CN116376315A - Preparation method and application of high-light fastness liquid crystal structure pigment - Google Patents

Preparation method and application of high-light fastness liquid crystal structure pigment Download PDF

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Publication number
CN116376315A
CN116376315A CN202310225017.6A CN202310225017A CN116376315A CN 116376315 A CN116376315 A CN 116376315A CN 202310225017 A CN202310225017 A CN 202310225017A CN 116376315 A CN116376315 A CN 116376315A
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CN
China
Prior art keywords
liquid crystal
pigment
crystal structure
light fastness
dispersing
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Pending
Application number
CN202310225017.6A
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Chinese (zh)
Inventor
付少海
吴燕祥
关玉
毛云山
范奇鸣
张晓芳
何红英
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Wujiang Shanhu Color Co ltd
Jiangnan University
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Wujiang Shanhu Color Co ltd
Jiangnan University
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Priority to CN202310225017.6A priority Critical patent/CN116376315A/en
Publication of CN116376315A publication Critical patent/CN116376315A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0001Post-treatment of organic pigments or dyes
    • C09B67/0004Coated particulate pigments or dyes
    • C09B67/0008Coated particulate pigments or dyes with organic coatings
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/006Preparation of organic pigments
    • C09B67/0066Aqueous dispersions of pigments containing only dispersing agents

Abstract

The invention discloses a preparation method of a high-light fastness liquid crystal structure pigment, which comprises the following steps: s1, adding pigment into deionized water, regulating the PH by using inorganic acid, dispersing to obtain pigment dispersion liquid, adding a composite liquid crystal finishing agent and an auxiliary emulsifier into the pigment dispersion liquid, and dispersing, homogenizing and emulsifying the pigment dispersion liquid to obtain liquid crystal homogeneous emulsion; s2, stirring the liquid crystal homogeneous emulsion at a high temperature, and cooling and standing to obtain the liquid crystal structure pigment with the lyotropic liquid crystal emulsified coating on the particle surface; s3, putting the liquid crystal structure pigment into a grinder for grinding and dispersing, adding a dispersing agent, grinding together with the dispersing agent, and obtaining the liquid crystal structure pigment with high light fastness after finishing grinding. The invention also provides application of the liquid crystal structure pigment. Compared with the prior art, the invention greatly improves the color fastness to sunlight of the pigment with poor color fastness to sunlight.

