CN111455693A - Modified long-acting photochromic microcapsule, preparation method thereof, photochromic dye printing paste containing modified long-acting photochromic microcapsule and application of photochromic dye printing paste - Google Patents
Modified long-acting photochromic microcapsule, preparation method thereof, photochromic dye printing paste containing modified long-acting photochromic microcapsule and application of photochromic dye printing paste Download PDFInfo
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- CN111455693A CN111455693A CN202010287140.7A CN202010287140A CN111455693A CN 111455693 A CN111455693 A CN 111455693A CN 202010287140 A CN202010287140 A CN 202010287140A CN 111455693 A CN111455693 A CN 111455693A
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 123
- 238000007639 printing Methods 0.000 title claims abstract description 109
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 239000004744 fabric Substances 0.000 claims description 52
- 238000000034 method Methods 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 19
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 18
- 239000011734 sodium Substances 0.000 claims description 18
- 229910052708 sodium Inorganic materials 0.000 claims description 18
- 239000004115 Sodium Silicate Substances 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 15
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- 239000003607 modifier Substances 0.000 claims description 8
- 238000010021 flat screen printing Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000010020 roller printing Methods 0.000 claims description 7
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- YGCOKJWKWLYHTG-UHFFFAOYSA-N [[4,6-bis[bis(hydroxymethyl)amino]-1,3,5-triazin-2-yl]-(hydroxymethyl)amino]methanol Chemical compound OCN(CO)C1=NC(N(CO)CO)=NC(N(CO)CO)=N1 YGCOKJWKWLYHTG-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000010022 rotary screen printing Methods 0.000 claims description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 11
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- 239000000975 dye Substances 0.000 description 29
- 239000000463 material Substances 0.000 description 23
- 238000012360 testing method Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 16
- 230000000694 effects Effects 0.000 description 14
- 239000010410 layer Substances 0.000 description 12
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 230000006750 UV protection Effects 0.000 description 6
- 239000011247 coating layer Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 239000003086 colorant Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000032798 delamination Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
- ZVFDTKUVRCTHQE-UHFFFAOYSA-N Diisodecyl phthalate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC(C)C ZVFDTKUVRCTHQE-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 150000004982 aromatic amines Chemical class 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 231100000315 carcinogenic Toxicity 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- -1 phthalic acid ester Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000037072 sun protection Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 241000122205 Chamaeleonidae Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 101150067256 MC69 gene Proteins 0.000 description 1
- 241000227425 Pieris rapae crucivora Species 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000011076 safety test Methods 0.000 description 1
- 238000009781 safety test method Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 231100000041 toxicology testing Toxicity 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/004—Dyeing with phototropic dyes; Obtaining camouflage effects
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
- D06P1/67383—Inorganic compounds containing silicon
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention provides a modified long-acting photochromic microcapsule, a preparation method thereof, photochromic dye printing paste containing the same and application thereof. The modified long-acting photochromic microcapsule deposits a layer of aluminum oxide or silicon dioxide on the surface of the photochromic microcapsule, and the coating structure can not only ensure that the organic shell of the photochromic microcapsule is not dissolved and damaged by printing paste, but also effectively improve the dispersibility and stability of the modified long-acting photochromic microcapsule powder in the printing paste. In addition, the modified long-acting photochromic microcapsule can be uniformly dispersed in the printing paste, so that the possible local precipitation of microcapsule powder in the printing paste is avoided, and the problem of uneven design and color in subsequent printing is further avoided.
Description
Technical Field
The invention relates to the technical field of garment materials, in particular to a modified long-acting photochromic microcapsule, a preparation method thereof, photochromic dye printing paste containing the same and application thereof.
Background
Photochromic materials have been developed in recent years, and garments made of the photochromic materials have the characteristics of receiving light for discoloration, bringing novel and attractive visual impact to garment wearers, and also have an ultraviolet indicating effect.
CN105167224A discloses a textile garment changing color along with light intensity, which comprises a garment body, wherein the garment body is provided with a plurality of photochromic ribbons, the photochromic ribbons are made of photochromic materials, and the photochromic materials comprise the following raw materials in parts by weight; 80-100 parts of photochromic material, 1-10 parts of antioxidant, 1-10 parts of dispersant and 1-10 parts of assistant. The photochromic material is preferably a mixture of spiropyrans and spirooxazines, the thermal stability and enhanced thermal stability of the photochromic material are good, the color of textile clothes can be changed along with the intensity of light, and the fatigue resistance of eyes is greatly improved.
