part of antioxidant 1010, 0.5 part of auxiliary antioxidant DSTP, 0.5 part of light stabilizer UV-327 and 1 part of photochromic agent.
The preparation method comprises the following steps:
(1) Preparation of photochromic agent
4 parts by weight of methyl methacrylate monomer and 2 parts by weight of acrylic acid are taken and added into anhydrous tetrahydrofuran, and the mixture is stirred uniformly. 0.3 part by weight of azodiisobutyronitrile is added in a nitrogen atmosphere, stirred, heated to 75 ℃ for reaction for 16 hours, 3 parts by weight of spiropyran compound with carboxyl is added, and the reaction is continued for 16 hours. Deionized water is added, filtered and dried.
(2) Mixing PC resin, an antioxidant, an auxiliary antioxidant, a light stabilizer and a photochromic agent, and extruding and granulating by a double-screw machine to obtain a photochromic coating master batch;
(3) Spraying the photochromic coating master batch on the surface of an external rubber layer of the integrated full rubber boot of the boot body, the sole and the heel to form a photochromic coating;
(4) And (3) spraying a bright oil layer outside the photochromic coating to obtain the photochromic fashionable rubber boot.
Example 5
A photochromic fashion rubber boot comprises a boot body, a sole, a heel, a photochromic coating sprayed on the surface of an external rubber layer and a bright oil layer outside the photochromic coating.
The preparation raw materials of the photochromic coating comprise the following components in parts by weight:
97 parts of PC resin, 1 part of antioxidant 1010, 0.5 part of auxiliary antioxidant DSTP, 0.5 part of light stabilizer UV-327 and 1 part of photochromic agent.
The preparation method comprises the following steps:
(1) Preparation of photochromic agent
2 parts by weight of methyl methacrylate monomer and 4 parts by weight of acrylic acid are taken and added into anhydrous tetrahydrofuran, and the mixture is stirred uniformly. 0.3 part by weight of azodiisobutyronitrile is added in a nitrogen atmosphere, stirred, heated to 65 ℃ and reacted for 28 hours, 3 parts by weight of spiropyran compound with carboxyl is added, and the reaction is continued for 28 hours. Deionized water is added, filtered and dried.
(2) Mixing PC resin, an antioxidant, an auxiliary antioxidant, a light stabilizer and a photochromic agent, and extruding and granulating by a double-screw machine to obtain a photochromic coating master batch;
(3) Spraying the photochromic coating master batch on the surface of an external rubber layer of the integrated full rubber boot of the boot body, the sole and the heel to form a photochromic coating;
(4) And (3) spraying a bright oil layer outside the photochromic coating to obtain the photochromic fashionable rubber boot.
Comparative example 1
The difference from example 1 is that the spiropyran compound with carboxyl group, which is added directly in the content of the photochromic agent, is supplemented with the missing weight by PC resin without the preparation step of the photochromic agent.
Comparative example 2
The difference from example 1 is that no secondary antioxidant is included, and the missing weight is supplemented with antioxidant, i.e. only 1.5 parts of antioxidant is included, no secondary antioxidant is included.
Experimental example
The photochromic coating master batches obtained in examples and comparative examples were formed into films, and LED (brightness 2000 CD/square meter) was continuously irradiated for 10day at 30 ℃ to determine initial light transmittance and light transmittance after treatment, respectively, and relative light transmittance (%) =light transmittance after treatment/initial light transmittance×100%, and the results are shown in table 1.
TABLE 1 influence on long-term light transmittance stability
| Relative light transmittance% | |
| Example 1 | 97.5 |
| Example 2 | 95.9 |
| Example 3 | 98.3 |
| Example 4 | 88.0 |
| Example 5 | 85.3 |
| Comparative example 1 | 77.4 |
| Comparative example 2 | 81.2 |
The results show that the relative light transmittance of examples 1-5 is significantly better than that of comparative examples 1 and 2, indicating the significant impact of the preparation method of the photochromic agent of the present invention and the stability of the light transmittance of the photochromic coating by the antioxidant, auxiliary antioxidant and light stabilizer.
The results show that the relative light transmittance of examples 1-3 is not significantly different, but is significantly better than that of examples 4 and 5, indicating the specific effect of the preparation method of the photochromic agent of the present invention, i.e., the significant effect of the different contents of the components on the stability of light transmittance.
