JPS62172065A - Concentrated solution of basic azo dye having storage stability - Google Patents

Abstract

PURPOSE:The titled solution having no irritating smell, no fear of corrosion of container, device, etc., and no fear of powder scattering, comprising a sulfamate of primary amino group-containing bisazo type basic dye and water. CONSTITUTION:The aimed dye solution consisting of (A) a sulfamate of primary amino group-containing bisazo type basic dye, optionally (B) an alkylamine type nonionic activator and (C) water.

Description

[Detailed Description of the Invention] Industrial Field of Application The present invention is the 1st v.! The present invention relates to a solution of a bisazo type basic dye having an amine group of t, which is stable and can be stored for a long period of time. Bisazo type basic dyes have strong dyeing power and are widely used for coloring paper, wood, etc. in addition to various fibers.

The object of the present invention is to produce this dye with a novel composition as a liquid that can be stored for a long period of time, and to provide it as a liquid product that is convenient to use.

Conventional technology: Documents related to converting basic dyes into liquids that can be stored for a long time include Japanese Patent Publication No. 39-4879 and Japanese Patent Publication No. 43
-18163, Special Publication No. 57-58384, etc.

The basic azo dye used in the present invention has been manufactured and provided in the form of a fine powder containing diluents, auxiliary agents, etc., like ordinary dyes. However, although basic dyes have strong coloring power, they have low solubility in water and require 20 to 30 times as much water to dissolve. Immediate and complete dissolution requires operations such as heating and stirring.

This fine powder with strong coloring power is easily scattered, and li! It has the disadvantage of easily contaminating the handler, instruments, equipment, etc. during construction and use.

The method disclosed in Japanese Patent Publication No. 39-4879 as a method for making such basic dyes into a concentrated liquid consists of using the basic dye base as a salt of a water-soluble nucleating acid and dissolving it in water to which various solvents have been added. This is the way to do it. This method has already become a commonly used technique, and liquid dyes prepared by dissolving dye acetate in highly concentrated acetic acid are commercially available. In Special Publication No. 43-18163,
A method is disclosed in which a sulfaminate salt of a general basic dye is dissolved in water together with an aqueous solvent, but in the detailed explanation, it is clearly stated that azo basic dyes are "difficult to be practically applied" and no examples are provided. However, nothing is disclosed regarding azo dye 10. Japanese Patent Publication No. 57-58384 discloses a method of bonding an alkylpenzole sulfonic acid with a dye base and liquefying this using various solvents.
The product is of a special type, has limited uses, and its solution is different from the aqueous solution according to the present invention.

Problems to be Solved by the Invention The conventional method of dissolving a dye base as a salt with a water-soluble organic acid is that the organic acid salt of the primary amino group bonded to the dye is easily dissociated, and the dye base is Separation and precipitation are likely to occur. In order to prevent this, a method of dissolving it in an organic acid, especially acetic acid at a high concentration, has been implemented. The product emits a strong pungent odor characteristic of acetic acid and is corrosive due to acid, requiring special care for handlers, equipment, containers, etc. during both manufacture and use. Also, the unit price naturally increases due to the price of acetic acid as a solvent. This is suitable for the current situation where there is a demand for liquid dyes that are easier to handle and produce and are cheaper. Also special public official 1816-1977
In No. 3, it is stated that the method of using a sulfamine salt as the dye base is difficult to practically apply to azo basic dyes, and no working examples are disclosed. Furthermore, Japanese Patent Publication No. 571'18384 discloses a method for producing printing ink using a solvent, which differs in purpose, structure, and effect from the present invention, and is related to the basic dye of the present invention. There are no disclosures to make.

Means for Solving the Problems In the present invention, these problems were solved by dissolving the dye base in the form of a salt with sulfamic acid in water. This is due to the discovery that only bisazo-type basic dyes with primary amino groups can have their sulfamates dissolved in water at high concentrations.

As mentioned above, Japanese Patent Publication No. 43-18163 discloses that it is practically difficult to prepare a sulfamic acid salt of an ordinary azo basic dye into a liquid composition using a mixture of water and a solvent. The inventor of the present application believes that it is impossible to apply the method of the present invention to monoazo dyes or basic azo dyes having secondary, tertiary amino groups, and quaternary alkylamino groups. So, number one! It has been discovered that the present invention can be practiced only with bisazo type azo dyes having &amino groups. Tokuko Showa 5
The method disclosed in No. 7-58384, in which an alkylbenzenesulfonic acid group is combined with a dye base and liquefied using a packaging solvent, cannot be carried out with the dye used in the present invention.

