JPH10330661A - Disperse dye ink for jet printing and ink jet printing - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a disperse dye ink high in a particle-forming ability, good in disperse stability and long period preservability and little in the clogging of filters and nozzles during the continuous extrusion of the ink. SOLUTION: This disperse dye ink for ink jet printing is used for an ink jet printing system comprising imparting an ink containing a dyeable dye to a fabric as ink drops from a nozzle by the ink jet printing method, subjecting the imparted ink to a color-developing treatment, washing and subsequently drying. Therein, the dye ink has the following characteristics. An anionic oligomer-dispersing agent having a functional group is used as a dispersing agent for the disperse dye for the ink jet printing. A water-soluble high boiling point organic solvent in the ink has a surface tension of >=46 dyne/cm. The value of an inorganic property/an organic property is 2-6. The water-soluble high boiling pint organic solvent is contained in an amount of 5-70 wt.% in the ink. The viscosity of the ink is <=10 cP at 25 deg.C.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a disperse dye ink for ink-jet printing, which prints a fabric by an ink-jet method (hereinafter, also simply referred to as "disperse dye ink").
And an inkjet printing method.

[0002]

2. Description of the Related Art At present, textile printing is performed by screen printing or roller printing. For these, prior to dyeing, it is necessary to prepare a printing plate or screen plate for printing.

[0003] The production of a plate is time-consuming and labor-intensive, very expensive and, unless production over a certain amount is performed, will not be cost effective.
Recently, a plateless electronic printing system has been demanded.

[0004] For example, in the current printing method, it takes 6 to 16 weeks from receiving an order to making the first production sample. However, recent retailers have only ordered a very small portion of the goods at the beginning of the season, and then, using real-time point-of-sale data, have been able to recreate only the styles, colors and sizes that are actually selling. I want to order.

[0005] Therefore, the order size is significantly reduced,
Manufacturers have come to demand the ability to supply small orders in a timely manner. At present, in the dyeing industry and the apparel industry, quick response that can respond quickly to customer demands is emphasized. Technology has been proposed.

[0006] Among them, ink jet printing is most expected. The reason for this is that the dye can be directly supplied to the cloth without the need to transfer intermediate toner or ink.

As described above, the features of ink-jet printing are as follows.
Eliminates the need for expensive engraving rolls and screen molds.

Since the time required for mold production is eliminated, production becomes possible immediately after receiving an order.

Further, it is easy to change the design and the color arrangement, and it is possible to immediately respond to the user's request.

[0010] Since it can be linked with the CAD system, it is easy to store the design, and there is no limitation on the design,
You can freely reproduce the design. In addition, dyes that have been used in conventional dyeing and have a proven track record can be used.

There are the following advantages.

On the other hand, the problem of ink-jet printing is that a sufficient density of color is formed. The nozzle is not clogged. The dispersion stability of the ink is good. The storage stability of the ink is good. The excessive bleeding is not caused. To get the average quality.

The ink jet system includes a thermal system in which a heater is rapidly heated to foam and discharge ink, and a piezo system in which a piezo element is vibrated to discharge ink.

In the thermal method, the head has no moving parts,
Since it can be manufactured by semiconductor technology, there is an advantage that the head can be arranged at a high density. However, since the head and the ink are overheated to a high temperature, the life of the head is short, and there are disadvantages that the thermal stability of the ink is greatly restricted.

The piezo method has the advantage that the ejection force is strong, the control of ink droplets is easy, and the image is excellent. However, since the head has a movable part, the structure becomes complicated and the nozzles cannot be arranged at high density. There are drawbacks.

However, as compared with the thermal method, there is a great advantage that the life of the head is longer and there is less restriction on ink.

In each of the methods, since the ink is ejected from a thin nozzle, clogging of the nozzle is the biggest problem.

Most of the current inkjet inks use a water-soluble dye, and the particle-dispersed inks cannot solve nozzle clogging and are hardly used.

The present invention relates to a disperse dye ink used for printing a polyester cloth as a cloth.

Since the polyester cloth is hydrophobic, the printing is performed by dispersing the hydrophobic disperse dye in water in the form of fine particles.

In the printing of a polyester cloth by an ink jet technique, an ink in which a disperse dye is dispersed in fine particles is discharged from a nozzle onto a cloth which has been subjected to a bleeding prevention treatment to form an image.

Further, the cloth is heated to a temperature equal to or higher than the glass transition temperature of the polyester (for example, at 150 to 220 ° C.), so that the dye penetrates into the fiber and is dyed.

The dyed cloth contains a large amount of a dispersant, an activator, a high-boiling solvent, a pretreatment agent, and the like in addition to the undyed disperse dye. Rinse with water to reduce wash resistance, give it a greasy feel, and give it a stiff feel.

