JPS60119265A - Alkali treatment of fiber material - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed Description of the Invention] Is the present invention a Fengxiong material? This invention relates to a method for obtaining a uniform and rapid treatment effect when carrying out alkali treatment using an alkali agent solution having various concentrations.

From the spinning process to the dyeing process, fibers are sometimes treated in an alkaline solution (hereinafter simply referred to as an alkaline solution) at a relatively high concentration. Examples of areas where alkaline solutions are used include the synthesis of alkaline cellulose in the rayon manufacturing stage, desizing scouring, bleaching, imparting gloss to fibers, dyeing with reactive dyes or vat dyes, mercerization, weight loss processing, and post-dyeing soaping. be.

When treating fiber materials with an alkaline solution, simply immersing the entire fiber in the alkaline solution or heating it depending on the purpose will not allow the alkali to penetrate quickly and uniformly into the inside of the fiber, so sufficient alkali treatment must be carried out. This will not be effective and will take a considerable amount of time.

Conventionally, in order to solve these problems, surfactants with good permeability or detergency, such as nonionic surfactants such as polyoxyethylene nonylphenyl ether, alkyl sulfates having 8 to 13 carbon atoms, or Anionic surfactants such as alkyl phosphates have been used.

However, nonionic surfactants have the disadvantage that sufficient effects can only be obtained in limited applications due to their own cloud points and salting-out phenomena in alkaline solutions of a certain concentration or higher.

Furthermore, although anionic surfactants such as alkyl sulfates and alkyl phosphates have good alkali resistance, they do not necessarily have good penetrating power or detergent power, and they have the drawback of high foaming properties.

The present inventors have arrived at the present invention as a result of intensive research in order to improve the drawbacks of conventionally used aids for alkali treatment of such fibers.
;l' When treating fiber materials with an alkaline solution, such as in processes such as scouring, bleaching, soaping, mercerization, or weight reduction processing, the following general formula (I) or (n) is used.
Compound i RI (where RI O) R1O- and R,0- have 1 carbon number
-18 alcohol residue or an alkylphenol residue t having an alkyl group having 1 to 12 carbon atoms.

Further, l t m and n are 0 or integers of 1-10,
and y represents an integer of 1-3. This invention relates to a method for alkali treatment of fiber materials characterized by using one or more of the following.

R@e in the formula represented by general formula (1) or (II)
R1 or R3 may be natural alcohol, synthetic alcohol, secondary alcohol, or alkylphenol as long as the number of carbon atoms is constant, but alcohols or alkylphenols should be selected depending on the degree of alkali of the treatment solution. Then, it is approximately as follows.

When used in an alkaline solution of 1.15% or less.

R, Q of the compound represented by general formula (13 or (If))
−.

It is preferable that R0-1 or R1α is a higher alcohol residue having 6 to 18 carbon atoms or an alkylphenol residue having an alkyl group having 1 to 12 carbon atoms.

When used in 215-30% alkaline solution.

R, O- of the compound represented by general formula (I) or (II)
.

Preferably, 0-2 or R,O- is an alcohol residue having 1-8 carbon atoms.

The details for each application are as follows.

(1) When fibers are treated with a solution having an alkaline concentration of approximately 5% or less, such as scouring, bleaching, reactive dyeing, or by-dye dyeing or soaping after dyeing.

R,0- of the compound represented by general formula (1) or (It)
, g, Q- or 4o- is a higher alcohol residue having 8-18 carbon atoms or an alkylphenol residue having 1-12 alkyl groups.

2. When used for gloss finishing of cotton fibers or as an alkali-containing textile detergent (alkali concentration is approximately 5-1
5chi).

R, O- of the compound represented by general formula (1) or (1)
R2O- or R,O- is a lower alcohol residue having 6 to 13 carbon atoms.

& When treating the fibers with a 1371% alkali solution of approximately 15-25%, such as mercerizing cotton fibers or reducing the weight of polyester fibers.

R10- or R,O- of the compound represented by the general formula [1] or (II) is an alcohol residue having 3-8 carbon atoms.

Not the same <Mercerization of Mf & fiber or weight loss processing of polyester fiber, etc., but the alkali concentration is 25-3
When used in 0% solution.

R, O- of the compound represented by general formula [1] or (II)
, R10- or R,0- is an alcohol residue having 1-6 carbon atoms.

