JPS63207865A - Production of water-based liquid composition of water-insoluble of hardly soluble dye - Google Patents

Abstract

PURPOSE:To obtain the titled composition storable over a long period without causing decomposition of dye and deposition of organic salt, by dispersing a surfactant, a specific crushing medium and a water-insoluble or hardly soluble dye having an inorganic salt content lower than a specific level in an aqueous medium. CONSTITUTION:The objective composition can be produced by dispersing (A) a water-insoluble or hardly soluble dye having an inorganic salt content of <=0.5wt.%, (B) a surfactant (preferably nonionic surfactant) having an inorganic salt content of <=3wt.% and (C) a crushing medium which does not generate inorganic salt by abrasion (e.g. glass bead containing <=5wt.% K2O and Na2O in total) in (D) an aqueous medium. The amount of the component B is preferably 5-30pts. based on 10-60pts. of the component A.

Description

DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for producing an aqueous liquid composition of a water-insoluble or sparingly soluble dye.

<Conventional technology> is often used.

<Problems to be Solved by the Invention> However, the method of pulverizing and dispersing using glass beads does not allow the Na and K contained in the glass beads to be pulverized and dispersed.

Inorganic salts such as Ca and mari are eluted to increase the pH of the product. If the dye is stored for a long period of time at this high pH, the dye will decompose and the density and hue will change.

On the other hand, in order to prevent this decomposition, it is possible to neutralize the product to near neutrality with sulfuric acid, etc., but in this case, it will contain a large amount of inorganic salts such as Glauber's Salt, and if stored at low temperatures, precipitates, causing various problems during dye weighing and dyeing operations.

In addition, in recent years, the method of using acrylic acid-based synthetic thickening agents has become popular during textile printing, and since this thickening agent is highly sensitive to ions, nonionic printing methods using nonionic surfactants as dispersants have become popular. Disperse dyes are preferably used. When producing this nonionic disperse dye, if glass beads are used as the crushing media, inorganic salts will be eluted due to abrasion of the beads and contain ionic substances, resulting in the viscosity of the acrylic acid synthetic glue. There were problems such as a decline in product quality and variations in product quality.

<Means for Solving the Problems> The present inventors have made extensive studies to solve the above-mentioned problems, and as a result, have arrived at the present invention.

That is, the present invention uses a water-insoluble or sparingly soluble dye with an inorganic salt content of 0.5% by weight or less, a surfactant with an inorganic salt content of 8% by weight or less as a dispersant, and a grinding media in which the inorganic salt is removed by abrasion. Provided is a method for producing an aqueous liquid composition of a water-insoluble or sparingly soluble dye, which is characterized by dispersing the dye in an aqueous medium using a medium that does not cause the dye.

The water-insoluble or poorly soluble dye used in the present invention is a dye that does not have a water-soluble group in its molecule, and examples include disperse dyes, vat dyes, and fluorescent dyes. Inorganic salts contained in these dyes, such as K, Na, Ca
, Mg, I'd, and Fe c7) The content of oxides, chlorides, sulfates, nitrates, phosphates, formates, acetates, etc. is not more than 0.5% by weight.

In the present invention, surfactants used as dispersants include formalin condensates of naphthalene sulfonates, anionic surfactants such as lignin sulfonates and alkylbenzene sulfonates, polyalkylene glycol alkyl phenyl ether compounds, polyalkylene glycols, etc. Examples include nonionic surfactants such as alkyl ether compounds, polyalkylene gellicol fatty acid ester compounds, polyalkylene glycol sorbitan fatty acid ester compounds, polypropylene glycol polyethylene glycol ether compounds, and N-polyalkylene glycol alkylamine compounds.
A species or two or more species may be used.

Among these surfactants, nonionic surfactants are preferred. The content of the above-mentioned inorganic salt contained in these surfactants is 8% by weight or less.

