KR100449383B1 - Manufacturing method of fire retardant polyester fiber having excellent mechanical properties - Google Patents

Abstract

PURPOSE: A manufacturing method of fire retardant polyester fiber having excellent mechanical properties is capable of increasing productivity, manufacturing and supplying the fiber immediately in accordance with various uses. CONSTITUTION: Fire retardant polyester is obtained by the steps of: using a dicarboxylic acid ingredient and a diol ingredient; preparing polyester copolymer added 0.6-4.0wt.% of phosphorus compound based on phosphorus; mixing the polyester copolymer and polyethylene terephthalate; and then spinning and drawing a mixture.

Description

Manufacturing method of flame retardant polyester fiber

The present invention relates to a method for producing a flame retardant polyester fiber, and more specifically to a flame retardant fiber having excellent mechanical properties by mixing and spun a polyester copolymerized by adding an excessive amount of flame retardant with pure polyethylene terephthalate (PET) It relates to a manufacturing method.

Usually polyester has excellent mechanical properties, chemical resistance, heat resistance, etc., so it is used in all fields such as fiber, film, etc., but it is inherently flammable material, so it is easy to ignite and burn.

In particular, in Europe and the United States, flame retardant standards are prescribed by law for infants and the elderly, curtains, carpets, etc., and thus, the necessity of flame retardant polyesters is urgently needed for the development of these applications.

The flame retardant method of polyester introduced so far can be divided into a method of adding a material that has a flame retardant effect during polymerization and a post-processing method of mixing a flame retardant component with a fiber emulsion. First, in the case of the post-processing method, there are economic advantages, but the surface of the product is rough and the flame retardant durability is degraded due to dropping of the flame retardant component by washing or the like. In addition, in the case of adding a flame retardant during polymerization, the flame retardant used generally has inorganic, halogen-based and phosphorus-based organic matters. Antimony trioxide is a representative example of the inorganic flame retardant component. In this case, there is a limit to use because it is not compatible with an organic polyester. Halogen-based flame retardants generate poisonous gases during coloring and thermal decomposition of polymers. Countries are restricting their use. Next, as a case of using a phosphorus-based flame retardant, it is most widely used due to the advantages of non-toxicity, durability, etc. among the methods for producing flame retardant fibers, and examples thereof include US Patent No. 3,941,752 and Japanese Patent Application No. 55-41610.

Such flame retardant polyesters are generally manufactured by copolymerization. When flame retardant yarns are manufactured by copolymerization, physical properties are degraded due to side reactions during the copolymerization reaction, resulting in poor workability during processing as well as color and mechanical properties of fibers. There are problems such as making things worse.

Therefore, in order to solve the above problems, by mixing and spinning pure polyethylene terephthalate (PET) in a polyester copolymer containing an excessive amount of a phosphorus-based flame retardant, it is easy to manufacture fibers having excellent mechanical properties and flame retardant performance of various grades. It is an object of the present invention to provide a method for producing a flame retardant polyester fiber.

The present invention is described in detail as follows.

Compared to the case of preparing a flame retardant polyester using a phosphorus compound, the color and mechanical properties of the fiber are mixed by using a method of mixing and spinning a polyester copolymer prepared by adding an excess amount of phosphorus compound and pure polyethylene terephthalate (PET). Flame retardant polyester fibers with excellent physical properties could be prepared.

At this time, the amount of phosphorus-based compound to be added is used 0.6% to 4.0% by weight based on phosphorus. If the amount of phosphorus compound is less than 0.6 wt% based on phosphorus, the improvement of color and mechanical properties after mixing spinning is insignificant. If the amount of phosphorus compound is more than 4.0 wt%, the reactivity becomes low, making it difficult to manufacture the spinning copolymer. Lose.

Flame retardancy in the case of adding the same amount of phosphorus compound remaining in the polyester fiber produced by the mixed spinning of the present invention in the conventional single spinning, and poly produced by the mixed spinning of the present invention Although the flame retardancy of the ester fiber was similar, the overall mechanical properties were superior to the polyester fiber produced by the present invention.

In addition, in the prior art, the amount of the phosphorus compound should be synthesized according to the required amount of flame retardant to synthesize the fibers, but in the present invention, the polyester copolymer with the excess phosphorus compound and pure polyethylene terephthalate (PET) may be used. By controlling the mixing ratio at the time of mixed spinning, it has the advantage of producing a flame retardant polyester fiber having various grades of flame retardancy simply as needed.

Example 1

In a stainless steel reactor equipped with a condenser and an agitator designed to reflux, dimethyl terephthalate and ethylene glycol have a molar ratio of 1: 1.5, followed by 4.0wt of phosphorus based on a polymer based on general formula (I). After the addition of%, a transesterification catalyst which is commonly used in the art to which the present invention pertains is added and heated and stirred to carry out transesterification while raising the temperature in the range of 220 ° C to 230 ° C.

Upon completion of the transesterification reaction, a polycondensation catalyst commonly used in the art to which the present invention pertains is added, and the temperature is gradually raised so that the final temperature is 265 ° C. to 285 ° C., and the pressure is gradually reduced so that the final pressure is 0.2 torr or less. The reaction was carried out for 150 minutes to obtain a polymer having an intrinsic viscosity of 0.55.

After drying the polymer and pure polyethylene terephthalate (PET), the ratio of the copolymer and the pure PET was mixed in a ratio of 1 to 7 to make a stretch yarn of 68 denier / 24 filaments according to a conventional method, and fabricated a flame retardant fabric. And other physical properties were measured. The measurement results are shown in Table 1.

Example 2 , Comparative Example 1-2

The polymers, filaments and fabrics were prepared in the same manner as in Example 1, except that the type and amount of the phosphorus compound added and the mixing ratio of the copolymer and the pure polyethylene terephthalate (PET) prepared were as shown in Table 1. Obtained, measured and evaluated the physical properties, the results are shown in Table 1.

TABLE 1

In the analysis of the polymer, the ultimate viscosity (IV) was measured by experimenting at 25 ° C. with o-chlorophenol solution to confirm the degree of polymerization, and the color was compared by measuring sulfur-blueness (b value).

The fabric is plain weave with a weight of 200g per yard. The color is measured by yellowish blue color (b-ga) and the flame retardancy is the limiting oxygen concentration according to the Limiting Oxygen Index (LOI) method indicated in ASTM D 2863-70. Was measured.

According to the present invention, it is possible to manufacture flame retardant fibers having excellent mechanical properties, and also to easily prepare fibers having various grades of flame retardant performances as necessary, thereby improving productivity in fiber manufacturing and promptly according to various uses. Has the advantage of manufacturing supply.

Claims (1)

In preparing a flame retardant polyester using a dicarboxylic acid component and a diol component, the compound is stretched and prepared by mixing and spinning pure polyester terephthalate with a polyester copolymer containing 0.6 wt% to 4.0 wt% of a phosphorus compound Method for producing a flame retardant polyester fiber characterized in that.