JPS61124625A - Easily dyeable polyester yarn - Google Patents

Abstract

PURPOSE:The titled yarn having improved basic dyeing properties with a small amount of a 5-metallic sulfoisophthalic acid component (SIP), improved strength and fastness to dyeing, obtained by adding a polyorganosiloxane to a polyester containing SIP. CONSTITUTION:Polyester yarn having 0.5-0.7 intrinsic viscosity, having 0.5-2mol% copolymerized SIP, containing 1-20wt% polyorganosiloxane having 600-150,000 molecular weight. SIP and the polyorganosiloxane (e.g., polydimethylsiloxanediol, etc.) are added to a polyester oligomer preferably before beginning of polycondensation reaction, the polyester is subjected to polycondensation to give a polyester, which is spun. SIP contains preferably an alkali metal as a metal, usually 5-metallic sulfoisophthalic acid, or an ester- forming derivative such as 5-metallic sulfoisophthalic acid lower alcohol ester, or its lower glycol ester may be used as SIP.

Description

Detailed Description of the Invention (Field of Industrial Application) The present invention provides an easy-to-dye product which can be easily dyed with a basic dye consisting of a polyester copolymerized with a 5-metal sulfoisophthalic acid component and containing a polyorganosiloxane. The invention relates to polyester fibers.

(Prior Art) Polyester, especially polyethylene terephthalate, has excellent mechanical and chemical properties and is used for clothing.

Widely used as an industrial fiber.

By the way, polyethylene terephthalate fibers do not have good dyeability, and various methods have been proposed to improve the dyeability.

The most typical method is to copolymerize polyester with a 5-metal sulfoisophthalic acid component (SIP) to make it dyeable with basic dyes (Japanese Patent Publication No. 34-10).
Publication No. 497). However, in order to obtain polyester fibers with satisfactory dyeability using this method, a large amount of SIP must be copolymerized.

Due to the thickening effect of SIP, if the intrinsic viscosity (degree of polymerization) of polyester is sufficiently increased, the melt viscosity will become extremely high, making melt spinning difficult, and if the intrinsic viscosity is decreased, only low-strength fibers can be obtained. Also, SI
If a large amount of P is copolymerized, there is a problem that the alkali resistance of the fiber will be reduced, which will limit the use of the fiber.Furthermore, since SIP is expensive, the cost will increase.

Attempts have also been made to improve the dyeability of monodisperse dyes by incorporating polyorganosiloxanes, but as described in Japanese Patent Publication No. 1834-1983, polyorganosiloxanes are compatible with polyesters. It has poor solubility, and when blended with polyester, it tends to become cloudy, and it has been considered difficult to sufficiently improve the dyeability of polyester by adding polyorganosiloxane.

(Problems to be Solved by the Invention) The present invention improves the technique of improving the dyeability of polyester fibers by SIP copolymerization, and provides dyed products that can be easily dyed with basic dyes, have a high light fastness, The object of the present invention is to provide easily dyeable polyester fibers with excellent alkali resistance and strength.

(Means for Solving the Problems) The present invention achieves the above objects, and the gist thereof is as follows.

5-Metal sulfoisophthalic acid component is copolymerized with 0.5 to 2 mol% of polyester containing 1 to 20% by weight of polyorganosiloxane with a molecular weight of 600 to 150,000, and has an intrinsic viscosity of 0.5 to 2 A polyester fiber characterized by having a polyester fiber of 0.7.

In the present invention, polyethylene terephthalate is preferred as the base polyester.

Isophthalic acid, p-oxybenzoic acid, adipic acid.

trimellitic acid, propylene glycol, 1.4-
It may also contain a small amount of butanediol, 1,4-cyclohexane dimetatool, pentaerythritol, etc. as a copolymer component.

In the present invention, SIP is 5-metal sulfoisophthalic acid and its lower alcohol ester.

An ester-forming derivative such as a lower glycol ester is used, and the metal thereof is preferably an alkali metal such as Na, Li, or Ni.