The compounds of the present invention represented by general formula CI) or (II) can be easily synthesized. That is, Al: 1-ru fJA or B
Alkylphenol 6 or ethylene oxide (hereinafter referred to as E) is added to the alcohol or argylphenol by a known method.

0°) or/and propylene oxide (hereinafter referred to as P, 0.
After phosphoric acid esterification of the tl-added compound t using phosphorus oxychloride or phosphoric anhydride, etc., it is converted to E, 0. Or/and p, o, etc. may be added and then neutralized with caustic soda, aqueous ammonia or alkanolamines.

F, O to the algol or argylphenol.

Or/and when adding p, o, the number of moles added is 1
-107 g, but as an auxiliary agent when used for fiber sound treatment in a solution with an alkali concentration of 15 g or more,
It is preferable that the number of added moles is less than 1 mole.

Furthermore, E, O, or/and P, 0. The number of added moles of OH of the phosphoric acid ester is
Addition of more than 3 moles per group is not preferred because the solubility in alcoholic solutions decreases rapidly.

The amount of the auxiliary agent used in the present invention varies depending on the purpose of processing the fiber material, the alkali concentration of the processing solution, the type of alkali agent, the processing temperature, etc., but it is usually α02% - 2% of the processing solution.
Below are examples of synthesis and performance tests of compounds of the present invention. show.

Synthesis Example 1 Tridecyl alcohol 2001r (1 mol) was charged into a four-eye flask, and phosphoric anhydride 57k (α4 mol) was added.
Add gradually at t-40-50°C and react for about 1 hour,
Next, the temperature was raised to 90-95°C and the reaction was continued for another 4 hours to synthesize a phosphoric acid ester.The phosphoric acid ester was then transferred to an autoclave with a total capacity of 1 klt, m[8 (J-90C, pressure L5''). ZOKf/c
Under the conditions of td, E-0,53J'r (3 moles per mole of phosphoric anhydride) was added to prepare a mixture of approximately equal amounts of monoester and diester of the compound of the present invention having the following structure ( I got Arashi 1). 1 liter of acid of this is 2
Met.

In a similar manner, a mixture of equal amounts of monoester and diester (ha2) and Nα3 of the compound of the present invention having the following structure was obtained.

Synthesis Example 2 50 2-ethylhexanol 1aoIIr (x mol)
Pour phosphorus oxychloride 153# into a 0-Yoturo flask.
After gradually adding r (1 mol) dropwise at a temperature below 40'C, the mixture was allowed to react at the same temperature for 2 hours.

Next, 36 gr (2 mol) of water was added, and dehydrochlorination was further carried out for 5 hours to synthesize a phosphoric acid ester.

After that, the temperature was raised to 180-90℃ and E and O were added at the same temperature.

Gas 44JFr (1 mol) was introduced and added, and then neutralized with 50% caustic soda to obtain 80% of the compound of the present invention (Nα4) having the following structure.

The acid value of the compound before neutralization was approximately 218.

Compound of the present invention (No. 5) having the following structure in a similar manner
A 90-piece product of (N16) and an 85-piece product of (N16) were obtained.

/ \ ON.

The compounds of the present invention shown in the above synthesis examples were used according to their respective uses, and performance tests shown in the following examples were conducted.

In the performance test, each sample was diluted with water to a concentration of 50%.

The structural formulas of the compounds shown in the above synthesis examples are all models.

Examples of the present invention Convex 1* Na2p Na4p and Ugly 5 as well as the solubility of the auxiliary agent in 0-5% Na0n solution,
Penetration and foaming? Examined.

The results are shown in Table 1. The measurement temperature was 20°C, and the amount of auxiliary agent used was 0.5 cm.

* Comparative product NaI CHH2gO801Nm (50
% product) (50chi product) From the results in Table 1, the present invention product N [L1+ N112p N
A4 and 5 are comparative products N[L 1. It can be seen that compared to p Nu 2 and 3, it has excellent solubility and permeability in 0-5% NaOH solution, and has low foaming properties.

Example 2 In order to investigate the scouring sound effect on polyester fibers, a desizing test using an acrylic acid sizing agent was conducted using the following method.

Test method: A 1% solution of acrylic acid-based sizing agent Plus Size J-21 (manufactured by Goo Kagaku Co., Ltd.) was impregnated into a scouring cloth of polyester processed yarn fabric, squeezed at a squeezing rate of IOO, and dried at 130°C x 5. A sample fabric was prepared by heat treatment, and this sample fabric was treated under the following conditions.

