CN112354493B - pH value sensitive microcapsule, preparation method and application - Google Patents
pH value sensitive microcapsule, preparation method and application Download PDFInfo
- Publication number
- CN112354493B CN112354493B CN202011041552.9A CN202011041552A CN112354493B CN 112354493 B CN112354493 B CN 112354493B CN 202011041552 A CN202011041552 A CN 202011041552A CN 112354493 B CN112354493 B CN 112354493B
- Authority
- CN
- China
- Prior art keywords
- sensitive
- value
- microcapsule
- molecular weight
- soluble prepolymer
- 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
Images
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a preparation method of a pH value sensitive microcapsule, which comprises the following steps: mixing pH value sensitive silica gel coated with an organic liquid layer and provided with a primary pore channel 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 two in ethanol, and dissolving the low molecular weight urea-formaldehyde resin into a secondary pore channel; cleaning and drying the microcapsule with the composite holes to obtain a target product; the invention also discloses the application of the pH value sensitive microcapsule; the pH value sensitive microcapsule with a composite structure is prepared by matching raw materials and a preparation process, and is sensitive to pH discoloration and stable in structure; the dye has obvious indication effect on acidity when being applied to textiles, and simultaneously, the rubbing color fastness and the washing fastness accord with corresponding national standards.
Description
Technical Field
The invention relates to the technical field of intelligent textiles, in particular to a pH value sensitive microcapsule, a preparation method and application.
Background
In daily life, the fabric needs to be crossed with textile products such as towels, bathroom ground mats and the like every day, and bacteria are easy to breed in an acidic and humid environment. The invention discloses a preparation method of a pH value color-changing fabric with application publication number CN 103590263A, which is specially used for preparing a dye solution by using a pH indicator dye and distilled water, and then accurately measuring and diluting the required dye solution to obtain a dye bath; squeezing the bleached cotton fabric wetted in water to dry, and immersing the cotton fabric into the dye bath to start dyeing; dyeing cotton fabric by using a water bath constant temperature oscillator, dyeing the fabric at 40 ℃, keeping the temperature for 30min after the temperature reaches 90 ℃, and then cooling to the normal temperature; after dyeing is finished, drying the cotton fabric after washing and soaping to obtain dyed cotton fabric; and soaking the dyed cotton fabric in a pH buffer solution to obtain the pH value color-changing fabric. The preparation process is simple and convenient, and the cost is low; according to the technical scheme, the pH indicator dye is directly impregnated in the textile, and the color change indicating effect of the pH indicator dye is difficult to maintain along with use and cleaning.
Disclosure of Invention
The invention aims to provide a preparation method of a pH value sensitive microcapsule, which prepares the pH value sensitive microcapsule with a composite structure by matching raw materials and a preparation process, and the pH value sensitive microcapsule is sensitive to pH discoloration and stable in structure.
In order to solve the technical problem, the technical scheme of the invention is as follows: a preparation method of a pH value sensitive microcapsule comprises the following steps:
step one, mixing pH value sensitive silica gel coated with an organic liquid layer and provided with a primary pore canal 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 two in ethanol, and dissolving the low molecular weight urea-formaldehyde resin into a secondary pore channel;
and cleaning and drying the microcapsule with the composite holes to obtain a target product.
Preferably, the preparation method of the pH-sensitive silica gel comprises the following steps:
s1 preparation of silica hydrosol
Stirring and mixing ethyl orthosilicate, carnation safflower pigment, absolute ethyl alcohol and deionized water to obtain yellow silicon dioxide hydrosol;
s2, adjusting the pH value of the yellow silicon dioxide hydrosol to 2;
s3, continuously adding the low-molecular-weight water-soluble prepolymer into the mixed solution of S2 under the stirring condition, and reacting to obtain a precipitate;
and S4, repeatedly washing the precipitate prepared in the S3 with ethanol and deionized water until the precipitate is colorless, and dissolving the low-molecular-weight urea-formaldehyde resin in the silicon dioxide precipitate to obtain the pH value sensitive silica gel particles with the primary pore channels. The carnation safflower pigment is used as a pH value color change indicator of silicon dioxide particles, is sensitive to an acid environment, and has the following color change along with the change of the pH value of the environment:
carnation safflower pigment reacts with acid to form a stable salt which is red, and the pH value is increased to form a colorless chromene derivative. Anthocyanidin is unstable under alkaline condition, easily discolors, and shows yellow color when combined with flavonoids (colorless in acid and yellow in alkaline). Compared with carnation safflower pigment, the carnation safflower pigment has the advantages of obviously improved safety of inorganic salt with color, rich color change and suitability for compounding with dye.
