JPS587756B2 - Polyamide resin - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention significantly increases the solubility of dyes by using the compounds used in the present invention in continuous dyeing of fabrics made of polyamide fibers, and further improves the solubility of dyes by reducing acidic substances or acid-generating substances. When used in combination, the dyeing rate after coloring treatment is significantly increased, and it is also effective for dyes for which it was not possible to obtain a thick pad solution due to the poor solubility of dyes (without using the compound used in the present invention). (For example, most dyes that are added with acidic substances or acid-generating substances gel, making it impossible to obtain a thick pad solution);
The present invention relates to a continuous dyeing method characterized in that the fibers are immersed in the pad liquid, squeezed, dried, and then subjected to a dry heat treatment and color development treatment to obtain a uniform deep color.

Conventionally, dyeing of polyamide fiber fabrics can be roughly divided into batch methods using a jitter or the like and continuous methods using a pad mangle or the like.

The general process for continuous polyamide dyeing is to uniformly apply the dye to the fabric to be dyed using a mangle, etc., evaporate moisture etc. in a suitable dryer, and then place the dye in an acid bath containing an acid such as sulfuric acid. After that, the color is developed by applying wet heat steam treatment without drying, and then continuously washed with water to fix the color.

This method dyes in a shorter time than the batch method, and is far more energy and labor-saving, and has attracted great interest for some time.

However, in the case of continuous dyeing, there are currently two or three major problems, which limit mass production.

b) Compared to immersion dyeing, the dye concentration in a pad bath is higher due to the bath ratio, but it is limited by the solubility of the dye, and the concentration can only be achieved up to a certain level. Due to instability, problems such as gelation and sedimentation of the dye occur, resulting in color variations and dye specks.
Can only be dyed in light colors.

When an acidic substance or an acid-generating substance is added to increase the dyeing rate, the solubility of the dye deteriorates and most of the dye turns into a gel.

b) Therefore, when a highly concentrated dye solution is required, it is common to use a dye dissolving agent such as urea, thiourea, thioglycol, ethylene glycol, or cellosolve, but It is not effective in dissolving dyes (more than 75 g/l), and it also inhibits the fixation of dyes, increases costs due to dye loss, and increases dye concentration in wastewater, which is one of the causes of pollution in the dyeing industry. It becomes.

c) Fabrics colored by the acid fixation method or the steam method using the above-mentioned highly concentrated dye solution have a very rough and hard feel, making them impractical.

The present invention has been made to improve the above-mentioned drawbacks and, as a result of intensive research, has achieved the practical application of a continuous dyeing method for polyamide fibers, which has high fixation properties, good bath stability, and does not inhibit dyeability and gives a good texture to dyed fabrics. It has been reached.

The compound used in the present invention has the general formula:
: Average number of added moles of ethylene oxide, an integer from 21 to 28. M : Represents K, Na, NH4, and alkanolamines and alkylamines having 5 or less carbon atoms.

), and examples of these compounds include the following.

Polyoxyethylene cetyl stearyl ether sulfate salt (yellowish brown paste) Polyoxyethylene dinonyl phenyl ether sulfate salt (yellow paste) Polyoxyethylene distyrenated phenyl ether sulfate salt (yellow paste) Ether sulfate salt ( Polyoxyethylene nonyl phenyl ether sulfate salt (pale yellow-white solid) The dyeing method of the present invention uses at least one of the above compounds.
g/l to 40 g/l and acidic substances, i.e. common organic and inorganic acids, from 50 g/l to 30 g/lf or acid generators, i.e. known ammonium phosphate, ammonium nitrate, ammonium persulfate, Ammonium sulfate, ammonium carbonate, ammonium tartrate, ammonium oxalate, ammonium acetate, etc. are so-called latent acids that exhibit acidity when NH4 is scattered at high temperatures, and their saturated aqueous solutions contain 50 g/l to 100 g/l. ℃~50℃. Polyamide fibers are immersed in the pad liquid, squeezed with a mangle, dried at 100°C and ~120°C, then dried at 180°C ~ 200°C, and then treated with unsaturated steam (HT) at 150°C ~ 180°C. law) kataha 9
This is a continuous dyeing method that does not involve color development using an acidic aqueous solution (acid shock method) at 0°C to 98°C.