The grinding media used in the present invention that does not produce inorganic salts due to abrasion is modified glass beads, that is, the total content of Na2O and Ni20 in the composition is 6% by weight.
Below, preferably 8% by weight or less, more preferably 1% by weight or less of glass beads, Ottawa sand, which is a high purity (99% or more) silica natural sand produced in Ottawa, Canada;
Examples include titania beads and ceramic beads such as zirconia beads or alumina beads.

The method of the present invention is carried out, for example, as follows. first,
Add 1 to 50 parts by weight, preferably 5 to 80 parts by weight of an anionic and/or nonionic surfactant to 5 to 80 parts by weight, preferably 10 to 60 parts by weight, of a water-insoluble or poorly soluble dye, and add water. After addition, the conventional decentralization method, namely 1. Methods using high-speed impeller disperser, sand mill, ball mill, and high-speed stone mill are 1.
It is carried out by applying seeds or 21 or more.

According to the production method of the present invention, since the contamination of inorganic salts during production is avoided, there is almost no increase in pH, and an aqueous liquid composition is provided that has no problems of dye decomposition or inorganic salt precipitation during long-term storage. be done.

Furthermore, when a nonionic surfactant is used, an aqueous liquid composition without viscosity reduction or variation of the acrylic acid-based synthetic sizing agent can be provided.

Hereinafter, the present invention will be explained in more detail with reference to Examples.

Note that the numbers in the middle of the text and % represent parts by weight.

Example 1 Sumikalon Blue 5-sRF Conch Cake (Disperse dye manufactured by Sumitomo Chemical Co., Ltd.; C0 process, Disperse
Bu JL/-257, Na2SO4- content 0.09
%, other inorganic salt content 410.01% or less) 28 parts,
Formalin condensate of sodium naphthalene sulfonate (Nissin Kasei Ichigo Co., Ltd. dispersant, heavy! Average molecular weight: 11 Approx. 11
00, Na2SO4 content 2.22%, other inorganic salt content 0.01% or less) and 62 parts of water were added, stirred well and mixed to form a slurry liquid, and adjusted to pH = 7 with a small amount of 70% sulfuric acid. Adjusted to .5. Then, the slurry liquid was mixed with NF beads (Ashizawa Iron Works Co., Ltd.) with an average particle size of 1 m.
A homogeneous dispersion was obtained by pulverizing and dispersing fine particles with an average particle size of 0.5 μm using a high-speed impeller stirrer into which 200 parts of the commercially available product (Na2O + K20 content 0%) had been added in advance. The pH of the obtained dye dispersion was 7.9, showing almost no increase, and the Na2SO4 content was 0.06.
It was as low as %.

For comparison, instead of the NF beads of the present invention, ordinary glass beads, GB502M beads (manufactured by Shiba Ballotini Co., Ltd., particle size range 1 to 1.4 m, Na2O+
K2O content 1t (7) Total = 14.0X, CaO+
MgO+ AA205+ Fe2O3 content=18.
1X) and then tested in the same manner, the pH of the dye dispersion obtained rose to 9.8. After processing this dye dispersion at 60°C for days, untreated products and 100% PE
High temperature staining method of T (180°C for 960 minutes, staining density = 1
．． When comparing the densities of 0, o, w, f), it was found that the dye in the treated product had decomposed, so the dyeing power was 8.
It had dropped to ON. (Comparative example) On the other hand, in order to suppress dye decomposition, a dye dispersion of P H = 9.8 was heated to 70 × H2
When neutralized with SO4 to pH=7.5, Na2
The SO4 content was 1.7%, and crystal precipitation was observed at -10'O.

(Comparative example 2) The above results are summarized in the table below.

Grinding Star Grinding Finished Product Na2SO460°C 7 Days Comparative Example 2 7.5 9.8 7.5 1.7
100 Example 1 7.5 7.9 7
．． 9 0.06 100 Example 2 Sumikalon Navy Blue 5-GL Conch Cake (disperse dye manufactured by Sumitomo Chemical Co., Ltd.; C, I, Disperse Blue 79°Na25O, content 1tO, 18%
, containing inorganic salts, ot% or less) 75 parts, anionic dispersant of the following formula-(1) (Hipposha Yushi Kogyo Co., Ltd.)
made into a slurry by adding 80 parts of Na2SO4 (Na2SO4 content: 0.76%, other inorganic salt content: 0.01%) and 150 parts of water and stirring well to form a slurry. It was .2.

