CN112516933A - Humidity-sensitive color-changing microcapsule, preparation method and application - Google Patents
Humidity-sensitive color-changing microcapsule, preparation method and application Download PDFInfo
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- CN112516933A CN112516933A CN202011043985.8A CN202011043985A CN112516933A CN 112516933 A CN112516933 A CN 112516933A CN 202011043985 A CN202011043985 A CN 202011043985A CN 112516933 A CN112516933 A CN 112516933A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/423—Amino-aldehyde resins
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Color Printing (AREA)
Abstract
The invention discloses a humidity-sensitive color-changing microcapsule and a preparation method thereof, wherein the preparation method comprises the following steps: step one, mixing allochroic silica gel coated with an organic liquid layer with an emulsifier aqueous solution; step two, adding a high molecular weight water-soluble prepolymer containing urea and formaldehyde and a low molecular weight water-soluble prepolymer into the mixed solution obtained in the step one; reacting at 45-55 deg.c for 2-3 hr to obtain microcapsule; step three, soaking the microcapsule prepared in the step three in ethanol, and forming holes on the side wall of the capsule; washing and drying the microcapsule with the holes to obtain a target product; the invention prepares the color-changing microcapsule with a core-shell structure when encountering moisture by matching the raw materials, the shell layer of the microcapsule has holes, the color-changing sensitivity is high, and the microcapsule can be repeatedly used.
Description
Technical Field
The invention relates to the technical field of humidity-sensitive color change, in particular to a humidity-sensitive color change microcapsule and a preparation method thereof.
Background
Microcapsules are micro-containers having a core-shell structure formed by coating a dispersible solid, liquid or gas with a film-forming material, and a coating film formed of the film-forming material is generally referred to as a wall material or a wall (generally, formed of a natural or synthetic polymer material), and a substance coated inside the film-forming material is referred to as a core material or a capsule core. The size and shape of the microcapsules can vary widely depending on the manufacturing process. Microcapsules are typically in the size range of 2 to 1000 μm, with capsules less than 1 μm in diameter being referred to as nanocapsules and capsules greater than 1000 μm in diameter being referred to as macrocapsules. The thickness of the capsule wall is 0.2-10 μm, and the proportion of the capsule core in the total mass of the microcapsule is also 20-95%. With the development of microcapsule technology, nanocapsules with a particle size of 1 to 1000nm have been prepared. Microencapsulation refers to the application of tiny solid particles, droplets, or bubbles with a coating film or shell material. The shape of the solid particle-containing microcapsules almost corresponds to the shape of the solid in the capsules, and the liquid or gas-containing microcapsules are generally spherical in shape. The microcapsule is composed of a coated material and a wrapping material. The material enclosed within is generally referred to as the active, active agent, core material, internal phase, core, payload, or filler. The encapsulating material, commonly referred to as a wall, carrier, shell, coating or membrane, may be an organic polymer, hydrosol, sugar, wax, fat, metal or inorganic oxide, or the like.
In the prior art, moisture-sensitive color change is used in textile technology, and moisture-sensitive dye is finished on textile in a printing and dyeing processing mode. The principle of humidity-sensitive color change is that the structure of the humidity-sensitive color change dye can change along with the change of the humidity in the environment, so that the absorption spectrum of visible light is changed, the final color is influenced, the humidity-sensitive color change material is complex, the repeated color change effect is poor, and the application of the color change fiber is limited.
Disclosure of Invention
The invention aims to provide a preparation method of a humidity-sensitive color-changing microcapsule, which prepares a color-changing microcapsule with a core-shell structure by matching raw materials, wherein the shell layer of the microcapsule has holes, the color-changing sensitivity is high, and the microcapsule can be repeatedly used.
In order to solve the technical problem, the technical scheme of the invention is as follows: a preparation method of humidity-sensitive color-changing microcapsules comprises the following steps:
step one, mixing allochroic silica gel coated with an organic liquid layer with an emulsifier aqueous solution;
step two, adding a high molecular weight water-soluble prepolymer containing urea and formaldehyde and a low molecular weight water-soluble prepolymer into the mixed solution obtained in the step one;
reacting at 45-55 deg.c for 2-3 hr to obtain microcapsule;
step three, soaking the microcapsule prepared in the step three in ethanol, and forming holes on the side wall of the capsule;
and washing and drying the microcapsule with the holes to obtain the target product.