CN108948786A discloses a photochromic dye, photochromic cloth and photochromic garment. The photochromic dye comprises dye, resin or paste, an auxiliary agent and a photochromic material, wherein the photochromic material comprises any one or the combination of more than two of inorganic photochromic compound, luminescent material, absorbent and material adopting complementary color principle. The photochromic dye provided by the invention can enable the cloth dyed by the photochromic dye to have color or change the color according to the absorbed light.
However, the photochromic materials are prepared by directly adding photochromic dyes into the fabric, and in the preparation process, the photochromic materials are inevitably influenced by active groups and pH value changes, so that the photochromic materials are invalid or the service life of the photochromic materials is greatly reduced.
Although there are many reports that the preparation method of microencapsulation can protect the photochromic material from being damaged in the processing process, the incomplete process conditions still cause the problems of failure, local damage and under color of the photochromic material in the manufacturing process.
Therefore, exploring and developing a novel photochromic microcapsule technology can avoid the damage of photochromic materials in the manufacturing process, and further, the manufacturing of fabrics with the service life meeting the requirements of clothes is a strong demand of the current market.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a modified long-acting photochromic microcapsule, a preparation method thereof, photochromic dye printing paste containing the same and application thereof. The modified long-acting photochromic microcapsule deposits a layer of alumina or silicon dioxide on the surface of the photochromic microcapsule, and the coating structure can not only ensure that the organic shell of the photochromic microcapsule is not dissolved and damaged by printing paste, but also increase the dispersibility and stability of the modified long-acting photochromic microcapsule powder in the printing paste.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a modified long-acting photochromic microcapsule, which is an alumina or silica coated photochromic microcapsule.
The modified long-acting photochromic microcapsule deposits a layer of aluminum oxide or silicon dioxide on the surface of the photochromic microcapsule, and the coating structure can not only ensure that the organic shell of the photochromic microcapsule is not dissolved and damaged by printing paste, but also effectively improve the dispersibility and stability of the modified long-acting photochromic microcapsule powder in the printing paste.
In the present invention, the term "long-lasting" means that after exposure for up to 70 hours, the photochromic effect still has a good photochromic effect, and the photochromic effect still can reach more than 3 grades (evaluation by the photochromic evaluation method).
In a second aspect, the present invention also provides a method for preparing the modified long-acting photochromic microcapsule according to the first aspect, comprising: and mixing sodium metaaluminate or sodium metasilicate and the photochromic microcapsule, reacting and aging to obtain the modified long-acting photochromic microcapsule.
The invention utilizes sodium metaaluminate or sodium metasilicate to form an alumina or silicon dioxide coating layer on the surface of the photochromic microcapsule, so that the finally obtained modified long-acting photochromic microcapsule has better dispersibility and stability.
In the reaction system, the weight portions of sodium metaaluminate or sodium metasilicate are 3-30 portions and the weight portions of photochromic microcapsule are 10-50 portions, and the weight portions of sodium metaaluminate or sodium metasilicate are more preferably 5-10 portions and the weight portions of photochromic microcapsule are 15-30 portions.
The sodium metaaluminate or sodium metasilicate is present in an amount of 3 to 30 parts by weight, for example, 4 parts by weight, 5 parts by weight, 6 parts by weight, 7 parts by weight, 8 parts by weight, 9 parts by weight, 10 parts by weight, 15 parts by weight, 20 parts by weight, 25 parts by weight, or the like.
10 to 50 parts by weight of the photochromic microcapsule, such as 15 parts by weight, 18 parts by weight, 20 parts by weight, 22 parts by weight, 25 parts by weight, 28 parts by weight, 30 parts by weight, 35 parts by weight, 40 parts by weight, 45 parts by weight and the like.
In the present invention, the 3-30 parts by weight of sodium metaaluminate or sodium metasilicate refers to 3-30 parts by weight of sodium metaaluminate or 3-30 parts by weight of sodium metasilicate.
In the invention, by controlling the weight of sodium metaaluminate or sodium metasilicate to be 3-30 parts and the weight of photochromic microcapsule to be 10-50 parts, the coating thickness of the finally obtained coating layer is moderate, so that the finally modified long-acting photochromic microcapsule has better dispersibility and stability and the photochromic effect of the microcapsule is not influenced.