The copolymerization ratio of SIP needs to be 0.5 to 2 mol%; if it is less than 0.5 mol%, sufficient dyeability cannot be obtained, and if it exceeds 2 mol%, the above-mentioned large amount of SIP copolymerization It shows the flaws.

Further, as the polyorganosiloxane in the present invention, compounds represented by the linear formula are preferably used.

I R'-04Si -0-f R' (where 11 to R4 are hydrogen atoms or carbon atoms 1 to 2
0 organic group, n indicates the average degree of polymerization. ) These include dialkylsilanediol, diarylsilanediol or alkylarylsilanediol, examples of which include polydimethylsiloxanediol.

Examples include polydiphenylsiloxane diol and polymethylphenylsiloxane diol. It is also possible to use polyorganosiloxanes in which alkoxy groups, thiol groups, carboxyl groups, amino groups, vinyl groups, epoxy groups, etc. are bonded to the terminal silicon atom. i The molecular weight of the liorganosiloxane must be between 600 and 150,000. If it is less than 600, the effect of improving dyeability is poor and is not preferable.

If it exceeds 150,000, the viscosity becomes extremely high (more than 3,000 Stix at 25° C.), which not only impairs workability but also reduces color fastness, which is not preferable.

What is the amount of polyorganosiloxane? It is necessary to set it at 1 to 20% by weight. If this amount is less than the lower limit of this range, the auxiliary effect of improving dyeability will not be substantially achieved, while if it exceeds the upper limit of this range, the degree of polymerization required to maintain the strength required for polyester fibers will not be achieved. This is undesirable because it may not reach the desired temperature, gelation may occur, or the good physical properties inherent to polyester may be impaired.

SIP and polyorganosiloxane can be added at any time before the single polycondensation reaction is completed.

Preferably, it is added to the polyester oligomer before the start of the polycondensation reaction for polycondensation.

The condensation reaction is carried out in the presence of a catalyst, and conventionally commonly used metal compounds such as antimony, titanium, germanium, and tin are used as catalysts, and antimony dioxide and dimethyltin maleate are particularly preferably used. The amount of catalyst added is 1:1 of the acid component constituting the polyester.
I X 10-' to I X 10-''% relative to moles
/L'+ Good* L < Ct 5 X 10-'~5
xlO-'mol, Yori t L < Ha1 xlO
-' to 3 xlO-' moles is appropriate.

In addition, if necessary, diethylene glycol binding by-product inhibitors such as alkali metal compounds, stabilizers such as hindered phenol compounds, cobalt compounds, fluorescent agents, color improvers such as dyes, and titanium dioxide may be added. Pigments etc. can be added.

The degree of polymerization of polyester is such that the intrinsic viscosity when made into fiber is 0.5 to 0°7. Preferably, it is necessary to set it to 0.55 to 0.65. If the intrinsic viscosity is less than 0.5, a fiber with sufficient strength (4 g/d or more) cannot be obtained, while if it exceeds 0.7, the melt viscosity is extremely high (which makes it difficult to carry out 9-poly condensation and spinning).

The polyester fiber of the present invention can be obtained by spinning the polyester thus obtained by a conventional method. In addition, it will be more effective if a high speed spinning method of 3.000 ta for 1 minute or more is adopted and ultrafine fibers with a single filament fineness of 1 denier or less are used.

(Function) Although the reason why the polyester fiber of the present invention exhibits excellent dyeability is not clear, the coexistence of polyorganosiloxane in the polyester makes the degree of dyeing to basic dyes of SIP extremely effective. It is surmised that this is to be used. Furthermore, since only a small amount of SIP is required and the polyorganosiloxane has some reactivity with polyester, it is presumed that the yarn strength is improved and the fastness after dyeing is also improved.

(Example) Next, the present invention will be specifically explained with reference to Examples.

In addition, in the examples, characteristic values etc. were measured as follows.

(1) Intrinsic viscosity Measured at 20°C using an equal weight mixture of phenol and tetrachloroethane as a solvent.

