JPH04194077A - Polyester fiber - Google Patents

Abstract

PURPOSE:To obtain the subject fiber having excellent yarn-making efficiency and good weaving efficiency by treating a polyester fiber with an oil produced by compounding a specific aliphatic monohydric alcohol ester, an aromatic ester and an alkylene oxide adduct of a triglyceride at specific ratios. CONSTITUTION:The surface of a polyester fiber is coated with 0.3-1wt.% of an oil containing, as essential components, (A) an aliphatic monohydric alcohol ester exhibiting liquid state at normal temperature and having a molecular weight of 550-750, (B) an aromatic ester exhibiting liquid state at normal temperature and expressed by formula I (R1 and R2 are 8-25C alkyl; A is 2-4C alkylene; (n) and (m) are 1 or 2), and (C) an alkylene oxide adduct of a triglyceride exhibiting liquid state at normal temperature and having one or more hydroxyl groups in one molecule. The amounts of A+B and C are 20-75wt.% and 2-15 wt.% based on the total active component of the oil, respectively, and the weight ratio of A/B is 95/5 to 60/40. The polyester fiber produced by the above process exhibits excellent heat-resistance and oligomer scum resistance in yarn-making process and good weaving efficiency in weaving even without desizing the product.

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to polyester fibers. More specifically, the present invention relates to polyester fibers, particularly low shrinkage polyester fibers, which have excellent spinning efficiency during fiber production and also have good weaving efficiency during sizing weaving.

(Prior art) In recent years, the progress of spinning technology in the production of synthetic fibers has been remarkable, and with the development of high-speed winders, the spinning speed is increasing more and more. (sometimes called direct extension)
However, as the spinning speed increases, friction between the traveling yarn and various yarn guides (rollers, guides, etc.) increases, causing single yarn breakage and reducing the quality of the yarn obtained. In addition to damaging the properties, heat setting at a higher temperature than before is required to impart the desired physical properties, especially heat shrinkage properties, resulting in increased smoke from the oil components and the formation of scum on the roller surface originating from the polyester oligomer. This also includes problems such as increased adhesion to the fibers and frequent thread breakage.

In particular, for polyester fibers for industrial materials used in sails, tents, etc., the dimensional stability of the yarn is extremely important compared to ordinary polyester fibers for clothing, and the thermal shrinkage rate is also required to be extremely low. Therefore, the heat setting mentioned above must be carried out at a higher temperature than that for clothing fibers, which means that the oil component produces less smoke (heat resistance) and generates less oligomer scum (oligomer scum resistance). Oil agents with excellent lubricity at high speeds are becoming important.

On the other hand, when the yarn obtained by such spinning is passed through weaving and knitting processes, it is often applied with a sizing agent that matches each process in order to increase the efficiency of the weaving and knitting processes. However, if the treating oil applied during the spinning process is inappropriate, it may soften the glue film formed on the thread and reduce the protective effect of the thread.
Alternatively, the sizing agent falls off and accumulates in various parts of the loom, which is called "gluing," increasing the friction with the threads, causing fuzz and yarn breakage, which impairs weaving and knitting efficiency.

For this reason, proposals have been made in the past to use an amide component in a spinning oil, but recent studies by the present inventors in high-speed silk spinning have shown that although such agents are good in terms of the above-mentioned sizing properties, It has been found that if too much is used, the heat resistance or lubricity will be impaired, which will impede the spinning efficiency.

In order to solve this problem, the present inventors first developed a polyester fiber to which an oil agent containing a high molecular weight monohydric alcohol ester and a polyhydric alcohol partial ester having a hydroxyl group in the molecule was added. I would like to propose a special application for Hei 2-
No. 125497). However, although such an oil agent improves heat resistance and scum resistance and improves yarn spinning efficiency, it still has some insufficiencies, such as staining of the surface of the heated roller due to long-term operation.

(Objective of the Invention) The present invention was made in view of the above background, and its purpose is to provide excellent heat resistance, oligomer scum resistance, and lubricity in the yarn spinning process, and to prevent "sizing removal" in the weaving process.
An object of the present invention is to provide a polyester fiber that does not induce scum and can provide good weaving efficiency.

