KR20130078537A - Low melting polyester binder resin, binder fiber and manufacturing method thereof - Google Patents
Low melting polyester binder resin, binder fiber and manufacturing method thereof Download PDFInfo
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- KR20130078537A KR20130078537A KR1020110147542A KR20110147542A KR20130078537A KR 20130078537 A KR20130078537 A KR 20130078537A KR 1020110147542 A KR1020110147542 A KR 1020110147542A KR 20110147542 A KR20110147542 A KR 20110147542A KR 20130078537 A KR20130078537 A KR 20130078537A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
- C09J167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
- C09J167/03—Polyesters derived from dicarboxylic acids and dihydroxy compounds the dicarboxylic acids and dihydroxy compounds having the carboxyl - and the hydroxy groups directly linked to aromatic rings
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/20—Presence of organic materials
- C09J2400/30—Presence of wood
- C09J2400/303—Presence of wood in the substrate
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Abstract
Description
The present invention relates to a low-melting point polyester binder resin, a binder fiber, a manufacturing method and a use thereof, and specifically, can be wet processed at a steam air temperature of 100 ° C. or less, and has excellent adhesive property. It relates to a resin, a binder fiber using the same and a method for producing the same.
In the case of traditional wood insulators and other building interior materials, dry heating type binders using wood fibers and adhesives have been commonly used. However, due to the increasing interest in environmental issues and increasing demand for stability and comfort for humans, low-melting polyester binder fibers with excellent price competitiveness and harmlessness to humans, as well as adhesive and heat resistance compared to other components, Mainly used.
However, in recent years, due to increased interest in eco-friendliness and human safety, demand for energy savings and productivity improvement, the dry heating type has been replaced to provide eco-friendly and human safety, high energy and production efficiency, and excellent price competitiveness. There has been a demand for a polyester fiber material that can be applied to steam air wet processing below 100 ° C that can realize all the properties such as adhesive strength and heat resistance of the dry heating type.
These low melting polyester binder fibers are prepared by synthesis of acid components such as terephthalic acid, isophthalic acid and aliphatic dicarboxylic acids having 30 or less carbon atoms and diol components such as diethylene glycol, tetra methylene glycol, neopentyl glycol, and polyethylene glycol. The physical properties such as melting point can be adjusted according to the type, content, etc. of the acid component and the diol component, and the properties such as workability and adhesiveness of the polyester binder fiber may be greatly influenced.
For example, US Pat. No. 4,296,475 introduced low melting point copolyesters mainly composed of terephthalic acid and isophthalic acid. However, this requires a temperature of more than 190 ° C for thermal bonding, which is uneconomical due to energy loss. Due to the nature of the heat resistance and formability is low, there is a disadvantage that easily causes thermal deformation.
In addition, the United States Patent Invention No. 44065439 introduced a low melting point polyester using terephthalic acid, isophthalic acid, adipic acid and ethylene glycol, neopentyl glycol, but the melting point is too low to 45 ~ 60 ℃ to cause strong and fusion problems There is concern.
In addition, Korean Patent Publication No. 2001-11548 uses terephthalic acid and phthalic anhydride as dicarboxylic acid components and ethylene glycol and diethylene glycol as diol components, but high temperature (270-290 ° C.), which is a general polyethylene terephthalate copolymerization condition, is used. , Pyrolysis and side reactions occur at high vacuum (less than 1torr), causing polymer color defects.
In addition, these low-melting polyester binder fibers are difficult to be wet processed by 100 ° C steam air, and their adhesive strength, heat resistance, and tear characteristics are greatly degraded during wet bonding, and their shape stability is degraded. It has a disadvantage.
Therefore, it is possible to wet process steam steam below 100 ℃ through the composition of acid component and diol component, so it is expected to save energy and improve productivity, and it is relatively harmless to the human body and has various physical properties such as adhesion, tearing property, touch, shape stability, etc. The development of low melting polyester binder fibers that can be applied to superior wood insulators and other building materials applications requires a high level of skill.
In order to solve the above problems, an object of the present invention is a polyester binder having a glass transition temperature (Tg) of 40 ° C. or higher and no melting point and a softening temperature of 100 ° C. or lower by condensing an acid component and a diol component at an extreme viscosity of 0.80 or lower. To provide a resin.
