JP2003253101A - Polyester highly containing manganese compound, manufacturing process of polytrimethylene terephthalate composition, and fiber with improved light resistance - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a polyester highly containing a manganese compound which is necessary to manufacture a polytrimethlene terephthalate polyester fiber having an improved light resistance. <P>SOLUTION: The polyester highly containing a manganese compound contains a manganese compound in the amount of 150 ppm or more and 10,000 ppm or less in terms of manganese. And the ratio of the contained manganese to phosphorus falls within the range as specified in the formula: (1) 0≤P/Mn≤1 (wherein, P is a mole equivalent of phosphorus, and Mn is a mole equivalent of manganese). <P>COPYRIGHT: (C)2003,JPO

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polyester containing a high concentration of manganese compound, a method for producing a polytrimethylene terephthalate composition using the same, and fibers, and more specifically, it has improved weather resistance with little yellowing after irradiation with light. The present invention relates to a method for producing a polytrimethylene terephthalate-based polyester composition and a fiber having improved light resistance.

[0002]

BACKGROUND OF THE INVENTION As is well known, polyester is
Due to its excellent performance, it is widely used for fibers, resins, films and the like. In particular, polyester fibers made of polyethylene terephthalate are excellent in dimensional stability, heat resistance, chemical resistance, light resistance and the like, and are used in various fields regardless of whether they are clothes or not.

Under such circumstances, in recent years, polytrimethylene terephthalate polyester fibers and woven and knitted fabrics thereof have been attracting attention in order to develop a texture and a dyeing property which are difficult to realize by conventional polyethylene terephthalate (for example, Japanese Patent Application Laid-Open No. 11-. No. 200175). However, this polytrimethylene terephthalate-based polyester fiber has a problem that the polyethylene terephthalate undergoes large yellowing upon irradiation with light and is inferior in light resistance.

As a method for improving the whiteness of this polytrimethylene terephthalate, for example, WO99 / 117 is used.
No. 09, etc. propose to add a phosphorus compound at the time of polymerization. However, even if the melt stability is improved by this method, improvement in light resistance cannot be expected.

On the other hand, as a method for improving the light resistance of polyester fibers, for example, Japanese Patent Laid-Open No. 3-234812 describes a method of adding a manganese compound, an antimony compound and a germanium compound to polyethylene terephthalate. However, this method relates to suppression of strength deterioration of polyethylene terephthalate fibers, and is a technique different from yellowing prevention, particularly yellowing prevention of polytrimethylene terephthalate fibers.

A technique for adding a manganese compound to polytrimethylene terephthalate is disclosed in US Pat. No. 58.
No. 72204 describes using a manganese compound as a catalyst that can be used in combination with an antimony compound catalyst, but there is no description that light resistance is improved by this method, and since an antimony compound is used, There is a problem that foreign substances are likely to be generated when the fiber is made.

[0007]

SUMMARY OF THE INVENTION The object of the present invention is to solve the problems of the prior art and to provide manganese necessary for producing a polytrimethylene terephthalate-based polyester fiber having improved light resistance. It is to provide a polyester containing a high concentration of a compound.

Still another object of the present invention is to provide a method for producing the above polyester composition.

[0009]

Means for Solving the Problems As a result of earnest studies to achieve the above object, the present inventor has found that a fiber obtained by melt spinning a specific polytrimethylene terephthalate polyester is yellow after light irradiation. As a result of further finding out that the change can be reduced, the present invention has been achieved.

That is, an object of the present invention is to make a manganese compound of polyester and convert the manganese compound to 150 manganese elements.
This is achieved by a polyester containing a high concentration of manganese compound, which is contained in an amount of more than 10,000 ppm and not more than 10,000 ppm, and the ratio of the contained manganese element amount to the phosphorus element amount is within the range of the following formula (I).