Preferably, the organic liquid layer in the step one is vegetable oil or glycerol. According to the invention, the organic liquid layer covering the surface of the color-changing silica gel ball is beneficial to leaving a gap between the color-changing silica gel particles and the urea resin, is beneficial to the inlet and outlet of water, and simultaneously ensures the stability of the color-changing silica gel in the preparation process.
Preferably, the prepolymer in the second step comprises a high molecular weight water-soluble prepolymer and a low molecular weight water-soluble prepolymer;
mixing 8 parts of urea, 24 parts of 37% formaldehyde solution and 50 parts of deionized water according to the mass parts of the high-molecular prepolymer, adjusting the pH value of a reaction system to 9, and carrying out constant-temperature reaction under stirring to obtain a high-molecular water-soluble prepolymer;
and mixing 0.5 part of urea, 1.6 parts of 37% formaldehyde solution and 50 parts of deionized water according to the mass parts of the low-molecular-weight water-soluble prepolymer, adjusting the pH value of a reaction system to 9, and carrying out constant-temperature reaction under stirring to obtain the low-molecular-weight water-soluble prepolymer. The shell structure formed by mixing the prepolymers with two molecular weights has urea-formaldehyde resins with two molecular weights, and the urea-formaldehyde resin with low molecular weight is dissolved in ethanol, so that the urea-formaldehyde resin of the high-molecular prepolymer is left in the shell structure, and the urea-formaldehyde resin with low molecular weight is removed, so that the side wall of the shell structure is provided with holes, the contact between the color-changing silica gel as a core and the moisture of the external environment is facilitated, the color-changing sensitivity of the color-changing silica gel is high, and meanwhile, part of the color-changing silica gel is exposed from the holes of the shell, and the observation.
Preferably, the regulating substances of the pH values of the high molecular weight water-soluble prepolymer and the low molecular weight water-soluble prepolymer system are triethanolamine; the invention uses triethanolamine to adjust the pH value of the system, is beneficial to improving the structural strength of the microcapsule and is beneficial to the application of the humidity-sensitive color-changing microcapsule in the textile field.
Preferably, the mass ratio of the high molecular weight water-soluble prepolymer to the low molecular weight water-soluble prepolymer is 1:4 to 1: 2. The invention effectively ensures the proportion of holes on the surface of the shell and ensures the sensitivity of color change when encountering moisture by controlling the dosage of the high molecular weight water-soluble prepolymer and the low molecular weight water-soluble prepolymer.
Preferably, the high molecular weight water-soluble prepolymer solution also comprises a coupling agent, wherein the coupling agent is KH550 or KH 560; the mass of the coupling agent is 5-10% of the mass of the high molecular weight water-soluble prepolymer solution. The presence of the coupling agent in the invention is beneficial to the roughness of the side wall surface of the shell structure, the grafting of the microcapsule and the fiber, and the color change function and the washability of the prepared fiber. Further preferably, the coupling agent is KH550 or KH 560. The two coupling agents which are optimized in the invention are effectively adsorbed or grafted on the surface of the shell structure, so that the combination and connection with the fiber are facilitated.
Preferably, the high molecular weight water-soluble prepolymer further comprises 0.5 to 1.5 parts by mass of melamine. The melamine with the amount is added into the high-molecular-weight water-soluble prepolymer, so that the structural strength of urea-formaldehyde resin formed by polycondensation of the high-molecular-weight water-soluble prepolymer is effectively improved, and a film layer formed by dissolving the low-molecular-weight prepolymer in ethanol is dissolved in the ethanol to form a hole structure with a clear structure.