(21 SIP and polyorganosiloxane content 57
The content of Si and Si was determined by quantitative determination using a fluorescent X-ray method.

(3) The drawn yarn with dyeability of 75d/36f is made into a tubular knitted fabric, and after scouring, washing with water and drying, it is dyed with basic dye Astrazone Blue.
10 in the first dye bath using eFRR (manufactured by Bayer)
The dyeing was carried out at 0° C. for 30 minutes, and the dye concentration in the dyed residual liquid was measured to determine the dye exhaustion rate.

Dye concentration 1%owf ゛ Sodium acetate 0.2g/l Acetic acid 0.2ra l/1 bath
Ratio 1:50 (Colorfastness) The tubular knitted fabric dyed using the above method was reduced and washed, washed with water, dried, and then placed in a fade meter with blue scale and exposed to light. JIS L-0842 and JIS L-084
The color was faded according to 3, and the light fastness was determined.

(5) Cylindrical knitted fabric made of drawn yarn with alkali resistance of 75d/36f at a concentration of 50g/
1 sodium hydroxide aqueous solution at 95°C, bath ratio 1:10
0 to give a weight loss rate of 10%, the strength of the yarn obtained by knitting was measured.

Example A slurry of terephthalic acid and ethylene glycol (molar ratio 1:1.6) was continuously fed into an esterification reactor containing bis-(β-hydroxyethyl) terephthalate and its low polymer (BHET). 250℃, 0
．． The reaction was carried out at 05 kg/aJ G for a residence time of 8 hours, and BHET with a reaction rate of 95% was continuously obtained.

The obtained BHET was transferred to a polymerization tank and heated to 270°C.

5-Sodium sulfoisophthalic acid (SIPA) and polydimethylsiloxane diol (PDMSO) were added (see Table 1), and then antimony dioxide was added as a catalyst at 2×10-' mol/mol of acid component to give 280
Polycondensation was carried out at a predetermined intrinsic viscosity at ``c, Q, 2+ueHg''.

The obtained polyester was spun at a spinning temperature of 360°C to a diameter of 0.
Using a spinneret with 36 15 m spinning holes,
Spinning at a discharge rate of 33 g per minute, winding at a speed of 1400 m/min, stretching temperature 80°C, heat treatment temperature 110°C.
℃ and stretched approximately 3.10 times at a stretching speed of 650 m/min.

A drawn yarn of 75d/36f was obtained.

Table 1 shows the characteristic values of the obtained drawn yarn.

In addition, reference examples are added to Table 1, and reference example 1 is ordinary polyethylene terephthalate fiber, and reference example 2 is 5IPA fiber.
Reference Example 3 is a polyethylene terephthalate polyester fiber copolymerized with SIP^ and 10% by weight of polyethylene glycol having a molecular weight of 2000.

(Effects of the Invention) As described above, according to the present invention, by coexisting polyorganosiloxane with SIP copolymerization, the dyeability with respect to basic dyes is significantly improved.

In addition, polyester fibers with excellent alkali resistance and yarn strength can be obtained, and such polyester fibers can be produced with good spinnability. In addition, the polyester fiber of the present invention has good spinnability and satisfactory dyeability even under normal spinning conditions without using any special equipment such as a heating tube.

Claims (2)

[Claims] (1) 0.5 to 2 mol% of 5-metal sulfoisophthalic acid component is copolymerized, and the molecular weight is 600 to 150,000.
1. A polyester fiber comprising polyester containing 1 to 20% by weight of polyorganosiloxane, and having an intrinsic viscosity of 0.5 to 0.7. (2) The polyester fiber according to claim 1, wherein the polyorganosiloxane is a compound represented by the following formula. ▲There are mathematical formulas, chemical formulas, tables, etc.▼ (Here, R^1 to R^4 are hydrogen atoms or 1 carbon atom.
~20 organic groups, n indicates the average degree of polymerization. )(3) The molecular weight of the polyorganosiloxane is 10,000 to 100,
000, the polyester fiber according to claim 1 or 2.