KR920001931B1 - Manufacturing method of modified polyester fiber - Google Patents

Abstract

The modified polyester fiber is prepd. by adding the cpd. (I) when end state of the esterification or inital stage of the polycondensation and reacting; spinning and alkali- shrinking then making uneven surface on the fiber after dyeing process. In the formula, R1 is monovalent org. gp.; X is hydroxy gp.; M is alkali (earth) metal; n1 is 0 or 1; R2 and R3 are a cpd. contg. C1-8 aliphatic hydrocarbon; n2 is 1 or 2. Pref. the cpd. of (I) is 1.0-4.0 wt. pts. w.r.t. the polymer. The obtd. fiber has excellent deep-coloring property and drapability.

Description

Method of Making Modified Polyester Fiber

The present invention relates to a method for producing a modified polyester fiber having good deep colorability and drapeability compared to general polyester fiber after alkali reduction and dyeing by imparting fine irregularities to the fiber surface.

Polyester fiber has various uses such as clothing and industrial materials because of its unique characteristics, but due to its high crystallinity, its dyeing effect is insufficient. Difficulties have arisen in the use of oriented high value-added products.

Therefore, in order to overcome such drawbacks, process modifications such as polymerization stages, weaving and dyeing processing steps have been developed. As a representative technique, a method of coating low refractive resin on the surface of polyester fiber, a method of imparting irregularities to the surface by plasma processing the polyester fiber surface, and an alkali reduction process in the post-spinning process by adding an additive during polymer polymerization Accordingly, a method of maximizing the light scattering effect by providing irregularities on the surface by removing insoluble fine particles has been published.

However, the method of coating the low refractive resin and the method of imparting the surface irregularities by the plasma processing treatment should be equipped with the difficulty of uniform adhesion formation and the expensive special device. A method of imparting color depth by a method of maximizing the light scattering effect has been put to practical use.

As a method of maximizing the light scattering effect, there is an external particle method in which silica-based dispersed particles are introduced during a polymer polymerization process and then eluted in an alkali-reduced state after spinning, but problems such as uneven surface irregularities and poor abrasion resistance, and particularly unreactive inorganic particles In the process of spinning the particles have problems such as poor radioactivity by coarse particles.

On the other hand, as a method using internal particles, a method of self-reacting a phosphorus compound and an alkaline earth metal compound during the polymerization process to form an insoluble alkaline earth metal salt and eluting it in an alkali-reduced state after spinning has been introduced. It is difficult to obtain a satisfactory deep color effect.

Such a method is disclosed in Korean Patent Publication Nos. 88-12803, 88-7833, Japanese Patent Laid-Open Nos. 59-21720, 60-59171, 61-152816, 61-160476, 61-258018, 62-238865 and the like.

The inventors of the present invention have studied ways to solve the process problems caused by the manufacturing method to maximize the light scattering effect, and to increase the deep color effect. The present invention has been achieved by the addition of late reaction or early polymerization condensation.

(Wherein R ₁ is a monovalent organic group, X is a hydroxyl group, M is an alkaline earth metal such as manganese, cobalt, zinc, nickel, etc., n1 is 0 or 1, and R ₂ and R ₃ have 1 to 8 carbon atoms). Compound containing an aliphatic hydrocarbon, n2 is 1 or 2.)

The compound of the general formula (I) is an externally synthesized alkaline earth metal compound, which is added after the reaction at the end of the ester reaction or the initial polycondensation reaction in a general polyester polymerization process using terephthalic acid or dimethyl terephthalate and ethylene glycol, followed by spinning Subsequently, after the reduction of alkali in the process, it is possible to form fine irregularities on the surface of the fiber.

That is, the present invention is 0.5 to 4.0 parts by weight of the compound of the general formula (I) to the end of the ester reaction or the initial polycondensation reaction when the polyester produced by the diol and dicarboxylic acid or ester reaction thereof is added, It relates to a method for producing a modified polyester fiber characterized in that the polycondensation reaction at the initial reaction temperature 140 ~ 245 ℃, the late reaction temperature 245 ~ 285 ℃ when described in detail, the present invention is diol and dicarboxylic acid or It is preferable that the input time is applied during the production of general polyester fiber produced by the ester reaction, and more specifically, the end of the ester reaction.

Hereinafter, the present invention will be described in detail based on examples.

Example 1

100 parts by weight of dimethyl terephthalate, 60 parts by weight of ethylene glycol, 0.083 parts by weight of calcium acetate, 0.038 parts by weight of antimony trioxide and the like were placed in a transesterification reactor and heated slowly at 140 ° C.