Description

Preparation method and application of high-light fastness liquid crystal structure pigment
Technical Field
The invention relates to the technical field of pigment production, in particular to a preparation method and application of a high-light fastness liquid crystal structure pigment.
Background
The organic pigment has the advantages of complete color spectrum, bright color, high tinting strength, no toxicity, no harm and the like. Most pigment varieties, except for a few high-end organic pigment varieties, currently suffer from more or less drawbacks in some respects, such as the poor light fastness of some scarce chromatographic (green, violet) pigments, which generally limits their range of application.
At present, most of the industry is to add an anti-ultraviolet finishing agent in the pigment use process or introduce a substituent group into the pigment to improve the color fastness to sunlight of the pigment, such as Chinese patent CN1 13755085A, CN1 13943495A and the like. However, the methods have the advantages that the improvement of the color fastness to sunlight of the pigment is not large, or the process is complex, the color light and the coloring strength of the pigment are easy to change, and the actual production requirements cannot be completely met.
Disclosure of Invention
The invention aims at: the preparation method and the application of the high-light fastness liquid crystal structure pigment are provided, the addition of an anti-ultraviolet finishing agent in the use process of the pigment is not needed, or substituent groups are introduced into the pigment, and the composite liquid crystal finishing agent is adopted to treat the organic pigment, so that the light fastness of the pigment with poor light fastness is greatly improved.
In order to achieve the above object, in one aspect, the present invention provides a method for preparing a high light fastness liquid crystal structure pigment, comprising the steps of:
s1, adding pigment into deionized water, regulating the PH by using inorganic acid, dispersing to obtain pigment dispersion liquid, wherein the PH of the pigment dispersion liquid is 3-6.5, adding a composite liquid crystal finishing agent and an auxiliary emulsifier into the pigment dispersion liquid, dispersing and homogenizing the mixture to emulsify the mixture to obtain liquid crystal homogenized emulsion, and the weight ratio of the pigment to the composite liquid crystal finishing agent to the auxiliary emulsifier to the deionized water is 1-5:5-20:0.2-1.1:100;
s2, stirring the liquid crystal homogeneous emulsion at a high temperature, and cooling and standing to obtain the liquid crystal structure pigment with the lyotropic liquid crystal emulsified coating on the particle surface;
s3, putting the liquid crystal structure pigment into a grinder for grinding and dispersing, adding a dispersing agent, grinding together with the dispersing agent, and obtaining the liquid crystal structure pigment with high light fastness after finishing grinding.
As a further description of the above technical solution:
in step S1, the pigment is one or more of azo pigments, lake pigments, heterocyclic pigments, and condensed ring ketone pigments.
As a further description of the above technical solution:
in step S1, the inorganic acid used for adjusting PH is one or more of formic acid, acetic acid, propionic acid, hydrochloric acid, and sulfuric acid.
As a further description of the above technical solution:
in the step S1, the composite liquid crystal finishing agent is one or more of glucosides, sucrose esters, glyceride, phosphonate esters and lecithin.
As a further description of the above technical solution:
in the step S1, the auxiliary emulsifier is one or more of a surfactant containing various acid radicals and long carbon chain fatty alcohol.
As a further description of the above technical solution:
in the step S1, the homogenizing and emulsifying rotating speed is 2000-8000r/min, and the homogenizing time is 2-10min.
As a further description of the above technical solution:
in the step S2, when stirring at high temperature, the temperature is 50-90 ℃, the stirring speed at the heat preservation is 300-1000r/min, and the stirring time at the heat preservation is 5-30min.
As a further description of the above technical solution:
in the step S2, the temperature is reduced to be between 20 and 40 ℃ and the standing time is between 2 and 8 hours.
As a further description of the above technical solution:
in step S3, the dispersant is one or more of fatty acid salts, oleate, alkyl sulfonate, aliphatic amides, paraffin, and metal soaps containing sulfonic acid groups.
On the other hand, the invention also provides application of the liquid crystal structure pigment in the fields of pigment printing, ink-jet printing, food coloring and painting ink.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
1. in the invention, after the prepared liquid crystal structure pigment is used for coloring the textile, the K/S value of the textile is even slightly improved compared with that of a common pigment printing textile, because part of finishing agent has a deepening effect. Meanwhile, compared with common pigment printed fabrics, the color fastness to sunlight of the liquid crystal structure pigment is greatly improved, so that the application range of the pigment with poor color fastness to sunlight is enlarged.