(Structure of the Invention) As a result of intensive studies to achieve the above object, the present inventors identified a specific monohydric alcohol ester, a specific aromatic ester, and an ethylene oxide adduct of a triglyceride having a hydroxyl group in the molecule. The present invention was achieved by discovering that by applying a blended amount of oil, it is possible to simultaneously improve unprecedented high heat resistance, lubricity, and excellent sizing properties, and to obtain extremely high-quality polyester fibers. did.

That is, according to the present invention, the following (A), (Bl and (
C) A lubricant containing component C) as an essential ingredient, the content of each of which satisfies the following formulas (i) to (iii) at the same time with respect to the active ingredient of the lubricant, is attached in an amount of 0.3 to 1.0% by weight. The polyester fiber (A) component is liquid at room temperature, and the aliphatic monohydric alcohol ester (B) component has a molecular weight of 550 to 750. , R2 is an anorexic group having 8 to 25 carbon atoms, A is an alkylene group having 2 to 4 carbon atoms, n, m (representing an integer of 1 or 2) component (C) is liquid at room temperature, Alkylene oxide adduct of triglyceride having one or more hydroxyl groups in the molecule (i) WA + WB: 20 to 75 (ii) Wc-
2~15 (iii) WA/WB =95/ 5~60/40[
However, WA, WB and W. are (A) and (B) respectively.
and the content (wt%) of component (C) relative to the active ingredients of the oil agent.
). ] is provided.

The aliphatic monohydric alcohol ester A), which is an essential component of the material 1 imparted to the polyester fiber of the present invention, is obtained from a monovalent higher alcohol and a monovalent or divalent aliphatic carboxylic acid. The ester compound must have a molecular weight of 550 to 750, preferably 600-L7oo, and be liquid at room temperature. Specifically, a higher alcohol having 20 to 34 carbon atoms is used as the monohydric higher alcohol, and higher fatty acids such as stearic acid, oleic acid, and palmitic acid or dibasic acids such as adipic acid, sebacic acid, and thiodipropionic acid are used. Examples include mono- or diester compounds using isoeicosylstearate, isobentacosyl palmitate, isobentacosyl oleate, isopentacosyl erucinate 2, or diisostearylthio. dipropionate,
Diorail adipate.

Examples include diesters such as diisostearyl sebacate.

Here, only aliphatic monohydric alcohol esters with a molecular weight exceeding 750 or solid at room temperature, or polyhydric alcohol esters without hydroxyl groups such as triglycerides such as coconut oil and rapeseed oil were used as component A. If this is the case, adhesive removal during weaving will increase, and friction between the running yarn and the yarn guide will increase during spinning, resulting in single yarn breakage, which is undesirable.

In addition, aliphatic monohydric alcohol esters with a molecular weight of less than 550 tend to volatilize due to the heat during spinning, producing smoke and contaminating the working environment.
This is undesirable because tar is formed on the thread guide, leading to single thread breakage, etc.

The aromatic ester (B), which is an essential component of the oil agent used in the present invention, is a diester compound represented by the following general formula, which is obtained by adding alkylene oxide to bisphenol A and then esterifying it with an aliphatic monocarboxylic acid.

In the formula, R1 and you represent an alkyl group having 8 to 25 carbon atoms, A represents an alkylene group having 2 to 4 carbon atoms, and n and m each represent an integer of 1 or 2. When the number of carbon atoms in R1 and R2 is less than 8, the lubricity decreases, the abrasion resistance deteriorates, and the number of yarn feathers tends to increase. On the other hand, when the number of carbon atoms exceeds 25, it is not preferred because it is difficult to obtain industrially. In addition, when the number of added moles (n or m) of alkylene oxide is O,
The properties of the aromatic ester become solid at room temperature, which inhibits the adhesion of the glue in the sizing process.On the other hand, if the aromatic ester is 3 or more, the hydrophilicity increases and the glue film becomes plasticized. A problem arises in that the protective effect of the glue film formed on the yarn is reduced and the efficiency of weaving and knitting is deteriorated.

As the component (B) which is usually preferably used, for example, dilaurate of bisphenol A added with 2 moles of ethylene oxide can be mentioned.