, M=Mn, n1과 n2=1인 상기 (I)의 화합물을 2.5중량부 투입하고 에틸렌 글리콜 회수공정이 끝난직후 에스테르 교환반응을 종료시켰다. 생성물을 중축합 반응조로 이행한 후 트리메틸 포스페이트 0.04중량부를 투입한뒤 0.1~0.2mmHg까지 감압하면서 280~285℃의 온도로 약 2시간 30분간 중축합 반응을 완료한 후 그 물성 및 심색도를 평가하였다. 그 평가치는 표 1과 같다.When methanol outflow reached about 400 ml and the final internal temperature of the reactor reached 240 ° C, R ₁ = -CH ₃ , X = -OH, R ₂ = -CH _2- , R ₃ =

2.5 parts by weight of the compound of (I), wherein M = Mn, n1 and n2 = 1, and terminated the transesterification reaction immediately after the ethylene glycol recovery process was completed. After the product was transferred to a polycondensation reactor, 0.04 parts by weight of trimethyl phosphate was added, and the polycondensation reaction was completed at a temperature of 280 to 285 ° C. for about 2 hours and 30 minutes under reduced pressure to 0.1 to 0.2 mmHg. It was. The evaluation value is shown in Table 1.

Example 2

1 part by weight of the compound (I) used in Example 1 was added and the same procedure as in Example 1 was carried out. The results are shown in Table 1.

Comparative Example 1

5 parts by weight of the compound (I) used in Example 1 was added thereto, and the same procedure as in Example 1 was carried out. The results are shown in Table 1.

Comparative Example 2

The addition time of the compound (I) used in Example 1 was added 2.5 parts by weight in the initial transesterification reaction was carried out in the same manner as in Example 1. The results are shown in Table 1.

Comparative Example 3

At the end of the transesterification reaction, the compound of formula (I) used in Example 1 was not administered, the transesterification reaction was terminated, the product was transferred to a polymerization reactor, and then 0.04 parts by weight of trimethyl phosphate was added to the same method as in Example 1. Was carried out. The results are shown in Table 1.

TABLE 1

The intrinsic viscosity of the prepared polymer was measured in an orthochlorophenol solution at 30 ° C., and melting point and glass transition temperature were measured using DuPont's Model 990 differential scanning heat analyzer.

The color depth is 4 hours after drying the polymer at 170 ° C. in a vacuum dryer, spinning and stretching in a conventional manner, and then weaving, dyeing with a black dispersion dye by a high temperature and high pressure method at 20% alkali reduction. It evaluated by the evaluation method.

[Method of evaluation of depth]

How to judge by water supply: Determine the water supply by visually comparing the color of the forge weaved with deep color yarn with the general forge of the same tissue (if the level 4 or higher, deep water effect).

Instrumental method:

1) Determined by measuring the reflectance by spectrophotometer measurement. (The larger the value of α, the deeper the color.)

K: extinction coefficient of the sample

S: light scattering coefficient of the sample

R: reflectance of monochromatic light

2) L * measurement by colorimeter measurement

(L * lower, better deep color)

In the results of Table 1, in Example 1, when compared with Comparative Example 1, which is a general polyester manufacturing method, the physical properties of the polymer is the least, the surface uneven structure, deep colorability was the best, in the case of Example 2 In the case of Comparative Example 1, the color depth was insufficient, and in the case of Comparative Example 1, the color depth was tended to be lowered due to the excessive input, and in Comparative Example 2 in which the timing was changed, the particle formation was poor and the color depth was decreased. Is showing.

Claims (2)

In the polyester polymerization produced by the reaction of diol with dicarboxylic acid or esters thereof, the compound of the general formula (I) is added to the end of the ester reaction or the initial stage of the polycondensation reaction, and then reacted. Method for producing a modified polyester fiber, characterized in that to give surface irregularities to the fiber after dyeing process by alkali reduction process.

(Wherein R ₁ is a monovalent organic group, X is a hydroxyl group, M is an alkali or earth metal, n1 is 0 or 1, and R ₂ and R ₃ are compounds containing an aliphatic hydrocarbon having 1 to 8 carbon atoms) , n2 is 1 or 2). The method for producing a modified polyester fiber according to claim 1, wherein 1.0 to 4.0 parts by weight of the compound of the general formula (I) is added to the polymer to perform a polycondensation reaction.