Since the above-mentioned compound which is a dye dissolving agent for acidic dyes, 1:2 type metal complex dyes, and chromium dyes is added to the pad solution, the dye does not precipitate even if the pad solution is acidic, which is different from conventional methods. It is possible to form a stable, concentrated solution that would otherwise be difficult to apply, and the pad liquid can be uniformly applied to the J polyamide fibers.

The dye on the knitted, squeezed, and dried polythemide fiber is fixed at a ratio of 80 to 85 in the dry heat treatment due to the dye solubility and fiber wettability of the compound.

Therefore, the elution into the bath in the acid shock method during the next coloring step, etc. is significantly reduced, and the adhesion to polyamide fibers, that is, the dyeing rate is improved.

Polyamide fibers treated in this manner can increase the dye dyeing rate and produce dyed fabrics with good texture.

In addition, if acidic substances or acid-generating substances are used alone,
Although the dyeing rate is improved, the degree of dissolution of the dye is extremely reduced, and most acid dyes, 1:2 type metal complex dyes and chromium dyes gel at concentrations of 759/l or higher and cannot be used.

The present invention uses the above-mentioned compound and an acidic substance or an acid-generating substance, and by their interaction, a padding liquid that has improved these various defects is attached to polyamide fibers, and most of the dye is fixed to the fibers by dry heat treatment, resulting in a uniform coating. In dark color,
Moreover, a durable dyed cloth can be obtained continuously.

Next, examples of the present invention will be shown.

Example I Commonly used dye solubilizers listed in Table 1,
A surfactant and an active agent according to the invention are dissolved in hot water and C.I. I. Acid Red 114 100g
After stirring sufficiently at 80 to 90°C for a certain period of time, the temperature was lowered to 40 to 50°C, and 75 g/l of an aqueous solution of ammonium 33-thiosulfate was added thereto, followed by thorough stirring again to prepare a pad liquid.

This pad liquid was subjected to suction filtration using Filter Paper Ni 2 manufactured by Tozen Roshi Paper Co., Ltd., and the filtration time was measured.

The results are shown in Table 1.

As can be seen from this result, compared to the conventional pad liquid using the dissolving agent 1 in Table 1, the compound 5 according to the present invention
It can be seen that this produces a stable and concentrated dye solution.

Example 2 C. I. A. cid Blue 113 100g/
l, ammonium tartrate (33% aqueous solution) 75g/
A comparison was made between a compound other than the present invention and a compound according to the present invention in the same manner as in Example 1 under the conditions of 1.

The results are shown in Table 2.

From the results in Table 2, similar to Example 1, in cases 1, 2, and 3 in the table, gelation was slight, whereas in cases of 4 according to the present invention.
The compounds form good dye solutions.

Example 3 Metal complex dye C. I. Acid Blue 127:
1 and C. I. A. cid Black 58 in the same manner as in Example 1 with 30 g/l of the activator of the polyoxyethylene distyrenated phenyl ether sulfate salt according to the invention and 45 g/l of ammonium tartrate (33% aqueous solution). The prepared solutions were visually observed for the presence or absence of precipitates after being left to stand for 1 hour, and the results shown in Table 3 were obtained.

inside. For comparison, a solution to which no dye dissolving agent was added is shown as "no auxiliary agent", and a solution to which thioethylene glycol is added as a dye dissolving agent is shown as "conventional solution".

The results are shown in Table 3.

Example 4C. I. A. cid Red 114 1 0 0
g/l, activator (pholyoxyethylene distyrenated phenyl ether sulfate salt) 30g/Cf! A staining solution was prepared in the same manner as in Example 1 using 75 g/l of ammonium acid (33% aqueous solution), and nylon taffeta (basis weight 70 g/rrt') was punctured in this dyeing solution ( Pick up 30%) Non-touch dryer drying → Cylinder heat treatment (190℃ x 60s
ec)→H.T.Steamer
The dyeing was carried out at 170°C x 5 sqm), followed by soaping and drying.