[0011]

## EQU00003 ## 0.ltoreq.P / Mn.ltoreq.1 (I) (where P is the molar equivalent of phosphorus element, and Mn is the molar equivalent of manganese element) Further, another object of the present invention is to provide the manganese according to claim 1. The compound high-concentration polyester is added to a polytrimethylene terephthalate-based polyester polymer comprising trimethylene terephthalate repeating units in an amount of 0.5 to 50% by weight based on the polyester polymer and melt-kneaded,
10 to 150 pp of manganese compound in terms of manganese element
A method for producing a poly (trimethylene terephthalate) -based polyester composition, which comprises a poly (trimethylene terephthalate) -containing polyester containing m and having the manganese element amount and the phosphorus element amount satisfying the relationship of the following formula (I): You can

[0012]

## EQU00004 ## 0.ltoreq.P / Mn.ltoreq.1 (I) (where P is the molar equivalent of phosphorus element, and Mn is the molar equivalent of manganese element).

[0013]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below.

The polyester containing a high concentration of manganese compound of the present invention has a manganese compound content of 150 in terms of manganese element.
Over 10,000 ppm is required. When the manganese element content is 150 ppm or less, it becomes necessary to use a large amount of a manganese compound high-concentration polyester in order to obtain a light resistance of the finally obtained fiber at a sufficient level. On the other hand, when it exceeds 10000 ppm, the yellow color of the polyester itself containing a high concentration of manganese compound becomes large, and the molecular weight is remarkably lowered by thermal decomposition, which makes it difficult to control the quality of the finally obtained fiber. The amount of elemental manganese in the polyester containing a high concentration of manganese compound is preferably in the range of 300 to 8000 ppm, more preferably in the range of 500 to 5000 ppm.

The manganese compound used in the present invention is preferably a divalent manganese salt, particularly preferably manganese acetate, manganese benzoate, manganese chloride, manganese sulfate, manganese borate, manganese formate and the like.

Further, in the polyester containing a high concentration of manganese compound of the present invention, the ratio of the content of manganese element to the content of phosphorus element must satisfy the relationship of the following formula (I).

[0017]

## EQU00005 ## 0.ltoreq.P / Mn.ltoreq.1 (I) (where P is the molar equivalent of phosphorus element, Mn is the molar equivalent of manganese element) In the above formula (I), when P / Mn is larger than 1 Results in insufficient light resistance of the finally obtained fiber. P / Mn
Is more preferably in the range of 0 to 0.8, and particularly 0
It is preferably in the range of to 0.6.

The high concentration manganese compound-containing polyester of the present invention is preferably at least one polyester selected from the group consisting of polytrimethylene terephthalate polyester, polyethylene terephthalate polyester and polytetramethylene terephthalate polyester. The polyester may be a blended polymer of two or more kinds, but it is particularly preferably a polytrimethylene terephthalate polyester.

The polytrimethylene terephthalate polyester in the method for producing the polytrimethylene terephthalate polyester composition of the present invention is a polytrimethylene terephthalate polyester mainly composed of trimethylene terephthalate repeating units.

Here, the "polytrimethylene terephthalate-based polyester mainly comprising trimethylene terephthalate repeating units" means that the trimethylene terephthalate repeating unit which is a constituent of the repeating unit is 85 mol% or more based on all repeating unit components. A poly (trimethylene terephthalate) -based polyester that occupies 90 mol% or more is preferable.

In the method for producing a polytrimethylene terephthalate type polyester composition of the present invention, when the polyester containing a high concentration of manganese compound is added to the polytrimethylene terephthalate type polyester, the high concentration of manganese compound is added to the polytrimethylene terephthalate type polyester. The contained polyester is melt-kneaded at 0.5 to 50% by weight, and the manganese compound in the polytrimethylene terephthalate-based polyester composition is converted into manganese element,
It is necessary to contain it so as to be 10 to 150 ppm. If the manganese element content is less than 10 ppm, the light resistance of the finally obtained fiber will be insufficient. On the other hand, 1
When it exceeds 50 ppm, the yellowness of the polymer itself becomes large, and the yellowing at the time of remelting and the decrease of the molecular weight become large, which is not preferable. The amount of manganese element is 15-120p
The range of pm is preferable, and the range of 20 to 100 ppm is more preferable. When the amount of the high-concentration manganese compound-containing polyester is 0.5% by weight or less, it becomes difficult to uniformly disperse the manganese compound in the polytrimethylene terephthalate-based polyester composition, and thus 50% by weight.
If it exceeds, the amount of the high-concentration manganese compound-containing polyester used is too large, which is not preferable because the efficiency of the polytrimethylene terephthalate-based polyester composition manufacturing process becomes poor. The amount of the high-concentration manganese compound-containing polyester is preferably in the range of 0.7 to 40% by weight, and 1 to 30% by weight.
Is more preferable.