If the addition amount of the sodium metaaluminate or the sodium metasilicate is too low or the addition amount of the photochromic microcapsules is too high, the dispersibility and the stability of the finally obtained photochromic microcapsules are influenced, the protection effect on the photochromic microcapsules is not good, and the photochromic microcapsules are easily damaged in subsequent printing paste; if the addition amount of the sodium metaaluminate or the sodium metasilicate is too high or the addition amount of the photochromic microcapsules is too low, the ultraviolet discoloration resistance of the finally obtained photochromic microcapsules can be affected.
In the present invention, the preparation method further comprises: the photochromic microcapsules are dispersed prior to mixing.
Preferably, the method of dispersing comprises: and premixing the photochromic microcapsules, water and a dispersing agent, and adjusting the pH value to obtain a dispersion liquid.
Preferably, the dispersant is any one or combination of at least two of sodium hexametaphosphate, sodium tripolyphosphate or sodium pyrophosphate.
The dispersant is preferably added in an amount of 0.5 to 20 parts by weight, for example, 1 part by weight, 2 parts by weight, 3 parts by weight, 4 parts by weight, 5 parts by weight, 8 parts by weight, 10 parts by weight, 12 parts by weight, 15 parts by weight, 18 parts by weight, etc., and more preferably 1 to 5 parts by weight.
In the invention, the addition of the dispersant can ensure the uniform coating thickness of the finally obtained modified long-acting photochromic microcapsule, and if the addition amount of the dispersant is too small, the uniformity of the coating layer of the modified long-acting photochromic microcapsule can be influenced, and the dispersion stability of the modified long-acting photochromic microcapsule in printing paste can be further influenced; if the amount of the dispersant is too high, the cost is affected.
Preferably, the water is added in an amount of 10 to 50 parts by weight, for example, 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight, 32 parts by weight, 35 parts by weight, 38 parts by weight, 40 parts by weight, 45 parts by weight, etc., and more preferably 30 to 40 parts by weight.
Preferably, the temperature of the pre-mixing is 60-65 ℃, such as 61 ℃, 62 ℃, 63 ℃, 64 ℃ and the like.
Preferably, the time of the premixing is 20-40min, such as 22min, 25min, 28min, 30min, 32min, 35min, 38min and the like.
Preferably, the pH is adjusted to a pH of 6.5-7.5, e.g., 6.6, 6.7, 6.8, 6.9, 7.0, 7.1, 7.2, 7.3, 7.4, etc.
Preferably, the pH of the mixing is 9.5-10.5, such as 9.5, 9.6, 9.7, 9.8, 9.9, 10, 10.1, 10.2, 10.3, 10.4, 10.5, or the like.
Preferably, the pH of the mixing is adjusted using sulfuric acid and/or sodium hydroxide.
In the invention, after the sodium metaaluminate or sodium metasilicate and the photochromic microcapsule are mixed, sulfuric acid and/or sodium hydroxide are needed to be added, and the pH value is 9.5-10.5.
Preferably, the aging time is 2-5h, such as 2.5h, 3h, 3.5h, 4h, 4.5h, and the like.
Preferably, the temperature of the aging is 60-65 ℃, such as 61 ℃, 62 ℃, 63 ℃, 64, etc.
Preferably, the preparation method further comprises crushing after the reaction is finished.
Preferably, the crushing method comprises the following steps: firstly, a high-speed pulverizer is used for primary pulverization, and then an airflow pulverizer is used for fine pulverization.
Conventional filtration is required before pulverization and cooling to room temperature for pulverization.
In a third aspect, the present invention also provides a photochromic dye printing paste comprising the modified long-acting photochromic microcapsule according to the first aspect.
The photochromic dye printing paste comprises the modified long-acting photochromic microcapsule, and a layer of alumina or silica is deposited on the surface of the powder of the modified long-acting photochromic microcapsule, so that the dispersity and stability of the microcapsule in the printing paste are effectively improved, the microcapsule can be uniformly dispersed in the printing paste, the possible local precipitation of the microcapsule powder in the printing paste is avoided, and the possible problem of uneven design and color in subsequent printing is avoided.
Preferably, the printing paste comprises the following components in parts by weight: 0.5-30 parts of modified long-acting photochromic microcapsule and 60-90 parts of printing paste.
The modified long-acting photochromic microcapsule is 0.5-30 parts, such as 0.5 part, 1 part, 3 parts, 5 parts, 7 parts, 9 parts, 10 parts, 15 parts, 20 parts, 25 parts or 30 parts.