The oil agent used in the present invention includes the above-mentioned (
The total amount of the Al component and component (B) must be 20 to 75% by weight, preferably 30 to 65% by weight based on the active ingredients of the oil agent. If this content is less than 20% by weight, it will not be possible to provide the lubricity required for high-speed spinning, and the occurrence of single yarn breakage will tend to increase, and problems such as "glue removal" during weaving will occur. There is little effect on improving the problem. On the other hand, if it exceeds 75% by weight, it is not preferable because it causes problems in the emulsion stability of the oil system.

Further, in the present invention, it is necessary that the weight ratio (A, /B) of the component (A) to the component (B) be within the range of 9515 to 60/40. If the proportion of component B is less than 5% by weight based on the total amount of A and B, the heat resistance of the oil will decrease, and if it exceeds 40% by weight, the friction of the thread will increase or post-processing will be difficult. When weaving with glue, the adhesion of the glue film on the yarn surface is reduced, and the cohesive force of the glue film is weakened, resulting in weakening of the sizing effect.

The alkylene oxide adduct of triglyceride having a hydroxyl group in its molecule, which is another essential component of the oil used in the present invention, needs to be liquid at room temperature.

Further, the content thereof needs to be 2 to 15% by weight, preferably 5 to 10% by weight based on the active ingredients of the oil agent.

The present invention is believed to be because the alkylene oxide adduct of glyceride has excellent compatibility with polyester oligomers (mainly cyclic trimers) and dissolves oligomers precipitated by treatments such as heating during polyester fiber production into the oil system. However, it has been found that this method is highly effective in suppressing the accumulation of oligomer scum on rollers, thread guides, etc. Therefore, if the amount used is too small, these effects will not be realized, while if it is too large, the effect of the above-mentioned A component (sizing resistance) will be reduced, and the friction between the running yarn and the yarn guide will also increase, making it difficult to use. Since thread breakage tends to increase, the amount used is 2 to 15% by weight as mentioned above.
It is necessary to do so.

In addition, in the case of glyceride alkylene oxide adducts that do not have hydroxyl groups in their molecules or are solid at room temperature, oligomers tend to accumulate on the cooling roller after heat setting, resulting in a lack of yarn runnability. This is undesirable because single yarn breakage may occur, adhesive removal may increase, and friction between the running yarn and the yarn guide during spinning may increase.

The alkylene oxide added in component (C) is an alkylene oxide having 2 to 4 carbon atoms, and ethylene oxide is particularly preferred. In addition, the number of moles added is 4 to 4 to the glyceride having a hydroxyl group.
30 mol, especially 8 to 15 mol is desirable. If the number of added moles is out of this range, it is presumed that the solubility of the polyester oligomer decreases, but the effect of suppressing oligomer scum deposition tends to decrease.

Examples of such component C include alkylene oxide adducts of hardened mustard oil, and aliphatic monocarboxylic acid monoesters or diesters thereof.

Specifically, P OE (81 hydrogenated castor oil ether (
POE (n) indicates that the number of moles of oxyethylene oxide added is n moles on average. (same below), PO
E (12> hydrogenated castor oil ether, P OE (25
+Hardened mustard oil dilaurate and the like are preferred.

The oil agent used in the present invention further includes the following (D+
It is particularly preferred that the acid component and component (E) are each used in an amount of 1% by weight or more. Among these components, the <D) component has its phosphate anion portion (phosphate residue) oriented on the metal surface such as the thread conductor, while its amine cation portion (organic amine residue) is oriented on the fiber surface. It is presumed that this combination with components (A) to (C) reduces friction under high contact pressure. Therefore, it is presumed that scum accumulation on the roller surface is reduced, drawability is improved, fluff of the drawn yarn is reduced, and the abrasion resistance of the fiber is improved. Ru.

As the (D+ acid component), a salt consisting of a phosphoric acid partial ester and an organic amine is used.

Preferably used phosphoric acid partial esters include C8-
22 higher alcohols, phenols having C8-22 alkyl groups, and alkylene oxide adducts thereof (10 moles or less),
Examples include phosphoric acid partial esters, such as octyl alcohol, lauryl alcohol, oleyl alcohol, and isostearyl alcohol.