Preferably, the organic liquid layer in the step one is vegetable oil or glycerol. According to the invention, the organic liquid layer covering the surfaces of the pH value sensitive silica gel particles is beneficial to leaving a gap between the pH value sensitive silica gel particles and the urea-formaldehyde resin, so that the moisture can enter and exit, and meanwhile, the stability of the pH value sensitive silica gel particles in the preparation process is ensured, the organic liquid layer coated on the surfaces of the pH value sensitive silica gel particles is cleaned in the washing process of the step three, and the preparation process is simple.
Preferably, the high-molecular water-soluble prepolymer is prepared by mixing 8 parts of urea, 24 parts of 37% formaldehyde solution and 50 parts of deionized water in parts by mass, adjusting the pH value of a reaction system to 9, and reacting at constant temperature under stirring;
according to the mass parts of the low-molecular-weight water-soluble prepolymer, 0.5 part of urea, 1.6 parts of 37% formaldehyde solution and 50 parts of deionized water are mixed, the pH value of a reaction system is adjusted to 9, and the mixture is stirred and reacts at constant temperature to obtain the low-molecular-weight water-soluble prepolymer. According to the invention, two prepolymers with two molecular weights are mixed, the shell structure is provided with urea-formaldehyde resin with two molecular weights, urea-formaldehyde resin with low molecular weight is dissolved in ethanol, urea-formaldehyde resin of a high-molecular prepolymer is left in the shell structure, the urea-formaldehyde resin with low molecular weight is removed, the side wall of the shell structure is provided with holes, which is beneficial for contact of pH value sensitive silica gel particles as cores with moisture of the external environment, the pH value sensitive silica gel particles have high color change sensitivity when the pH value of the moisture in the external environment changes, and meanwhile, part of the pH value sensitive silica gel particles are exposed from the holes of the shell, so that the color change is beneficial to observation.
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 along with pH value 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 coupling agent has the advantages that the surface of the side wall of the rough shell structure is favorable for the grafting of the microcapsule and the fiber, and the prepared fiber has washing fastness while the color is changed due to the pH value. 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 secondary pore 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 invention also provides a pH value sensitive microcapsule, which is provided with a composite pore channel structure, is sensitive to pH color change and has a stable structure.
In order to solve the technical problem, the technical scheme of the invention is as follows: a pH-sensitive microcapsule comprises pH-sensitive silica gel particles and a capsule shell surrounding the pH-sensitive silica gel particles;
the pH value sensitive microcapsule has a composite pore passage structure, and the composite pore passage comprises a primary pore passage formed by dissolving urea formaldehyde of pH value sensitive silica gel particles in ethanol and a secondary pore passage formed by dissolving low molecular weight urea formaldehyde resin in ethanol in a capsule shell.
A third object of the present invention is to provide the use of pH sensitive microcapsules in textiles.
By adopting the technical scheme, the invention has the beneficial effects that:
1. the invention prepares the pH value sensitive microcapsule with a core-shell structure by matching of preparation processes, the pH value sensitive silica gel particles as the core are provided with a primary pore passage, the capsule shell which surrounds the outside of the pH value sensitive silica gel particles is provided with a secondary pore passage, and a gap obtained by dissolving an organic liquid layer in ethanol is matched between the primary pore passage and the secondary pore passage to form a water inlet and outlet passage; the pH value sensitive silica gel plays a role in indicating the pH value along with the change of the pH value of the external environment moisture;
2. according to the pH value sensitive microcapsule with the core-shell structure, the capsule shell with the hole structure effectively protects the pH value sensitive silica gel particles, the color change of the pH value sensitive silica gel particles is more sensitive, and the structure is stable;
3. the capsule shell is formed by polycondensation of two prepolymers with different molecular weights on the surfaces of pH value sensitive silica gel particles coated with an organic liquid layer to form a shell layer of urea-formaldehyde resin; urea 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 a gap between the pH value sensitive silica gel particles and the shell layer, and a hole with a clear capsule shell layer structure is also formed; the microcapsule prepared by the invention has rich pore canals, rapid water in and out of the environment and high indicating sensitivity;
4. the microcapsule provided by the invention has a composite pore channel, particularly the surface of a capsule shell has a certain roughness, so that the firm connection between the microcapsule and the surface of a textile is facilitated, and the microcapsule provided by the invention is applied to the textile so that the textile has a pH value sensitive function and effectively prompts whether the textile needs to be cleaned;
5. the pH value sensitive silica gel particles are not easy to fall off under the protection of the capsule shell, and the washability of the pH value sensitive silica gel particles is obviously improved.
