CN108716141B - High-settling-resistance and high-color-depth pigment nanocapsule coating, and preparation method and application thereof - Google Patents
High-settling-resistance and high-color-depth pigment nanocapsule coating, and preparation method and application thereof Download PDFInfo
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- CN108716141B CN108716141B CN201810387621.8A CN201810387621A CN108716141B CN 108716141 B CN108716141 B CN 108716141B CN 201810387621 A CN201810387621 A CN 201810387621A CN 108716141 B CN108716141 B CN 108716141B
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- 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
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1818—C13or longer chain (meth)acrylate, e.g. stearyl (meth)acrylate
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Textile Engineering (AREA)
- Polymerisation Methods In General (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a high-settling-resistance and high-color-depth pigment nanocapsule coating with good settling resistance, and also discloses a preparation method of the pigment nanocapsule coating, which comprises the following steps: a large amount of low-density, inert and volatile decamethylcyclopentasiloxane or octamethylcyclotetrasiloxane is added into acrylate monomers, and the organic pigment is subjected to nano-encapsulation treatment through miniemulsion polymerization to prepare the uniform and stable nano-capsule coating. The method has the advantages of green and environment-friendly preparation process, easily obtained raw materials, simple process and high pigment coating efficiency. The invention also provides a method for applying the pigment nanocapsule coating to fabric coating printing to obtain a dark color fabric with a K/S value of more than or equal to 25, wherein the air permeability retention rate of the printed fabric is more than 70%, the stiffness is increased by less than 30%, the dry and wet rubbing fastness is more than or equal to level 4, and the hand feeling subjective rating is more than or equal to level 4.
Description
Technical Field
The invention relates to the technical field of pigment capsule coatings in fine chemical engineering, in particular to in-situ miniemulsion polymerization preparation and application of a pigment nano capsule coating with high settling resistance and high color depth.
Background
Pigment printing is a printing technology which utilizes the principle that a binder forms a film on the surface of a fabric and adheres colorant particles which have no affinity and reactivity with the fabric to the fabric by virtue of the adhesion effect of the binder so as to obtain the required coloring effect. The coloring principle has wide applicability to fabrics, especially has no selectivity to coloring of a large number of blended fabrics, can greatly simplify the coloring processing flow, and improve the rate of certified products and the processing speed when processing products.
The nano encapsulation of the pigment can coat the adhesive polymer on the surface of the organic pigment in advance, thereby greatly improving the dispersibility and dispersion stability of the organic pigment in water. The emulsion after the organic pigment nano encapsulation is applied to pigment printing, so that the dosage of the adhesive is greatly reduced and the utilization efficiency of the adhesive is improved on the premise of ensuring the fastness.
However, the current organic pigment nano-capsule coating generally has the key problems of poor anti-settling property, difficulty in preparing dark fabrics and the like, and limits the application range of the coating. The poor anti-settling property is mainly caused by the fact that the density of most organic pigments is generally 1.3-2.1 g/cm3In between, much more than water, and thus the density of the pigment capsules is also generally greater than water, naturally tending to settle to the bottom. More importantly, the polymer on the surface of the pigment capsule has strong adhesion capability, and once the pigment capsules collide with each other, the polymer is easy to aggregate into blocks, so that the phenomenon of caking is generated, and the stability of the system is not facilitated. At present, the common solution in industry is to add a large amount of emulsifier and dispersant to solve the problems, but the practical situation shows that even if a large amount of emulsifier and dispersant is added to the emulsion, the emulsion cannot be kept non-settling for a long time, and once the pigment capsule settles to the bottom of the container, the polymer on the surface of the capsule is bonded to form irreversibleThe agglomerates, which are transferred, seriously affect the coating quality.
The difficulty in producing dark fabrics is mainly due to the fact that with pigment capsules prepared by in situ miniemulsion polymerization, too much organic pigment can gel the original pigment/monomer dispersion and cannot be prepared by miniemulsion polymerization. At present, researches show that the mass fraction of organic pigments in a pigment capsule film is difficult to exceed 12%, and the total amount of the coatings used by pigment capsules in pigment printing is small, so that the color depth and brightness of the current pigment capsule pigment printing fabric are difficult to guarantee while the hand feeling and the fastness are guaranteed.