As described above, the ink jet ink for textile printing in which the disperse dye is dispersed in the form of fine particles is required to have a small dispersed particle diameter, a narrow distribution range of the particle diameter, and good dispersion stability. That is, no agglomerates are generated, and nozzles and filters are not blocked. For this reason, disperse dye
It is necessary to disperse such that the particle diameter is as fine as possible and the distribution range of the particle diameter is as narrow as possible, and this state must be maintained for a long time.

The process of dispersing hydrophobic particles in water consists of wetting, mechanical disintegration and dispersion stabilization.

A suitable wetting agent is added to the hydrophobic dye to bring the secondary aggregates of the disperse dye into intimate contact with water,
A mechanical impact force and a shear force are applied to achieve atomization.

Further, the dispersed particles are bound again,
The polymer activator is adsorbed on the particle surface to cover the surface so as not to generate aggregates, and the particles are three-dimensionally stabilized.

The disperse dye has a solubility in water of 0.1 g.
/ L or less and extremely hydrophobic.

When such a hydrophobic dye is finely dispersed in water, if the interfacial energy of the particles and water is large, it is difficult to atomize the hydrophobic dye. Therefore, a surfactant having a strong wetting action is applied to the surface of the hydrophobic dye. It is necessary to adsorb and hydrophilize and reduce the interfacial energy between water and particles.

Further, in order to maintain the dispersion stability for a long period of time, it is necessary to prevent the activator from being desorbed from the particle surface.

However, an active agent having a strong wetting action has a low affinity for a disperse dye, and is easily desorbed from the particle surface during storage, particularly when the environmental temperature changes.

Therefore, in order to maintain the dispersion stability for a long period of time even when environmental conditions change, it is necessary to share a surfactant which is strongly adsorbed on the particle surface and is not easily desorbed.

In order to strongly adsorb the surfactant to the disperse dye, it is preferable that the structure of the hydrophobic part of the activator is similar to the structure of the disperse dye.

Further, in order to maintain the dispersion stability for a long period of time even under extreme environmental conditions such as high temperature and low temperature, an activator having a functional group capable of binding to a functional group of the disperse dye is preferable.

Further, to effectively cover the particle surface, a high molecular weight, high molecular weight activator is preferable.

Since the polymer activator has a plurality of hydrophobic parts and hydrophilic groups in one molecule, it is advantageous because it can effectively coat the particle surface and stabilize the particle three-dimensionally.

The present invention relates to an ink in which a disperse dye is finely dispersed in water. The solubility of the disperse dye in water of a medium has a great influence on the storage stability and stability of the dispersed particles. Disperse dyes are sparingly soluble in water but have some water solubility.

In particular, as the particle size decreases, the solubility increases. If the particle size distribution is broad, so-called Ostwald ripening, in which small particles dissolve and precipitate on large particles during storage, occurs, and the particle size gradually increases, causing sedimentation and aggregation.

Further, the solubility of the disperse dye is greatly affected by a water-soluble high-boiling organic solvent coexisting in the ink.

In the ink-jet ink, use of a water-soluble high-boiling organic solvent is indispensable to prevent drying of the nozzle.

This water-soluble high-boiling organic solvent dissolves the disperse dye. The water-soluble high-boiling organic solvent usually has an ink amount of 5%.
Since 〜50% is used, the dissolving action of the water-soluble high-boiling organic solvent has a very large effect on the dispersion stability.

In general, the solubility of the disperse dye increases as the environmental temperature increases, and decreases as the environmental temperature decreases. If the ink is exposed to temperature changes during storage, it will gradually increase in particle size and eventually aggregate. For this reason, even at room temperature, even if the ink maintains dispersion stability for a long time, it easily aggregates at a high temperature. If the particle size increases during storage, the filter, the ink chamber inlet nozzle and the discharge nozzle inside the head are more likely to be closed.

JP-A-60-133076 and JP-A-60-2
29969, 61-215783, 61-24
No. 1371, No. 61-247762, No. 62-101
No. 73, No. 62-11780, No. 62-121776
No. 63-159484, No. 61-31469,
JP-A-61-213273, JP-A-4-59282, and the like, which disperse a disperse dye by using a nonionic dispersant obtained by adding ethylene oxide to a styrenated phenol or an anionic dispersant obtained by sulfonating the same. Ink has been published.

However, since the nonionic dispersant does not impart a charge to the particles, the dispersion is not stabilized by the repulsion of the charge, so that the dispersion stability is inferior to the anionic dispersant.

Further, since the ethylene oxide chain in the nonionic dispersant binds to the disperse dye to form a complex, the effect of solubilizing the disperse dye is large, which is not preferable in terms of stability.

Accordingly, these dispersants are widely used in conventional screen printing and the like, but are not necessarily suitable as dispersants for ink-jet inks because of the high solubility of the disperse dye.

JP-A-6-41878, JP-A-61-1
No. 48275 discloses a disperse dye ink dispersed using a formalin condensate of naphthalenesulfonic acid. However, this dispersant does not have a functional group capable of binding to the functional group of the disperse dye, and thus has insufficient storage stability. In particular, if the temperature rises to 60 ° C. or higher during storage, it will settle.

