JPS5953395B2 - Spinning oil composition for polyester fibers - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a spinning oil for polyester fibers suitable for high-speed spinning processes.
It improves the antistatic property of blends such as polyester-rayon blends and polyester-linen blends, and also reduces spinning scum caused by white powder scum and oligomer precipitation or falling off due to fiber damage, making it easier to use in the spinning process. It is an object of the present invention to provide a spinning oil composition for polyester fibers that can reduce troubles as much as possible.

In recent years, in the spinning industry for polyester fibers and other products, efforts have been made to save labor in order to reduce processing costs, and there is a strong desire for a spinning oil suitable for high-speed spinning.

Moreover, a spinning oil agent that is fully satisfactory even when spinning with 100% polyester fibers or when blending with other fibers has not yet appeared.

On the other hand, since polyester fibers exhibit a smoother surface than cotton or wool, it is extremely difficult for the conventionally used oils to pass through the spinning process without any problems.

For example, experience has shown that winding on a cylinder or on a filament roller during the carding process is greatly influenced by the nature and type of the oil attached to the fiber surface.

Therefore, research has been intensely conducted on spinning oils for polyester fibers, and there is a particular need for oils that improve fiber cohesiveness and streamline the spinning process while requiring as few cleanings as possible. That's why.

In general, spinning oils consist of a smoothing agent component and an antistatic component, and the smoothing agent components include animal and vegetable oils, mineral oils, fatty acid ester compounds, aliphatic higher alcohols, fatty acid esters of polyhydric alcohols, ethylene oxide, propylene oxide, or both. Nonionic activators consisting of adducts are used, while antistatic agents include cationic activators such as alkyl sulfonates, alkyl phosphates, alkyl sulfates, alkylamine-ethylene oxide adducts, quaternary ammonium salts, or alkyl betaines. Types of amphoteric active agents are used.

These components are usually combined and used as a spinning oil.

However, it is generally well known that nonionic activators, animal and vegetable oils, mineral oils, or fatty acid esters used alone or in combination mainly increase the friction between fibers and improve cohesiveness. During the opening process and filament process, sticky substances adhere to the surfaces of rubber rolls and metal rolls, and the stickiness of the oil itself can cause the rollers to wrap around, and even worsen the electrical conductivity, causing spinning problems. Problems in the process will increase.

On the other hand, anionic activators are generally used as alkali metal salts, and many have good antistatic properties, but their properties change greatly with changes in temperature and humidity. It has low stickiness on rollers and is less likely to wrap around the filament roller, but it is well known that when the humidity is high, the amount of roller wrapping increases rapidly, resulting in spinning trouble.

In addition, cationic activators are generally known to have excellent antistatic properties, even at low humidity levels, but on the other hand, due to their high hygroscopicity, they may cause roller wrapping or yellowing of the fibers due to heating. It is also known that there are some drawbacks.

On the other hand, amphoteric activators also have excellent antistatic properties even at low humidity levels, but like cationic activators, they have high hygroscopicity, so they have the drawback of causing old-layer winding and yellowing of the fibers when heated.

In addition, compounds based on alkyl phosphate ester compounds, which are said to have relatively good performance these days, have the advantage of being less likely to wrap around the roller under normal conditions, but they still have insufficient performance at low humidity. It is also known to have a disadvantage of poor fiber cohesiveness.

In order to improve these drawbacks, proposals have been made to adjust the degree of phosphorylation, select the type of alkyl group, select the degree of neutralization, and introduce an ethylene oxide chain into the molecule.

However, it is extremely difficult to improve antistatic properties during blending, prevent white powder scum, and oligomer precipitation while maintaining good spinnability.

Therefore, in order to improve spinnability, an alkyl phosphate ester is used, and as a way to overcome the drawbacks of the alkyl phosphate ester, a spinning oil in which the alkyl phosphate ester is blended with other surfactants has recently been proposed. It is well known that it has been put into practical use.

For example, according to JP-A-48-33193, 40 to 60% of potassium salt of alkyl phosphate is added with 2 polyoxyalkylene ether or polyoxyalkylene ester.
In JP-A-52-63497, a block copolymer of propylene oxide and ethylene oxide with a molecular weight of 5000 or more is blended with 30% by weight of the total oil component. A blended oil agent containing the above-mentioned alkyl phosphates is known as a spinning oil agent.