Preferably, the emulsifier is sodium dodecyl sulfate, and the mass of the emulsifier is 3 to 7 percent of that of the high molecular weight water-soluble prepolymer solution. According to the invention, the emulsifier is matched with the melamine to effectively improve the strength and the wear resistance of the reticular shell structure formed by the high molecular weight prepolymer.
The second purpose of the invention is to provide a humidity-sensitive color-changing microcapsule, the color-changing silica gel and urea resin form a core-shell structure, the sensitivity of color change is high when meeting water, and the repeatability is good.
In order to solve the technical problem, the technical scheme of the invention is as follows: the humidity-sensitive color-changing microcapsule is a core-shell structure formed by color-changing silica gel and urea resin, a gap is formed between the color-changing silica gel coated by the urea resin and the urea resin, and the urea resin layer is provided with holes for water to enter and exit.
It is a third object of the present invention to provide the use of moisture sensitive color-changing microcapsules in textiles.
By adopting the technical scheme, the invention has the beneficial effects that:
1. the shell layer of the urea-formaldehyde resin is formed by polycondensation of two prepolymers with different molecular weights on the surfaces of the allochroic silica gel particles coated with the organic liquid layer; urea-formaldehyde resin with small molecular weight and an organic liquid layer wrapped in the shell are contacted with ethanol and dissolved in the ethanol to form gaps between the color-changing particles and the shell layer, and holes of the shell layer are also formed;
2. the moisture-sensitive color-changing microcapsule prepared by the invention has rich shell hole structure, is beneficial to quickly transferring external water to the color-changing silica gel, and the color-changing silica gel changes color after contacting water, thereby improving the color-changing sensitivity and color development degree;
3. the humidity-sensitive color-changing capsule prepared by the invention is suitable for being attached to the surface of textile fibers or the surface of textiles, effectively indicates the dry and wet conditions of products, and is beneficial to judging the dry and wet conditions of the products in actual use by people.
Thereby achieving the above object of the present invention.
Drawings
FIG. 1 is a schematic diagram of a humidity-sensitive color-changing microcapsule preparation route according to the present invention.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
Example 1
The invention discloses a humidity-sensitive color-changing microcapsule and a preparation method thereof, wherein the specific synthetic route is shown in figure 1, and the preparation method comprises the following steps:
step one, mixing allochroic silica gel coated with an organic liquid layer with an emulsifier aqueous solution;
the organic liquid layer in the first step is vegetable oil or glycerol; the mass ratio of the organic liquid layer to the allochroic silica gel is shown in table 1.
The emulsifier is sodium dodecyl sulfate, and the dosage of the sodium dodecyl sulfate is shown in table 1.
Step two, adding a high molecular weight water-soluble prepolymer containing urea and formaldehyde and a low molecular weight water-soluble prepolymer into the mixed solution obtained in the step one;
mixing 8 parts of urea, 24 parts of 37% formaldehyde solution and 50 parts of deionized water according to the mass parts of the high-molecular prepolymer, adjusting the pH value of a reaction system to 9 by using triethanolamine, and carrying out constant-temperature reaction under stirring to obtain a high-molecular water-soluble prepolymer;
mixing 0.5 part of urea, 1.6 parts of 37% formaldehyde solution and 50 parts of deionized water according to the mass parts of the low-molecular-weight water-soluble prepolymer, adjusting the pH value of a reaction system to 9 by using triethanolamine, and carrying out constant-temperature reaction under stirring to obtain the low-molecular-weight water-soluble prepolymer;
the mass ratio of the high molecular weight water-soluble prepolymer to the low molecular weight water-soluble prepolymer is shown in Table 1.
Preferably, the high molecular weight water-soluble prepolymer further comprises melamine in parts by weight as listed in table 1.
Preferably, the high molecular weight water-soluble prepolymer solution also comprises a coupling agent, and the coupling agent is KH550 or KH 560; the mass of the coupling agent is 5-10% of the mass of the high molecular weight water-soluble prepolymer solution.