Disclosure of Invention
Aiming at the technical problems, the invention provides the pigment nanocapsule coating with high settling resistance and high color depth, which has good settling resistance, can be used for preparing deep color fabrics with K/S value of more than or equal to 25, the air permeability retention rate of printed fabrics is more than 70%, the stiffness amplification is less than 30%, the dry and wet rubbing fastness is more than or equal to level 4, and the subjective hand feeling rating is more than or equal to level 4.
The pigment nano-capsule coating provided by the invention is obtained by an in-situ miniemulsion preparation method, the preparation process of the method is green and environment-friendly, the used raw materials are easy to obtain, the process is simple, and the pigment coating efficiency is high.
A preparation method of a pigment nanocapsule coating with high sedimentation resistance and high color depth comprises the following steps:
1) carrying out ultrasonic homogenization on octamethylcyclotetrasiloxane (D4) or decamethylcyclopentasiloxane (D5), acrylate monomer and organic pigment to obtain an oil phase mixed solution serving as a phase A, wherein the mass of D4 or D5 accounts for 30-60% of that of the phase A;
the structural formula of D4 is shown in formula I; d5 has a structural formula shown in formula II:
2) adding an emulsifier into the aqueous solution until the emulsifier is completely dissolved to serve as a phase B, mixing the phase A and the phase B in the step 1), and performing ultrasonic homogenization to obtain a fine emulsion; then transferring the miniemulsion into a reaction device, and carrying out polymerization reaction of the miniemulsion under the protection of inert gas and the action of an initiator to obtain the pigment nanocapsule coating with high settling resistance and high color depth;
the ultrasonic homogenization temperature is-5-0 ℃, and the ultrasonic time is 10-20 min.
The acrylate monomer in the step 1) is a mixture of Methyl Methacrylate (MMA), Octadecyl Acrylate (OA), Butyl Acrylate (BA), Ethylene Glycol Dimethacrylate (EGDMA), hydroxyethyl acrylate (HEMA) and glycidyl acrylate (GMA).
In the step 1), the acrylic ester monomer is selected mainly according to the polarity and the functionality, wherein methyl methacrylate, octadecyl acrylate and butyl acrylate are used as main adhesive monomers to provide main adhesive force; ethylene glycol dimethacrylate and glycidyl acrylate are used as cross-linking agents to improve the cross-linking degree of the adhesive; hydroxyethyl acrylate is mainly used to increase the hydrophilicity of the adhesive.
The organic pigment in the step 1) is one or more of C.I. pigment blue 15, C.I. pigment green 36, C.I. pigment violet 19, C.I. pigment red 122, C.I. pigment yellow 191, C.I. pigment yellow 81, C.I. pigment yellow 1, C.I. pigment yellow 3, carbon black and graphene; the addition amount of the pigment is 5-12% of the mass of the phase A.
The organic pigment filter cake is mainly based on organic pigments with strong lipophilicity and good compatibility with organic silicon, wherein the organic pigments comprise C.I. pigment blue 15, C.I. pigment green 36, C.I. pigment violet 19, C.I. pigment red 122, C.I. pigment yellow 191, C.I. pigment yellow 81, C.I. pigment yellow 1, C.I. pigment yellow 3, carbon black, graphene and the like, have stable chemical structures, have strong lipophilicity on the surface, and thus have good compatibility with organic silicon and acrylate monomers.
Step 1) the preferable dosage of D4 or D5 is 30-60% of the mass of the phase A, D4 and D5 are two liquids with low density, low viscosity and no double bond, do not participate in the free radical polymerization reaction of vinyl monomers, and exist in the fine emulsified liquid drop and the final pigment capsule in a liquid form in the system all the time, so that the density of the pigment capsule can be effectively reduced, and the pigment capsule is prevented from settling to the bottom of a container. In addition, in the film forming process of the pigment capsule emulsion, D4 and D5 are gradually volatilized in the heating and baking process, the mass proportion of pigment particles in the pigment capsule emulsion is gradually increased, the thickness of the adhesive film is also continuously reduced, and finally, the thin pigment composite adhesive film with high color depth is obtained. When the amount of D4 or D5 is less than 30%, the content is too low to lower the density of the pigment capsules well, and thus the settling resistance of the nanocapsule emulsion is not good. When the D4 or D5 is more than 60 percent, the density of the pigment capsules is reduced to be low enough, and the anti-settling property of the emulsion is excellent, but because the D4 or D5 is too high, the content of the acrylate polymer is too low, the cohesive force of the pigment composite adhesive film is greatly reduced, and the dry-wet rubbing fastness of the pigment capsule printed fabric is reduced to 1 level.