Table 4 shows the dye dyeing rate in each step.

For comparison, the results of a conventional method in which thiodiethylene glycol was used as a dye dissolving agent and cylinder heat treatment was omitted are also shown.

The results are shown in Table 4.

However, the dyeing rate was measured by an extraction method using the amount of dye attached to the pad as a reference amount.

As is clear from Table 4, the method of the present invention achieved 88.0% adhesion by heat treatment, and 99.0% by steaming treatment.
Shows a high dyeing rate of 5%, 1% compared to conventional Zitzker dyeing.
/4 times showed similar effects.

Amazingly, there was no selective adsorption of the dye to the dyed object during the process, resulting in a uniform scarlet red color with a good texture.

Example 5 C. I. A. cid Red 114 1 0 0
g/l, activator (pholyoxyethylene nonyl phenyl ether sulfate salt) 30 g/l1 tartaric acid (5
A staining solution was prepared in the same manner as in Example 1 using 40 g/l of 0% aqueous solution, and nylon taffeta (basis weight 70 g/d) was padded into this dyeing solution (Pick up 3).
0%) Non-touch dryer drying → cylinder heat treatment (
190℃ x 60'sec) "Acid treatment" (sulfuric acid
5°Be3cc/l 96°C x 3 minutes) to dye and soap dry.

The dye dyeing rate and texture in each step are shown in Table 5 in comparison with the conventional method (same as Example 4).

As is clear from Table 5, the method of the present invention allows most of the dye to be dyed by dry heat treatment.

By the way, when the dye dissolving agent used in the method of the present invention was used and the cylinder heat treatment was omitted and acid treatment was performed, the dyeing rate was 86.
．． It is 0%.

Further, the dye dissolving agent used in the present invention hardly hardened the texture of the dyed material, resulting in a good texture that could not be obtained with conventional acid shock dyeing.

Example 6 C. I. A. cid Blue 230 1 0 0
9/l, C. I. A. cid Yellow 49
5 fl/l, C. I. A. cidBlue
113 509/l1 activator (polyoxyethylene cetyl stearyl ether sulfate salt) 40g/l,
A staining solution consisting of 75 g/l of ammonium tartrate (33% aqueous solution) was prepared according to the method of Example 1, nylon baby taffeta (basis weight 174 g/rrl) was placed in this dyeing solution (Pick up 35%), and then dried using a non-touch dryer. Drying → Cylinder heat treatment (190℃ x 6
0 sec )→Acid treatment (H2S0455°Be 3c
c/l9 6°C x 3 minutes) for dyeing and soaping drying.

The obtained dyed fabric was dyed using the conventional method (using Levegar KS (manufactured by Bayer) as a dye solubilizer, as shown in Table 6).
This method shows a significantly superior effect compared to the method (method in which cylinder heat treatment is omitted).

Example 7 Table 7 shows the names of dyes that can obtain a long-term stable and thick pad solution consisting of the compound used in the present invention, an acid generating substance, and an acid dye or a metal complex dye. Table 7 shows the results regarding the solution stability of the pad bath for the conventional product and the conventional product.

Claims (1)

[Claims] 1 General formula R-0-(CH2CH20)m-SO3M (wherein R is an alkyl group having 8 to 20 carbon atoms, an alkylaryl phenyl residue or an alkylphenyl residue, and m is The average number of added moles of ethylene oxide is 21 to 28, M is K
, Na, NH, and alkanolamines and alkylamines having 5 or less carbon atoms. ) A polyamide fiber is immersed in a pad bath consisting of at least one or more compounds represented by the following formulas, an acidic substance or an acid-generating substance, and an acidic dye or a metal complex dye, and after being squeezed and dried, it is subjected to a dry heat treatment. , a continuous dyeing method for polyamide fibers, which is then subjected to a coloring treatment.