The printing paste is 60 to 90 parts, and may be, for example, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, or 90 parts.
The printing paste of the present invention is a commonly used printing paste, and is exemplified by a printing paste provided by Densitan Fine chemical Co., Ltd. with a model number of FS-404R.
Preferably, the printing paste further comprises 0.1-10 parts of bridging agent, which can be 0.1 part, 0.5 part, 1 part, 2 parts, 5 parts, 8 parts or 10 parts, for example.
Preferably, the bridging agent comprises hexamethylol melamine and/or etherified hexamethylol melamine.
Preferably, the printing paste further comprises 0.01-1 part of a hand feeling modifier, which may be, for example, 0.01 part, 0.05 part, 0.1 part, 0.3 part, 0.5 part, 0.8 part, 1 part, or the like.
Preferably, the hand feeling modifier is silicone oil type hand feeling modifier.
In a fourth aspect, the present invention also provides a preparation method of the photochromic dye printing paste according to the third aspect, comprising the following steps: and uniformly mixing the modified long-acting photochromic microcapsule, the printing paste, the optional bridging agent and the optional hand feeling regulator to obtain the photochromic dye printing paste.
Preferably, the preparation method comprises the following steps: and uniformly mixing the modified long-acting photochromic microcapsules and the printing paste, filtering (filtering by using a 160-mesh silk screen), and then adding a bridging agent and a hand feeling regulator to obtain the photochromic dye printing paste.
In the present invention, the term "uniformly mixing" means uniformly mixing in the presence or absence of ultraviolet rays.
In a fifth aspect, the invention also provides a photochromic fabric, which is printed on the surface of the fabric by using the photochromic dye printing paste of the third aspect.
The photochromic fabric can intelligently change colors according to the intensity of ultraviolet rays, the stronger the ultraviolet rays are, the darker the fabric color is, and the color change can prompt people whether to need sun protection or not. Meanwhile, the photochromic fabric is obtained by printing the photochromic dye printing paste on the surface of the fabric, and a layer of alumina or silica is deposited on the surface of the photochromic microcapsules in the printing paste, so that the photochromic microcapsules can be prevented from being damaged in the fabric printing process, and the fabric with the service life meeting the clothing requirements is manufactured.
Preferably, the printing method is any one or a combination of at least two of flat screen printing, rotary screen printing or roller printing, preferably flat screen printing and/or roller printing.
The flat screen printing can print fine patterns, does not transmit colors, has a large amount of printing paste, is accompanied by a three-dimensional sense, is suitable for printing woven fabrics and knitted fabrics such as silk, cotton, chemical fiber and the like, and is more suitable for printing high-grade fabrics of various varieties in small batches.
The roller printing can continuously press color paste in the concave lines onto the fabric, can print in large batch, and can realize continuous printing of colorful patterns when a plurality of cylinders are arranged on the equipment at the same time.
Preferably, the method of flat screen printing comprises: selecting a screen frame and a screen mesh with proper specifications, coating the photochromic dye printing paste on the surface of the fabric in a scraping way, and setting the temperature at 100-180 ℃.
It should be noted that, in the flat screen printing process, whether heat setting finishing is needed or not is selected according to the type of the fabric, so as to reduce shrinkage deformation in the printing process, and the required photochromic fabric can be prepared.
Preferably, the roller printing method comprises the following steps: the paste feeding roller with the cylinder transfers the color paste to the cylinder, and the printing can be printed on the surface of the fabric through the continuous roller of the cylinder and the continuous transmission of the fabric.