2. Most organic pigments have bright color light and excellent color development performance, but partial scarce color spectrum pigments have higher symmetry degree of molecular structures, and certain groups in the structures are activated by selective absorption of light in different wave bands, so that substitution and ring opening reactions are easy to occur, and the pigments fade. Compared with the common pigment, the prepared lyotropic liquid crystal emulsion coated liquid crystal structure pigment with high light fastness has excellent light fastness and can be applied to the coloring of various textiles.
3. In the preparation process of the pigment with the liquid crystal structure, the composite liquid crystal finishing agent cooperates with the auxiliary emulsifier to form a lyotropic liquid crystal emulsion coating structure on the surface of the pigment particles, so that the charge property of the surface of the pigment is changed, and the pigment is dispersed more uniformly. The pigment is easy to generate substitution reaction and ring-opening reaction after absorbing light energy and being activated, and the finishing agent with negative electricity on the surface of the pigment can effectively prevent the reaction. Starting from the sun-drying and fading reaction mechanism of the pigment, the liquid crystal structure inhibits or blocks the progress of the fading reaction, and can enhance the sun-drying resistance of the pigment. By the method, a series of liquid crystal structure pigments with high light fastness can be obtained.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the structure of the prepared lyotropic liquid crystal emulsion coated liquid crystal structure pigment.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention.
Embodiment one: preparation of liquid crystal structure pigment purple P.V.3 with high light fastness
The preparation method of the liquid crystal structure pigment violet P.V.3 lake pigment with high light fastness comprises the following steps: 10g of pigment violet P.V.3 was weighed into 250mL of deionized water, pH was adjusted to 5 using acetic acid, and dispersed to prepare a pigment dispersion. To the pigment dispersion was added 50gEmulsifier HP 30 liquid crystal emulsifier and 2.5g of sodium dodecylbenzenesulfonate. Homogenizing for 5min at 3000r/min, heating the solution to 70deg.C, maintaining the temperature, and stirring for 30min to obtain the liquid crystal structure pigment with emulsion coating of lyotropic liquid crystal. And then 5g of the liquid crystal structure pigment violet P.V.3 is taken and put into a sand mill together with 50g of dispersant NNO and zirconium beads to be ground for 2 hours, and finally the liquid crystal structure pigment violet P.V.3 with high light fastness is obtained.
Experimental example
The liquid crystal structured pigment with high light fastness prepared in example 1 was printed, comprising the steps of:
1g of pigment prepared in example 1 is taken, 3g of adhesive SP, 0.2g of thickener and deionized water are then taken to prepare 10g of color paste, and the polyester fabric is printed, pre-baked and baked. The fabrics were tested for apparent color depth values and light fastness.
Table 1: example 1 printing Property
Examples K/S value Fastness to light
1 21.749 5-6
Comparative example 1
1g of commercial pigment violet P.V.3 is taken, then 3g of adhesive SP, 0.2g of thickener and deionized water are directly prepared into 10g of color paste, and the polyester fabric is printed, pre-baked and baked. The fabrics were tested for apparent color depth values and light fastness.
Comparative example 2
1g of commercial pigment violet P.V.3 is taken, then 3g of adhesive SP, 0.2g of thickener, 2.5g of sodium dodecyl benzene sulfonate and deionized water are directly prepared into 10g of color paste, and the polyester fabric is printed, pre-baked and baked. The fabrics were tested for apparent color depth values and light fastness.
Table 2: comparative examples 1 and 2 printing Properties
Comparative example K/S value Fastness to light
1 20.1 3
2 21.413 3
Comparative example 3
1g of commercial pigment violet P.V.3 is taken, then 3g of adhesive SP, 0.2g of thickener, and ultraviolet-resistant finishing agents UV 360, 400, 531, 928 and 1577 with different concentrations are directly prepared into 10g of color paste, and the polyester fabric is printed, pre-baked and baked. The fabrics were tested for apparent color depth values and light fastness.
Table 3: printing Property of comparative example 3
Comparative example Amount of fabric reuse K/S value Fastness to light
UV 360 1% 22.031 3
UV 360 10% 22.98 4-5
UV 400 1% 22.529 3
UV 400 10% 22.73 3-4
UV 531 1% 23.424 3
UV 531 10% 21.989 4
UV 928 1% 20.817 3
UV 928 10% 21.8 3-4
UV 1577 1% 18.367 3-4
UV 1577 10% 20.489 4-5
Conclusion: referring to tables 1-3, compared with the commercial organic pigment, the liquid crystal structure pigment prepared by the method effectively improves the color fastness to sunlight, and meanwhile, the color fastness to sunlight of the liquid crystal structure pigment prepared by the method is better than that of the commercial organic pigment added with the anti-ultraviolet finishing agent.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (10)