In addition, the object of the present invention is made of a polyester binder resin in the sheath-core or side-by-side type of composite fiber, excellent adhesion, heat resistance and tear characteristics, so that steam air wet processing at 100 ℃ or less It is possible to provide a low melting point polyester binder fiber with heat adhesion, heat resistance and excellent hand and shape stability after processing.
Still another object of the present invention is to provide a low melting point polyester binder fiber which can be applied for building materials, in particular, for wood insulation, in addition to adhesion between fibers, and having excellent adhesion.
In order to achieve the above object, the present invention provides 40 to 84 mol% of terephthalic acid, 15 to 40 mol% of isophthalic acid, and 1 to 20 mol% of adipic acid, and 60 to 75 mol% of ethylene glycol and 1,4-butanediol. Condensation polymerization of a diol component containing 20 to 40 mol% and 1 to 10 mol% of 1,4-cyclohexanedimethanol provides a low melting point polyester binder resin having no melting point and a softening temperature of 60 to 100 ° C.
The present invention also provides a low melting polyester binder resin having an intrinsic viscosity of 0.60 to 0.80 of the low melting polyester resin.
The present invention also provides a low melting point polyester binder fiber which is a composite fiber of sheath-core or side-by-side type including the low melting point polyester binder resin.
The present invention also provides a low melting point polyester binder fiber having a fineness of 0.3 to 15 mono denier and having a length of 1 to 100 mm.
In another aspect, the present invention provides a low-melting polyester binder fiber having a processing temperature of 80 ~ 100 ℃ by steam air (Steam Air) wet processing.
In another aspect, the present invention provides a low melting polyester binder fiber in which the polyester binder fiber is used as a building material.
In another aspect, the present invention provides a low-melting polyester binder fiber is a building material is a wooden insulation.
In addition, the present invention is a method for producing a low-melting polyester binder resin, the acid component containing 40 to 84 mol% of terephthalic acid, 15 to 40 mol% of isophthalic acid and 1 to 20 mol% of adipic acid and 60 to 75 mol of ethylene glycol % And diol components containing 20 to 40 mol% of 1,4-butanediol and 1 to 10 mol% of 1,4-cyclohexanedimethanol are mixed, and the reaction ratio of acid component to diol component is 1: 1.1 to 1: 2. Mix as much as possible Ester reactant preparation step of esterification reaction at 200 ~ 270 ℃, 700 ~ 1500 torr; To the ester reactant, 0.01 to 0.04 parts by weight of antimony trioxide and 0.001 to 0.01 part by weight of tetrabutyl titanate were added to 100 parts by weight of the ester reactant, and the temperature was gradually raised to a temperature of 250 to 300 ° C, and reduced to 0.1 to 1.0 torr Condensation polymerization step of polymerizing to form a polymer while; And a viscosity control step of terminating the reaction when the intrinsic viscosity becomes 0.60 to 0.80 while continuing the polymerization reaction of the polycondensed polymer. It provides a method for producing a low melting polyester binder resin comprising a.
In addition, the present invention is a method for producing a low-melting polyester binder fiber, the low-melting polyester binder resin produced by the method of claim 8 and the polyester resin having a melting point of 230 ~ 280 ℃ cis-core or side-by-side type The composite spinning step of spinning so as to have a fineness of 0.3-15 monodenier fibers at an area ratio of 8: 2 to 2: 8, and an elongation ratio of 2.0 to 4.5; And it provides a method for producing a low melting polyester binder fiber comprising the step of cutting the composite spun fiber to 1 ~ 100mm.
As described above, the low-melting-point polyester binder resin of the present invention has the effect of being capable of wet adhesive processing by steam air of 100 ° C. or less even at high intrinsic viscosities exceeding 0.60 equivalent to conventional resins.
In addition, the low-melting polyester binder fiber of the present invention can be bonded by fusion by steam air without using an organic solvent when used as a binder has an environmentally friendly effect, at the same time high energy saving and productivity improvement effect There is.
In addition, the low-melting polyester binder fiber of the present invention is not only capable of wet processing steam air at 100 ° C or less, 60 ~ 90 ° C but also excellent adhesiveness and heat resistance, it is also excellent in tear characteristics and toughness.