It should be noted that, in the process of roller printing, the color paste of the non-pattern part can be scraped by the doctor blade, and the small yarn-removing scraper on the side surface of the tube can prevent the fluff on the fabric from entering the color paste through the tube, so that the color paste can better transfer color.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the modified long-acting photochromic microcapsule, a layer of aluminum oxide or silicon dioxide is deposited on the surface of the photochromic microcapsule, and the coating structure can not only ensure that the organic shell of the photochromic microcapsule cannot be dissolved and damaged by printing paste, but also effectively improve the dispersibility and stability of the modified long-acting photochromic microcapsule powder in the printing paste;
(2) the photochromic dye printing paste comprises the modified long-acting photochromic microcapsule, and a layer of alumina or silica is deposited on the surface of the powder of the modified long-acting photochromic microcapsule, so that the dispersity and stability of the microcapsule in the printing paste are effectively improved, the microcapsule can be uniformly dispersed in the printing paste, the possible local precipitation of the microcapsule powder in the printing paste is avoided, and the problem of uneven design and color in subsequent printing is further avoided;
(3) the photochromic garment fabric can intelligently change colors according to the ultraviolet intensity, the stronger the ultraviolet rays are, the darker the fabric color is, and the color change can prompt people whether to need sun protection or not. Meanwhile, the photochromic garment fabric is obtained by printing the photochromic dye printing paste on the surface of the garment fabric, and because a layer of aluminum oxide or silicon dioxide is deposited on the surface of the photochromic microcapsules in the printing paste, the photochromic microcapsules can be prevented from being damaged in the fabric printing process, and the fabric with the service life meeting the garment requirement is manufactured;
(4) the printing paste provided by the invention has good dispersion stability, obvious layering can not occur after the printing paste is placed at 60 ℃ for 3 days, the photochromic garment fabric provided by the invention has good weather resistance, and after being exposed for 70 hours, the photochromic garment fabric still has a good photochromic effect, and the photochromic effect can still reach more than 3 grades.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The manufacturers and the brands of partial raw materials used in the embodiment and the application example of the invention are as follows:
photochromic microcapsules are available from L CRHallcrest, USA, under the model numbers 1797U (red) and 2995U (blue);
the hand feeling regulator is purchased in Dongguan for peak chemical industry and is brand smooth and ice feeling silicone oil C922.
The following examples and comparative examples each prepared modified long-acting photochromic microcapsules using the photochromic microcapsules of 1797U (red) and 2995U (blue), respectively, i.e., each example and each comparative example obtained two different modified long-acting photochromic microcapsules, and each application example and each comparative example also obtained two different photochromic fabrics.
Example 1
A modified long-acting photochromic microcapsule is an alumina-coated photochromic microcapsule, and the preparation method comprises the following steps:
1) mixing 30g of photochromic microcapsules and 40g of water, adding 5g of sodium hexametaphosphate into the mixed system, mixing at 60 ℃ for 30min, and adjusting the pH value to 7.0 to obtain a mixed solution;
2) adding 10g of sodium metaaluminate into the mixed solution obtained in the step 1), titrating by using 1 mol/L sulfuric acid solution, adding sodium hydroxide to adjust the pH value to 9.5 after titration is finished, aging for 2h at 62 ℃, performing suction filtration on the aged solution in a Buchner funnel, cooling the block powder obtained by suction filtration to 30 ℃, primarily crushing by using a high-speed crusher, and finely crushing by using a jet mill to obtain the modified long-acting photochromic microcapsule.
Examples 2 to 3
The difference from example 1 is that, in this example, the photochromic microcapsules are added in an amount of 10g (example 2) and 50g (example 3).
Examples 4 to 5
The difference from example 1 is that, in the present example, the amount of sodium metaaluminate added is 3g (example 4) and 30g (example 5).
Examples 6 to 7
The difference from example 1 is that in this example, the sodium hexametaphosphate was added in an amount of 0.5g (example 6) and 20g (example 7).
Example 8
A modified long-acting photochromic microcapsule is a silica-coated photochromic microcapsule, and the preparation method comprises the following steps:
1) mixing 30g of photochromic microcapsules and 40g of water, adding 5g of sodium tripolyphosphate into the mixed system, mixing for 30min at 62 ℃, and adjusting the pH value to 7 to obtain a mixed solution;
2) adding 10g of sodium metasilicate into the mixed solution obtained in the step 1), adjusting the pH to 10.5 by utilizing 0.2 mol/L sulfuric acid solution and sodium hydroxide together, aging for 4h at 65 ℃, performing suction filtration on the aged solution in a Buchner funnel, cooling the block powder obtained by suction filtration to 25 ℃, primarily crushing by utilizing a high-speed crusher, and finely crushing by utilizing a jet mill to obtain the modified long-acting photochromic microcapsule.
Comparative example 1
This comparative example provides photochromic microcapsules used in example 1, which have no alumina or silica coating deposited on their surface.
Application example 1
A photochromic fabric is prepared by the following steps:
and printing the photochromic dye printing paste on the surface of the clothing fabric in a flat screen printing mode to obtain the photochromic fabric.
The photochromic dye printing paste consists of the following components:
the printing paste is purchased from Dengzhong Fine chemical Co., Ltd, and the model is FS-404R, and the bridging agent is purchased from Dengzhong fine chemical Co., Ltd, and the model is DF-810.