1. The preparation method of the high-light fastness liquid crystal structure pigment is characterized by comprising the following steps of:
s1, adding pigment into deionized water, regulating the PH by using inorganic acid, dispersing to obtain pigment dispersion liquid, wherein the PH of the pigment dispersion liquid is 3-6.5, adding a composite liquid crystal finishing agent and an auxiliary emulsifier into the pigment dispersion liquid, dispersing, homogenizing and emulsifying the pigment dispersion liquid to obtain liquid crystal homogeneous emulsion, and the weight ratio of the pigment to the composite liquid crystal finishing agent to the auxiliary emulsifier to the deionized water is (1-5): 5-20:0.2-1.1:100;
s2, stirring the liquid crystal homogeneous emulsion at a high temperature, and cooling and standing to obtain the liquid crystal structure pigment with the lyotropic liquid crystal emulsified coating on the particle surface;
s3, putting the liquid crystal structure pigment into a grinder for grinding and dispersing, adding a dispersing agent, grinding together with the dispersing agent, and obtaining the liquid crystal structure pigment with high light fastness after finishing grinding.
2. The method for preparing a high light fastness liquid crystal structure pigment according to claim 1, wherein in the step S1, the pigment is one or more of azo pigments, lake pigments, heterocyclic pigments, condensed ring ketone pigments.
3. The method for preparing a high light fastness liquid crystal structure pigment according to claim 1, wherein in the step S1, the inorganic acid used for adjusting PH is one or more of formic acid, acetic acid, propionic acid, hydrochloric acid and sulfuric acid.
4. The method according to claim 1, wherein in the step S1, the composite liquid crystal finishing agent is one or more of glucosides, sucrose esters, glycerides, phosphonates, and lecithins.
5. The method according to claim 1, wherein in the step S1, the co-emulsifier is one or more of a surfactant containing various acid groups and a long-carbon chain fatty alcohol.
6. The method for preparing a high light fastness liquid crystal structure pigment according to claim 1, wherein in the step S1, the homogenizing emulsifying rotation speed is 2000-8000r/min, and the homogenizing time is 2-10min.
7. The method according to claim 1, wherein in the step S2, the temperature is raised to 50-90 ℃ during high temperature stirring, the stirring speed is maintained at 300-1000r/min, and the stirring time is maintained at 5-30min.
8. The method for preparing a high light fastness liquid crystal structure pigment according to claim 1, wherein in the step S2, the temperature is reduced to be at a temperature of 20-40 ℃ and the standing time is 2-8h.
9. The method according to claim 1, wherein in the step S3, the dispersant is one or more of fatty acid salts, oleic acid salts, alkyl sulfonic acid salts, aliphatic amides, paraffins, and metal soaps containing sulfonic acid groups.
10. Use of a liquid crystal structured pigment according to any one of claims 1 to 9 in the field of pigment printing, inkjet printing, food coloring, painting inks.
CN202310225017.6A 2023-03-07 2023-03-07 Preparation method and application of high-light fastness liquid crystal structure pigment Pending CN116376315A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101423672A (en) * 2007-10-31 2009-05-06 张瑞 Technology for preparing lyotropic liquid crystal template to separation and purification of natural pigment
CN107956168A (en) * 2017-11-22 2018-04-24 辽宁恒星精细化工有限公司 A kind of printing with reactive dye fabric increases the gorgeous finishing agent of deep increasing and preparation method
JP2021109123A (en) * 2020-01-08 2021-08-02 旭化成ワッカーシリコーン株式会社 Liquid crystal emulsification method and liquid crystal emulsion
CN115584143A (en) * 2022-07-18 2023-01-10 吴江山湖颜料有限公司 Preparation method of fast type basic lake pigment

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101423672A (en) * 2007-10-31 2009-05-06 张瑞 Technology for preparing lyotropic liquid crystal template to separation and purification of natural pigment
CN107956168A (en) * 2017-11-22 2018-04-24 辽宁恒星精细化工有限公司 A kind of printing with reactive dye fabric increases the gorgeous finishing agent of deep increasing and preparation method
JP2021109123A (en) * 2020-01-08 2021-08-02 旭化成ワッカーシリコーン株式会社 Liquid crystal emulsification method and liquid crystal emulsion
CN115584143A (en) * 2022-07-18 2023-01-10 吴江山湖颜料有限公司 Preparation method of fast type basic lake pigment

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈冬芝: "一种液晶乳化剂在个人护理产品中的研究", 《中国洗涤用品工业》, no. 6, 30 June 2022 (2022-06-30), pages 61 - 70 *

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