Polyoxyalkylene glycol monoalkyl ether, polyoxyalkylene glycol monoalkyl phenyl ether, which is obtained by adding 10 moles or less of ethylene oxide and/or propylene oxide to phosphoric acid mono- or diester such as nonylphenol, or these higher alcohols or alkylphenols. Examples include phosphoric acid mono- or diesters such as.

Further, as the organic amine used in combination with the phosphoric acid partial ester, an organic amine represented by the following general formula is preferable.

However, R1' is a 08-2° saturated or unsaturated alkyl group, R2' and R3' are each hydrogen or a 01-5 alkyl group, A' is a C2-4 alkylene group, n', m
' represents an integer satisfying m' + n' - 0 to 10, respectively.

If the number of carbon atoms in R1' is 7 or less, extreme pressure lubrication performance deteriorates and friction increases), while if the number of carbon atoms in R1' is 23 or more, it becomes difficult to obtain commercially, which is not preferable. In addition, R2', R
More preferably, both 3' groups are alkyl groups.

Specific examples of component (D) include the above-mentioned phosphoric acid mono- or diester, stearylamine, laurylmethylamine, ethylene oxide and propylene oxide adducts thereof, as well as octyldimethylamine and lauryldimethylamine.

Examples include reaction products with oleyldimethylamine, instearyldimethylamine, lauryldiethylamine, and the like.

In the present invention, although component (D) as described above reduces friction under high contact pressure, this component is likely to be colored by heating, so it is desirable to use component (E) in combination.

As for such component (E), the phosphate residue may be the same as or different from the phosphate residue of the above-mentioned (D+ acid component), for example, a 08-22 higher alcohol, a C8-22 alkyl group. phenol having
and an alkali metal salt of at least one phosphoric acid partial ester selected from these alkylene oxide adducts (10 moles or less). Among them, lauryl phosphate potassium salt, isoseti I rephosphate potassium salt, instearyl phosphate sodium salt, etc. are preferable.

On the other hand, when the above-mentioned (DJ acid component and (E) component) are contained in the oil agent, the (E) component is liberated from the oil agent as an incompatible component during high-temperature heating (for example, during heat setting after stretching), and the heating roller, Problems such as easy accumulation of scum on hot plates, etc. may occur.Such problems can be solved by reducing the degree of neutralization of the fE component used, but in this case, it is necessary to reduce friction under high contact pressure. Another problem arises in that the effectiveness of the wire is reduced and metals used for thread guiding etc. are corroded.

It has been found that this problem can be solved by using component (F) (0(CH2CH20)) and H (where n is an integer of 11 to 20) in combination. That is, the compound is a highly polar organic compound. Since it is a compound, it is thought to suppress the free precipitation of the El component and suppress the generation of scum. Preferably used component (F) includes ethylene glycol and low molecular weight ethylene such as diethylene glycol and triethylene glycol. Oxide polymers can be used, but if the molecular weight becomes too large, the viscosity of the oil agent will increase, which may cause fluffing and yarn breakage, so the degree of polymerization is preferably 20 or less.

Further, the content of the component (F) is desirably 10% by weight or less, preferably 2 to 5% by weight based on the active ingredients of the oil agent. Even if it is used in excess of this range, no improvement in compatibility will be observed, and rather the emulsion stability of the oil agent will be impaired, which is not preferable.

As mentioned above, the polyester fiber of the present invention has (A), (
Bl and (C) component are essential components, (i) to (iii)
) is a fiber to which an oil agent containing an oil agent that simultaneously satisfies the formula, preferably an oil agent that further contains components (D), (E), and (F), but within a range that does not impair the purpose of the present invention. It goes without saying that an oil agent containing other oil components may also be applied. Such compounding agents include, for example, a heat-resistant 1,000-onyster leveling agent, an emulsifier for use as an emulsion, an antistatic agent to prevent static electricity, an antioxidant to improve heat resistance, and even an extreme pressure agent for oil agents. Examples include organic or inorganic additives for increasing lubricity and oil film strength.

The oil agent may be applied to the polyester fibers at any time after the spun yarn has solidified, but it is usually applied to the yarn before the take-up roller.