Thereby achieving the above object of the present invention.
Drawings
FIG. 1 is a schematic view of the structure of the pH-sensitive microcapsules of the present invention.
In the figure:
a pH value sensitive microcapsule 4; pH sensitive silica gel particles 41; a primary duct 411; the capsule shell 42; secondary channels 421; the gap 43; the antenna 44 is connected.
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
This example discloses a method for preparing pH-sensitive microcapsules,
the method comprises the following steps:
step one, mixing pH value sensitive silica gel coated with vegetable oil or glycerin layer and provided with a primary pore canal with an emulsifier aqueous solution;
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.
The preparation method of the pH value sensitive silica gel comprises the following steps:
s1 preparation of silica hydrosol
Stirring and mixing ethyl orthosilicate, carnation safflower pigment, absolute ethyl alcohol and deionized water to obtain yellow silicon dioxide hydrosol;
s2, adjusting the pH value of the yellow silicon dioxide hydrosol to 2;
s3, continuously adding the low-molecular-weight water-soluble prepolymer into the mixed solution of S2 under the stirring condition, and reacting to obtain a precipitate;
and S4, repeatedly washing the precipitate prepared in the S3 with ethanol and deionized water until the precipitate is colorless, and dissolving the low-molecular-weight urea-formaldehyde resin in the silicon dioxide precipitate to obtain the pH value sensitive silica gel particles with the primary pore channels.
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;
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.
Mixing 8 parts of urea, 24 parts of 37% formaldehyde solution and 50 parts of deionized water according to the parts by mass of the high-molecular prepolymer, adjusting the pH value of a reaction system to 9, and reacting at constant temperature under stirring to obtain a high-molecular water-soluble prepolymer;
the solution of the high molecular weight water-soluble prepolymer also comprises a coupling agent which 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 high molecular weight water-soluble prepolymer also comprises 0.5 to 1.5 parts by weight of melamine.
According to the mass parts of the low-molecular-weight water-soluble prepolymer, 0.5 part of urea, 1.6 parts of 37% formaldehyde solution and 50 parts of deionized water are mixed, the pH value of a reaction system is adjusted to 9, and the mixture is stirred and reacts at constant temperature to obtain the low-molecular-weight water-soluble prepolymer.
Reacting at 45-55 deg.c for 2-3 hr to obtain microcapsule;
step three, soaking the microcapsule prepared in the step two in ethanol, and dissolving the low molecular weight urea-formaldehyde resin into a secondary pore channel;
and cleaning and drying the microcapsule with the composite holes to obtain a target product.
The specific amounts of each of the substances in this example are shown in Table 1.
The specific structure of the microcapsule with pH sensitivity prepared in this embodiment is shown in fig. 1, in which the microcapsule with pH sensitivity 4 includes a particle 41 of pH-sensitive silica gel and a capsule shell 42 wrapping the particle 41 of pH-sensitive silica gel; the pH value sensitive microcapsule 4 has a communicated composite pore structure; the composite pore channel structure comprises a primary pore channel 411 distributed in the pH value sensitive silica gel particles 41 and a secondary pore channel 421 uniformly distributed in the capsule shell 42. In the invention, the communication between the water in the external environment and the pH value sensitive microcapsule 4 is ensured through the matching of the primary pore 411 and the secondary pore 421, and the reliable indication of the embodiment is ensured.
The composite pore structure in this embodiment further includes a gap 43 between the pH-sensitive silica gel particle 41 and the capsule shell 42. The gap 43 is beneficial to the contact of water in the external environment with the outer surface of the pH-sensitive silica gel particle 41 from various directions and angles, and is also convenient for external water to enter the pH-sensitive silica gel particle 41 from the primary pore 411, so that the pH-sensitive silica gel particle 41 is sensitive to color change.
The exterior of the capsule shell 42 in this embodiment is grafted with a connecting antenna 44. In the embodiment, the connecting antenna 44 is arranged on the outer surface of the capsule shell 42 in a surface grafting manner, and the surface of the capsule shell 42 is roughened, so that the improvement of the connecting strength between the pH value sensitive microcapsule 4 and the textile is facilitated.
The pH-sensitive microcapsule prepared in this embodiment is adhered to the surface of a textile by an adhesive, and the test of color fastness to rubbing, color fastness to washing, pH-sensitive discoloration performance and washing times is performed on the microcapsule, and the specific test data are detailed in tables 2 and 3.