However, in general, this does not mean that any combination of alkyl phosphates and other surfactants is acceptable, but there is a difference between the type of alkyl phosphates themselves, the type of other surfactants used in combination, and the mixing ratio. has fairly severe selectivity.

In other words, even if the properties of the alkyl phosphate and the properties of the other surfactants blended with them are excellent individually, when they are combined, these properties are not always exhibited and, on the contrary, the tackiness increases. In many cases, it becomes negative.

Moreover, since there is no formability in terms of blending ratio, it is not possible to estimate the properties of the oil based on the blending, and the current situation is that the spinnability must be confirmed each time.

Furthermore, polyester fibers are not only spun alone, but are also often blended with other fibers such as cotton, rayon, wool, and hemp, and from this point of view, there are quite severe restrictions on the composition. In particular, it is known that in blended spinning, the transfer of polyester oil to other fibers causes a decrease in electrical conductivity and poor spinning stability.

Against this background, the present inventors achieved high efficiency and high convergence in spinning at high speed, which is the object of the present invention.
The present invention was achieved as a result of extensive research aimed at developing a spinning oil that also produces less spinning scum.

That is, according to the present invention, the alkyl phosphate ester is obtained by reacting a linear or side chain alcohol having an average carbon number of 10 to 16 with P2O, and the degree of phosphorylation thereof is 0.6 to 1. 0 and an acid value of 0 to 50 (component A) to 50 to 7
0% (weight) [However, R is a linear or side chain carbon number 8 to 18
represents a saturated or unsaturated alkyl group (wherein R' is the same group as R), and X represents a hydrogen atom, a lower alkyl group having 1 to 4 carbon atoms, -COCH3, or a cyanoethyl group.

] T? n1v) rlT-T [However, R represents a hydrocarbon residue with a total number of carbon atoms of the substituents from 8 to 12, n is from 3 to 13, and Y represents polyoxyethylene, polyoxypropylene, or polyoxyethylene and polyoxy Indicates that it is a propylene copolymer.

It has been found that the object of the present invention can be achieved by using an oil composition containing 10 to 30% of the compound (component C) represented by the following.

To explain the present invention more specifically, first, the phosphoric ester compound used in the present invention is obtained from higher alcohols that have been widely used in the past, and exhibits the effects of the present invention even among known phosphoric esters. In particular, alcohols with a phosphorylation degree of 0.6 to 1.0 obtained by reacting an alcohol with a straight chain or side chain with an average carbon number in the range of 10 to 16 and P2O5 at a temperature of 100°C or less are used. The reaction product is neutralized with, for example, potassium hydroxide so that the acid value of the reaction product is in the range of 0 to 50.

As the alcohol, linear and side-chain alcohols having an average carbon number of 10 to 16, such as thiocyl, tritecan, and tetrathecan, and more preferably higher alcohols having 12 to 14 carbon atoms are used.

If longer or shorter chains are used as the main ingredients, the object of the present invention cannot be achieved even if the composition of the present invention is obtained.

In other words, if the alkyl chain length is too short, the hygroscopicity increases, physical changes in the properties of the phosphoric acid ester itself increase, and roller wrapping during spinning increases.

Furthermore, if the chain length is long, the phosphoric acid ester salt will not be able to maintain convergence, making it unsuitable.

Moreover, if the degree of phosphorylation exceeds the range of 0.6 to 1.0, that is, if the degree of phosphorylation is less than 0.6, white powder scum during spinning will increase and the cohesiveness will be poor.

Moreover, if the degree of phosphorylation exceeds 1.0, the original properties as an alkyl phosphate ester will be lost, the hygroscopicity will increase, and the heat resistance will also decrease, which is not preferable.

On the other hand, the degree of neutralization with potassium hydroxide greatly affects the spinnability, and when the acid value is 50 or more, the heat resistance is greatly reduced and the solubility becomes poor.

Therefore, in the present invention, a linear or branched alkyl group having an average carbon number of 10 to 16, preferably 12 to 14, and a degree of phosphorylation of 0.6 to 1.0, preferably 0.7 to 0.9
A potassium salt having an acid value of 0 to 50, preferably 10 to 40 is used.

In the present invention, the degree of phosphorylation refers to the phosphorus content (weight) obtained by the phosphomolybdic acid colorimetric method based on the known quantitative analysis method for phosphorus.
The degree of phosphorylation was determined by calculating how many moles of phosphorus were bonded to 1 mole of the alcohol used.