JP-A-8-143802, JP-A-8-143
Nos. 803 and 8-143804 use a styrene-acrylic acid-methyl methacrylate copolymer as a dispersant and use a nonionic activator of ethylene oxide or a copolymer of ethylene oxide and propylene oxide. A thermal inkjet ink has been disclosed.

However, since these dispersants have no functional group, the dispersion has poor stability at high temperatures. Further, a nonionic activator containing ethylene oxide or propylene oxide forms a complex with a disperse dye, so that the solubility of the disperse dye is high, which is not preferable.

JP-A-8-176482 discloses an agglomerated dispersion type ink in which a disperse dye is dissolved in a water-soluble high-boiling organic solvent and poured into water to form fine particles. Among them, in order to enhance the dispersion stability, the solubility of the disperse dye in a mixture of water and a water-soluble high-boiling organic solvent is specified to be 0.5 wt% or less. This method is not practical because the solubility and precipitation of the disperse dye greatly affect the dispersibility.

JP-A-8-67848 describes dispersing a disperse dye with a styrene-maleic anhydride copolymer dispersant, but the styrene-maleic anhydride copolymer has a low affinity for the disperse dye, Dispersion stability cannot be expected.

[0052]

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide an ink jet printing system which has a high ability to form fine particles, has a good dispersion stability, has a good long-term storage property, and has little clogging of filters and nozzles during continuous discharge. An object of the present invention is to provide a disperse dye ink and an ink jet printing method.

[0053]

The object of the present invention is achieved by the following constitution.

1. A disperse dye for inkjet printing used in an inkjet printing system in which an ink containing a dye that can be dyed is applied to the fabric as ink droplets from a nozzle by an inkjet method, and then subjected to color development, washing, and drying. An anionic oligomer dispersant having a functional group is used as the dispersant, and the water-soluble high-boiling organic solvent in the ink has a surface tension of 46 dyne / cm or more and an inorganic / organic value of 2 to 6 Wherein the ink contains the water-soluble high-boiling organic solvent in an amount of 5 to 70% by weight and has a viscosity at 25 ° C. of 10 cp or less.

2. (1) The disperse dye ink for ink-jet printing has an average particle diameter of 0.25 μm or less and a maximum particle diameter of 0.4 μm or less.
5. The disperse dye ink for inkjet printing according to item 1.

3. 3. The disperse dye ink for ink-jet printing described in 1 or 2, wherein the disperse dye ink for ink-jet printing contains 1 wt% or less of the disperse dye particles for ink-jet printing having a particle size of 0.1 μm or less.

4. An ink jet nozzle for applying the disperse dye ink for ink jet textile printing according to any one of the above items 1 to 3 to a fabric, ejects the ink using mechanical energy due to deformation of a piezo, and has a nozzle diameter of 1
An ink-jet printing method, characterized in that an ink is applied to a cloth by an ink-jet printer having 0 to 40 μm and having 60 or more nozzles.

Hereinafter, the present invention will be described in more detail.

The biggest problem with particle-dispersed inks is that coarse particles block nozzles, orifices, and filters. In order to prevent this, it is necessary to make the particles as fine as possible.

However, if the particles are excessively finely divided, the surface area increases, the dispersion becomes unstable, and the solubility of the particles increases, so that the particle diameter increases during storage. Therefore, there is an optimum range. .

The present invention solves the incompatibility problem of making fine particles and stabilizing dispersion by using a surfactant having a wetting action, an anionic oligomer dispersant having a functional group, and a disperse dye for inkjet printing (hereinafter simply referred to as a disperse dye). This problem has been solved by combining a water-soluble high-boiling organic solvent which hardly dissolves (also referred to as a dye) and controlling the particle size range.

Usually, an ink jet printer is used in an environment at around room temperature, for example, at a temperature of 10 to 50 ° C., and it is sufficient that the dispersion of the ink is maintained within this range. However, considering long-term storage, it is necessary to be stable in a temperature range of -10 to 70C. However, when the temperature exceeds 60 ° C., the dispersion stability is extremely reduced.

The reason is presumed that the dispersant adsorbs on the surface of the particles of the disperse dye and achieves fine dispersion of the disperse dye, thereby maintaining the dispersion stability. (60 ° C. or higher), the dispersant seems to be easily desorbed.

At a high temperature, the solubility of the disperse dye increases, and Ostwald ripening is likely to occur. At room temperature, for a long time,
Even if the dispersion stability can be maintained, if the temperature is increased and stored, aggregation occurs in a short time for the above-described reason. For example,
A dispersion that can maintain dispersion stability at 25 ° C. for 2 years can be stored at 70 ° C. for only 2 weeks.

The dispersant of the present invention has a hydrophobic portion having a polycyclic structure, and the hydrophobic portion can form a hydrogen bond with a functional group of a disperse dye.
It is characterized by having a functional group.