In addition, the low-melting point polyester binder fiber of the present invention can be bonded between wood fibers (Wood Fiber) in addition to the conventional fiber adhesion, it is applied as a binder for building materials, preferably wood insulation material has been developed for new uses and excellent adhesion It has the effect of providing resistance, heat resistance, toughness and form stability.
1 is a manufacturing process diagram of a low melting polyester binder fiber according to an embodiment of the present invention.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. First, it should be noted that, in the drawings, the same components or parts have the same reference numerals as much as possible. In describing the present invention, detailed descriptions of related well-known functions or configurations are omitted in order not to obscure the subject matter of the present invention.
The terms " about ", " substantially ", etc. used to the extent that they are used herein are intended to be taken to mean an approximation to or in the numerical value of the manufacturing and material tolerances inherent in the meanings mentioned, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure.
The present invention relates to a polyester binder resin and a binder fiber prepared using the same, and in particular, an acid component and ethylene glycol in the form of a dicarboxylic acid including terephthalic acid (TPA) and isophthalic acid (IPA). Diol components including (Ethylene Glycol; EG), 1,4-butanediol (BD) and 1,4-cyclohexanedimethanol are condensed, and the ultimate viscosity is 0.80 or less, more preferably 0.60 A polyester binder resin is prepared by condensation polymerization to exhibit an intrinsic viscosity of ˜0.70, and no melting point, and a softening temperature of 100 ° C. or less, more preferably 60 to 100 ° C.
In addition, the prepared polyester binder resin is made of a sheath-core (Sheath-Core) or side-by-side (Side-by-Side) composite fiber to make a uniform fiber cross-section to steam air below 100 ℃ (Steam) Wet processing is possible in the air, and it shows excellent adhesion, heat resistance, and touch, and it is excellent for wet adhesion processing by steam air below 100 ° C not only for bonding between fibers but also for bonding between wood fibers. It is a polyester binder fiber which can be applied as a binder for wood insulation.
Figure 1 shows a manufacturing process of the low melting polyester binder fiber according to an embodiment of the present invention.
The present invention comprises 40 to 84 mol% of terephthalic acid, 15 to 40 mol% of isophthalic acid and 1 to 20 mol% of adipic acid, 60 to 75 mol% of ethylene glycol, 20 to 40 mol% of 1,4-butanediol, and Condensation polymerization of the diol component containing 1 to 10 mol% of 1,4-cyclohexanedimethanol provides a low melting point polyester binder resin having no melting point and a softening temperature of 60 to 100 ° C.
Specifically, the low melting polyester binder resin of the present invention is a method for producing polyethylene terephthalate by condensation polymerization of terephthalic acid (TPA) and ethylene glycol (EG), in addition to 40 to 84 mol% of terephthalic acid as an acid component in the form of dicarboxylic acid. 15 to 40 mol% of isophthalic acid (IPA), preferably 20 to 30 mol% and 1 to 20 mol% of adipic acid (AA), preferably 5 to 15 mol%, are added as a copolymerization component of ethylene glycol ( EG) 60-75 mol%, 20-40 mol% of 1, 4- butanediol and 1-10 mol% of 1, 4- cyclohexane dimethanol are added as a copolymerization component of a diol component, and reaction ratio of a dicarboxylic acid component and a diol component is carried out. 1 to 1.1 to 1.2 Prepare an ester reactant which is esterified at 200-270 ° C. and 700-1500 Torr. (S100 step)
0.01 to 0.04 parts by weight of antimony trioxide and 0.001 to 0.01 parts by weight of tetrabutyl titanate were added to the prepared ester reactant, and the temperature was gradually raised to a temperature of 250 to 300 ° C., preferably 0.1 to 1.0 Torr. The polymerization reaction was carried out to form a polymer with a reduced pressure of 0.5 Torr (S200), and then the polymerization reaction of the polycondensation polymer was continued, and the ultimate viscosity was 0.60 to 0.70. When the reaction is terminated by adjusting the viscosity (step S300), the low melting point polyester binder resin of the present invention can be prepared.
Antimony trioxide and tetrabutal titanate used in the present invention are catalysts which are added to increase the reactivity of the copolymerization components of the present invention and to adjust the viscosity required. Therefore, when the temperature, pressure and catalyst content of the present invention is less than the above range, the polymerization of each reactant does not occur smoothly, polymer formation is difficult and there is a fear that the viscosity of the formed polymer (Polymer) is too low. In addition, the overall physical properties of the polymer thus formed is deteriorated so that the function of the general polymer can not be exhibited. If the above range is exceeded, a side reaction may occur due to a sudden increase in the reaction rate, polymer color defects, and gelation of the polymer inside the reaction tube are expected.