Next, titania beads (manufactured by Toyama Ceramic Co., Ltd., composition = Ti02g2%) were added to this slurry.

5iOz 14%, kH2's 8%, average particle size 2■)
The eQO portion was added and ground and dispersed using a 1/4G6 cylindrical sand grinder (manufactured by Igarashi Kikai Seizo Co., Ltd.) until the average particle size became 0.8 μm to obtain a uniform dispersion.

When the pH of the resulting dispersion was measured, it was 7.8, which was <
No increase in pH was observed.

For comparison, the general glass beads used in Example 1 were used instead of the titania beads of the present invention, and the test was conducted under the same conditions. The pH of the resulting dispersion was 9.
．． It had risen to 5. Divide this in half and make one side 70
% H, So4tePH=7.2tt' Neutralized, Example-
When eight samples were compared in the same manner as in Example 1, the comparative example had either a problem of concentration reduction due to dye decomposition or Na2SO4 precipitation.

Example 8 Sumikalon Red 5-BDF (Sumitomo Chemical Co., Ltd.)
Manufactured disperse dye; C, I, Disperse Red 843
) 10 parts of conch cake, 10 parts of a Pluronic nonionic dispersant having a molecular weight of about 11,000 and 70% polyethylene oxide, and 80 parts of water were added and thoroughly stirred and mixed to form a slurry. I checked the pH here and it was 7.
It was 6.

Next, this slurry was added to Ottawa Sand (Igarashi Machine Manufacturing Co., Ltd.).
A homogeneous dispersion liquid was obtained by adding 200 parts of a product sold by Ashizawa Iron Works Co., Ltd. and pulverizing and dispersing the mixture into fine particles with an average particle size of 0.5 μm using a pearl mill (manufactured by Ashizawa Iron Works Co., Ltd.).

The pH of the obtained dye dispersion was 8.0, which showed almost no increase, and the viscosity of the color paste using the acrylic acid-based synthetic paste described below was 25,000 CP, showing almost no change in viscosity.

Acrylic acid-based color paste composition Hi-Print DA" 2 parts Hi-Print DB*2 1 part water 87 parts Dye dispersion 10 parts Total 100 parts 4.2 Comparison of acrylic acid-based synthetic paste for textile printing manufactured by Hayashi Kagaku Co., Ltd. Example 1 instead of the Ottawa sandwich of the present invention
When the test was carried out in the same manner using the general glass beads used in the above, the pH of the resulting dye dispersion was 9.
It rose to 8.

Divide this dye dispersion in half and divide one half into 70XH2SO4
"C' Neutralized L, PH = 7.51!: L, 1", Tension When the same printing dyeing paste as above was prepared, the viscosity of the colored paste was 14000CP for the unneutralized product (Comparative Example 3) The viscosity of the neutralized product (Comparative Example 4) decreased to 8500 CP.

The above results are summarized in the table below.

Claims (1)

[Scope of Claims] 1) Water-insoluble or poorly soluble dye with an inorganic salt content of 0.5% by weight or less, a surfactant with an inorganic salt content of 3% by weight or less as a dispersant, and abrasion as a grinding media. 1. A method for producing an aqueous liquid composition of a water-insoluble or poorly soluble dye, which comprises dispersing it in an aqueous medium using a medium that does not produce inorganic salts. 2) The manufacturing method according to claim 1, wherein the surfactant is a nonionic surfactant. 3) The manufacturing method according to claim 1, wherein the grinding media is glass beads, Ottawa sand, titania beads, or ceramic beads having a total content of K_2O and Na_2O of 5% by weight or less.