A preferred method for applying the oil is to form an aqueous emulsion into the oil and apply it through a metering oiling nozzle. It is necessary to set the content to .0% by weight, thereby improving the weaving efficiency of the resulting fibers. If the applied amount is less than 0.3% by weight, a sufficient effect will not be obtained, while if it exceeds 1.0% by weight, the effect will not increase any further, and excess oil will be applied to rollers, thread guides, etc. It is undesirable because it adheres to the surface.

Furthermore, the oil agent used in the present invention exhibits its effects when applied to polyester fibers that are heat-treated at high temperatures. Therefore, the present invention is particularly effective when targeting polyester fibers that need to be heat-set at high temperatures, particularly low-shrinkage polyester fibers with a dry heat shrinkage rate of 5% or less at 150°C. When the dry heat shrinkage rate exceeds 15%, it is not necessarily necessary to perform high-temperature heat treatment during spinning, so it is not necessarily necessary to use the oil agent according to the present invention.

(Effects of the Invention) The polyester fiber of the present invention has low friction under high contact pressure, is heat resistant, and is provided with an oil agent that has good polyester oligomer solubility. In addition, it exhibits excellent performance in heat resistance, scum resistance, and lubricity, and good spinning efficiency can be obtained. Furthermore, when the fibers are pasted and weaved, no adhesive loss occurs and good weaving efficiency can be obtained.

(Example) The present invention will be explained in more detail below with reference to Examples.

In addition, in the examples, heat resistance, white powder stain on heat set roller, oligomer scum resistance, yarn fuzz, abrasion resistance,
The properties of the glue film and the adhesive removal properties were evaluated by the following methods.

(1) When spinning heat-resistant yarn, the state of the smoke generated from the heat set roller heated to 220'C and the occurrence of stains on the surface of the heat roller (thermal deterioration of the attached oil) are visually observed, and the following standards are checked. Judgment was made by

Resistance to roller staining Low grade staining 2 Medium: △ High: × Smoke resistance Grade low smoke 2 Medium 2 △ High: × (2) Oligomer scum resistance Silk spinning was carried out by the method shown in the example, and spinning started 1 Days later,
Visually observe the occurrence of oligomer scum that adheres to the cold roller immediately after the heat set roller heated to 220 ° C.
Judgment was made based on the following criteria.

Grade Oligomer scum Almost none: ○ Little to medium: △ Much: × (3) White powder stains Same as (2) above, stains on the heat set roller heated to 220°C one day after the start of yarn spinning, except for deterioration of the oil agent. The degree of white powder stain was visually judged according to the following criteria.

Grade Almost no white powder stains 2 〇 Few, medium: △ Many: × (4) Collect 160 yarns with fluff, and count and add up the number of fluffs (single yarn breaks) for each 200,000 m. From these, the number of fuzz per 106 m was determined and evaluated in the three stages shown below.

Number of fuzz (ri/106m) Grade 0-0.2:
◎ 0.2~0.52 〇0.5~2. O: △ 2.0 or more: × (5) Abrasion resistance Evaluate the abrasion resistance of fiber to metal (F/M) and fiber to fiber (F/F) according to the measurement methods shown in the following table.

Evaluation Criteria Fluff Occurrence Condition Grade: Almost no fluff: ◎) Slight fluff present: ○ Large fluff: △ Yarn breakage: × (6) Evaluation of glue film properties: Glue on the fibers when the fibers are glued The following model experiment was used as a substitute for evaluating the physical properties of the film.

A mixed aqueous solution of a sizing agent and an oil agent mainly composed of polyvinyl alcohol and polyacrylic acid ester in an active ingredient ratio of 5/1 was poured onto a glass plate, followed by air drying and heat treatment to obtain a casting film. A strip sample was taken from the film and subjected to a tensile test, and evaluated according to the following criteria.

Comparing film samples obtained only with adhesives that are not mixed with oil, those with film strength of 30% or more or elongation of 250% or less are marked "○", and those outside this range are marked "x".
And so.

(7) Evaluation of “sizing removal” property As a substitute property for the “sizing removal” phenomenon in the actual weaving process, the size of the glue film on the yarn surface is Evaluation was made based on the peeling frequency at which the part peeled off from the yarn surface.