Isophthalic acid (IPA) used in the present invention is used to lower the melting point of the polyester to form low melting point polyester.
The content of isophthalic acid may be used in 15 ~ 40mol%, if the content is used in less than 15mol% adhesive processing in steam air below 100 ℃, preferably 60 ~ 90 ℃ required by the present invention It is difficult to have this possible low melting point function, and when used in excess of 40 mol% acts as a factor in lowering the adhesive strength, as is generally known, no further melting point lowering effect appears.
In addition, adipic acid (AA) added as another acid component increases the fluidity of the entire molecular chain of the copolyester, is included as a diol component, and has a high surface area due to its molecular structure when processing steam air. It is easy to bond between fibers or wood by (Steam Air), can maintain high adhesive strength, and improve the tearing property at the time of binding by securing the ductility of the molecular chain. The content of such adipic acid (AA) may be used in a range of 1 to 20 mol%. If the content is less than 1 mol%, the desired melting point decreases and the flexibility of the polyester may not be obtained. The glass transition temperature is too low to obtain a glass transition temperature of 40 ℃ or more there is a limit to use as a low-melting polyester having a heat resistance.
Meanwhile, 1,4-butanediol (BD), which is used as the diol component of the present invention, lowers the melting point of the polyester and is advantageous for forming a low melting point polyester, and has excellent molecular chain fluidity and molding processability, as well as steam. When air processing (Steam Air), the heat adhesion surface area is high can have excellent adhesion. It is preferable that the content of 1,4-butanediol is 20 to 40 mol%. If the content of 1,4-butanediol is less than 20 mol%, a low melting point polyester having excellent desired moldability may not be obtained, and more than 40 mol%. If there is a large amount of tetrahydrofuran (THF) during the polycondensation reaction, there is a fear that the thermal stability and operating efficiency when spinning.
In addition, 1 to 10 mol% of 1,4-cyclohexanedimethanol is included as a diol component, but less than 1 mol% of 1,4-cyclohexanedimethanol does not show a desired glass transition temperature improvement effect, and 10 mol% If exceeded, the glass transition temperature improvement effect is high, but wet processing is difficult or the problem that the adhesive strength is impaired after wet processing occurs.
The low-melting polyester resin of the present invention may be provided with a binder fiber capable of wet air processing of steam air (100 ° C or less, preferably 60 ° C to 90 ° C) of which the ultimate viscosity is 0.60 to 0.80. . If the intrinsic viscosity is less than 0.60, the target adhesive strength after the 100 ° C steam air bonding process can not be secured, and in the range of the intrinsic viscosity greater than 0.80, it is difficult to secure the radiation stability.
However, the present invention overcomes the problems of low adhesion, heat resistance and shape stability, toughness of the binder resin caused by the low limit viscosity as well as the control of the limit viscosity 0.8 or less, preferably 0.60 ~ 0.80 to overcome this problem. In the present invention, a low melting point polyester binder resin is prepared by adding adipic acid (AA) to the acid component and 1,4-butanediol (BD) to the diol component during polyester copolymerization.
Accordingly, the low melting polyester binder resin thus prepared has no melting point and exhibits a softening temperature of 60 to 100 ° C., and this feature enables wet processability even in steam air of 100 ° C. or less, and provides excellent adhesion and tear characteristics. to provide.
In another embodiment, the present invention provides a low melting point polyester binder fiber which is a composite fiber of a sheath-core or side-by-side type including the low melting point polyester binder resin.
Referring to Figure 1, the low melting point polyester binder fiber of the present invention is a composite spinning in a low melting point polyester binder resin prepared through the ester reactant preparation step (S100), condensation polymerization step (S200), viscosity control step (S300) Step (S500), may be manufactured to further include a cutting step (S600).