The acid value was determined by titrating the obtained potassium salt of the alkyl phosphate ester into a glacial acetic acid solution, using crystal violet as an indicator, and a perchloric acid glacial acetic acid solution.
The acid value was determined from the titration value.

In other words, 0 oxidation means complete neutralization,
An acid value of 50 indicates that the alkyl phosphate salt is half neutralized.

On the other hand, a component to be used in combination with 50 to 70% of the alkyl phosphate ester (component A) in order to exhibit the effects of the present invention is represented by the general formula (I) [wherein R is a straight chain or a side chain]. A saturated or unsaturated alkyl group having 8 to 18 carbon atoms, (wherein R' is the same group as R.

)X is a hydrogen atom, a lower alkyl group having 1 to 4 carbon atoms, - Indicates COCH3 or a cyanoethyl group.

A phosphate salt (component B) of a compound obtained by adding 5 to 15 moles of ethylene oxide to an alkylamine or a substituted alkylamine shown in ] is added in an amount of 10% or more by weight.

Specifically, alkyl groups include octyl, lauryl,
Typical examples include stearyl and oleyl.

Also, examples of alkyl having a side chain include 2-ethylhexyl,
Examples include alkylamines such as isotridecyl, isocetyl, and α-methylalkyl, but the present invention is not limited thereto.

Further, there are ethylene oxide adducts of hydroxyalkylamines, alkoxypropylamines, and amines of alkyl monoglycerides in which R is represented by R-COOC)12- and H-L;M2-.

Furthermore, in the general formula RN
Phosphates of ethylene oxide adducts such as N-cyanoethylamine, N-lauryl-N-ethylamine, and N-stearyl-N-butylamine are used.

Further, ethylene oxide adducts of amines of hydroxyamines, alkoxyhydroxypropylamines, and alkyl monoglycerides in which R is also used.

The addition of ethylene oxide is carried out in the usual manner.

It is then obtained by neutralization with phosphoric acid.

If the number of moles of ethylene oxide added is small, the heat resistance will decrease and the weight loss on heating will increase, which poses a practical problem.If the number of moles of ethylene oxide added is too large, the hydrophilicity will become high and the hygroscopicity will increase unnecessarily, resulting in adhesiveness. Since the amount also increases, those having a mole range of 5 to 15 moles are preferably used.

Compounds with ethylene oxide added to them are neutralized by phosphoric acid, but when completely neutralized, the aqueous solution itself becomes acidic, so Compound 1 with ethylene oxide added to amines
Neutralization using 0.2 to 0.7 moles of phosphoric acid is preferred.

The B component can suppress the antistatic properties of the A component and can improve the heat resistance of the blended oil composition.

Furthermore, in order to achieve the object of the present invention, in addition to the above-mentioned components A and B, as a component C, the general formula (1) [However, R represents a hydrocarbon residue having a total number of carbon atoms of 8 to 12 as a substituent. , n is 3 to 13, and Y represents polyoxyethylene, polyoxypropylene, or a copolymer of polyoxyethylene and polyoxypropylene.

] 10 to 30% (by weight) of the compound (C component) is blended.

Specifically, ethers in which ethylene oxide or propylene oxide, or ethylene oxide and propylene oxide are added to alkylphenols such as octylphenol and nonylphenol, or dialkylphenols such as dibutylphenol, are used.

What is very interesting about these ethers is that component C is soluble especially with component A when hot, but they are poorly miscible when cold.

This phenomenon is effective even in a mixed system of components A, B, and C, so that when the water in the composition evaporates, a solid layer is deposited on the surface.

That is, although it has a paste-like property, it appears to be solid at first glance.

The details of how this effect affects spinnability are unknown, but the feature of the oil composition of the present invention is that it can reduce spinning scum while maintaining a high level of spinning performance. It is presumed that the important meaning lies in the fact that they have poor compatibility.

In addition, the features of the compounded oil of the present invention include polyester 1
It is possible to improve the spinability not only of 0.00% polyester fibers, but also of polyester-cotton blends, polyester-rayon blends, polyester-wool blends, polyester-linen blends, and blended products mainly made of polyester fibers.

Therefore, it is an extremely versatile spinning oil and deserves special mention.

However, as mentioned above, if component A, component B, and component C are used together, it does not mean that good results can be obtained at any blending ratio, but rather the following blending composition should be used.

In other words, the A component is 50 to 70% (weight), the B component is 10% (weight) or more, and the C component is 10 to 30%.
limited to.