Further, in the polytrimethylene terephthalate type polyester in the method for producing the polytrimethylene terephthalate type polyester composition of the present invention, the ratio of the manganese element amount and the phosphorus element amount contained satisfies the relationship of the following formula (I). There is a need to.

[0023]

0 ≤ P / Mn ≤ 1 (I) (where P is the molar equivalent of phosphorus element, and Mn is the molar equivalent of manganese element) In the above formula (I), when P / Mn is larger than 1, Results in insufficient light resistance of the finally obtained fiber. P / Mn
Is more preferably in the range of 0 to 0.8, and particularly 0
It is preferably in the range of to 0.6.

In the method for producing the polytrimethylene terephthalate-based polyester composition of the present invention, the method of melt-kneading the polyester containing a high concentration of manganese compound with the polytrimethylene terephthalate-based polyester is not particularly limited. Method of adding solid or molten manganese compound high-concentration polyester in a side feeder or the like to the polytrimethylene terephthalate-based polyester melted by, after chip-blending the polytrimethylene terephthalate-based polyester and manganese compound high-concentration polyester, melted A method of kneading, a method of adding polyester chips containing a high concentration of manganese compound to a polymerization reaction vessel at a polymerization reaction stage of a polytrimethylene terephthalate-based polyester polymerized by a batch method, It is below.

The polytrimethylene terephthalate-based polyester in the method for producing the polytrimethylene terephthalate-based polyester composition of the present invention is in the range that does not impair the characteristics thereof, preferably in the range of 10 mol% or less based on the total dicarboxylic acid component. Components other than the terephthalic acid component and the trimethylene glycol component may be copolymerized.

Examples of these copolymerization components include isophthalic acid, orthophthalic acid, naphthalenedicarboxylic acid, diphenyldicarboxylic acid, diphenyletherdicarboxylic acid, diphenylsulfonedicarboxylic acid, benzophenonedicarboxylic acid, phenylindanedicarboxylic acid, 5-sulfoxyisophthalic acid metal salt. Aromatic carboxylic acids such as 5-sulfoxyisophthalic acid phosphonium salt, ethylene glycol, tetramethylene glycol, pentamethylene glycol, hexamethylene glycol, octamethylene glycol, decamethylene glycol, neopentylene glycol, diethylene glycol, triethylene glycol, Aliphatic glycols such as polyethylene glycol, polytetramethylene glycol, cyclohexanediol, 1,4- Cyclohexane dimethanol, 1,
Alicyclic glycol such as 4-cyclohexanediol, o
-Xylylene glycol, m-xylylene glycol,
p-xylylene glycol, 1,4-bis (2-hydroxyethoxy) benzene, 1,4-bis (2-hydroxyethoxyethoxy) benzene, 4,4'-bis (2-
Hydroxyethoxy) biphenyl, 4,4'-bis (2
-Hydroxyethoxyethoxy) biphenyl, 2,2-
Bis [4- (2-hydroxyethoxy) phenyl] propane, 2,2-bis [4- (2-hydroxyethoxyethoxy) phenyl] propane, 1,3-bis (2-hydroxyethoxy) benzene, 1,3- Bis (2-hydroxyethoxyethoxy) benzene, 1,2-bis (2-
Hydroxyethoxy) benzene, 1,2-bis (2-hydroxyethoxyethoxy) benzene, 4,4′-bis (2-hydroxyethoxy) diphenylsulfone, 4,
Aromatic glycol such as 4′-bis (2-hydroxyethoxyethoxy) diphenyl sulfone, hydroquinone,
Examples thereof include diphenols such as 2,2-bis (4-hydroxyphenyl) propane, resorcin, catechol, dihydroxynaphthalene, dihydroxybiphenyl and dihydroxydiphenylsulfone. These may be used alone or in combination of two or more.