Preferably, the phase A adopts the following weight portion:
in the step 2), the emulsifier is prepared by compounding Sodium Dodecyl Sulfate (SDS), nonylphenol polyoxyethylene ether (OP-10) and sodium hydroxypropyl methacrylate sulfonate (HMPS). Due to the low surface energy of D4, D5, a strong emulsifying power is required to stabilize the polymerized monomer droplets containing a large amount of D4, D5. SDS and HMPS are two ionic emulsifiers with stronger emulsifying capacity, OP-10 is a commonly used non-ionic emulsifier, and the three emulsifiers are mixed and compounded to effectively improve the emulsifying stability of the phase B. The preferable dosage of the emulsifier is 5-10% of phase A.
In the step 2), the initiator is dibenzoyl peroxide or potassium persulfate, and the using amount of the initiator is 2-3% of that of the phase A; the reaction temperature of the miniemulsion polymerization is 60-70 ℃, and the reaction time is 1-2 h. Because D4 and D5 in the invention are volatile at high temperature, the polymerization temperature of the miniemulsion adopted in the invention cannot be too high, the reaction time cannot be too long, otherwise D4 and D5 can be volatilized in a large amount, and the D4 and D5 are difficult to store in the pigment capsule, so the preferable reaction temperature in the invention is 63-66 ℃. Meanwhile, in order to reduce the reaction time, the dosage of the initiator is properly increased, and the preferable dosage is 2.3-2.5% of the mass of the phase A.
In the step 2), the inert gas is selected from inert gases in a wide range in the field, and can be selected from one of nitrogen, argon, helium and the like, and from the viewpoint of saving cost, nitrogen is preferred.
The invention also provides application of the pigment nanocapsule coating with high settling resistance and high color depth in the field of textile pigment printing, which specifically comprises the following steps:
adding a thickening agent and water into the pigment nanocapsule coating with high settling resistance and high color depth, adjusting the viscosity according to the actual application requirement to prepare a pigment printing paste, and then applying the pigment printing paste to fabric printing by adopting a flat screen printing technology.
The pigment printing paste is prepared from the following raw materials in parts by weight:
80-90 parts of nano capsule coating;
1-5 parts of a thickening agent;
10-15 parts of water.
The thickening agent is an anionic thickening agent PTF formed by copolymerization of polyacrylate, the viscosity of the thickening agent PTF is less than or equal to 60cps, the pH value is 4-5, and the solid content is 18-29%.
In the invention, the stirring, the ultrasonic treatment, the flat screen printing and the like are typical unit operations in chemical and dye printing processes and can be realized by adopting the conventional device.
According to the invention, a large amount of low-density, low-viscosity and inert organosilicon component octamethylcyclotetrasiloxane (D4) or decamethylcyclopentasiloxane (D5) is added into a preparation formula of a miniemulsion of a conventional pigment capsule, so that the density and surface properties of the pigment capsule are changed, and the anti-settling property of the pigment capsule in an aqueous phase is enhanced. The coating provided by the invention is applied to fabric coating printing, after being heated and baked, D4 or D5 is heated and volatilized, the mass fraction and the color depth of the pigment in a final solid adhesive film are improved, the thickness of the adhesive film is reduced, and finally a composite capsule film with good pigment dispersion, ultra-thin and deep color can be formed on the surface of a fiber, so that a printed fabric with good fastness, hand feeling, air permeability and color depth is obtained, the color depth (K/S value) of the printed fabric exceeds 25, the air permeability retention rate of the printed fabric is greater than 70%, the stiffness is increased by less than 30%, and the dry-wet friction fastness is greater than or equal to level 4.
Compared with the prior art, the invention has the following beneficial effects:
(1) on the basis of nano encapsulation of the organic pigment, the invention introduces the low-density, low-viscosity and inert organic silicon component (D4 or D5) into the capsule, changes the density of the capsule and improves the anti-settling property of the pigment capsule in the water phase.
(2) The novel coating provided by the invention is applied to textile pigment printing, after being heated and baked, D4 and D5 attached to the interior of the nanocapsules on the surface of the textile volatilize together with water, and in the volatilization process, the thickness of the pigment composite adhesive film gradually decreases, and the color gradually becomes dark. Therefore, the coating can obtain the pigment printed fabric with the color depth (K/S value) of more than 25, the air permeability retention rate of the printed fabric of more than 70 percent, the stiffness amplification of less than 30 percent and the dry and wet rubbing fastness of more than or equal to grade 4 under the condition of lower pigment consumption.