The preparation method comprises the following steps:
the modified long-acting photochromic microcapsule prepared in the embodiment 1 and the printing paste are uniformly mixed at room temperature, a 160-mesh silk screen is used for filtering, and then the bridging agent and the hand feeling modifier are added into the mixed system to obtain the photochromic dye printing paste.
Application examples 2 to 8
The difference from application example 1 is that the modified long-acting photochromic microcapsules provided in example 1 in the photochromic dye printing paste were replaced with the modified long-acting photochromic microcapsules provided in examples 2 to 8.
Application example 9
A photochromic fabric is prepared by the following steps:
and printing the photochromic dye printing paste on the surface of the clothing fabric in a roller printing mode to obtain the photochromic fabric.
The photochromic dye printing paste consists of the following components:
the printing paste is purchased from Dengzhong Fine chemical Co., Ltd under the model of FS-404R, and the bridging agent is purchased from Dengzhong fine chemical Co., Ltd under the model of DF-810.
The preparation method comprises the following steps:
the modified long-acting photochromic microcapsule prepared in the embodiment 1 and the printing paste are uniformly mixed at room temperature, a 160-mesh silk screen is used for filtering, and then the bridging agent and the hand feeling modifier are added into the mixed system to obtain the photochromic dye printing paste.
Comparative application example 1
The only difference from application example 1 is that the modified long-acting photochromic microcapsule prepared in example 1 was replaced with the photochromic microcapsule in comparative example 1.
Performance test 1:
the printing pastes prepared in application examples 1-9 and comparative application example 1 were subjected to a performance test by the following method:
(1) dispersion stability: the printing pastes prepared in the application examples and the comparative application examples are placed at 60 ℃ for 3 days, and the layering condition of the printing pastes is visually observed.
The test results are shown in table 1.
TABLE 1
As can be seen from the data in Table 1, the application examples 1-9 show that no obvious delamination occurs when the printing paste prepared by the invention is placed at 60 ℃ for 3 days, which indicates that the modified long-acting photochromic microcapsule prepared by the invention can stably exist in the printing paste, i.e. the dispersibility and stability of the photochromic microcapsule in the printing paste are obviously improved.
Application example 6 showed slight delamination compared to application example 1. The reason is that the addition amount of the dispersing agent is less, so that the dispersibility and the stability of the modified long-acting photochromic microcapsule in the printing paste are reduced
Compared with application example 1, the printing paste prepared in comparative application example 1 showed significant delamination. This is because no alumina layer is deposited on the surface of the photochromic microcapsule contained in the printing paste of comparative application example 1, which results in that the wall material of the microcapsule is easily dissolved by the organic substance in the printing paste, the structural stability is reduced, and the obvious layering phenomenon occurs.
Performance test 2
The photochromic fabrics prepared in application examples 1-9 and comparative application example 1 were subjected to a performance test by the following method:
(1) weather resistance, referring to appendix A of Q/CPT L Z0014.11-2019, the Test conditions are that the blackboard temperature is 50 +/-2 ℃, 65 +/-4 percent RH, the exposure time is 70h, and the instrument manufacturers are U.S. Q-SUN, Xenon Test Chamber Xenon aging boxes;
the standard value requirement of the test is as follows: the application example 1 is taken as a standard sample, and the photochromic performance of the insolation test sample relative to the standard sample is evaluated by a photochromic evaluation method, wherein the photochromic performance is more than or equal to 3 grade;
the test results of the application examples and the comparative application examples are shown in table 2.
TABLE 2
Before and after the photochromic fabric provided by the embodiment 1 of the invention is exposed for 70 hours, the photochromic fabric is placed under a 365 ultraviolet flashlight to be irradiated for 5 seconds for rating, the color difference is small, and the photochromic fabric meets the requirements, so that the photochromic fabric is used as a standard sample in the invention.
From the test results in table 2, it can be seen from application examples 1 to 9 that all performance indexes of the photochromic fabric prepared by the method can meet the standard requirements.
The level of the light-variable effect was slightly reduced after exposure to light for 70 hours in application example 2 and application example 5, compared to application example 1. The reason is that the lower adding amount of the photochromic microcapsules and the higher adding amount of the sodium metaaluminate cause the thicker alumina layer deposited on the surfaces of the photochromic microcapsules, and the level of the color development effect is degraded after the photochromic microcapsules are exposed to the sun.