The high-concentration manganese compound-containing polyester of the present invention and the polytrimethylene terephthalate polyester used in the present invention may optionally contain a small amount of additives such as lubricants, pigments, dyes, antioxidants and solid-state polymerization. It may contain an accelerator, an optical brightener, an antistatic agent, an antibacterial agent, an ultraviolet absorber, a light stabilizer, a heat stabilizer, a light shielding agent, a matting agent and the like.

Fibers made of the poly (trimethylene terephthalate) type polyester of the present invention include the poly (trimethylene terephthalate) type polyester of the present invention at 238 ° C. to 275 ° C.
It may be produced by melt spinning in the range of ° C, and if the melt spinning temperature is in this range, yarn breakage during spinning will not occur. The melt spinning temperature is more preferably in the range of 239 to 270 ° C, and particularly preferably in the range of 240 ° C to 265 ° C. In addition, the spinning speed at the time of melt spinning may be set in the range of 400 to 5000 m / min. If the spinning speed is in this range, the strength of the obtained fiber is sufficient and the fiber is stably wound. You can also take it.
The spinning speed is more preferably in the range of 500 to 4700 m / min, and particularly preferably in the range of 600 to 4500 m / min.

There are no particular restrictions on the shape of the spinneret used during spinning, and any shape such as circular, irregular, solid or hollow can be used.

The polytrimethylene terephthalate polyester stretched yarn in the present invention may be obtained by winding the above-mentioned polytrimethylene terephthalate polyester fiber, or by continuously stretching it without winding it once. Can be obtained.

The polytrimethylene terephthalate polyester fiber and the polyester drawn yarn of the present invention preferably have an intrinsic viscosity in the range of 0.5 to 1.5.
When the intrinsic viscosity is within this range, the mechanical strength of the fiber finally obtained is sufficiently high and the handling becomes good. The intrinsic viscosity is more preferably in the range of 0.52 to 1.4, and particularly preferably in the range of 0.55 to 1.3.

By using the polyester fiber and / or the polyester undrawn yarn of the present invention, a fabric having an increase in the hue b value of 2 or less after being irradiated at 60 ° C. for 80 hours by using a sunshine weather meter can be obtained. You can

[0033]

EXAMPLES The present invention will be described in more detail below with reference to examples, but the present invention is not limited thereto. In addition, the part in an Example shows a weight part. Further, various characteristics were obtained by the following methods.

(1) Intrinsic viscosity: Measured at 35 ° C. with orthochlorophenol as a solvent and determined from its relative viscosity according to a conventional method.

(2) Measurement of manganese amount, phosphorus amount, and cobalt amount in polyester: A sample is heated and melted to form a circular disk, and a fluorescent X-ray apparatus 327 manufactured by Rigaku Corporation is used.
It was quantified using type 0.

(3) Amount of dipropylene glycol: A sample was sealed with an excess amount of methanol, decomposed with methanol in an autoclave at 260 ° C. for 4 hours, and the decomposed product was subjected to gas chromatography (HP6890 Series GC System manufactured by HEWLETTPACKARD).
The amount of dipropylene glycol was quantified using m) and the weight percentage of dipropylene based on the measured polymer weight was determined.

(4) Cyclic dimer content: Waters
Waters G made by 486 type liquid chromatograph
PC column TSKgel G2000H8 was connected to two devices, chloroform was used as a developing solvent, 1 mg of sample was dissolved in 1 ml of hexafluoroisopropanol, and a sample diluted with 10 ml of chloroform was injected to calibrate the standard cyclic dimer. The weight percentage in the polymer was determined from the line.

(5) Hue b value: The hue of the chip is 130 ° C.
After drying for 2 hours, the hue of the fiber is
It was measured using a color difference meter manufactured by Minolta Co., Ltd. (model: CR-200).

(6) Tensile strength and tensile elongation: JIS L1
The measurement was performed according to the method described in 070.