(3) The preparation process of the pigment nanocapsule coating with high settling resistance and high color depth, which is prepared by the invention, is green and environment-friendly, the used raw materials are easy to obtain, the process is simple, and the product can be directly used in the production process of the existing pigment printing, so that the quality of printed fabrics is comprehensively improved.
Drawings
FIG. 1 is a schematic view of the in-situ miniemulsion polymerization preparation and application process of the pigment nanocapsule coating with high sedimentation resistance and high color depth in examples 1-15 of the present invention.
FIG. 2 is a surface SEM image of a nano-capsule emulsion polyester printed fabric in examples 4-5 and comparative example 2 of the invention, wherein a is a surface SEM image of a nano-capsule emulsion polyester printed fabric in comparative example 2; b is a surface SEM image of the nano-capsule emulsion polyester printed fabric of example 5; and c is the surface SEM picture of the nano-capsule emulsion terylene printed fabric of the example 4.
FIG. 3 is a graph comparing the particle size of the nanocapsule emulsions of examples 1, 4, 7, 8, 12 of the present invention and comparative example 2.
FIG. 4 is a transmission electron micrograph of the nanocapsule emulsion in example 4 of the present invention.
FIG. 5 is a transmission electron micrograph of the nanocapsule emulsion in example 8 of the present invention.
Detailed Description
The compositions of the synthetic formulas in the examples and comparative examples of the specific embodiment of the present invention are shown in table 1, the emulsifier components are shown in table 2, and the corresponding performance test results are shown in table 3.
The characterization methods referred to in the examples and comparative examples illustrate:
1. testing the settleability of the nano-capsule emulsion:
weighing a certain amount of the nano-capsule emulsion, and testing the solid content (marked as W)1) Then the emulsion was centrifuged at 10000 r.min in a TGL-16G model high speed centrifuge-1Centrifuging at rotating speed for 60min, taking out the upper liquid, and measuring the solid content (W)2)。
Define weight loss rate W ═ W2/W 1100% by weight, the sedimentation resistance is evaluated in terms of the W value, the W value ranges from 0 to 100%, and a larger W value indicates a better sedimentation resistance of the emulsion.
2. And (3) determining the printing effect of the pigment:
1) measurement of the colorimetric value of printed textiles
The pigment depth refers to the visual depth feeling or color concentration given to people by the color of an opaque solid substance, and the size of the pigment depth is usually influenced by various factors such as the content of the colored substance in the solid substance, the physical state of the colored substance, the optical property of the solid surface and the like, the size of the color depth value is usually represented by a K/S value, and the larger the K/S value is, the darker the color is represented; the smaller the K/S value, the lighter the color.
The testing method adopts a Datacolor650 type color measuring and matching instrument to measure the K/S value of a dyed sample, and five different points of each sample are used for measuring color and calculating the average value of the five different points.
2) Measurement of Dry and Wet rub fastness
The dry and wet rubbing fastness test refers to GB/T3920-1997 standard. The sample was 50mm X200 mm, two each in warp and weft direction, and the standard rubbing cotton cloth was 50mm X50 mm.
3) Hand feeling Performance test
Grading the fabric subjected to eye-closing touch finishing by a small group of 5-10 people, and evaluating the hand feel of the printed fabric according to different hand feels, wherein the specific evaluation method comprises the following steps: the hand feeling grading is carried out from two aspects of softness and smooth feeling, the grade is 5, the grade 1 is the worst, the fabric hand feeling is hard, the smooth feeling is poor, the grade 5 is the best, and the fabric hand feeling is soft and smooth.
4) Air permeability test
The air permeability of the printed fabric was measured by using a digital air permeability instrument, model YG461E, manufactured by Ningbo textile instruments and factories, according to GB/T5453-1997 determination of air permeability of textile fabrics.
The air permeability retention rate is the air permeability of the printed fabric/the air permeability of the original cloth.
Examples 1 to 15
The first step is as follows: according to the formula of the formula shown in the table 1, D4 or D5 with a certain mass is stirred and mixed with an organic Pigment (Pigment) and an acrylate monomer (Acr), and the mixture is subjected to uniform ultrasonic treatment to obtain an oil phase mixed solution as an A phase.
The second step is that: three emulsifiers were added to the aqueous solution according to the formulation of table 2 until completely dissolved as phase B.