The hydrophobic part of the dispersant of the present invention has a high affinity because it has a similar structure to the disperse dye having a polycyclic structure, so that the dispersant has not only a strong physical adsorption to the disperse dye but also a functional property of the disperse dye. Hydrogen bonding to the group causes extremely strong adsorption, and it is considered that the substance is hardly desorbed even when stored at a high temperature or for a long time at room temperature.

Further, since a water-soluble high-boiling organic solvent which does not dissolve the disperse dye is used, an increase in particle size due to a change in environmental temperature or an increase in solubility is unlikely to occur.

The disperse dye used for dyeing polyester fibers generally has a polycyclic structure such as a benzene ring, a naphthalene ring, an anthraquinone ring or a quinophthalone ring.

The polycyclic structure has an —OH group, an —NH ₂ group,
-N (R) and a hydrophilic group such as ₂ group, -NO ₂ group, -CN group,
A functional group such as a —COOR group, a —SO ₂ R group, a —CO group, or a halogen atom is bonded. R represents a C ₁ -C ₄ linear or branched alkyl group.

The anionic oligomeric dispersant having a polycyclic structure having a functional group used in the present invention has not only strong physical adsorption but also a strong physical adsorption because its polycyclic structure is similar to the polycyclic structure of the disperse dye. Since the functional group is hydrogen-bonded with the functional group of the disperse dye, it does not desorb even under severe conditions such as high temperature, and can maintain dispersion stability for a long period of time.

The polycyclic structure of the anionic oligomer dispersant having a functional group of the present invention refers to a condensed ring of benzene, naphthalene, anthracene, phenanthrene or the like.

The functional groups of the anionic oligomer dispersant of the present invention are a phenolic hydroxyl group and an alcoholic hydroxyl group, and a phenolic hydroxyl group is particularly preferable.

The degree of polymerization of the anionic oligomer dispersant having a functional group of the present invention is preferably from 2 to 10 nuclei obtained by condensing a hydrophobic part with formalin. Alternatively, a molecular weight of 5,000 to 10,000 is preferred.

The higher the molecular weight, the better the dispersibility but the lower the water solubility and the higher the viscosity. Therefore, 2 to 5 nuclei or a molecular weight of 5,000 to 10,000 are preferred.

The dispersant of the present invention is an anionic oligomer dispersant in which the hydrophobic part has the same aromatic polycyclic structure as the disperse dye and has a functional group capable of bonding to the functional group of the disperse dye in the hydrophobic part. Preferably, there is.

Since one molecule contains a plurality of anionic groups, it is possible to effectively impart a charge to the particles and stabilize the dispersion by repelling the charges.

The anionic oligomer dispersant having a functional group is strongly adsorbed on the particle surface, exhibits an excellent dispersion stabilizing effect, and makes the effect of the present invention more remarkable.

The nozzle diameter of the ink jet head of the present invention is becoming smaller in order to increase the resolution of an image.
４０40 μm, and the number of nozzles is 60 or more in order to increase the printing speed. The diameter of a filter provided between the ink tank and the head for removing foreign matter and removing bubbles is about 50 microns. The diameter of the inlet nozzle of the ink chamber of the piezo type inkjet head is 4
It is about 0 microns.

For this reason, the average particle diameter of the disperse dye ink is preferably as small as possible, usually 0.5 μm or less, more preferably 0.15 to 0.25 μm or less.

If the particle diameter exceeds 0.5 μm, the particles precipitate during storage and pass through agglomeration and block the nozzle or filter.

The average particle size is more preferably 0.15 to 0.25 microns or less. At 0.25 microns or less, Brownian motion predominates over sedimentation.
It is difficult for sedimentation and clogging.

However, if it is less than 0.15 μm, dispersion becomes difficult and a large amount of a dispersant is required, so that the viscosity of the ink is undesirably increased. Further, since the solubility of the particles increases and the particles easily aggregate during storage, it is preferable that particles of 0.1 μm or less exist in the ink at 1 wt% or less.

The blockage of the nozzle or the filter depends not only on the average particle diameter but also on the maximum particle diameter. The maximum particle size is preferably 0.8 μm or less, more preferably 0.5 μm or less. More preferably, it is 0.4 microns or less. The maximum particle size can be controlled by selecting a dispersant, a dispersion time, and a filter.

The particle diameter is measured using a Shimadzu laser diffraction type particle size distribution analyzer, and the average diameter and 99% cumulative frequency distribution are expressed as an average diameter and a maximum particle diameter, respectively.

A dispersant whose hydrophobic part does not have an aromatic polycyclic structure is not preferred because it has low affinity with a disperse dye and low long-term dispersion stability and high-temperature dispersion stability.

Those having no functional group such as phenolic hydroxyl group in the hydrophobic part are not preferred because they have low affinity for disperse dyes and low long-term dispersion stability and high-temperature dispersion stability.

