KR102249081B1 - Spinning oil composition for polyester industrial yarns, Spinning oil using the same and Manufacturing method thereof - Google Patents

Abstract

The present invention relates to a spinning emulsion composition and a spinning emulsion prepared using the same, and more specifically, to a spinning emulsion composition that can reduce fluff or single yarn by reducing yarn vibration by improving focusing properties by being applied to a high-temperature and high-speed spinning process when spinning polyester industrial yarn (synthetic fiber), a spinning emulsion containing the same, and a method for preparing the same.

Description

Spinning oil composition for polyester industrial yarns, spinning oil using the same and manufacturing method thereof

The present invention is a polyester that can reduce fluff or single yarn by reducing the vibration of the yarn by improving the binding property by applying it to a high-temperature and high-speed spinning process when spinning yarn (synthetic fiber) for the polyester industry. It relates to a spinning oil composition for industrial use, a spinning oil comprising the same, and a method of manufacturing the same.

In general, the method of manufacturing polyester-based industrial yarn is to melt polyester chips at 250 ~ 300℃ in an extruder and pass them through a spinneret at high speed to wind them up in a filament state (4,000 ~ 6,000m/min of yarn speed). In order to further improve the production speed, high-temperature heat treatment and high-speed production are being performed.

Increasing the production speed leads to problems of increasing fluff or single yarn due to increased damage to the surface of the yarn, generation of static electricity, and poor collection properties.

In addition, in the heat treatment, high temperature is accompanied in order to eliminate the lack of thermal energy required for orientation and stabilization of the fiber polymer chain due to the high speed. In other words, in order to manufacture yarns with high functionality, such as high strength with high morphological stability, it is necessary to increase the temperature of the heat set roller. The high temperature of the heat set roller causes an increase in contamination of the heat set roller due to deterioration of the spinning oil for synthetic fibers, and there is a problem of deteriorating the production environment and lowering the productivity.

Therefore, the selection of a suitable spinning oil according to the high temperature and high speed of the spinning process has a great influence on the fiber quality. Important factors in the spinning emulsion of synthetic fibers include smoothness, antistatic properties, and binding properties. In other words, the spinning emulsion includes a smoothing agent to reduce friction generated when filamentous fibers pass through a high-speed metal surface, an antistatic agent to reduce the generation of static electricity on the surface of various machinery and fibers, and a uniform aggregate of yarns composed of several short fibers. It requires a binding agent for physical properties. In particular, in the case of industrial companies, unlike general medical applications, the thermal stability of the spinning oil is also emphasized along with these as the high temperature and high speed of the process.

Since the friction between fiber-metal and fiber-fiber is low and fluff and single yarn can be reduced, most of the conventional spinning oils have been proposed treatment agents having excellent lubricity by focusing on smoothness among these factors. However, with the recent high temperature of the heat set roller, four flows (shaking) increase during spinning, and the amount of fume generated due to pyrolysis and volatilization of the spinning oil due to high heat increases, deteriorating the work environment. In addition, the contamination of the rollers increased, and it was necessary to frequently clean the rollers, and high-quality fibers could not be obtained.

In addition, a treatment agent using a polyhydric alcohol ester as a lubricant has been proposed in order to improve contamination of the heat set roller. Although this treatment agent has good heat resistance, the friction between fiber-metal and fiber-fiber is high, and lubricity, which is a necessary characteristic as a treatment agent for synthetic fibers, is inferior. As a result, damage to the fibers in the fiber manufacturing process and the processing process increased, fluff and single yarn increased, and the high demands required for the current fibers could not be satisfied.

As described above, the conventional treatment agent for synthetic fibers cannot cope with the above-described problem, and the treatment agent for synthetic fibers that is capable of producing high-quality recently highly functional fibers and has excellent heat resistance and does not deteriorate the production environment is urgently needed. Is being demanded.

Korean Patent Application Publication No. 10-2004-0061347 (July 7, 2004) Korean Registered Patent Publication No. 1993-0005935 (1993.06.29)

As a result of careful examination to solve the problems of the existing spinning emulsions, the inventors of the present invention have shown that a specific ester (A) and a specific polyhydric alcohol condensate (B) have an excellent effect of reducing the flow of yarn at a high temperature. The present invention was completed by knowing a spinning oil composition for synthetic fibers that essentially contains. That is, the present invention is to provide a spinning oil composition for polyester-based synthetic fibers and a spinning oil comprising the same.

The spinning oil composition for polyester industry of the present invention for solving the above problems comprises: an ester compound obtained by polymerizing an aliphatic dihydric alcohol and a straight-chain fatty acid; And polyhydric alcohols and polyhydric alcohol polymers.

In addition, the spinning oil for industrial use of the polyester of the present invention includes the spinning oil composition and a diluent.

In addition, the present invention relates to a method of manufacturing the spinning oil for the polyester industry, the first step of preparing a mixture of the spinning oil composition; And a second step of preparing a spinning oil having ^{a viscosity of 3 to 100 mm 2} /sec at 25° C. by adding and stirring a diluent to the mixture.

Synthetic fiber produced by applying the spinning emulsion made of the spinning emulsion composition of the present invention to a high-speed, high-temperature spinning process for the production of polyester synthetic fibers, thereby reducing the flow of yarn at high temperature with appropriate smoothness and excellent binding properties. Alternatively, it is possible to improve the quality of synthetic fibers and obtain excellent yarn spinning properties by remarkably reducing the occurrence of single yarn and fluffing (including filaments and yarns). In addition, there are advantages of less contamination of the rollers due to tar during heat treatment, excellent heat resistance, and prevention of deterioration of the production environment. The spinning emulsion of the present invention can be applied to industrial materials such as tarpaulin, tire cords, seat belts of automobiles, and synthetic fiber filament yarns.

Hereinafter, the present invention will be described in more detail.

The present invention is used when manufacturing an industrial yarn composed of a polyester synthetic fiber (hereinafter, referred to as'synthetic fiber' or "industrial yarn"), it is possible to significantly reduce the occurrence of fluff and single yarn, and also has excellent heat resistance. It is to provide a spinning oil for industrial use that does not deteriorate the production environment.

The composition used in the production of the spinning oil for industrial use of the present invention includes an ester compound and a polyhydric alcohol polymer.

The ester polymer is a compound that does not have a polyoxyalkylene group in its molecule as it acts as a leveling agent in a spinning oil.

The ester polymer is a polymer obtained by polymerizing an aliphatic dihydric alcohol and a straight-chain fatty acid, preferably the aliphatic dihydric alcohol and a straight-chain fatty acid in a molar ratio of 1: 1.0 to 2.0, more preferably an aliphatic dihydric alcohol and a straight-chain fatty acid It is a polymer obtained by polymerizing at a molar ratio of 1: 1.5 to 2.0.

When only an ester having a structure in which a monohydric alcohol and a linear fatty acid are ester-bonded is used as the ester compound, the smoothness is excellent, but the oil film strength protecting the fiber is weak, and the fluff is rather increased. Further, when an ester having a structure in which a polyhydric alcohol and a branched fatty acid are ester-bonded is used, smoothness is insufficient and fluff increases.

Accordingly, the aliphatic dihydric alcohol used in the preparation of the ester compound of the present invention is ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, 1,4-butanediol, 2-methyl-1,3-propanediol, It may contain at least one selected from 1,6-hexanediol, neopentyl glycol, and cyclohexanediol, and preferably 2-methyl-1,3-propanediol in terms of smoothness and fluff reduction due to the oil film steel , 1,6-hexanediol and neopentyl glycol, more preferably 1,6-hexanediol.

The straight-chain fatty acid refers to an aliphatic monocarboxylic acid having a straight-chain carbon skeleton. The straight-chain fatty acid may also contain hydroxy fatty acid, but if the hydroxy fatty acid is included, the role of the treatment agent as a leveling agent is insufficient, so it is preferable that the hydroxy fatty acid is not included.

Therefore, the straight-chain fatty acid used in the preparation of the ester compound of the present invention may include a saturated fatty acid and/or an unsaturated fatty acid, and specifically, a straight-chain fatty acid having 12 to 22 carbon atoms, preferably 12 to 20 carbon atoms. Phosphorus straight-chain fatty acids can be used. At this time, when the number of carbon atoms is less than 12, sufficient oil film strength cannot be obtained, and fluff is generated. When the number of carbon atoms exceeds 22, the smoothness of the ester is insufficient, and fluff increases. For a preferred embodiment of the straight-chain fatty acid, the straight-chain fatty acid having 12 to 22 carbon atoms is lauric acid, myristic acid, myristoleic acid, and palmitic acid. , Palmitolenic acid, stearic acid, stearic acid, oleic acid, elaidic acid, linolenic acid, eicosenoic acid, and henicosanoic acid ) May include one or more selected from.

And, in the composition of the present invention, the ester compound may have an acid value of 0.5 to 7, preferably 0.5 to 5, more preferably 0.5 to 3. At this time, when the acid value of the ester polymer exceeds 7, a large amount of smoke occurs during heat treatment, or an odor is generated, which deteriorates the use environment.

In addition, the weight average molecular weight of the ester compound is preferably 500 to 1,000, preferably 500 to 900, more preferably 500 to 800. At this time, if the weight average molecular weight is less than 500, the oil film strength is insufficient, fluff increases, or smoke during heat treatment may increase.If the weight average molecular weight exceeds 1,000, the smoothness is insufficient and fluff occurs. In addition, since high-quality fibers cannot be obtained, and the quality in the weaving or knitting process may be inferior, it is preferable to use an ester polymer having a weight average molecular weight within the above range.

In addition, the content of the ester compound in the industrial spinning oil composition of the present invention is the remaining amount of the total weight of the composition components described below.

Next, the polyhydric alcohol polymer among the compositions used in the production of the industrial spinning oil of the present invention is used to improve the lubricity and binding properties of the spinning oil and to improve high spinning performance, and condensation of a polyhydric alcohol and a dihydric fatty acid Polyhydric alcohol polymers can be used. In addition, the polyhydric alcohol polymer is an essential component of the spinning emulsion composition of the present invention together with the ester polymer, and includes the ester compound and the polyhydric alcohol polymer in a weight ratio of 1: 0.1 to 2, preferably in a weight ratio of 1: 0.10 to 1.00. , More preferably, it is good to use in a weight ratio of 1:0.10 to 0.50. At this time, if the weight ratio of the polyhydric alcohol polymer is too low, there may be a problem in that lint increases due to a decrease in the binding property, and if it exceeds 2 weight ratio, there may be a problem in that the lubricity is deteriorated.

The polyhydric alcohol used for condensation of the polyhydric alcohol polymer may include at least one selected from ethylene glycol, glycerin, sorbitol, sorbitan, trimethylolpropane, and pentaerythritol, preferably 1 selected from glycerin and sorbitol. It may contain more than one species.

In addition, the divalent fatty acid used for condensation of a polyhydric alcohol polymer may include at least one selected from fumaric acid, succinic acid, maleic acid, adipic acid and sebacic acid, and preferably maleic acid, adipic acid, and seba It may include at least one selected from among the acidic acids, and more preferably at least one selected from adipic acid and sebacic acid.

It is preferable to prepare a polyhydric alcohol condensate by performing a condensation reaction of the polyhydric alcohol and the dihydric fatty acid in a molar ratio of 1: 0.5 to 1.0, preferably in a molar ratio of 1: 0.65 to 1.00. At this time, if the weight ratio of the divalent fatty acid is less than 0.5 molar ratio, a polymer having a desired amount of binding cannot be obtained, and if the weight ratio of the divalent fatty acid exceeds 1.0 molar ratio, the polymer is gelled or flowable due to an excessive increase in the weight average molecular weight. Since it disappears and there may be a problem in use, it is preferable to prepare a polymer by condensation within the above range. In addition, the polyhydric alcohol polymer prepared by performing the condensation reaction preferably has a weight average molecular weight of 3,500 to 8,000, preferably 4,500 to 8,000, and more preferably about 5,000 to 7,800. At this time, if the weight average molecular weight of the polyhydric alcohol condensate is less than 3,500, the desired binding property may not be obtained, and there may be a problem of increasing fluff, and if it exceeds 8,000, there may be a problem that the single yarn decreases due to low smoothness.

In addition, the content of the polyhydric alcohol polymer in the spinning oil composition for synthetic fibers of the present invention is 2 to 25% by weight, preferably 2 to 20% by weight, more preferably about 3.5 to 13.0% by weight of the total weight of the composition. And, while satisfying the weight ratio with the ester polymer described above, it is preferable to use within the above weight% range. At this time, when the content of the polyhydric alcohol polymer in the total weight of the composition is less than 2% by weight, the binding property may decrease and fluff may increase, and when it exceeds 25% by weight, there is a problem that the smoothness is insufficient, but rather the fluff increases. It is recommended to use within the above range.

Next, the spinning oil composition of the present invention may include a polyol alkylate in order to impart thermally stable smoothness to the spinning oil in addition to the ester compound and the polyhydric alcohol polymer.

In addition, the polyol alkylate may include at least one selected from trimethylolpropane trilaurate, trimethylolpropane trioleate, pentaerythritol trilaurate, and glycerin trioleate, preferably trimethylolpropane trioleate. It may contain at least one selected from laurate and glycerin trioleate.

In addition, the content of the polyol alkylate in the composition may include 25 to 32% by weight, preferably 27 to 30% by weight of the total weight of the composition. At this time, if the polyol alkylate content is less than 25% by weight, the amount of the polyol alkylate is less than that, and the effect of imparting thermally stable smoothness may be insufficient, and if it is used in excess of 32% by weight, the amount of ester compound used is relatively reduced. Since there may be a problem of reducing the value, it is recommended to use it within the above range.

Next, the spinning oil composition of the present invention may further include a nonionic surfactant in order to have binding properties and emulsification properties, and as the nonionic surfactant, polyoxyalkylene polyhydric alcohol ether, polyoxyalkylene polyhydric alcohol fatty acid Ester, polyoxyalkylene aliphatic alcohol ether, fatty acid ester of polyalkylene glycol, polyoxyalkylene castor oil ether and/or polyhydric alcohol fatty acid ester. Oxyalkylene aliphatic alcohol ether and polyoxyalkylene castor oil ether can be mixed and used, more preferably polyoxyalkylene aliphatic alcohol ether and polyoxyalkylene castor oil ether are mixed in a weight ratio of 1: 0.3 to 0.7 Can be used.

In addition, the content of the nonionic surfactant is preferably 12 to 25% by weight, preferably 13.0 to 22.0% by weight, more preferably 14.0 to 20.0% by weight of the total weight of the composition, and the nonionic surfactant content If it is less than 12% by weight, the oil film strength decreases and fluff may increase, and if it is used in excess of 25% by weight, there may be a problem that the fluff increases due to insufficient smoothness due to excessive use. It is good.

Next, the spinning oil composition of the present invention may further include an antistatic agent to impart antistatic properties, lubricity, and binding properties to the fibers, and as the antistatic agent, a metal salt or an amine salt of alkyl phosphate ; Metal salt or amine salt of polyoxyethylene alkyl phosphate; Anionic surfactants such as alkanesulfonic acid salts and fatty acid soaps; Cationic surfactants such as alkylamine salts, alkylimidazolinium salts, and/or quaternary ammonium salts; And amphoteric surfactants such as lauryl dimethyl betaine and/or stearyl dimethyl betaine; It may include one or more selected from among.

In addition, the content of the antistatic agent is preferably 0.1 to 10% by weight, preferably 0.5 to 5.0% by weight, more preferably 0.5 to 2.0% by weight of the total weight of the composition, and at this time, the content of the antistatic agent is 0.1 If the content is less than% by weight, the effect of using the antistatic agent may be insufficient, and if the content exceeds 10% by weight, heat resistance may deteriorate due to excessive use, and as a result, there may be a problem that the properties of fluff and single yarn deteriorate. It is recommended to use within the range.

Next, the spinning oil composition of the present invention may further include an antioxidant in order to impart heat resistance. As the antioxidant, one or more known antioxidants such as phenol-based antioxidants, thio-based antioxidants, and phosphite-based antioxidants may be used. In addition, the content of the antioxidant is preferably 0.1 to 5.0% by weight, preferably 0.1 to 2.0% by weight, more preferably 0.2 to 1.5% by weight of the total weight of the composition, and at this time, the antioxidant content is 0.1 If it is less than wt%, the content may be too small to prevent oxidation and improve heat resistance, and if it is used in excess of 5.0 wt%, there may be a problem of yellowing of the yarn during storage or storage due to excessive use, so it is recommended to use it within the above range. good.

The spinning emulsion composition described above can be prepared as a spinning oil for polyester industry (hereinafter, referred to as a spinning oil) by the following method.

1 step of preparing a mixture of the spinning emulsion composition described above; And a second step of preparing a spinning oil by adding and stirring a diluent to the mixture, thereby producing a spinning oil for use in the polyester industry.

The spinning emulsion composition in step 1 is as described above, and the mixture in step 1 is in a non-volatile state.

In the second step, the mixture of the composition of the first step is mixed and stirred with a diluent so that the viscosity at 25°C is 3 to 100 mm ² /sec, preferably 5 to 70 mm ² /sec, more preferably 10 to 60 mm. ^{It is preferable to be about 2} /sec, and it is advantageous in terms of uniformly imparting the spinning oil to the fiber material that the viscosity is in the above range.

In addition, it is appropriate in terms of viscosity control that the second-stage spinning emulsion has a nonvolatile content concentration of 65 to 75% by weight, preferably 66.0 to 73.5% by weight, and more preferably about 67.5 to 72.5% by weight.

In addition, the diluent may be a general diluent used in the art, preferably a low-viscosity mineral oil having 12 to 15 carbon atoms, more preferably one selected from normal dodecane, tridecane, and tetradecane The above low viscosity mineral oil can be used.

When the spinning emulsion of the present invention is applied to the production of polyester synthetic fibers, a preferred example, can be applied as a spinning emulsion for polyester-based industrial yarn high-speed spinning (SDY, Spin draw yarn), and tarpaulin (Tapaurin), It can be applied to tire cords, industrial materials such as automobile seatbelts, and synthetic fiber filament yarns.

Hereinafter, the present invention will be described in more detail by the following Examples and Experimental Examples. However, the following Examples and Experimental Examples are for illustrative purposes only, and the scope of the present invention is not limited by these Examples and Experimental Examples.

[Example]

Preparation Example 1-1: Synthesis of Ester Polymer

In the reactor, 49.3 parts of ethylene glycol, an aliphatic dihydric alcohol, and 50.6 parts of lauric acid, which are linear fatty acids, were mixed, and 0.1 part of paratoluenesulfone was mixed as a reaction catalyst.

Next, the temperature was raised to 150°C under a nitrogen stream and reacted for 4 hours, and then the temperature was continuously raised to 200°C, followed by polymerization reaction for 8 hours. After the polymerization reaction, the reaction catalyst and unreacted fatty acid were removed from the reaction product to prepare an ester polymer having an acid value of 0.8 (Mw=710).

Preparation Example 1-2 ~ Preparation Example 1-3

The ester polymer was synthesized by using an aliphatic dihydric alcohol and a straight-chain fatty acid under the same conditions and composition ratio as in Preparation Example 1-1, but the ester polymer was synthesized by different aliphatic dihydric alcohols and straight-chain fatty acids as shown in Table 1 below. Thus, Preparation Example 1-2 and Preparation Example 1-3 were carried out, respectively.

division Preparation Example 1-1 Preparation Example 1-2 Preparation Example 1-3 Straight-chain fatty acids Lauric acid Stearic acid Oleic acid Aliphatic dihydric alcohol Ethylene glycol 1,4 butanediol 1,6 hexanediol Acid 0.8 1.3 0.7 Weight average molecular weight (Mw) 710 650 680

Preparation Example 2-1: Synthesis of polyhydric alcohol polymer

In a reactor, 29.5 parts of glycerin as a polyhydric alcohol and 70.3 parts of adipic acid as a dihydric fatty acid were mixed, and 0.3 parts of paratoluenesulfone as a reaction catalyst were mixed.

Next, the temperature was raised to 200° C. under a nitrogen stream, condensation reaction was performed for 1 hour, and then the temperature was continuously raised to 220° C. and condensation reaction was performed for 12 hours. After the condensation reaction, the reaction catalyst and unreacted fatty acid were removed from the reaction product, and a polyhydric alcohol polymer having a weight average molecular weight of 5,500 was prepared.

Preparation Example 2-2 and Comparative Preparation Example 1-1

A polyhydric alcohol polymer was synthesized using a polyhydric alcohol and a dihydric fatty acid under the same conditions and composition ratio as in Preparation Example 2-1, but the ester polymer was synthesized by different polyhydric alcohols as shown in Table 2 below, and Preparation Example 2-2 and Comparative Preparation Example 2-1 was carried out, respectively.

division Preparation Example 2-1 Preparation Example 2-2 Comparative Preparation Example 2-1 Divalent fatty acids Adipic acid Adipic acid Adipic acid Polyhydric alcohol glycerin Trimethylolpropane Pentaerythritol Weight average molecular weight 5,500 7,500 10,000

Examples 1 to 3 and Comparative Examples 1 to 3: Preparation of spinning oil composition and spinning oil for use in polyester industry

(1) Spinning oil composition for polyester industry

The composition and composition ratio as described in Table 3 were mixed to prepare a spinning oil composition for use in polyester industry, respectively.

Next, the composition was mixed and stirred to prepare a mixture, and then tridecane, a low-viscosity mineral oil having 13 carbon atoms, was mixed and stirred to dilute the mixture to prepare a spinning emulsion having a nonvolatile content of 70% by weight. Examples 1 to 3 and Comparative Examples 1 to 3 were carried out, respectively.

At this time, when preparing the composition, trimethylolpropane trilaurate was used as the polyol alkylate, and polyoxyethylene oleyl ether and castor oil EO (ethylene oxide) were added as an aliphatic alcohol EO (ethylene oxide) adduct as a nonionic surfactant. Water polyoxyethylene castor oil ether was used. In addition, as an antistatic agent, an alkyl phosphate salt, isotridecyl alcohol phosphate Na salt was used, and as an antioxidant, thiodiethylenebis[3-(3,5-ditert-butyl-4-hyde), a phenolic antioxidant Roxyphenyl propionate)] (Thiodiethylenbis[3-(3,5-ditert-butyl-4-hydroxyphenyl propionate)) was used.

Experimental Example 1: Spinning emulsion physical properties experiment

Using each of the prepared spinning oils, roller contamination, fluff, and single yarn were evaluated by the following method, and the results are shown in Table 3 below.

(1) roller contamination

For the 1500d/144f non-lubricating polyester filament yarn, the spinning oil prepared above was applied so that the amount of non-volatile matter was 0.5% by using the guide lubrication method, and allowed to stand in an atmosphere at a temperature of 25° C. for 24 hours and humidity controlled.

The moistened yarn was brought into contact with a friction body at 230° C. by a friction tester, and the yarn was run for 8 hours at a load of 250 g and a scanning speed of 200 m/min. The adhered contamination of the friction body was determined under the following conditions, and roller contamination was evaluated. . The results are shown in Table 3.

(○: No or very few tardates / ×: Remarkable tars are recognized)

(2) Evaluation of single yarn and fluff generation

In the melt spinning step, the polyester polymer was melt-spinned, and the spinning oil agent was applied so that the amount of non-volatile matter was 0.5% by using the guide lubrication method. The yarn to which the oil agent was applied was continuously stretched and stretched through a 230° C. hot roller to obtain a filament of 1500 d//144f.

Single yarn and fluff were evaluated under the following conditions, and the results are shown in Table 4.

① Single yarn: For each spinning emulsion, the number of yarn breaks per ton of yarn was evaluated, and if less than one was set as ○, and more than one was set as ×

② Fluff: Each treatment agent-applied yarn was checked for fluff with a fluff counter, and the case where the value per million m is less than 1 was set to ○, and 1 or more was set to x.

Spinning emulsion component Example Comparative example One 2 3 One 2 3 Ester polymer Preparation Example 1-1 45 - - - 45 - Preparation Example 1-2 - 40 - - - - Preparation Example 1-3 - - 45 - - 45 Polyhydric alcohol
Condensate Preparation Example 2-1 5 - - - - - Preparation Example 2-2 - 10 5 - - - Comparative Preparation Example 2-1 - - - - - 5 Polyol
Alkylate Trimethylolpropane
Tryster 30 30 30 75 30 30 Nonionic
Surfactants Aliphatic alcohol EO adduct 12 12 12 12 12 12 Caster Oil EO Additives 6 6 6 11 6 6 Antistatic agent Alkyl phosphate salt One One One One One One Antioxidant Phenolic antioxidant One One One One One One Total weight% of spinning emulsion composition 100 100 100 100 100 100 Spinning emulsion Concentration of non-volatile matter 70% by weight 70% by weight 70% by weight 70% by weight 70% by weight 70% by weight Viscosity (25℃, ㎜ ² /sec) 28 35 27 24 22 38 The degree of single yarn occurrence ○ ○ ○ × × ○ The degree of fluffing ○ ○ ○ × × × Roller contamination ○ ○ ○ ○ × ○

Looking at the measurement results of the physical properties of Table 3, Examples 1 to 3, the occurrence of single yarn and fluff is significantly reduced. Further, it was confirmed that there was little roller contamination, excellent heat resistance, and did not deteriorate the production environment.

On the contrary, in Comparative Example 1 using only polyol alkylate and Comparative Example 2 without using a polyhydric alcohol polymer, there was a serious problem in the occurrence of single yarn and fluff, and Comparative Example 2 also showed poor roller contamination. In addition, in the case of a spinning emulsion prepared using a polyhydric alcohol polymer having a weight average molecular weight of more than 8,000, there is a problem that a lot of fluff occurs.

Examples 4 to 5 and Comparative Examples 4 to 6: Preparation of spinning oil composition and spinning oil for use in polyester industry

In the same manner as in Example 1, a spinning oil composition for polyester industry and a spinning oil were prepared, but the spinning emulsions were prepared by varying the composition of the spinning emulsion as shown in Table 4 below, and Examples 4 to 5 and Comparative Examples 4 to 6 were prepared. Was carried out.

Spinning emulsion component Example Comparative example 4 5 4 5 6 Ester polymer Preparation Example 1-1 45 45 45 45 37 Polyhydric alcohol polymer Preparation Example 2-1 20 13 30 15 5 Polyol alkylate Trimethylolpropane
Tryster 15 28 5 29 38 Nonionic
Surfactants Aliphatic alcohol EO adduct 12 8 12 5 12 Caster Oil EO Additives 6 4 6 4 6 Antistatic agent Alkyl phosphate salt One One One One One Antioxidant Phenolic antioxidant One One One One One Total weight% of spinning emulsion composition 100 100 100 100 100 Spinning emulsion Concentration of non-volatile matter 70% by weight 70% by weight 70% by weight 70% by weight 70% by weight Viscosity (25℃, ㎜ ² /sec) 35 29 48 36 28 The degree of single yarn occurrence ○ ○ × × ○ The degree of fluffing ○ ○ × × × Roller contamination ○ ○ × ○ ○

Looking at Table 4, in the case of Comparative Example 4 in which the polyhydric alcohol polymer was used in excess of 25% by weight, the viscosity was high, the degree of occurrence of single yarn and the occurrence of fluff was high, as well as poor roller contamination. In addition, in the case of Comparative Example 5 in which a nonionic surfactant was used in an amount of less than 10% by weight, a result was shown that the frequency of occurrence of single yarn and fluff was high, and in the case of Comparative Example 6 in which a polyol alkylate was used in an amount of more than 32% by weight, the incidence of fluff was It was confirmed that there was a problem of increasing.

Claims (11)

delete delete delete delete delete delete delete delete Polyhydric alcohol polymer 2 to 20% by weight, polyol alkylate 25 to 32% by weight, nonionic surfactant 12 to 25% by weight, antistatic agent 0.1 to 10% by weight, antioxidant 0.1 to 5% by weight, and the balance of ester compound Spinning oil composition; And
Including; a diluent containing a low viscosity mineral oil having 12 to 15 carbon atoms,
The ester compound includes a polymer obtained by polymerizing an aliphatic dihydric alcohol and a linear fatty acid having 12 to 22 carbon atoms in a molar ratio of 1: 1.0 to 2.0,
The aliphatic dihydric alcohol is ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, 1,4-butanediol, 2-methyl-1,3-propanediol, 1,6-hexanediol, neopentyl glycol, and cyclohexane It contains at least one selected from among diols,
The straight-chain fatty acids having 12 to 22 carbon atoms are lauric acid, myristic acid, myristoleic acid, palmitic acid, palmitoleic acid, and stearic acid. ,(stearic acid) oleic acid, elaidic acid, linolenic acid, eicosenoic acid, and heneicosanoic acid,
The polyhydric alcohol polymer is a condensation product obtained by condensing a polyhydric alcohol and a dihydric fatty acid in a molar ratio of 1: 0.5 to 1.0,
The polyhydric alcohol polymer has a weight average molecular weight of 3,500 to 8,000,
The polyhydric alcohol includes at least one selected from glycerin and trimethylolpropane,
The divalent fatty acid includes at least one selected from fumaric acid, succinic acid, maleic acid, adipic acid, and sebacic acid,
Spinning oil for polyester industrial yarn manufacturing, characterized in that the non-volatile content concentration of the spinning oil is 65 to 75% by weight. The method of claim 9, wherein the spinning emulsion
Spinning oil for polyester industrial yarn production, characterized in that the viscosity at 25 ℃ 3 ~ 100㎜ ^{2 /sec.} 1 step of preparing a mixture in which the spinning emulsion composition is mixed; And
A second step of preparing a spinning emulsion having ^{a viscosity of 3 to 100 mm 2} /sec at 25°C by adding and stirring a diluent to the mixture; and performing a process including,
The spinning oil composition is a polyhydric alcohol polymer 2 to 20% by weight, polyol alkylate 25 to 32% by weight, nonionic surfactant 12 to 25% by weight, antistatic agent 0.1 to 10% by weight, antioxidant 0.1 to 5% by weight and the balance Containing an ester compound of,
Including; a diluent containing a low viscosity mineral oil having 12 to 15 carbon atoms,
The ester compound includes a polymer obtained by polymerizing an aliphatic dihydric alcohol and a linear fatty acid having 12 to 22 carbon atoms in a molar ratio of 1: 1.0 to 2.0,
The aliphatic dihydric alcohol is ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, 1,4-butanediol, 2-methyl-1,3-propanediol, 1,6-hexanediol, neopentyl glycol, and cyclohexane It contains at least one selected from among diols,
The straight-chain fatty acids having 12 to 22 carbon atoms are lauric acid, myristic acid, myristoleic acid, palmitic acid, palmitoleic acid, and stearic acid. (stearic acid), oleic acid, elaidic acid, linolenic acid, eicosenoic acid, and heneicosanoic acid,
The polyhydric alcohol polymer is a condensation product obtained by condensing a polyhydric alcohol and a dihydric fatty acid in a molar ratio of 1: 0.5 to 1.0,
The polyhydric alcohol polymer has a weight average molecular weight of 3,500 to 8,000,
The polyhydric alcohol includes at least one selected from glycerin and trimethylolpropane,
The divalent fatty acid comprises at least one selected from fumaric acid, succinic acid, maleic acid, adipic acid, and sebacic acid.