The bisazo basic dye having a primary amino group used in the present invention includes Bismarck Brown (CI, 2100
0 Basic Brown 1 and Cl21010 Basic Brown 4).

The conditions that made the present invention possible include the Kt degree of the dye base, the amount of sulfamic acid, 784 degrees of dissolution, etc.
In particular, the amount of sulfamic acid is limited by the final pH of the solution.

Furthermore, it has been found that the addition of a ruamino-type nonionic activator in alcohol is effective when a more stable solution at a higher concentration is dissolved with suryafamine acid, which is a dye base.As this activator, penzol sulfoamine or toluene sulfoamine A compound in which ethylene oxide is added to is particularly effective.

As the latter, Nippon Nyukazai-PHG-55 can be used, and as the latter, Levalin EX-BNS (Bayer, Germany) can be used. The parts in the examples below indicate weight.

Example 1 10 parts of metaphenylene diamine, 3 parts of sodium nitrate.
9 parts, hydrochloric acid (21°Be) 12.8 parts, water and ice 1
A dye is synthesized using 00 parts by a known method (eg, Yutaka Hosoda, Theoretical Manufacturing Dye Chemistry, p. 588). The resulting reaction solution is neutralized at low temperature with 5.5 parts of commercially available industrial ammonia water to precipitate the dye base.

This precipitate is thoroughly washed with water to remove water-soluble impurities. The dye base thus obtained was added to 6.5 parts of sulfamic acid and 33.5 parts of water and stirred at 25°C for 20 hours.

50 parts of a fluid dark brown viscous liquid was obtained.

The amount of sulfamic acid is set to the amount necessary to dissolve the dye base, and excess is not preferable, and the final pH of the bath solution is adjusted to 2. This concentrated solution thus prepared has a dyeing power comparable to that of a commercially available powdered dye (Bismarck Brown B). After this solution was left at room temperature for 6 months, the staining power before and after was compared. There is no difference in staining power,
Also, no change was observed in quality such as fluidity.

Example 2 The dye base obtained by the method of Example 1 was mixed with 33 parts of water,
It is dissolved in the same manner as in Example 1 using 0.5 part of Levalin EX-BNS (manufactured by Bayer) and 6 parts of sulfamic acid. 2
It was completely dissolved in about 4 hours at 0'C. 50 parts of a dark brown viscous liquid was obtained. This dye had the same dyeing power as the commercially available powder dye as in Example 1, and no change in dyeing power, quality, etc. was observed even after being left for 6 months.

Example 3 13 parts of metatolylene diamine, 3.9 parts of sodium nitrate, 12.8 parts of hydrochloric acid (21° Ben, water and 1 ml).

A dye was synthesized using the method of Example 1. The resulting reaction solution is neutralized by adding 5.7 parts of 5'CC TODO commercially available industrial aqueous ammonia to precipitate the dye base. The precipitated dye base is thoroughly washed with water to remove impurities. The dye base thus obtained was added to 6.5 parts of sulfamic acid and 33 parts of water, and further 0.3 part of PHG-55 (Nippon Nyukazai ■) was added, and the mixture was stirred with a trowel for 8 hours at a temperature below 10°C. and dissolved.

55 parts of a dark brown viscous liquid was obtained. This corresponds to Basic Bron R (CI 21010), which dyes a reddish hue compared to Example It, and has almost the same dyeing strength. No change in dyeing power, color tone, or liquid quality was observed even if it was left at room temperature for more than 6 months.

EFFECTS OF THE INVENTION The novel composition of the present invention has been made. Concentrated and stable solutions of bisazo basic dyes with primary amino groups are used for various dyeings. Compared to the conventional liquid oak dye, it has the characteristic that it does not have a pungent odor because it uses water instead of acetic acid. Because it does not contain excess acid, the container
It also has the characteristic of being less likely to corrode the manufacturing equipment 4, etc.

Also, the handler will not be bothered by the strong pungent odor that is found in conventional products. It goes without saying that it does not scatter as compared to powdered dyes, and by implementing the present invention, dye production,
It is extremely convenient to use, more streamlined, and can be provided to users at a lower cost than conventional products.

Man patent applicant Nobuaki Takaki

Claims (1)

[Claims] 1. A concentrated storage-stable solution comprising a sulfamate salt of a bisazo-type basic dye having a primary amino group and water. 2. A concentrated storage-stable aqueous solution consisting of a sulfamate salt of a bisazo-type basic dye having a primary amino group, an alkylamine-type nonionic activator, and water.