Nonionic dispersants are not preferred because the ethylene oxide chains solubilize the disperse dye.

The nonionic dispersant does not impart a charge to the particles, and therefore is not preferred in terms of dispersion stability.

The viscosity of the ink is 10 cp or less at 25 ° C. If the viscosity exceeds 10 cp, the flow resistance of the nozzle portion increases, and the discharge amount decreases. The viscosity is controlled by the amount of the dispersant and the dispersion time.

The dispersant of the present invention is, for example, a formalin condensate of sodium creosote oil sulfonate, (1) a formalin condensate of sodium cresol sulfonate and sodium 2-naphthol-6-sulfonate, (2) cresol sulfonic acid Formalin condensate of sodium, (3) Formalin condensate of sodium phenolsulfonate, (4) Formalin condensate of sodium β-naphtholsulfonate, (5) Formalin condensation of sodium β-naphtholsulfonate and sodium β-naphtholsulfonate (6) Lignin sulfonate, (7) and the like.

Creosote oil has a polycyclic structure such as naphthalene, anthracene, phenanthrene and the like.

Cresol and naphthol have a phenolic hydroxyl group. Lignin is a product obtained by condensing a plurality of phenylpropane structures and has an alcoholic hydroxyl group and a phenolic hydroxyl group.

Among the above-mentioned dispersants, an activator using creosote oil as a raw material is superior to the disperse dye of the present invention in the form of fine particles and excellent stability, does not cause foaming or gelation, and has good properties. It was found to give fluidity.

Further, the lignin sulfonate has a dispersibility,
It was found that the dispersion stability was excellent and the viscosity of the dispersion was low, which was preferable. This is thought to be due to sulfonic acid groups, carboxyl groups, alcoholic hydroxyl groups, and phenolic hydroxyl groups, which are produced from pulp manufacturing wastewater.

Preferred wetting agents for the present invention are wetting agents such as sodium dodecylbenzenesulfonate, sodium 2-ethylhexylsulfosuccinate, ethylene oxide adduct of sodium alkylnaphthalenesulfonate and nonylphenol, and ethylene oxide adduct of acetylene diol. Activators that are excellent in are preferred.

Depending on the structure of the disperse dye to be used, foaming, gelling, or poor fluidity may occur during dispersion. Therefore, the dispersant or wetting agent has a wetting ability, a fine-graining ability, and dispersion stability. In addition, it is necessary to take into consideration foaming during dispersion, gelation of the dispersion, fluidity of the dispersion, and the like.

Since there is no dispersant that satisfies all of the above requirements, it is necessary to select an optimal dispersant according to the dye to be dispersed and to add an antifoaming agent or the like as necessary.

The amount of the dispersant used is 5 to the disperse dye.
0-200% is preferred. If the dispersant exceeds this range, it is not preferable because fine particles and dispersion stability are poor or the viscosity is high.

These dispersants may be used alone or in combination. For example, the dispersibility at high temperature is bad,
When a formalin condensate of sodium naphthalenesulfonate having extremely good dispersibility at room temperature is used in combination, good dispersibility and stability can be maintained over a wide temperature range due to a synergistic effect. The mixing ratio is 0.1: 1.0 to 1.0:
0.1 is preferable, and 1: 1 is more preferable.

In order to prevent nozzle drying of the ink-jet ink, a water-soluble high-boiling organic solvent such as glycol or glycol ether is used for the ink. The solubility of the preferred water-soluble, high-boiling organic solvent used in the present invention in a disperse dye is preferably 0.1% by weight.

The solubility of the organic compound can be represented by the (inorganic / organic) value of the organic compound.

The method of obtaining this value is described in detail in Yoshio Koda, Organic Conceptual Diagram, Sankyo Publishing.

The (inorganic / organic) value of the disperse dye used in the present invention is in the range of 0.8 to 1.5, and it is well dissolved in an organic solvent in this range. The high-boiling organic solvent has an (inorganic / organic) ratio in the range of 2 to 6.

The water-soluble high-boiling organic solvent of the present invention is preferably, for example, glycols such as ethylene glycol (5), glycerin (5) and diethylene glycol (2.8). The figures in parentheses are (inorganic / organic)
Is the value of The surface tension of these glycols is 46 dyne / cm or more.

In particular, since glycerin has a high specific gravity, the specific gravity of the ink is also high, which is preferable from the viewpoint of preventing the sedimentation of particles. Glycol ethers usually used in ink jets have an inorganic / organic value in the range of 1 to 2 and are not preferred because they readily dissolve the disperse dye.

Further, the glycol ethers have a surface tension of 40 dyne / cm or less, while the anionic oligomer dispersant having a functional group of the present invention has a surface tension of 50 dyne / cm or more, which hinders dispersion. Might be.

Preferred hydrotropes for the present invention are:
Urea and urea derivatives are preferred.