The level of the light-variable effect was slightly reduced after exposure to light for 70 hours in application example 3 and application example 4, compared to application example 1. The reason is that the aluminum oxide layer deposited on the surface of the photochromic microcapsules is thinner due to more addition of the photochromic microcapsules and less addition of the sodium metaaluminate, so that the wall materials of part of the microcapsules are easily dissolved by organic matters in the printing paste, the structural stability is reduced, and the level of the color development effect after exposure to the sun is finally reduced.
Compared with the application 1, the light variability performance of the application example 6 after being exposed for 70h just meets the standard value of the application example. The reason is that the addition amount of the dispersing agent is less, so that the dispersibility and stability of the modified photochromic microcapsules in the printing paste are reduced, and the level of the photochromic effect is reduced.
Compared with application example 1, the light variability performance is poorer after the application example 1 is exposed for 70 h. This is because the photochromic microcapsules contained in the printing paste of comparative application example 1 have no alumina layer deposited on the surface thereof, which results in that the wall materials of the microcapsules are easily dissolved by the organic substances in the printing paste, the structural stability thereof is lowered, and the optically variable effect is deteriorated.
(2) And (3) safety testing: the safety of the photochromic fabric prepared in application example 1 and application example 8 of the invention was tested according to GB 31701-2015 technical safety Specification (class A) for infant and child textile products.
The specific test items, detection methods and detection standards are as follows:
(a) content of formaldehyde: testing the content of formaldehyde according to GB/T2912.1-2009, wherein the standard value is less than or equal to 20 mg/kg;
(b) pH value: performing pH value test according to GB/T7573-2009, extracting potassium chloride, and the standard value range is 4.0-7.5;
(c) and (3) decomposing carcinogenic aromatic amine dye: the test for decomposing the carcinogenic aromatic amine dye is carried out according to GB/T17592-2011, and the standard values are as follows: forbidding;
(d) heavy metals: the heavy metal content is tested according to GB/T30157-2013, and the standard value is as follows: the total lead is less than or equal to 90mg/kg, and the total cadmium is less than or equal to 100 mg/kg;
(e) phthalic acid ester: the phthalate content was tested according to GB/T20388-2016, and the main detection substances: di (2-ethyl) hexyl phthalate (DEHP), dibutyl phthalate (DBP) and Butyl Benzyl Phthalate (BBP), diisononyl phthalate (DINP), diisodecyl phthalate (DIDP) and dioctyl phthalate (DNOP), with the standard value of less than or equal to 0.1%;
the test results are shown in Table 3.
TABLE 3
As can be seen from the data in Table 3, all safety tests of the photochromic fabric prepared by the application example of the invention meet the requirements of various national legal and regulatory standards, namely the prepared photochromic fabric has no potential safety hazard to human bodies.
(3) And (3) ultraviolet performance test: and respectively carrying out red printing and blue printing on the sample to be tested of the photochromic printing paste on the fabric of the common white skin garment, carrying out ultraviolet resistance index test on the prepared printed skin garment, and taking the non-printed white skin garment as a blank control.
The test method comprises the following steps: GB/T18830-.
The test results are shown in Table 4 below.
TABLE 4
As can be seen from the data in Table 4, after the red printing or the blue printing is performed on the skin clothes fabric by the printing pastes prepared in the application example and the comparative application example, the ultraviolet resistance indexes are both obviously improved, the deeper the optically variable color is, the better the ultraviolet resistance index is, and the ultraviolet resistance index after the color change is more obviously higher than the ultraviolet resistance index before the color change, which shows that the ultraviolet resistance function of the fabric can be obviously improved after the printing is performed by the photochromic printing paste.
(4) And (3) weather resistance test: the modified long-acting photochromic microcapsules of examples 1 and 8 of the present invention and comparative example 1 were subjected to a weather resistance test. A commercially available domestic ultraviolet-proof toner (purchased from Qianhong new color change material science and technology Limited in Shenzhen, model: MC14/MC69) and a commercially available imported ultraviolet-proof toner (purchased from Korean Chameleon UVC, model: Bichrom P) are used as control groups.
The Test method refers to appendix A of Q/CPT L Z0014.11-2019, the Test conditions are that the blackboard temperature is 50 +/-2 ℃, 65 +/-4 percent RH, the exposure time is shown in Table 5, and the equipment manufacturer is a Xenon Test Chamber of Q-SUN company;
the standard value requirement of the test is as follows: the application example 1 is used as a standard sample, and the photochromic performance of the insolation test sample relative to the standard sample is evaluated by a color change evaluation method, and the result is more than or equal to grade 3.