The third step: mixing the phase A and the phase B, and performing ultrasonic homogenization to obtain a fine emulsion; and then transferring the miniemulsion into a reaction device, and carrying out miniemulsion polymerization under the protection of nitrogen and the action of an initiator dibenzoyl peroxide to obtain the pigment nanocapsule coating with high settling resistance and high color depth.
The fourth step: and (3) uniformly mixing 20g of the prepared nano-capsule emulsion with 0.5g of a thickening agent PTF (anionic thickening agent, the viscosity of the nano-capsule emulsion is 40cps to 50cps, the pH value of the nano-capsule emulsion is 4.5, and the solid content of the nano-capsule emulsion is 23 percent), adding water, stirring to a certain consistency, and performing flat screen printing on the fabric. The printed fabric is pre-dried in a low-temperature (60 ℃) oven for 5min, and then is placed in an oven for baking at 120 ℃ to obtain a printed finished product.
The preparation and application flow diagrams of the in-situ miniemulsion polymerization described in the above examples are shown in FIG. 1. Surface SEM images of the nano-capsule emulsion polyester printed fabrics in examples 4-5 and comparative example 2 are shown in FIG. 2, and it can be seen from FIG. 2 that the adhesive film becomes thinner gradually and the protrusions are increased obviously with the increase of the content of D4. The nanocapsule emulsion of example 4 has a high D4 content and is pigment printed with it, and the polymer film on the baked surface of the printed fabric is found to be very thin and to fit tightly to the surface of the fibre (panel c in figure 2). The structure can ensure that the printed fabric has good fastness and can ensure that the printed fabric has soft hand feeling.
Further, a comparison graph of the particle size of the nanocapsule emulsions of examples 1, 4, 7, 8, 12 and comparative example 2 is shown in FIG. 3. The transmission electron micrograph of the nanocapsule emulsion in example 4 is shown in fig. 4; the transmission electron micrograph of the nanocapsule emulsion in example 8 is shown in fig. 5.
Comparative example 1
The organic pigment mass (10g) in example 4 was mixed with an aqueous emulsifier solution and then ball milled with zirconium beads for 3 hours to obtain an organic pigment suspension. Then, a proper amount of commercially available polyacrylate adhesive is added into the organic pigment suspension, the mixture is uniformly mixed and stirred, the anti-settling performance of the mixture is tested, and then the mixed solution (20g) is mixed with the same mass of thickening agent in the embodiment 4 to prepare the printing paste with certain viscosity. And (3) performing warp-wise manual scraping printing on the polyester plain weave fabric, pre-drying the printed fabric in a 60 ℃ drying oven for 5min, and then placing the printed fabric in a 120 ℃ drying oven for baking to obtain a printed finished product.
Comparative example 2
The first step is as follows: according to the formula of the formula shown in the table 1, D4 or D5 with a certain mass is stirred and mixed with an organic Pigment (Pigment) and an acrylate monomer (Acr), and the mixture is subjected to uniform ultrasonic treatment to obtain an oil phase mixed solution as an A phase.
The second step is that: three emulsifiers were added to the aqueous solution according to the formulation of table 2 until completely dissolved as phase B.
The third step: mixing the phase A and the phase B, and performing ultrasonic homogenization to obtain a fine emulsion; and transferring the miniemulsion into a reaction device, carrying out miniemulsion polymerization under the protection of nitrogen and under the action of an initiator dibenzoyl peroxide to obtain the high-settling-resistance and high-color-depth pigment nanocapsule coating, and testing the settling resistance of the pigment nanocapsule coating.
The fourth step: and (3) uniformly mixing the prepared nano-capsule emulsion (20g) with a proper amount of thickening agent, stirring and adjusting to a certain consistency, and printing the polyester plain weave fabric by using a flat screen. The printed fabric is pre-dried in a low-temperature (60 ℃) oven for 5min, and then is placed in an oven for baking at 120 ℃ to obtain a printed finished product.
As can be seen from Table 3, when the pigment nanocapsule coating with high settling resistance is used for fabric pigment printing, the pigment printed fabric with dry and wet rubbing fastness of 4-5 grades, the highest air permeability retention rate of the printed fabric can reach more than 90 percent, the color depth is high, and the hand feeling is soft can be obtained. Compared with the blended printing pigment color paste of the pigment and the coating and the conventional polyacrylate pigment capsule coating color paste, the pigment nanocapsule coating prepared by the invention has extremely high sedimentation resistance and stability.