(7) Evaluation of light resistance: A sample in which fibers were knitted with Melias was irradiated with a sunshine weather meter (manufactured by Suga Test Instruments Co., Ltd.) under the conditions of 60 ° C., 80 hours, 50% humidity and no rain. . For the samples before and after irradiation, the hue b value was measured and the increase in b value was calculated.

[Reference Example 1] Production of polytrimethylene terephthalate type polyester: 100 parts of dimethyl terephthalate, 70.5 parts of trimethylene glycol, and titanium tetrabutoxide having a function as a transesterification catalyst and a polymerization catalyst 0.05
26 parts were charged into a reactor equipped with a stirrer, a rectification column and a methanol distillation condenser, and the ester exchange reaction was carried out while gradually raising the temperature from 140 ° C. while distilling out the methanol produced as a result of the reaction. I went. The internal temperature reached 210 ° C. 3 hours after the start of the reaction.

Next, the obtained reaction product was transferred to another reactor equipped with a stirrer and a glycol distilling condenser, and the temperature was gradually raised from 210 ° C. to 265 ° C., and from normal pressure to high vacuum of 70 Pa. The polymerization reaction was carried out while lowering the pressure. While tracing the melt viscosity of the reaction system, the polymerization reaction was terminated when the predetermined intrinsic viscosity was reached.

The molten polymer was extruded from the bottom of the reactor in a strand shape into cooling water and cut into chips by using a strand cutter. The results are shown in Table 1.

Example 1 Production of Polyester Containing High Concentration of Manganese Compound: 100 parts of dimethyl terephthalate, trimethylene glycol 7
0.5 parts and 0.0316 parts of manganese diacetate tetrahydrate as a transesterification catalyst were charged into a reactor equipped with a stirrer, a rectification column and a methanol distillation condenser, while gradually heating from 140 ° C, The transesterification reaction was carried out while distilling the methanol generated as a result of the reaction out of the system. The internal temperature reached 210 ° C. 3 hours after the start of the reaction.

Next, 0.0526 parts of titanium tetrabutoxide as a polymerization catalyst and 0.5995 parts of manganese diacetate tetrahydrate as a light resistance improver were added to the obtained reaction product, followed by stirring and glycol distillation. The mixture was transferred to another reactor equipped with an output condenser, the temperature was gradually raised from 210 ° C. to 265 ° C., and the polymerization reaction was performed while lowering the pressure from normal pressure to a high vacuum of 70 Pa. While tracing the melt viscosity of the reaction system, the polymerization reaction was terminated when the predetermined intrinsic viscosity was reached.

The molten polymer was extruded from the bottom of the reactor in a strand form into cooling water and cut into chips by using a strand cutter. The results are shown in Table 1.

Example 2 Production of Polyester Containing High Concentration of Manganese Compound: In Example 1, the addition amount of manganese diacetate tetrahydrate was 0.28.
The same operation was performed except that 4 parts were used. The results are shown in Table 1.
Shown in.

Example 3 Production of Polyester Containing High Concentration of Manganese Compound: The same operation as in Example 1 was carried out except that 0.135 parts of 56% phosphoric acid aqueous solution was added after the transesterification reaction. The results are shown in Table 1.

Example 4 Production of Polyester Containing High Concentration of Manganese Compound: In Example 1, 0.0316 parts of manganese diacetate tetrahydrate and cobalt diacetate tetrahydrate were used as the transesterification catalyst before the transesterification reaction. The same operation was performed except that 0.0064 parts was used in combination. The results are shown in Table 1.

Example 5 Production of Polyester Containing High Concentration of Manganese Compound: 100 parts of dimethyl terephthalate, 70 parts of ethylene glycol and manganese diacetate tetrahydrate as an ester exchange catalyst.
0316 parts were charged into a reactor equipped with a stirrer, a rectification column and a methanol distillation condenser, and the ester exchange reaction was carried out while gradually raising the temperature from 140 ° C. while distilling out the methanol produced as a result of the reaction. I went. 3 after starting the reaction
The internal temperature reached 210 ° C. in time.