The pH value sensitive discoloration test method comprises the following steps:
measuring the initial weight of the dried square textile with the area of 5cm x 5cm, spraying water with different pH values to the square textile, changing the textile from initial colorless to fixed chroma and standard red (M100; Y60), measuring the weight of the textile, calculating the water consumption for color change, drying the textile after color change and observing the reversible state of the color change.
Example 2
The main difference between this example and example 1 is detailed in table 1, the pH-sensitive microcapsules prepared in this example are prepared into textiles by the same method as in example 1, the specific performance test is the same as in example 1, and the specific test results are detailed in tables 2 and 3.
Example 3
The main difference between this example and example 1 is detailed in table 1, the pH-sensitive microcapsules prepared in this example are prepared into textiles by the same method as in example 1, the specific performance test is the same as in example 1, and the specific test results are detailed in tables 2 and 3.
Example 4
The main difference between this example and example 1 is detailed in table 1, the pH-sensitive microcapsules prepared in this example are prepared into textiles by the same method as in example 1, the specific performance test is the same as in example 1, and the specific test results are detailed in tables 2 and 3.
Example 5
The main difference between this example and example 1 is detailed in table 1, the pH-sensitive microcapsules prepared in this example are prepared into textiles by the same method as in example 1, the specific performance test is the same as in example 1, and the specific test results are detailed in tables 2 and 3.
Example 6
The main difference between this example and example 1 is detailed in table 1, the pH-sensitive microcapsules prepared in this example are prepared into textiles by the same method as in example 1, the specific performance test is the same as in example 1, and the specific test results are detailed in tables 2 and 3.
Comparative example
In this example, a 5cm by 5cm textile was prepared by loading the textile surface with an equal amount of carnation safflower pigment as in example 1, and the performance of the textile was tested as in example 1, and the results are shown in tables 2 and 3.
Table 1 amounts of each substance (parts by weight) in examples 1 to 6
Table 2 examples 1 to 6 and comparative examples the performance test conditions for pH sensitive textiles
Table 3 amount and reversibility of examples 1 to 6 and comparative example textiles for development to the same color with aqueous solutions of different pH values
| Item | Acidic aqueous solution with pH value of 2 | Acidic aqueous solution with pH value of 3 | Acidic aqueous solution with pH value of 5 |
| Example 1 | Reversible, 0.4g/cm 2 | Reversible, 0.6g/cm 2 | Reversible, 1.2g/cm 2 |
| Example 2 | Reversible, 0.3g/cm 2 | Reversible, 0.5g/cm 2 | Reversible, 1.1g/cm 2 |
| Example 3 | Reversible, 0.3g/cm 2 | Reversible, 0.5g/cm 2 | Reversible, 1.0g/cm 2 |
| Example 4 | Reversible, 0.2g/cm 2 | Reversible, 0.4g/cm 2 | Reversible, 0.9g/cm 2 |
| Example 5 | Reversible, 0.2g/cm 2 | Reversible, 0.3g/cm 2 | The reverse-direction-changeable rubber can be used for reversing,0.9g/cm 2 |
| example 6 | Reversible, 0.3g/cm 2 | Reversible, 0.5g/cm 2 | Reversible, 1.2g/cm 2 |
| Comparative example | Reversible, 0.15g/cm 2 | Reversible, 0.2g/cm 2 | Reversible, 0.6g/cm 2 |
As can be seen from data in tables 1 to 3, the pH sensitive microcapsule with a core-shell structure is prepared by matching the preparation processes, the pH sensitive silica gel particles serving as the core have a primary pore channel, the capsule shell surrounding the pH sensitive silica gel particles has a secondary pore channel, and a gap formed by dissolving an organic liquid layer in ethanol is matched between the primary pore channel and the secondary pore channel to form a water inlet and outlet channel; the pH value sensitive silica gel plays a role in indicating the pH value of the environmental moisture along with the change of the pH value of the external environmental moisture, and the table 3 shows that the textile prepared by the method is sensitive to acidity, the sensitivity degree of the textile is almost close to that of single use of carnation safflower pigment, but the friction color fastness, the washing fastness and the washing times of the textile are all obviously improved.