The specific test results are shown in table 5 below:
TABLE 5
From the results in table 5, it can be seen that the weather resistance of the modified long-acting photochromic microcapsule with deposited alumina coating layer prepared in example 1 of the present invention or the modified long-acting photochromic microcapsule with deposited silica coating layer prepared in example 8 is significantly better than that of the commercially available uv-blocking toner in home or import. This shows that the stability of the photochromic microcapsule can be obviously improved by depositing a layer of alumina or silica on the surface of the photochromic microcapsule, and further the weather resistance of the photochromic microcapsule is obviously improved.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. The modified long-acting photochromic microcapsule is characterized in that the modified long-acting photochromic microcapsule is an alumina or silica coated photochromic microcapsule.
2. A method of preparing a modified long-acting photochromic microcapsule according to claim 1, wherein the method of preparation comprises: and mixing sodium metaaluminate or sodium metasilicate and the photochromic microcapsule, reacting and aging to obtain the modified long-acting photochromic microcapsule.
3. The method according to claim 2, wherein the reaction system comprises 3 to 30 parts by weight of sodium metaaluminate or sodium metasilicate and 10 to 50 parts by weight of photochromic microcapsule, more preferably 5 to 10 parts by weight of sodium metaaluminate or sodium metasilicate and 15 to 30 parts by weight of photochromic microcapsule.
4. The production method according to claim 2 or 3, characterized by further comprising: before mixing, dispersing the photochromic microcapsules;
preferably, the method of dispersing comprises: premixing photochromic microcapsules, water and a dispersing agent, and adjusting the pH value to obtain a dispersion liquid;
preferably, the dispersant is any one or combination of at least two of sodium hexametaphosphate, sodium tripolyphosphate or sodium pyrophosphate;
preferably, the addition amount of the dispersant is 0.5 to 20 parts by weight, more preferably 1 to 5 parts by weight;
preferably, the addition amount of the water is 10 to 50 parts by weight, and further preferably 30 to 40 parts by weight;
preferably, the temperature of the pre-mixing is 60-65 ℃;
preferably, the pre-mixing time is 20-40 min;
preferably, the pH is adjusted to 6.5-7.5.
5. The production method according to any one of claims 2 to 4, wherein the mixed pH is 9.5 to 10.5;
preferably, the pH of the mixing is adjusted with sulfuric acid and/or sodium hydroxide;
preferably, the aging time is 2-5 h;
preferably, the temperature of aging is 60-65 ℃;
preferably, the preparation method further comprises, after the reaction is finished, pulverizing;
preferably, the crushing method comprises the following steps: firstly, a high-speed pulverizer is used for primary pulverization, and then an airflow pulverizer is used for fine pulverization.
6. A photochromic dye printing paste comprising the modified long-acting photochromic microcapsules of claim 1.
7. The printing paste according to claim 6, wherein the printing paste comprises the following components in parts by weight: 0.5-30 parts of modified long-acting photochromic microcapsule and 60-90 parts of printing paste;
preferably, the printing paste also comprises 0.1-10 parts of bridging agent;
preferably, the bridging agent comprises hexamethylol melamine and/or etherified hexamethylol melamine;
preferably, the printing paste also comprises 0.01-1 part of hand feeling modifier;
preferably, the hand feeling modifier is silicone oil type hand feeling modifier.
8. A method for preparing the photochromic dye printing paste according to claim 6 or 7, wherein the method comprises the following steps: and uniformly mixing the modified long-acting photochromic microcapsule, the printing paste, the optional bridging agent and the optional hand feeling regulator to obtain the photochromic dye printing paste.
9. A photochromic fabric, wherein the photochromic fabric is printed on the surface of the fabric by using the photochromic dye printing paste according to claim 6 or 7.
10. The photochromic fabric of claim 9, wherein the printing method is any one of flat screen printing, rotary screen printing or roller printing or a combination of at least two of them.
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| CN114621694A (en) * | 2022-03-18 | 2022-06-14 | 宁波百仕高联合工业有限公司 | Preparation method of photochromic flash glue |
| CN115120504A (en) * | 2022-07-20 | 2022-09-30 | 武汉大学 | Photochromic orthodontic bracket adhesive and preparation method and application thereof |
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