Next, 0.0405 parts of diantimony trioxide as a polymerization catalyst and 0.5995 parts of manganese diacetate tetrahydrate as a light resistance improver were added to the obtained reaction product, followed by a stirrer and a glycol. The mixture was transferred to another reactor equipped with a distillation condenser, the temperature was gradually raised from 210 ° C. to 285 ° C., and the polymerization reaction was carried out while lowering the pressure from normal pressure to a high vacuum of 70 Pa. While tracing the melt viscosity of the reaction system, the polymerization reaction was terminated when the predetermined intrinsic viscosity was reached.

The molten polymer was extruded in the form of a strand from the bottom of the reactor into cooling water and cut into chips by using a strand cutter. The results are shown in Table 1.

Example 6 Production of Polyester Containing High Concentration of Manganese Compound: 100 parts of dimethyl terephthalate, tetramethylene glycol 6
7 parts and 0.0316 parts of manganese diacetate tetrahydrate as a transesterification catalyst were placed in a reactor equipped with a stirrer, a rectification column and a methanol distillation condenser, and the temperature of the reaction was gradually raised from 140 ° C. The transesterification reaction was carried out while distilling the resulting methanol out of the system. The internal temperature reached 210 ° C. 3 hours after the start of the reaction.

Next, 0.0526 parts of titanium tetrabutoxide as a polymerization catalyst and 0.5995 parts of manganese diacetate tetrahydrate as a light resistance improver were added to the obtained reaction product, followed by stirring and glycol distillation. The reaction mixture was transferred to another reactor equipped with an output condenser, the temperature was gradually raised from 210 ° C. to 245 ° C., and the polymerization reaction was performed while lowering the pressure from normal pressure to a high vacuum of 70 Pa. While tracing the melt viscosity of the reaction system, the polymerization reaction was terminated when the predetermined intrinsic viscosity was reached.

The molten polymer was extruded from the bottom of the reactor in a strand shape into cooling water and cut into chips by using a strand cutter. The results are shown in Table 1.

Comparative Example 1 Production of Manganese Compound-Containing Polyester: 0.5995 parts of manganese diacetate tetrahydrate added after completion of transesterification reaction as a light resistance improving agent in Example 1 was not added. Performed the same operation. The results are shown in Table 1.

Comparative Example 2 Production of Polyester Containing High Concentration of Manganese Compound: The same operation as in Example 1 was carried out except that 0.495 parts of 56% phosphoric acid aqueous solution was added after the transesterification reaction. The results are shown in Table 1.

Example 7 Production of Polytrimethylene Terephthalate Composition and Fibers Composed of the Same: 95 parts of the chip obtained in Reference Example 1 and 5 parts of the chip obtained in Example 1 were uniformly chip-blended. Using an extrusion spinning machine having a spinneret with 36 circular spinning holes with a hole diameter of 0.27 mm and a kneader, 255 ° C.
Melted and spun at a discharge rate of 34 g / min and a take-up speed of 2400 m / min, and the resulting undrawn yarn is subjected to a drawing treatment machine having a heating roller at 60 ° C. and a plate heater at 160 ° C., and a draw ratio of 1 Stretched at 7 times 83 dtex / 3
A drawn filament of 6 filaments was obtained. The manganese and phosphorus element amounts in the obtained drawn yarn, the fiber physical properties, and the light resistance evaluation results are shown in Table 2.
Shown in.

[Example 8] Production of polytrimethylene terephthalate composition and fiber comprising the same: In Example 7, 90 parts of the chip obtained in Reference Example 1 and 10 parts of the chip obtained in Example 2 were prepared. The same operation was performed except that it was used. The results are shown in Table 2.

[Example 9] Production of polytrimethylene terephthalate composition and fiber comprising the same: In Example 7, 95 parts of the chip obtained in Reference Example 1 and 5 parts of the chip obtained in Example 3 were prepared. The same operation was performed except that it was used. The results are shown in Table 2.

Example 10 Production of polytrimethylene terephthalate composition and fiber made thereof: In Example 7, 95 parts of the chip obtained in Reference Example 1 and 5 parts of the chip obtained in Example 4 were prepared. The same operation was performed except that it was used. The results are shown in Table 2.