The capsule shell with the hole structure of the core-shell structure of the pH value sensitive microcapsule effectively protects the pH value sensitive silica gel particles, the color change of the pH value sensitive silica gel particles is more sensitive, and the structure is stable;
the capsule shell is formed by polycondensation of two prepolymers with different molecular weights on the surfaces of pH value sensitive silica gel particles coated with an organic liquid layer to form a shell layer of urea-formaldehyde resin; 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 a gap between the pH value sensitive silica gel particle and the shell layer, and a hole with a clear capsule shell layer structure is formed at the same time; the microcapsule prepared by the invention has rich pore canals, rapid water in and out of the environment and high indicating sensitivity;
the microcapsule has a composite pore passage, particularly the surface of a capsule shell has a certain roughness, so that the microcapsule is favorably and firmly connected with the surface of a textile;
the pH value sensitive silica gel particles are not easy to fall off under the protection of the capsule shell, and the washability of the pH value sensitive silica gel particles is obviously improved.
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 (8)
1. A preparation method of pH value sensitive microcapsules applied to textiles is characterized by comprising the following steps:
the method comprises the following steps:
mixing pH value sensitive silica gel coated with an organic liquid layer and provided with a primary pore channel 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 two in ethanol, and dissolving the low molecular weight urea-formaldehyde resin into a secondary pore channel;
washing and drying the microcapsule with the composite holes to obtain a target product;
the preparation method of the pH value sensitive silica gel comprises the following steps:
s1 preparation of silica hydrosol
Stirring and mixing ethyl orthosilicate, carnation safflower pigment, absolute ethyl alcohol and deionized water to obtain yellow silicon dioxide hydrosol;
s2, adjusting the pH value of the yellow silicon dioxide hydrosol to 2;
s3, continuously adding the low-molecular-weight water-soluble prepolymer into the mixed solution of S2 under the stirring condition, and reacting to obtain a precipitate;
and S4, repeatedly washing the precipitate prepared in the S3 with ethanol and deionized water until the precipitate is colorless, and dissolving the low-molecular-weight urea-formaldehyde resin in the silicon dioxide precipitate to obtain the pH value sensitive silica gel particles with the primary pore channels.
2. The process for preparing pH-sensitive microcapsules according to claim 1, wherein: the organic liquid layer in the first step is vegetable oil or glycerol.
3. The process for preparing pH-sensitive microcapsules according to claim 1, wherein:
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;
according to the mass parts of the low-molecular-weight water-soluble prepolymer, 0.5 part of urea, 1.6 parts of 37% formaldehyde solution and 50 parts of deionized water are mixed, the pH value of a reaction system is adjusted to 9, and the mixture is stirred and reacts at constant temperature to obtain the low-molecular-weight water-soluble prepolymer.
4. A process for the preparation of microcapsules sensitive to pH according to claim 3, characterized by: 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.
5. The process for preparing pH-sensitive 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.
6. The process for preparing pH-sensitive microcapsules according to claim 5, wherein: the high molecular weight water-soluble prepolymer also comprises 0.5 to 1.5 parts by weight of melamine.
7. The process for preparing pH-sensitive microcapsules according to claim 6, 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.
8. A pH-sensitive microcapsule prepared by the preparation method according to any one of claims 2 to 7, characterized in that: comprises pH value sensitive silica gel particles and a capsule shell which surrounds the outside of the pH value sensitive silica gel particles;
the pH value sensitive microcapsule has a composite pore passage structure, and the composite pore passage comprises a primary pore passage formed by dissolving urea formaldehyde of pH value sensitive silica gel particles in ethanol and a secondary pore passage formed by dissolving low molecular weight urea formaldehyde resin in ethanol in a capsule shell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011041552.9A CN112354493B (en) | 2020-09-28 | 2020-09-28 | pH value sensitive microcapsule, preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011041552.9A CN112354493B (en) | 2020-09-28 | 2020-09-28 | pH value sensitive microcapsule, preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112354493A CN112354493A (en) | 2021-02-12 |
| CN112354493B true CN112354493B (en) | 2022-09-16 |
Family