The amount of the oil composition of the present invention attached to polyester fibers is 0.07 to 0.3% (by weight), preferably 0.1 to 0.3% (by weight).

It is preferable to keep it within the range of 0.2% (by weight).

If the amount of adhesion is less than this range, uneven adhesion occurs and static electricity is likely to occur during spinning, while if the amount of adhesion is greater than this range, the tendency for spinning scum and roller winding will increase somewhat.

Since the spinning oil composition of the present invention is water-soluble or water-dispersible, components A, B, and C are diluted as they are and used as an aqueous solution for dipping or dipping to tow or cut cotton in the spinning and drawing process. It can be attached using one spray method.

The polyester fiber thus obtained has good high-speed card passing properties, passes through the filament process very smoothly, and raw cotton with little shedding of spinning scum and the like can be obtained.

In addition, the oil composition of the present invention may contain nonionic activators, anionic activators,
A small amount of a cationic activator or an amphoteric activator may be added, and other additives such as brighteners, dyes, and antioxidants may also be added.

EXAMPLES Hereinafter, the present invention will be explained with reference to Examples, but the present invention is not limited in any way by the following Examples.

In addition, as an evaluation of spinnability, convergence, spinning scum, coiling form, etc. were determined.

(1) Convergence: The electrical properties of the wraps were determined by cT113/g and compared with each other.

(2) Spinning scum: 100 kg of cotton was passed through the filament process, and the scum adhering to the rubber roller and metal roller was collected and measured.

(3) Coiling form: The shape of the sliver obtained through the filament process was evaluated by grade.

Example 1 The intrinsic viscosity measured with an orthochlorophenol solution was 0.
No. 65 polyethylene terephthalate fiber (1.5 denier) was cut into a length of 38 mm and immersed in each of the 10 solutions shown in Table 1. % (weight), then heat-treated cotton at 120°C and aged for 24 hours at 25°C and relative humidity of 70% RH to reach the equilibrium moisture content, then opened, batted, and carded.・The fibers were passed through each step of the filament, and the bulk specific gravity of the wrap, spinning scum, and coiling form were measured for convergence.

Regarding convergence, spinning scum, and coiling form, those with good results are marked as ○ and the rest are △-○, △, △.
It was qualitatively shown that the defects become worse in the order of −× and ×.

As can be seen from the results in Table 2, it can be seen that the present invention exhibits excellent spinnability.

Example 2 In the same way as in Example 1, oil agent B in Table 1 was used, and after changing the blending ratio and applying the oil agents shown in Table 3, the behavior after time was measured in the same way as in Example 1. conducted and evaluated.

The results are shown in Table-3. As can be seen from the table, the spinnability of the blended composition of the present invention is very stable.

Example 3 Each treatment was performed using the oil composition shown in Table 4 in the same manner as in Example 1, and the spinnability was determined at 25°C x 70% RH using the treated 100% polyester cotton as a standard. Polyester/cotton 65%/35%
The spinnability of a cotton blend of (by weight) and the spinnability of a polyester/rayon blend of 50% polyester/rayon and 150% (by weight) were tested.

The results are summarized in Table 5. As can be seen from Table 5, the examples of the present invention exhibit very stable spinnability.

Claims (1)

[Scope of Claims] 1. An alkyl phosphoric acid ester obtained by reacting a linear or side chain alcohol having an average carbon number of 10 to 16 with P2O5, the degree of phosphorylation of which is 0.6 to 1.0.
50 to 70% (by weight) of a potassium salt of an alkyl phosphoric acid ester (component A) having an acid value of 0 to 50 [However, R is a straight chain or a side chain having 8 to 18 carbon atoms]
saturated or unsaturated alkyl group, R'-CH-CH2-
, R' COOCH2CHCH2,11 0HOH or R'-0-C, CH-CH2-OH (however, R' is the same group as R), and X is a hydrogen atom, a lower alkyl group having 1 to 4 carbon atoms, or -COCH3 indicates a cyanoethyl group. 10% (by weight) or more of a phosphate (component B) of a compound obtained by adding 5 to 15 moles of ethylene oxide to an alkylamine or a substituted alkylamine represented by 8 to 12 hydrocarbon monohydrogen residues, n is 3 to 13, Y is polyoxyethylene,
Indicates that it is polyoxypropylene or a copolymer of polyoxyethylene and polyoxypropylene. ] A spinning oil composition for polyester fibers containing 10 to 30% of the compound (C component).