While the preferred embodiments and examples of the present invention have been described in detail, the present invention is not limited to the above-described embodiments and examples, and various changes may be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (9)
1. The photochromic fashion rubber boot comprises a photochromic coating sprayed on the surface of an external rubber layer, and is characterized in that the photochromic coating comprises the following raw materials in parts by weight:
90-100 parts of resin, 0.5-3 parts of antioxidant, 0.1-1 part of auxiliary antioxidant, 0.1-1 part of light stabilizer and 0.5-3 parts of photochromic agent;
the antioxidant is antioxidant 1010;
the auxiliary antioxidant is an auxiliary antioxidant DSTP;
the preparation method of the photochromic agent comprises the following steps:
s11, dissolving a monomer of methyl methacrylate and acrylic acid in a solvent;
s12, adding azodiisobutyronitrile in a nitrogen atmosphere for reaction;
s13, adding a spiropyran compound with carboxyl, and continuing the reaction;
s14, adding deionized water, filtering and drying.
2. The photochromic fashion boot of claim 1 wherein the resin is a PC resin;
and/or, the light stabilizer is a light stabilizer UV-327;
and/or the photochromic agent comprises a spiropyran compound with carboxyl.
3. The photochromic fashion boot according to claim 1 or 2, wherein in S11, the solvent is anhydrous tetrahydrofuran;
and/or, in S12, reacting for 15-25h at 65-75 ℃;
and/or, in S13, reacting for 15-25h at 65-75 ℃.
4. The photochromic fashion boot according to claim 1 or 2, wherein the weight ratio of the monomer of methyl methacrylate, acrylic acid, azobisisobutyronitrile and the spiropyran compound with carboxyl group is (2-4): (2-4): (0.2-0.4): (2.5-3.5).
5. The photochromic fashion boot of claim 4 wherein the weight ratio of monomers of methyl methacrylate, acrylic acid, azobisisobutyronitrile and the carboxyl group bearing spiropyran compound is (3:3:0.3:3).
6. The photochromic fashion rubber boot according to claim 1 or 2, wherein the raw materials for preparing the photochromic coating comprise the following components in parts by weight:
96.6-97.2 parts of PC resin, 1 part of antioxidant, 0.4-0.7 part of auxiliary antioxidant DSTP, 0.4-0.7 part of light stabilizer and 1 part of spiropyran compound with carboxyl.
7. The photochromic fashion rubber boot of claim 1 or 2 wherein the outer rubber layer is an integrally formed outer rubber layer of a full rubber boot of a boot body, sole, heel.
8. The photochromic fashion boot of claim 1 or 2 further comprising a glossy layer over the photochromic coating.
9. A method of making a photochromic fashion boot according to any one of claims 1 to 8, comprising the steps of:
s01, preparing a photochromic agent;
s02, mixing resin, an antioxidant, an auxiliary antioxidant, a light stabilizer and a photochromic agent, and extruding and granulating by a double-screw extruder to obtain a photochromic coating master batch;
s03, spraying the photochromic coating master batch on the surface of an external rubber layer of the integrated full rubber boot of the boot body, the sole and the heel to form a photochromic coating;
and optionally, S04, spraying a bright oil layer outside the photochromic coating to obtain the photochromic fashion rubber boot.
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| KR20160127900A (en) * | 2015-04-27 | 2016-11-07 | (주)디와이엠 | Resin composition of photochromic film, Photochromic film and Photochromic lenz |
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| CN107778510A (en) * | 2017-11-10 | 2018-03-09 | 江苏视客新材料股份有限公司 | Spiro-pyrans class photochromic optical material and preparation method thereof |
| CN109942861A (en) * | 2019-03-12 | 2019-06-28 | 无锡创彩光学材料有限公司 | A kind of photochromic composite membrane of flexibility and preparation method thereof |
| CN113832717A (en) * | 2021-11-04 | 2021-12-24 | 武汉纺织大学 | Novel spiropyran photochromic cotton fabric and preparation method thereof |
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2022
- 2022-12-01 CN CN202211544117.7A patent/CN115746367B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101704921A (en) * | 2008-06-27 | 2010-05-12 | 上海金发科技发展有限公司 | Method for synthesizing spiropyran polymers |
| KR20160127900A (en) * | 2015-04-27 | 2016-11-07 | (주)디와이엠 | Resin composition of photochromic film, Photochromic film and Photochromic lenz |
| CN105970625A (en) * | 2016-05-20 | 2016-09-28 | 广州鼎昊纺织品有限公司 | Photochromic spun silk and fabric and preparation method of photochromic spun silk |
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| CN113832717A (en) * | 2021-11-04 | 2021-12-24 | 武汉纺织大学 | Novel spiropyran photochromic cotton fabric and preparation method thereof |
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