A sizing yarn was obtained by sizing the polyester fibers with a sizing agent mainly composed of polyvinyl alcohol and polyacrylic acid ester using a normal roller sizing method so that the target adhesion amount was 5.0% by weight. Next, 20 of these sizing threads were arranged at equal intervals, fixed terminals were installed so that both ends would not be disturbed, one end was fixed with a chuck 4 as shown in Figs. 1 and 2, and 25 g / load 6 is applied and tension is applied to the entire sample through pulley 5. In the figure, 1, 2, and 3 are reeds installed at intervals of 10α, and are fixed to a movable table 7, which is parallel to the yarn axis.
It can reciprocate over n width. The sample sizing thread is set so as to have an opening angle of 108° in the central reed 2, as shown in FIG.

Next, the movable table 7 is reciprocated from side to side, and after 10 reciprocations, the state of peeling of the glue film at the abraded area between the reed and the thread is carefully observed, and the ratio of the number of peeled samples per 20 samples is determined as follows. Expressed by grading.

Note that here, the determination was made based on the average of the results obtained three times each.

Peeling number ratio Grade Less than 25%　2　　 25-50%: △ Over 50%: × (8) Overall evaluation It is expressed in the following four stages.

Very good 20 Good: ○ Slightly unsatisfactory: △ Unsatisfactory / × Example 1 Polyethylene terephthalate having an intrinsic viscosity of 1.00 was melted and discharged to form 48 filament yarns.

An oil emulsion shown in Table 1 was applied to this yarn through an oiling roller so that the pure oil amount was 0.5% by weight of the yarn weight. Then 600m with the take-up roller
After being preheated at 90°C while being taken off at a speed of 1/min, the material is heat set at 220°C while being stretched 5.0 times between the takeoff roller and a stretching heat set roller, and then rolled via an empty roller. Take 250d/48f, strength 8. OK/d,
A drawn yarn with a dry yield of 5% at 150°C was obtained.

Table 2 summarizes the results of evaluation using the above-mentioned measuring method using the drawn yarn obtained at this time.

As is clear from these results, the polyester fibers to which the oil agent within the range of the present invention is attached are heat resistant.

It has excellent lubricity and adhesive properties in the weaving process, and has remarkable effects on spinning and post-processing properties.

Example 2 Processing was carried out in the same manner as in Example 1, except that the amount of oil applied in Experiment ~α6 was changed. The results obtained at this time are summarized in Table 3.

[Brief explanation of the drawing]

FIGS. 1 and 2 are schematic diagrams of the apparatus used to evaluate adhesive removal characteristics, with FIG. 1 being a side view and FIG. 2 being a plan view.

Claims (1)

[Claims] 1. The surface of the polyester fiber contains the following components (A), (B), and (C) as essential components, and the content of each of them is as follows (i) with respect to the active ingredient of the oil agent. A polyester fiber characterized in that 0.3 to 1.0% by weight of an oil agent that satisfies formula (iii) is adhered thereto. (A) Component is an aliphatic monohydric alcohol ester that is liquid at room temperature and has a molecular weight of 550 to 750. (B) Component is an aromatic ester that is liquid at room temperature and is represented by the following formula ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ [ However, R_1 and R_2 are alkyl groups having 8 to 25 carbon atoms, A is an alkylene group having 2 to 4 carbon atoms, and n and m are 1 or 2.
represents an integer. ] (C) Component alkylene oxide adduct of triglyceride that is liquid at room temperature and has one or more hydroxyl groups in the molecule (i) W_A+W_B=20-75 (ii) W_C=2-15 (iii) W_A/W_B= 95/5 to 60/40 [However, W_A, W_B and W_C are (A) and (B), respectively.
, and the content (% by weight) of component (C) relative to the active ingredient of the oil agent. ] 2. The polyester fiber according to claim 1, wherein the oil agent contains the following components (D) and (E) at 1% by weight or more based on the active ingredients of the oil agent, and the following component (F) at 10% by weight or less: . (D) Component Salt of alkyl phosphate and/or alkylene oxide adduct of alkyl phosphate and alkylamine and/or its alkylene oxide adduct (E) Component alkali metal salt of alkyl phosphate (F) Component Glycol represented by the following formula ▲ There are mathematical formulas, chemical formulas, tables, etc.▼ [However, n = 1 to 20. ]