TABLE 1
TABLE 2
| Examples | SDS/g | OP-10/g | HMPS/g |
| Example 1 | 4 | 1 | 2 |
| Example 2 | 1 | 1 | 5 |
| Example 3 | 1 | 3 | 5 |
| Example 4 | 2 | 3 | 2 |
| Example 5 | 3 | 1 | 2 |
| Example 6 | 3 | 2 | 2 |
| Example 7 | 3 | 1 | 1 |
| Example 8 | 2 | 3 | 2 |
| Example 9 | 2 | 3 | 2 |
| Example 10 | 5 | 2 | 1 |
| Example 11 | 2 | 3 | 2 |
| Example 12 | 2 | 3 | 2 |
| Example 13 | 2 | 4 | 2 |
| Example 14 | 2 | 3 | 2 |
| Example 15 | 4 | 3 | 1 |
| Comparative example 2 | 2 | 3 | 2 |
TABLE 3
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description herein, since various changes and modifications can be made in the details of the embodiment and the application range according to the spirit of the present invention.
Claims (10)
1. A preparation method of a pigment nanocapsule coating with high sedimentation resistance and high color depth comprises the following steps:
1) d4 or D5, an acrylate monomer and an organic pigment are subjected to ultrasonic homogenization to obtain an oil phase mixed solution serving as a phase A, wherein the mass of D4 or D5 accounts for 30-55.3% of the mass of the phase A;
the structural formula of D4 is shown in formula I;
the structural formula of D5 is shown in formula II:
2) adding an emulsifier into the aqueous solution until the emulsifier is completely dissolved to serve as a phase B, mixing the phase A and the phase B in the step 1), and performing ultrasonic homogenization to obtain a fine emulsion; under the protection of inert gas and the action of an initiator, carrying out polymerization reaction of miniemulsion to obtain the pigment nanocapsule coating with high settling resistance and high color depth.
2. The method for preparing a pigment nanocapsule coating material with high sedimentation resistance and high color depth according to claim 1, wherein in step 1), the acrylic ester monomer is a mixture of methyl methacrylate, octadecyl acrylate, butyl acrylate, ethylene glycol dimethacrylate, hydroxyethyl acrylate and glycidyl acrylate.
3. The preparation method of the pigment nanocapsule coating with high sedimentation resistance and high color depth according to claim 1, wherein in step 1), the phase A adopts the following weight parts:
4. the method for preparing the pigment nanocapsule coating material with high sedimentation resistance and high color depth according to claim 1, wherein in the step 2), the emulsifier is prepared by compounding sodium dodecyl sulfate, nonylphenol polyoxyethylene ether and sodium hydroxypropyl methacrylate sulfonate; the addition amount of the emulsifier is 5-10% of the mass of the phase A.
5. The method for preparing pigment nanocapsule coating material with high sedimentation resistance and high color depth according to claim 1, wherein in step 2), the initiator is dibenzoyl peroxide or potassium persulfate, and the amount of the initiator is 2-3% of phase A.
6. The method for preparing a pigment nanocapsule coating material having a high sedimentation resistance and a high color depth according to claim 1, wherein in step 2), the reaction temperature of the polymerization reaction of the miniemulsion is 60 to 70 ℃ and the reaction time is 1 to 2 hours.
7. The method for preparing a pigment nanocapsule coating material having a high sedimentation resistance and a high color depth according to claim 6, wherein the reaction temperature of the polymerization reaction of the miniemulsion in step 2) is 63 to 66 ℃.
8. The pigment nanocapsule coating with high settling resistance and high color depth prepared by the preparation method according to any one of claims 1 to 7.
9. Use of the pigment nanocapsule coating having high sedimentation resistance and high color depth according to claim 8 in the field of textile pigment printing.
10. The application of the printing paste as claimed in claim 9, wherein the required pigment printing paste for textiles is prepared from the following raw materials in parts by weight:
80-90 parts of nano capsule coating;
1-5 parts of a thickening agent;
10-15 parts of water;
the thickening agent is an anionic thickening agent PTF formed by copolymerization of polyacrylate, the viscosity of the thickening agent PTF is less than or equal to 60cps, the pH value is 4-5, and the solid content is 18-29%.
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| CN113088142A (en) * | 2021-04-26 | 2021-07-09 | 宇虹颜料股份有限公司 | Method for preparing acrylic paint by directly using organic pigment filter cake |
| CN113308915B (en) * | 2021-05-17 | 2022-04-15 | 英德科迪颜料技术有限公司 | Printing paste and preparation method thereof |
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