Reacting at 45-55 deg.c for 2-3 hr to obtain microcapsule;
step three, soaking the microcapsule prepared in the step three in ethanol, and forming holes on the side wall of the capsule;
the microcapsule with holes is cleaned and dried to obtain the discoloring silica gel and the urea-formaldehyde resin to form a core-shell structure, and the discoloring sensitivity is high when the microcapsule meets water, and the repeatability is good.
The moisture-sensitive color-changing capsules prepared by the method are adhered to the surface of a textile, and are subjected to the test of rubbing color fastness, washing fastness, moisture-sensitive color-changing performance and washing fastness times, and specific test data are shown in table 2 in detail.
The humidity sensitivity test method is as follows:
measuring the initial weight of the dried square textile with the area of 5cm by 5cm, spraying water to the textile, comparing the textile with a corresponding color card when the textile is changed from the initial blue color to standard blue with fixed chroma (CMYK: C40; M0; Y10; K0), measuring the weight of the textile, calculating the water consumption for color change, and drying the textile after color change to observe the reversible state of the color change.
Example 2
The main differences between the present example and example 1 are detailed in table 1, the moisture-sensitive color-changing microcapsules prepared in the present example are prepared into textiles by the same method as in example 1, the specific performance tests are the same as in example 1, and the test results are detailed in table 2.
Example 3
The main differences between the present example and example 1 are detailed in table 1, the moisture-sensitive color-changing microcapsules prepared in the present example are prepared into textiles by the same method as in example 1, the specific performance tests are the same as in example 1, and the test results are detailed in table 2.
Example 4
The main differences between the present example and example 1 are detailed in table 1, the moisture-sensitive color-changing microcapsules prepared in the present example are prepared into textiles by the same method as in example 1, the specific performance tests are the same as in example 1, and the test results are detailed in table 2.
Example 5
The main differences between the present example and example 1 are detailed in table 1, the moisture-sensitive color-changing microcapsules prepared in the present example are prepared into textiles by the same method as in example 1, the specific performance tests are the same as in example 1, and the test results are detailed in table 2.
Example 6
The main differences between the present example and example 1 are detailed in table 1, the moisture-sensitive color-changing microcapsules prepared in the present example are prepared into textiles by the same method as in example 1, the specific performance tests are the same as in example 1, and the test results are detailed in table 2.
Comparative example
In this example, the same amount of the allochroic silicagel particles as in example 1 was loaded on the surface of the textile, and the textile thus obtained was prepared into a 5cm by 5cm textile, and the performance test thereof was the same as in example 1, and the specific test results are detailed in table 2.
Table 1 amounts of each of the materials used in examples 1 to 6
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Mass ratio of organic liquid to allochroic silicagel | 1:3 | 1:3 | 1:4 | 1:5 | 1:4 | 1:5 |
| The mass percentage of the emulsifier in the high molecular weight prepolymer | 3％ | 5％ | 7％ | 7％ | 5％ | 3％ |
| Mass ratio of high molecular weight prepolymer to low molecular weight prepolymer | 1:2 | 1:3 | 1:4 | 1:4 | 1:3 | 1:2 |
| Mass fraction of melamine | / | 0.5 | 0.8 | 1.0 | 1.2 | 1.5 |
| The coupling agent accounts for the mass percent of the high molecular weight prepolymer | / | / | 5％ | 8％ | 10％ | / |
TABLE 2 Performance test cases for moisture sensitive color-changing textiles obtained in examples 1 to 6 and comparative example
The data in tables 1 and 2 show that the humidity-sensitive color-changing microcapsule prepared by the invention has a shell-core structure with abundant holes, so that a channel for the color-changing silica gel to contact with water is effectively ensured, and the color change of the color-changing silica gel coated with the microcapsule can be effectively displayed through the holes after the color-changing silica gel absorbs water, so that the color-changing microcapsule prepared by the invention has high color-changing sensitivity and can be compared favorably with the color-changing silica gel directly loaded on textiles; however, the shell structure of the color-changing microcapsule prepared by the invention effectively surrounds and protects the color-changing silica gel and effectively improves the connection strength between the color-changing microcapsule and textile fibers from the washing times, and the textile loaded with the humidity-sensitive color-changing microcapsule has better friction color fastness and washing color fastness, and the reversible humidity-sensitive color change and the water amount for realizing the humidity-sensitive color change can be seen.