Processing conditions> Bath ratio: l220 Processing temperature: 80°C
E type), the reflectance was measured, the dyeing density was calculated, and the shedding rate of the glue was calculated using the following formula.

Staining conditions> Rnodmine 11 0.1% o, w, fpH5
, 0 (adjusted with acetic acid) Bath ratio 1:20 Dyeing temperature 60°C x 10ml The results are shown in Table 2.

The test aids were the same as in Example 1.

From the results in Table 2, it can be seen that the auxiliary agent of the present invention product has an excellent desizing effect compared to the case where no auxiliary agent was added and the comparative product.

Example 3 A hydrogen peroxide bleaching test was conducted using unscoured cotton knit cloth under the following conditions.

Motani ratio: 20 Treatment temperature: 85° C. x 45 min The whiteness of the bleached cloth treated under the above conditions was measured using a T-Hunter whiteness meter. The results are shown in Table 3.

The test aids were the same as in Example 1.

Below is a blank Table 3 Hydrogen peroxide bleaching test results From the results in Table 3, the auxiliary agent of the present invention product is superior in white discoloration improvement effect compared to the product without the auxiliary agent and the comparative product.

Example! In order to examine the penetrating power of vat dye in a reducing bath, a test was conducted under the following conditions.

Composition of reducing bath〉 Auxiliary agent α31 Test method 2 Heat the above reducing bath to 70°C, and add cotton gabardine (2
x21) sedimentation start time was measured.

The results are shown in Table 4. The test aids were the same as those in Example 1, but comparative product No. 3 was excluded because it was insoluble.

Table 4. As is clear from Table 4, the auxiliaries of the present invention have excellent penetration power in the reducing bath compared to the comparative products.

Example 5 Inventive product t4113. Using N11L4 and No. 6 and comparative product No. 1 # No. 2 and N[L4i, the solubility permeability and foaming property in 5-15% Na0HI'4 solution were investigated in the same manner as in Example 1. The results are shown in Table 5.

*Comparative product N114 C, H, 70SO, Na (50% product) Table 5 Solubility, permeability and foaming test results (Display method is exactly the same as in Example fIIl) Example 6 Invention 8 Fly 3 and Na6 and comparative products Na4 and Na
? As in Example 1, 5-25 tN, O
The solubility, permeability and foaming property in H solution were investigated. The results are shown in Table 6.

*Comparison product Sho 5 C1H70SO1NB (50% product) Table 6. As is clear from the results of solubility, permeability, and foaming test results (the display method is exactly the same as in Example 1) in Tables 5 and 6, the auxiliary agent of the present invention product has a higher It can be seen that both have excellent solubility and permeability, and low foaming properties.

Example 7 In order to investigate the effect on cotton mercerization, the shrinkage rate of cotton thread was measured by the following method.

Test method: A weight was hung with a cotton thread, and the shrinkage rate of the thread was measured from the height of the weight using the following formula (see the figure below).

The results are shown in Table 7.

Dark, the test auxiliary agent was the same as in Example 6, but the comparative product FJa
4 was excluded because it was insoluble.

1゜Table 7 Shrinkage rate of cotton thread (ch) As is clear from Table 7, the auxiliary agent of the product of the present invention is superior in the shrinkage of cotton yarn compared to the comparative product or the case where no auxiliary agent is added. I understand.

Patent applicant: Toho Chemical Industry Co., Ltd.

Claims (1)

[Claims] Compounds represented by the following general formula [1] or (1()) when treating fll fiber materials with alkaline agents such as scouring, bleaching, nooping, mercerization, or thickness reduction processing. R/ n/ (However, R,0-+ R, O- and o-, represent an alcohol residue having 1-18 carbon atoms or an alkylphenol residue having an alkyl-j&wo having 1-12 carbon atoms. Alkali treatment of fiber material using -dan or two or more of (where t + m and is an integer t of 0 or !-10, and X and y are integers a of 1-3) Method. r2) RlO-, R0- and R,O- have 6 carbon atoms
-18 Kla alcohol residues or alkylphenol residues having 1-12 alkyl groups; A method for alkali treatment of Goku material, characterized in that it is used. (3) R, O-, bird 0- and R, O-, have 1 carbon number
Compound t-1 according to claim 1, consisting of an alcohol residue of No. 8. An alkali agent for textile materials, characterized in that it is used when textile materials are treated with an alkali solution of 15% to 30%. Processing method.