The hydrotrope means solubilization,
It functions to dissolve and redisperse the disperse dye deposited at the nozzle outlet. Unlike a water-soluble high-boiling organic solvent, the dissolving action of the hydrotrope is small and does not hinder dispersion stability.

Preferred are urea, thiourea, buret, semicarbazide, dimethylol urea, dimethylol ethylene urea, 1,3 dimethyl imidazolidinone and the like. The addition amount is preferably 1 to 10% of the ink, more preferably 1 to 5%.

In the present invention, any of the conventionally known disperse dyes can be used.

The disperse dyes of the present invention include, for example, C.I. I. D
ispersel Yellow 3,4,5,7,9,
13, 24, 30, 33, 34, 42, 44, 49, 5
0, 51, 54, 56, 58, 60, 63, 64, 6
6,68,71,74,76,79,82,83,8
5,86,88,90,91,93,98,99,10
0, 104, 114, 116, 118, 119, 12
2,124,126,135,140,141,14
9,160,162,163,164,165,17
9,180,182,183,186,192,19
8,199,202,204,210,211,21
5,216,218,224; C.I. I. Dispers
e Orange 1,3,5,7,11,13,1
7, 20, 21, 25, 29, 30, 31, 32, 3
3,37,38,42,43,44,45,47,4
8,49,50,53,54,55,56,57,5
8,59,61,66,71,73,76,78,8
0, 89, 90, 91, 93, 96, 97, 119, 1
27, 130, 139, 142; I. Disper
se Red 1,4,5,7,11,12,13,1
5,17,27,43,44,50,52,53,5
4,55,56,58,59,60,65,72,7
3,74,75,76,78,81,82,86,8
8, 90, 91, 92, 93, 96, 103, 105,
106, 107, 108, 110, 111, 113, 1
17, 118, 121, 122, 126, 127, 12
8,131,132,134,135,137,14
3,145,146,151,152,153,15
4,157,159,164,167,169,17
7,179,181,183,184,185,18
8,189,190,191,192,200,20
1,202,203,205,206,207,21
0, 221, 224, 225, 227, 229, 23
9,240,257,258,277,278,27
9, 281, 288, 298, 302, 303, 31
0, 311, 312, 320, 324, 328;
I. Disperse Violet 1,4,8,2
3,26,27,28,31,33,35,36,3
8, 40, 43, 46, 48, 50, 51, 52, 5
6, 57, 59, 61, 63, 69, 77; I. D
isperse Green 9; I. Dispe
rs Brown 1,2,4,9,13,19;
C. I. Disperse Blue 3,7,9,1
4,16,19,20,26,27,35,4 3,4
4,54,55,56,58,60,62,64,71
0, 72, 73, 75, 79, 81, 82, 83, 8
7, 91, 93, 94, 95, 96, 102, 106,
108, 112, 113, 115, 118, 120, 1
22, 125, 128, 130, 139, 141, 14
2,143,146,148,149,153,15
4,158,165,167,171,173,17
4,176,181,183,185,186,18
7,189,197,198,200,201,20
5,207, 211, 214, 224, 225, 25
7,259,267,268,270,284,28
5,287,288,291,293,295,29
7, 301, 315, 330, 333; I. Dis
perse black 1, 3, 10, 24; and the like.

The ink of the present invention can be obtained by mixing the above-mentioned disperse dye, dispersant, medium and optional components and dispersing them by using a disperser. As the disperser, a conventionally known ball mill, sand mill, line mill, high-pressure homogenizer and the like can be used.

[0113]

EXAMPLES The present invention will be described in more detail with reference to the following Examples, but it should not be construed that the present invention is limited thereto.

Example 1 Yellow Disperse Dye Ingredient (CI Disperse Yellow 160) 25 parts Glycerin (50 dyne / cm) 10 parts Formalin condensate of creosote oil sodium sulfonate (Demol C manufactured by Kao Corporation) 10 Part 2- (2-ethylhexyl) sodium sulfosuccinate 0.05 part Nonylphenol ethylene oxide 10 mol adduct 1 part Water 40 parts The above mixture was mixed with ceramic beads having a diameter of 0.5 mm, and was used by IMEX (former name, Igarashi Seisakusho). The mixture was dispersed for 5 hours at a rotation speed of 2500 rpm using a sand grinder made by the company. This dispersion was diluted with water / glycerin = 1: 4 so as to have a dye concentration of 5% to prepare an ink.

After degassing for one hour under a reduced pressure of 30 mmHg, the mixture was discharged using a piezo type ink jet tester manufactured by Konica Corporation.

Number of discharge nozzles = 64, nozzle diameter = 40 μm,
At a discharge frequency of 7 KHZ, 100 million dots were discharged, and the discharge amount was measured with a precision balance.

The particle size of the particles in the ink was measured with a Shimadzu laser diffraction type particle size distribution analyzer. Further, to examine the high-temperature dispersion stability of the ink, the ink was placed in a constant temperature layer at 60 ° C.
Left for a week.