The above embodiments and drawings are not intended to limit the form and style of the present invention, and any suitable changes or modifications thereof by those skilled in the art should be considered as not departing from the scope of the present invention.
Claims (10)
1. A preparation method of humidity-sensitive color-changing microcapsules is characterized in that:
the method comprises the following steps:
step one, mixing allochroic silica gel coated with an organic liquid layer with an emulsifier aqueous solution;
step two, adding a high molecular weight water-soluble prepolymer containing urea and formaldehyde and a low molecular weight water-soluble prepolymer into the mixed solution obtained in the step one;
reacting at 45-55 deg.c for 2-3 hr to obtain microcapsule;
step three, soaking the microcapsule prepared in the step three in ethanol, and forming holes on the side wall of the capsule;
and washing and drying the microcapsule with the holes to obtain the target product.
2. The method for preparing moisture-sensitive color-changing microcapsules according to claim 1, wherein: the organic liquid layer in the first step is vegetable oil or glycerol.
3. The method for preparing moisture-sensitive color-changing microcapsules according to claim 1, wherein: the prepolymer in the second step comprises a high molecular weight water-soluble prepolymer and a low molecular weight water-soluble prepolymer;
mixing 8 parts of urea, 24 parts of 37% formaldehyde solution and 50 parts of deionized water according to the mass parts of the high-molecular prepolymer, adjusting the pH value of a reaction system to 9, and carrying out constant-temperature reaction under stirring to obtain a high-molecular water-soluble prepolymer;
and mixing 0.5 part of urea, 1.6 parts of 37% formaldehyde solution and 50 parts of deionized water according to the mass parts of the low-molecular-weight water-soluble prepolymer, adjusting the pH value of a reaction system to 9, and carrying out constant-temperature reaction under stirring to obtain the low-molecular-weight water-soluble prepolymer.
4. The process for preparing moisture-sensitive color-changing microcapsules according to claim 3, wherein: the regulating substance of the pH value of the high molecular weight water-soluble prepolymer and the low molecular weight water-soluble prepolymer system is triethanolamine.
5. The process for preparing moisture-sensitive color-changing microcapsules according to claim 3, wherein: the mass ratio of the high molecular weight water-soluble prepolymer to the low molecular weight water-soluble prepolymer is 1:4 to 1: 2.
6. The method for preparing moisture-sensitive color-changing microcapsules according to claim 1, wherein: the high molecular weight water-soluble prepolymer solution also comprises a coupling agent, wherein the coupling agent is KH550 or KH 560; the mass of the coupling agent is 5-10% of the mass of the high molecular weight water-soluble prepolymer solution.
7. The method for preparing moisture-sensitive color-changing microcapsules according to claim 6, wherein the method comprises the following steps: the high molecular weight water-soluble prepolymer also comprises 0.5 to 1.5 parts by weight of melamine.
8. The method for preparing moisture-sensitive color-changing microcapsules according to claim 7, wherein: the emulsifier is sodium dodecyl sulfate, and the mass of the emulsifier is 3-7% of that of the high molecular weight water-soluble prepolymer solution.
9. A moisture-sensitive color-changing microcapsule according to any one of claims 1 to 8, characterized in that: the microcapsule is a core-shell structure formed by the color-changing silica gel and the urea-formaldehyde resin, a gap is formed between the color-changing silica gel coated by the urea-formaldehyde resin and the urea-formaldehyde resin, and the urea-formaldehyde resin layer is provided with holes for water to enter and exit.
10. Applying the moisture-sensitive color-changing microcapsules of claim 9 to a textile.
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| CN113713727A (en) * | 2021-06-07 | 2021-11-30 | 江南大学 | Humidity-sensitive color-changing microcapsule and preparation method and application thereof |
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| CN113713727A (en) * | 2021-06-07 | 2021-11-30 | 江南大学 | Humidity-sensitive color-changing microcapsule and preparation method and application thereof |
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