[Example 11] Production of polytrimethylene terephthalate composition and fiber comprising the same: In Example 7, 95 parts of the chip obtained in Reference Example 1 and 5 parts of the chip obtained in Example 5 were prepared. The same operation was performed except that it was used. The results are shown in Table 2.

[Example 12] Production of polytrimethylene terephthalate composition and fiber comprising the same: In Example 7, 95 parts of the chip obtained in Reference Example 1 and 5 parts of the chip obtained in Example 6 were prepared. The same operation was performed except that it was used. The results are shown in Table 2.

[Comparative Example 3] Production of polytrimethylene terephthalate and a fiber made of polytrimethylene terephthalate: The same operation as in Example 7 was carried out except that only the chip obtained in Reference Example 1 was used. The results are shown in Table 2.

Comparative Example 4 Production of Polytrimethylene Terephthalate Composition and Fibers Composed of the Same: In Example 7, 90 parts of the chips obtained in Reference Example 1 and 10 parts of the chips obtained in Comparative Example 1 were prepared. The same operation was performed except that it was used. The results are shown in Table 2.

Comparative Example 5 Production of Polytrimethylene Terephthalate Composition and Fibers Composed of the Same: In Example 7, 95 parts of the chips obtained in Reference Example 1 and 5 parts of the chips obtained in Comparative Example 2 were prepared. The same operation was performed except that it was used. The results are shown in Table 2.

[0067]

[Table 1]

[0068]

[Table 2]

[0069]

Industrial Applicability According to the present invention, the light resistance of polytrimethylene terephthalate type polyester fiber can be improved, and the spinning conditions are not severely restricted. A methylene terephthalate-based polyester can be provided.

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Claims (7)

[Claims] 1. A polyester comprising a manganese compound in an amount of more than 150 ppm in terms of manganese element of 10,000.
A high-concentration manganese compound-containing polyester, which contains ppm or less and the ratio of the contained manganese element amount to the phosphorus element amount is within the range of the following formula (I). ## EQU1 ## 0.ltoreq.P / Mn.ltoreq.1 (I) (where P is the molar equivalent of phosphorus element, and Mn is the molar equivalent of manganese element) 2. The manganese compound in high concentration according to claim 1, wherein the polyester is at least one polyester selected from the group consisting of polytrimethylene terephthalate polyester, polyethylene terephthalate polyester and polytetramethylene terephthalate polyester. polyester. 3. The manganese compound high-concentration polyester according to claim 1 is added to a polytrimethylene terephthalate-based polyester polymer comprising trimethylene terephthalate repeating units in an amount of 0.5 to 50% by weight based on the polyester polymer and melted. Kneading, containing 10 to 150 ppm of manganese compound in terms of manganese element,
A method for producing a poly (trimethylene terephthalate) polyester composition, which obtains a poly (trimethylene terephthalate) polyester in which the content of manganese element and the content of phosphorus element satisfy the relationship of the following formula (I). ## EQU00002 ## 0.ltoreq.P / Mn.ltoreq.1 (I) (where P is the molar equivalent of elemental phosphorus and Mn is the molar equivalent of elemental manganese). 4. A polytrimethylene terephthalate-based polyester composition according to claim 3 having a melting temperature of 238 to 27.
Polytrimethylene terephthalate-based polyester fiber obtained by melt spinning at 5 ° C. and a spinning speed of 400 to 5000 m / min. 5. A polytrimethylene terephthalate polyester stretched yarn obtained by winding the fiber according to claim 4 once or continuously drawing the fiber without once winding it. 6. A polyester comprising the polytrimethylene terephthalate-based polyester fiber according to claim 4 and having an increase of a hue b value of 2 or less after irradiation with a sunshine weather meter at 60 ° C. for 80 hours. Cloth that becomes. 7. A polyester comprising the stretched polytrimethylene terephthalate polyester yarn according to claim 5 and having an increase in hue b value of 2 or less after irradiation with a sunshine weather meter at 60 ° C. for 80 hours. A fabric made of.