Example 2 Disperse Dye Bulk (CI Disperse Yellow 160) 25 parts Ethylene glycol (48 dyne / cm) 10 parts Formalin condensate of sodium cresol sulfonate and sodium 2-naphthol-6-sulfonate ( Kao Corporation Demol SSL) 25 parts Acetylene glycol (Surfinol 465) 5 parts Urea 5 parts Water 26 parts Dispersion and ink were prepared in the same manner as in Example 1,
evaluated.

Example 3 Disperse Dye Ingredient (CI Disperse Red) 25 parts Glycerin (50 dyne / cm) 10 parts Formalin condensate of sodium cresol sulfonate (Demol SC30 manufactured by Kao Corporation) 25 parts Nonylphenol ethylene oxide Additive (Emulgen 920) 1 part Urea 5 parts Water 20 parts Ink was prepared in the same manner as in Example 1 to prepare an ink, which was then tested and evaluated.

Example 4 Disperse Dye Ingredient (CI Disperse Blue 60) 25 parts Glycerin (50 dyne / cm) 10 parts Formalin condensate of sodium phenolsulfonate 25 parts Acetylene glycol defoamer (Surfinol 104E) 0 .1 part Urea 5 parts Water 20.9 parts Dispersed in the same manner as in Example 1 to prepare an ink,
evaluated.

Example 5 Disperse dye precursor (CI Disperse Yellow 160) 25 parts Glycerin (50 dyne / cm) 10 parts Sodium β-naphthalenesulfonate (20%) and sodium β-naphtholsulfonate (80%) 25 parts of formalin condensate of sodium dodecylbenzenesulfonate 1 part urea 5 parts water 20 parts Dispersed in the same manner as in Example 1 to prepare an ink,
evaluated.

Example 6 Disperse Dye Material (CI Disperse Red) 25 parts Glycerin (50 dyne / cm) 10 parts Formalin condensate of creosote oil sodium sulfonate (Demol C manufactured by Kao Corporation) 15 parts β -Formalin condensate of sodium naphthalene sulfonate (Demol N manufactured by Kao Corporation) 10 parts Water 26 parts Dispersed in the same manner as in Example 1, ink was prepared, and ejected with an ink tester.

Example 7 Disperse Dye Ingredient (CI Disperse Blue 60) 25 parts Glycerin (50 dyne / cm) 10 parts Lignin sulfonate 25 parts Aerosol OT (di (2-ethylhexyl) sulfosuccinate) 1 Part Urea 5 parts Water 20 parts Ink was prepared and dispersed in the same manner as in Example 1 and ejected with an ink tester.

Example 8 Yellow Disperse Dye Ingredient (CI Disperse Yellow 160) 25 parts Glycerin (50 dyne / cm) 10 parts Formalin condensate of sodium creosote oil sulfonate (Demol C manufactured by Kao Corporation) 30 Part: sodium di (2-ethylhexyl) sulfosuccinate (Aerosol OT) 1 part: urea: 5 parts: water: 25 parts The ink was prepared in the same manner as in Example 1 to prepare an ink, which was then tested and evaluated.

In order to reduce the particle size of the ink, 0.3 mm
The amount of the dispersant was increased by using ceramic beads, the dispersion time was doubled to 10 hours, and further atomization was achieved.

Examples 1 to 8 were prepared by dispersing a disperse dye precursor using a polycyclic anionic oligomeric dispersant having a phenolic hydroxyl group and having a disperse dye solubility of 0.1. % Or less of glycerin and ethylene glycol as water-soluble high-boiling organic solvents. The inorganic / organic value of glycerin and ethylene glycol is 5.

Comparative Example 1 Disperse dye precursor (CI Disperse Yellow 160) 25 parts Glycerin (50 dyne / cm) 10 parts Formalin condensate of sodium β-naphthalenesulfonate (Kao Co., Ltd. Demol N) 25 parts Sodium di (2-ethylhexyl) sulfosuccinate (Aerosol OT) 1 part Urea 5 parts Water 20 parts Ink was prepared in the same manner as in Example 1 to prepare an ink, which was then tested and evaluated.

Comparative Example 2 Disperse dye precursor (CI Disperse Yellow 160) 25 parts Glycerin (50 dyne / cm) 10 parts Ethylene oxide 14 mol adduct of tribenzylphenol (Newcol-714 manufactured by Nippon Emulsifier Co., Ltd.) 25 parts) Di (2-ethylhexyl) sodium sulfosuccinate (Aerosol OT) 1 part Urea 5 parts Water 20 parts Ink was prepared in the same manner as in Example 1 to prepare an ink, which was then subjected to experiments and evaluation.

Comparative Example 3 Disperse dye precursor (CI Disperse Yellow 160) 25 parts Glycerin (50 dyne / cm) 10 parts β-naphthol 13 mol sulfuric acid ester of ethylene oxide adduct (Nippon Emulsifier Co., Ltd. New Coal B-13SN) 25 parts Di (2-ethylhexyl) sodium sulfosuccinate (Aerosol OT) 1 part Urea 5 parts Water 20 parts Ink was prepared in the same manner as in Example 1 to prepare an ink, which was then subjected to experiments and evaluation.