ID=74508083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011041552.9A Active CN112354493B (en) | 2020-09-28 | 2020-09-28 | pH value sensitive microcapsule, preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112354493B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113713727A (en) * | 2021-06-07 | 2021-11-30 | 江南大学 | Humidity-sensitive color-changing microcapsule and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102466638A (en) * | 2010-11-12 | 2012-05-23 | 中国科学院大连化学物理研究所 | Indicator fixation test paper for heavy metal ion detection, preparation thereof and application thereof |
| CN105126715A (en) * | 2015-08-29 | 2015-12-09 | 复旦大学 | Magnetic mesoporous silica microsphere material with yolk structure and preparing method thereof |
| CN106706611A (en) * | 2015-11-12 | 2017-05-24 | 中国科学院大连化学物理研究所 | Method for immobilizing indicator by utilizing porous silica gel material and gas sensor and application |
| CN111073763A (en) * | 2019-12-27 | 2020-04-28 | 武汉材料保护研究所有限公司 | Slow-release urea formaldehyde microcapsule antifouling agent for reserved channel and preparation method thereof |
| CN111662702A (en) * | 2020-06-17 | 2020-09-15 | 厦门安踏体育用品有限公司 | Inductive color-changing material and application thereof in garment fabric |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9227221B2 (en) * | 2005-09-19 | 2016-01-05 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Hydrophilic-core microcapsules and their formation |
| JP2021512176A (en) * | 2018-02-06 | 2021-05-13 | スリーエム イノベイティブ プロパティズ カンパニー | Microcapsules with a porous or hollow core and a pH sensitive shell and their use |
-
2020
- 2020-09-28 CN CN202011041552.9A patent/CN112354493B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102466638A (en) * | 2010-11-12 | 2012-05-23 | 中国科学院大连化学物理研究所 | Indicator fixation test paper for heavy metal ion detection, preparation thereof and application thereof |
| CN105126715A (en) * | 2015-08-29 | 2015-12-09 | 复旦大学 | Magnetic mesoporous silica microsphere material with yolk structure and preparing method thereof |
| CN106706611A (en) * | 2015-11-12 | 2017-05-24 | 中国科学院大连化学物理研究所 | Method for immobilizing indicator by utilizing porous silica gel material and gas sensor and application |
| CN111073763A (en) * | 2019-12-27 | 2020-04-28 | 武汉材料保护研究所有限公司 | Slow-release urea formaldehyde microcapsule antifouling agent for reserved channel and preparation method thereof |
| CN111662702A (en) * | 2020-06-17 | 2020-09-15 | 厦门安踏体育用品有限公司 | Inductive color-changing material and application thereof in garment fabric |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112354493A (en) | 2021-02-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112354493B (en) | pH value sensitive microcapsule, preparation method and application | |
| CN103769021A (en) | Preparation method of organic-inorganic composite capsule wall energy-storage microcapsule | |
| CN103410007A (en) | Sol-gel pH discoloration finishing method for fabric | |
| CN109758990A (en) | Preparation method and application with highly sensitive temperature induced color changing microcapsules | |
| CN107386009A (en) | A kind of wet sensitive colour changing wall paper and preparation method thereof | |
| CN102115987A (en) | Formula of foam reactive dyeing system and preparation method thereof | |
| CN112852402A (en) | Durable thermochromic material, preparation method thereof and application thereof in textiles | |
| CN108755174B (en) | Preparation method of pH color-changing sol and textile based on natural dye | |
| CN111662702A (en) | Inductive color-changing material and application thereof in garment fabric | |
| CN107739035B (en) | A kind of coloring stabilized colored silicon dioxide granule and preparation method thereof | |
| CN112516933B (en) | Humidity-sensitive color-changing microcapsule, preparation method and application | |
| CN113249973A (en) | Modified long-acting photochromic microcapsule and preparation method thereof | |
| CN108905915A (en) | The preparation method and its resulting materials of a kind of thio chitosan photochromic micro-encapsulation and application | |
| CN110409196A (en) | A kind of preparation method of natural colorants functional agent | |
| CN102965912B (en) | Be suitable for cotton type fabric thermal transfer printing alkaline reaction type silicon titanium colloidal sol preparation method | |
| CN107904689B (en) | Preparation method of natural pigment colored fiber | |
| TWI625441B (en) | A dyeing composition for nylon fiber material and using the same method for dyeing process | |
| CN113559017A (en) | Hair dye based on copolymerization of 5, 6-dihydroxyindole and 6-hydroxyindole, and preparation method and use method thereof | |
| CN113713727A (en) | Humidity-sensitive color-changing microcapsule and preparation method and application thereof | |
| CN106770268B (en) | Preparation method of non-permeation pH test paper | |
| CN107987552B (en) | A kind of preparation method and applications of water-soluble natural pigment microcapsule | |
| WO2021232496A1 (en) | Colored silicon dioxide with core-shell structure, preparation method therefor and use thereof | |
| JP2908654B2 (en) | Manufacturing method of thermosensitive fiber structure | |
| CN115385905B (en) | PH color-changing reactive dye capable of dyeing cotton fabric and preparation method thereof | |
| CN115011327B (en) | Packaged photochromic microsphere and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |