KR100714782B1 - Process for preparing flameproof polyester based synthetic hair - Google Patents

Abstract

Flame retardant polyester wig yarn of the present invention is a thermal stabilizer and a process stabilizer 500 to 60 to 90% by weight of the polyester resin pulverized to 1 mm or less and 10 to 40% by weight of the polymeric brominated flame retardant pulverized to 1 mm or less, respectively. The composition was added at a concentration of 5,000 ppm to prepare a uniformly mixed composition, and the composition was added to a melt extruder in which a compression ratio of the screw was in the range of 3.5 to 6.5 and a plurality of metal mesh filters of 300 to 400 mesh were inserted into the screw tip. It is prepared by the step of melting and spinning, and drafting the spun filament at a draft ratio of 5 to 30 times.

Index words: Flame retardant, Polyester, Wig yarn, Heat stabilizer, Screw compression ratio, Filter, Draft

Description

Process for Preparing Flameproof Polyester based Synthetic Hair

Field of invention

The present invention relates to a flame retardant wig yarn made of polyester. More specifically, the present invention has self-extinguishing and anti-dripping, the strength of the human hair level, elongation, curl formation, curl retention, curl elasticity, vivid A method for producing a flame retardant polyester wig yarn with color and the like.

Background of the Invention

Artificial hair, which is mainly used as a wig yarn, requires flame retardancy with vivid color, natural luster, lightness, heat resistance, soft touch and flexibility, and curl formation. Flame retardancy is explained by self-extinguishing and drip resistance. Polyester yarns have not been widely used as wig yarns because they do not have the properties required for such artificial hair.

In order to solve the above problems of the polyester wig yarn, the present inventors have developed a polyester artificial hair yarn having improved physical properties such as flexibility, curl formability, light weight, glossiness, etc., and have been registered in Korean Patent No. 426685.

In addition, the present inventors developed a mixed spinning method of a polyester resin and a polymer brominated flame retardant in order to solve the flame retardancy problem of polyester wig yarn to develop a polyester wig yarn having a flame retardancy as well as the characteristics required for artificial hair. I was registered as a ho.

Looking at the trend of the conventional technology related to the production of flame retardant polyester wig yarn as follows.

Japanese Patent Laid-Open No. 2003-0064622 and Japanese Patent Laid-Open No. 2005-76147 include a method of producing a flame retardant polyester wig yarn from a thermoplastic copolymerized polyalkylene terephthalate resin copolymerized with a reactive phosphorus flame retardant, but this method is also a wig yarn. In order to satisfy the flame retardancy required by 5 to 10% by weight of the flame retardant in terms of phosphorus atomic weight is added, in this case, the flame retardancy is improved, but it is difficult to form the fiber is not a practical method.

As the most practical method, a method of flame retarding a polyethylene terephthalate resin or a polybutylene terephthalate resin, and adding a polymeric brominated epoxy or phenoxy flame retardant is disclosed in Japanese Patent Application Laid-Open No. 60-71713, Known from US Pat. Nos. 59-129253, 59-149954 and 58-101145. These patents disclose a method of melt kneading a reaction product obtained by polymerizing a brominated bisphenol A diglycidyl ether and a brominated bisphenol A as a main component as a flame retardant.

However, when the flame retardant polyester wig yarn having a fineness of 30-100 denier is produced by these methods, the wig yarn which requires uniform fineness cannot be manufactured due to the increase in fineness variation in the fiber axis direction, and pyrolysis as the spinning time elapses. As the generation of carbides increases, pyrolysis carbides accumulate around nozzle holes through which nozzle holes are clogged or molten resin is discharged, and trimming occurs due to the curvature phenomenon, thereby making continuous production difficult. In addition, these methods are limited in flame retardants that can be used, and there is a great difference in productivity problems such as trimming, cleaning around the nozzle hole, and nozzle replacement in the fiber manufacturing process by pyrolysis of the flame retardant, and in melt flowability of the polyester resin and the flame retardant. In this case, it is difficult to manufacture a uniform quality wig yarn, and there is a limit to long-term continuous production. Therefore, stably producing flame-retardant wig yarn of uniform quality without trimming is an urgently required technique in terms of production well. In particular, the technique of extending the nozzle hole cleaning cycle from the conventional method is important in terms of economical efficiency that can reduce the number of workers required for cleaning and reduce waste generation.

The present inventors improve the manufacturing process conditions to solve the problems of the prior art as described above, the new polyester wig according to the present invention can improve the workability by maintaining the physical properties of the wig yarn as well as flame retardancy and reducing the occurrence of trimming It is about to develop a method of manufacturing yarn.

An object of the present invention is to provide a method of continuously producing a flame-retardant polyester wig yarn without melt trimming for a long time by melt mixing spinning at least one polyester resin and a polymeric brominated flame retardant.

It is another object of the present invention to provide a method for producing an excellent flame retardant polyester wig yarn having a blend of various thermoplastic polyester resins and a polymeric brominated flame retardant and having self-extinguishing and drip resistance when ignited.

Another object of the present invention is to minimize the amount of pyrolysis material attached around the nozzle hole as the spinning time elapses in the spinning process of flame retardant polyester wig yarn to significantly reduce the number of times cleaning the nozzle surface to reduce the generation of waste due to cleaning yield It is to provide a method for producing a polyester wig yarn of uniform quality by increasing the amount of trimming.

Another object of the present invention is a polyester capable of minimizing the occurrence of trimming due to nozzle hole clogging, fine sanding, and howling in the process of melt spinning a high melting point polyester resin and a flame retardant mixture composition at a melt extruder temperature of 270-350 ° C. It is to provide a method for manufacturing a wig yarn.

Another object of the present invention is to provide a method for producing a flame retardant polyester wig yarn having a vivid color, curl formability, curl retention, curl elasticity, moderate strength and elongation as a wig yarn.

The above and other objects of the present invention can be achieved by the present invention described below.

Summary of the Invention

Flame retardant polyester wig yarn of the present invention is a thermal stabilizer and a process stabilizer 500 to 60 to 90% by weight of the polyester resin pulverized to 1 mm or less and 10 to 40% by weight of the polymeric brominated flame retardant pulverized to 1 mm or less, respectively. The composition was added at a concentration of 5,000 ppm to prepare a uniformly mixed composition, and the composition was added to a melt extruder in which a compression ratio of the screw was in the range of 3.5 to 6.5 and a plurality of metal mesh filters of 300 to 400 mesh were inserted into the screw tip. It is prepared by the step of melting and spinning, and drafting the spun filament at a draft ratio of 5 to 30 times.

Hereinafter, specific contents of the present invention will be described in detail below.

Detailed Description of the Invention

The flame retardant polyester wig yarn of the present invention is added to a basic resin consisting of a polyester resin pulverized to 1 mm or less and a polymeric bromine flame retardant pulverized to 1 mm or less by adding a small amount of a heat stabilizer and a process stabilizer to mix uniformly, The composition was melt-spun into a melt extruder in which a compression ratio of the screw was in the range of 3.5 to 6.5 and a plurality of 300-400 mesh mesh filters were inserted into the screw tip, and the spun filament was drafted at a draft ratio of 5 to 30 times. Prepare by drafting.

In the present invention, the reason why the polyester resin and the flame retardant resin composition are pulverized to 1 mm or less and mixed and mixed into the melt spinning apparatus is to minimize the formation of thermal decomposition products due to excessive shear stress and excessive heat from the external heater in the compounding process of the two resins. It is for.

The reason for adding the heat stabilizer in the present invention is to prevent the thermal decomposition of the flame retardant to minimize the production of radicals.

The reason why the process stabilizer is added in the present invention is to reduce the adhesion of the two resin mixture compositions in a molten state to metal surfaces such as screws, cylinders, and nozzles.

Polyester resin

Suitable polyester resins in the present invention are resins having a thermoplastic linear polyester structure and having a molecular weight having an intrinsic viscosity of 0.5 to 1.2. More specifically, polyetherene terephthalate (PET) resin, polybutylene terephthalate (PBT) resin, polypropylene terephthalate (PPT) resin, polynaphthalene terephthalate (PEN) resin, polycyclohexanedimethanol tere Phthalate (PCT) resin). The polyester resins used in the present invention may be used alone, or two or more resins may be mixed and used depending on the purpose of the wig yarn. However, polycyclohexane dimethanol terephthalate (PCT) resin is not compatible with other polyether resin due to its molecular structure. If necessary, a compatibilizer may be used.

In the present invention, by melting and spinning at least one resin selected from polyethylene terephthalate, polybutylene terephthalate, polypropylene terephthalate, polyethylene naphthalate, polycyclonucleic acid dimethylene terephthalate and polymer type brominated flame retardant without continuous generation of trimming Flame retardant polyester wig yarn can be produced.

Flame retardant

The flame retardant used in the present invention is a polymeric bromine flame retardant. More specifically, flame retardants suitable for the present invention are suitable flame retardants having a molecular weight ranging from 10,000 to 120,000 and a bromine content of 40 to 80% by weight. Examples of flame retardants include polystyrene bromo flame retardants, polybromoepoxy flame retardants, polybrophenoxy flame retardants, polybromocarbonate flame retardants, and polybromoacrylate flame retardants. More preferably, a polybromoepoxy or polybromophenoxy flame retardant composed of a reaction product polymerized with bisphenol A diglycidyl ether and brominated bisphenol A as a main component is suitable.

It is preferable that the said flame retardant is as large as possible. The higher the molecular weight, the better the fiber formability during the melt spinning of the polyester resin and the flame retardant composition, the higher the softening temperature, and the higher the secondary transition temperature, thereby increasing the heat deformation temperature as the wig yarn. When using a flame retardant having a molecular weight of 10,000 or less, self-extinguishing can be obtained, but it will not function as an anti-dripping function when ignited. As a result of the experiment in the present invention, it was found that the flame retardant having a molecular weight in the range of 30,000 to 90,000 has the best self-extinguishing, melt-dripping inhibitory, fiber forming property, and heat distortion temperature of the wig yarn.

Grinding step

A polyester resin, a polybromoepoxy flame retardant, or a polybromophenoxy flame retardant was ground and used, respectively. That is, in order to mix the flame retardant with the polyester chip uniformly, the flame retardant resin and the polyester resin are respectively ground in a grinder to make powder. If the chip is not made in a powder state, the polyester resin and the flame retardant resin are not uniformly mixed, and after the fiber is made, the flame retardancy is uneven and the flame retardancy is locally different.

The smaller the particle size, the better the homogeneous mixing of the two resins and the less trimming in the spinning process. In this invention, it is preferable to grind the average particle diameter of the said polyester resin and a flame retardant resin to 1 mm or less. If it exceeds 1 mm, uniform mixing of the resin is difficult. The grinding method may use a conventional method, which can be easily carried out by those skilled in the art.

additive

The flame retardant used in the present invention is a polymer flame retardant resin having a melting temperature of 200 to 230 ° C. Since the melt spinning temperature of the polyester resin is in the range of 270 to 330 ° C., which is 70 to 100 ° C. higher than the flame retardant resin melting temperature, the pyrolysis tends to occur because of kneading under a large shear force inside the cylinder of the extruder. When pyrolysis occurs, a three-dimensional crosslinked material is formed and gelation occurs. When long-term operation, these materials block the fine nozzle hole and become impossible to radiate. The fine material passing through the nozzle hole accumulates around the nozzle hole and eventually acts as an obstacle to the polymer flow, causing fine yarn and howitz. Cause. This causes a decrease in productivity and the unevenness of the produced wig yarn.

In the present invention, the thermal stabilizer to minimize thermal decomposition products of the flame-retardant polyester composition, to improve the compatibility between the polyester resin and the flame-retardant resin and to prevent the flame-retardant resin composition from sticking to the metal surface such as cylinders, screws and nozzles of the melt extruder Spinning is carried out using Iganox 1010 as the process and Structol TR 065 as the process stabilizer. These additives can achieve a significant improvement when using a polybromoepoxy flame retardant or a polybromophenoxy flame retardant. The amount of the additive added in the present invention is preferably in the range of 500 to 5,000 ppm, more preferably in the range of 700 to 2,000 ppm.

Composition Mixing Step

The pulverized polyester resin and the flame retardant resin are mixed uniformly. In the present invention, the mixing ratio of the polyester resin and the flame retardant resin is preferably mixed with 60 to 90 wt% of the polyester resin and 10 to 40 wt% of the flame retardant resin. If the flame retardant resin is less than 10% by weight, the flame retardancy of the wig yarn is insufficient, whereas if it exceeds 30% by weight, the flame retardancy is increased, but the elasticity of the molten polymer rapidly decreases directly under the nozzle, leading to a sharp increase in trimming and an irradiated state. do. The mixing conditions of the pulverized product are stirred for 30 minutes at a speed of 30 revolutions / minute in a tumbler mixer.

Melt spinning step

In producing a flame retardant polyester wig yarn by mixing a polyester resin and a flame retardant resin, a melt extrusion machine is suitable for a single screw extruder, and a screw is suitable for a full-flight screw. This screw is usually used for polyester fiber melt spinning. In the present invention, the fiber forming property when melt spinning the flame retardant resin mixture depends on the compression ratio of the screw. The compression ratio of the screw with favorable processability is 3.5-6.5, More preferably, it is 4.5-6.0. If the compression ratio is 3.5 or less, the kneading state is poor. If the compression ratio is 6.5 or more, the discharge amount decreases, resulting in a decrease in productivity.

In the present invention, the density of the metal mesh filter was adjusted at the screw tip as a method for increasing the kneading effect with the screw compression ratio of the melt extruder and effectively removing the pyrolysis oxide. Conventionally, three sheets of 100 to 200 mesh filters were used overlapping, but in the present invention, three sheets of 300 to 400 mesh were inserted in front of the breaker plate. In the case of the compact filter, the kneading effect is improved by increasing the back pressure in the cylinder, and the removal of the pyrolysis material is effective, but the discharge amount is reduced and the pyrolysis is promoted more than 400 mesh.

Draft steps

In the melt spinning process, draft refers to the elongation of the yarn until the molten polymer is wound up out of the nozzle hole. That is, it can be displayed by the discharge speed / spinning speed of the molten polymer in the nozzle hole.

The present inventors have found that the draft ratio is important in continuously producing a flame retardant polyester wig yarn having a uniform fineness for a long time in the spinning process of melt spinning a flame retardant polyester resin composition to produce a wig yarn. The suitable draft ratio for producing a flame retardant polyester wig yarn is 3 to 35, more preferably 5 to 20. If the draft ratio is 3 or less, productivity is considerably reduced, and it is difficult to control thread shaking at the lower portion of the nozzle, so that there is a problem in that trimming occurs. If the draft ratio is 35 or more, the occurrence of trimming increases, the fineness unevenness problem occurs, the strength decreases significantly, and the value as a wig yarn is lost.

The invention can be better understood by the following examples, which are intended to illustrate the invention and are not intended to limit the scope of protection defined by the appended claims.

Example

Example 1-7

The blending ratio of the polyester resin, the flame retardant resin, the heat stabilizer and the process stabilizer used in the embodiment of the present invention is shown in Table 1. The polyester chip was dried at 140 ° C. for 8 hours using a vacuum dryer, and the flame retardant was dried at 90 ° C. for 5 hours and then ground. At this time, the pulverized particle size was 0.1-0.8 mm. Measured according to the mixing ratio of Table 1, put into a tumbler type stirrer and stirred for 30 minutes at 30 rpm, and then shortened it to a cylinder diameter of 50 mm with a 160-hole spinneret having an octagonal, hexagonal, pentagonal and peanut-shaped cross section. The unstretched yarn was prepared so that the monofilament fineness was 180 denier by feeding it to an extruder and spinning at a speed of 150 m / min. At this time, the cylinder temperature of the extruder was set to 270-330 ° C, the spinneret temperature to 270 ° C. The extruder screw used was a compression ratio of 5, and the filter mesh attached to the extruder tip was mounted in front of the breaker plate by overlapping three 300 meshes. The melt spinning draft ratio was set to 10 and wound up. The resulting undrawn yarn was heat-stretched at 80 ° C. at a draw ratio of 3.6 times, followed by tension heat treatment at 120 to 200 ° C. to obtain 50 denier fibers, and the physical properties thereof are shown in Table 1.

Comparative Example 1-7

The blending ratio of polyester resin, flame retardant resin, thermal stabilizer, process stabilizer, screw compression ratio of melt extruder, density of gold mesh filter, draft ratio are shown in Table 2. The polyester chip was dried at 140 ° C. for 8 hours in a vacuum dryer, and the flame retardant was dried at 90 ° C. for 5 hours. The grinding process was not carried out, and the same procedure as in Example 1 was carried out except that it was immediately added to a tumbler stirrer. The results are shown in Table 2.

The present invention melt-mixed spinning at least one polyester resin and a polymeric brominated flame retardant to produce a flame-retardant polyester wig yarn continuously without the occurrence of trimming for a long time, blending various thermoplastic polyester resins and polymeric brominated flame retardant to magnetic Has the effect of the invention to produce excellent flame retardant polyester wig yarn having digestibility and drip resistance.

In addition, the present invention in the flame retardant polyester wig yarn spinning process minimizes the amount of pyrolysis material adhered to the nozzle hole as the spinning time elapses, significantly reducing the number of times cleaning the nozzle surface to reduce the generation of waste due to cleaning to increase the yield and trimming Reduced generation of polyester wig yarn of uniform quality, and melt hole spinning of high melting point polyester resin and flame retardant resin mixed composition at melt extruder temperature of 270-350 ° C. It is possible to minimize the occurrence of trimming, and has the effect of producing a flame retardant polyester wig yarn having a vivid color, curl formation, curl retention, curl elasticity, moderate strength and elongation as a wig yarn.

Simple modifications or changes of the present invention can be easily carried out by those skilled in the art, and all such modifications or changes can be seen to be included in the scope of the present invention.

Claims (5)

60 to 90% by weight of polyester resin pulverized to 1 mm or less and 10 to 40% by weight of polymer brominated flame retardant pulverized to 1 mm or less are added to the mixture of heat stabilizer and process stabilizer at a concentration of 500 to 5,000 ppm, respectively. Preparing a composition; The composition is melt-spun into a melt extruder in which a compression ratio of the screw is in the range of 3.5 to 6.5 and a plurality of 300-400 mesh metal mesh filters are inserted into the screw tip; And Drafting the spun filaments at a draft ratio of 5 to 30 times; Method for producing a flame retardant polyester wig yarn, characterized in that the step of manufacturing. The polyester resin of claim 1, wherein the polyester resin has an intrinsic viscosity in the range of 0.6 to 1.2, polyethylene terephthalate (PET) resin, polybutylene terephthalate (PBT) resin, polypropylene terephthalate (PPT) resin, polyethylene or At least one selected from the group consisting of a phthalate (PEN) resin and a polycyclomethylene terephthalate (PCT) resin. The flame retardant resin according to claim 1, wherein the flame retardant resin has a bromine content of 50 to 70 wt% and an average molecular weight in the range of 10,000 to 120,000, and a polybromostyrene flame retardant, a polybromophenoxy flame retardant, a polybromoepoxy flame retardant, and a polybro A method for producing a flame retardant polyester wig yarn, which is selected from the group consisting of a mocarbonate flame retardant. The method for producing a flame retardant polyester wig yarn according to claim 1, wherein three metal mesh filters are inserted. A flame retardant polyester wig yarn prepared according to any one of claims 1 to 4.