Comparative Example 4 Disperse dye precursor (CI Disperse Yellow 160) 25 parts Glycerin (50 dyne / cm) 10 parts Styrene-maleic anhydride copolymer dispersant 25 parts Urea 5 parts Water 21 parts Example 1 The ink was prepared by dispersing in the same manner as described above, and an experiment and evaluation were performed.

Comparative Example 5 Yellow disperse dye base material (CI Disperse Yellow 160) 25 parts Ethylene glycol monobutyl ether (inorganic / organic value: 1) 10 parts Formalin condensate of sulfonated creosote oil (Kao Demol C) 10 parts Di (2-ethylhexyl) sodium sulfosuccinate (Aerosol OT) 1 part Urea 5 parts Water 35 parts Ink was prepared in the same manner as in Example 1 to prepare an ink, which was then subjected to experiments and evaluation.

Comparative Example 1 is an example of a polycyclic dispersant having no functional group.

Comparative Example 2 is a nonionic dispersant used in conventional screen printing, and has a strong solubilizing power for the disperse dye.

Comparative Example 3 was used for screen printing.
It is an anionized nonionic dispersant and has high solubility of disperse dyes.

Comparative Example 4 is an example of a dispersant having no functional group and no polycyclic structure.

Comparative Example 5 is an example in which an organic solvent having high solubility in a disperse dye having an inorganic / organic value of 1 is used.

[0137]

[Table 1]

In the anionic oligomer dispersant having a functional group of the present invention, the hydrophobic portion has an affinity for the polynuclear structure of the disperse dye and has a functional group capable of strongly binding to the disperse dye.
Good dispersion stability. Even after storage at 60 ° C. for one week, the change in particle size is small.

In Examples 1 to 7, a polycyclic anionic dispersant having a functional group was used, and the solubility in disperse dyes was low, and the inorganic / organic value was 5 in water-soluble high-boiling organic compounds. The use of a solvent and avoiding excessive dispersion prevent the presence of particles of 0.1 μm or less in the ink at 1 wt% or less, so that the particles do not become large even when stored at a high temperature, and the average particle diameter of the ink. Is 0.25 μm or less and the maximum particle diameter of the ink is 0.4 μm or less, so that even when 100 million drops are continuously ejected, clogging of filters and nozzles is small.

Example 8 is within the scope of the present invention, but the addition amount of the dispersant was increased and the dispersion time was increased to 10 hours.
Even when 100 million droplets are continuously ejected, the filter and the nozzle are less clogged, but the proportion of particles of the disperse dye having a particle diameter of 0.1 μm or less in the ink is 3.00%. , The largest).

On the other hand, if a dispersant having no functional group or an organic solvent having high dye solubility, which is outside the scope of the present invention, is used, the particle size becomes large during storage and the high-temperature stability is poor.
Further, the discharge amount decreases in a long-time continuous discharge test, and the one using conventional screen printing is not preferred because the dissolving power of the disperse dye is strong.

[0142]

As has been demonstrated in the examples, the disperse dye ink for textile printing according to the present invention has a high ability to form fine particles, good dispersion stability, good long-term storage properties, and clogging of filters and nozzles during continuous discharge. Excellent effect with less.

Claims (4)

[Claims] 1. A disperse dye ink for ink-jet printing used in an ink-jet printing system in which an ink containing a dye which can be dyed is applied to a fabric as ink droplets from a nozzle by an ink-jet method, color-developed, washed and dried. An anionic oligomer dispersant having a functional group is used as a dispersant for a disperse dye for inkjet printing, and the water-soluble high-boiling organic solvent in the ink has a surface tension of 46 dyne / cm or more, and an inorganic / organic organic solvent. 2 to 6, the ink contains the water-soluble high-boiling organic solvent in an amount of 5 to 70% by weight, and has a viscosity of 1 at 25 ° C.
A disperse dye ink for ink-jet printing, which has a molecular weight of 0 cp or less. 2. An ink jet printing disperse dye ink having an average particle size of 0.25 μm or less and a maximum particle size of 0.4 μm or less.
5. The disperse dye ink for inkjet printing according to item 1. 3. The dispersion for ink-jet printing according to claim 1, wherein the disperse dye ink for ink-jet printing contains 1% by weight or less of disperse dye particles for ink-jet printing having a particle size of 0.1 μm or less. Dye ink. 4. An ink jet nozzle for applying the disperse dye ink for ink jet textile printing according to any one of claims 1 to 3 to a fabric, and discharges the ink using mechanical energy due to deformation of a piezo. Nozzle diameter is 1
An ink-jet printing method, characterized in that an ink is applied to a cloth by an ink-jet printer having 0 to 40 μm and having 60 or more nozzles.