In the method for producing a low melting polyester binder fiber of the present invention, a low melting polyester binder resin prepared in the above method and a polyester resin having a melting point of 230 to 280 ° C. have a cis-core or side-by-side type with an area ratio of 8: 2. It includes a composite spinning step (S500) to spin the fibers so that the fineness of 0.3 to 15 monodenier at ~ 2: 8, the draw ratio 2.0 to 4.5 (S600); and cutting the composite spun fibers to 1 ~ 100mm (S600);
Specifically, the low-melting polyester binder fiber of the present invention comprises a sheath portion of the low-melting-point polyester binder resin prepared by the method described above, and a general polyester resin having a melting point of 230 to 280 ° C. as a core portion. : Core = 8: 2-2: 8, Preferably the composite spinning at 6: 4-4: 6 can improve adhesiveness and a touch. In addition, a draw ratio of 1.0 to 4.5, preferably 2.5 to 4.0, can provide spin stability so that the fibers are not cut. In addition, adjusting the fineness to be 0.3 to 15 deniers (De), preferably 2 to 6 deniers and 1 to 100 mm in length, can improve adhesiveness and feel.
The low melting polyester binder fiber of the present invention prepared as described above is characterized in that wet processing by steam air below 100 ° C is possible. Accordingly, the low melting point polyester binder fiber of the present invention is wet even at low steam air temperature of 100 ° C. or less, while the conventional binder fiber is thermally bonded by a dry heating method exceeding 100 ° C. Thermal bonding is possible, so that high energy savings and productivity can be ensured, resulting in a highly stable work environment. In addition, even when wet adhesion by steam air (adhesion) it is possible to maintain the adhesion and tear characteristics, excellent touch and shape stability.
Due to these characteristics, the low melting point polyester binder fiber of the present invention is not only used for bonding between existing fibers but also used as a polyester binder for building materials, in particular, a binder for wood insulation, and thus exhibits excellent adhesion. Applicable to the application.
Hereinafter, the present invention will be described in more detail.
Example One
Low melting point Preparation of Polyester Binder Resin
Terephthalic acid (TPA) / isophthalic acid (IPA) / adipic acid (AA) (60/25/15, mol%) as acid component and ethylene glycol (EG) / 1,4-butanediol (BD) / 1 as diol component , 4-cyclohexanedimethanol (CHDM) (65/30/5, mol%) was adjusted to the reaction ratio of the acid component and the diol component 1: 1.1, and esterified by esterification at 250 ° C. under 1140 Torr pressure. Formation was obtained and the reaction rate was 97.5%. The formed ester reactant was transferred to a polycondensation reactor, and 0.02 parts by weight of antimony trioxide and 0.005 parts by weight of tetrabuttal titanate were added to 100 parts by weight of the ester reactant, and the temperature was raised to 280 ° C. while gradually depressurizing to a final pressure of 0.5 Torr. The polycondensation reaction was carried out until 0.65.
Low melting point Preparation of Polyester Binder Fiber
The low melting polyester binder resin prepared as described above was used as a sheath component, and the core component was a mono 4 having an area ratio of 6: 4 and an elongation ratio of 3.5 using a conventional polyethylene terephthalic acid chip (melting point of 260 ° C.). Spinning with denia to prepare a low-melting polyester binder fiber made of a composite fiber having a fiber length of 6mm.
Physical properties of the binder resin and the fiber prepared as described above are shown in Table 2 below.
Example 2
The acid component is terephthalic acid (TPA) / isophthalic acid (IPA) / adipic acid (AA) (60/30/10, mol%) and the diol component is ethylene glycol (EG) / 1,4-butanediol (BD) / 1 , 4-cyclohexanedimethanol (CHDM) (60/30/10, mol%), and the reaction was carried out in the same manner as in Example 1 except that the reaction was carried out to an intrinsic viscosity of 0.67.
Example 3
The acid component is terephthalic acid (TPA) / isophthalic acid (IPA) / adipic acid (AA) (84/15/1, mol%) and the diol component is ethylene glycol (EG) / 1,4-butanediol (BD) / 1 , 4-cyclohexanedimethanol (CHDM) (70/20/10, mol%), and the reaction was carried out in the same manner as in Example 1 except that the reaction was carried out to an intrinsic viscosity of 0.68.
Comparative example One
Except that the acid component was adjusted to terephthalic acid (TPA) / isophthalic acid (IPA) (60/40, mol%) and the diol component with ethylene glycol (EG) (100 mol%) and reacted to an intrinsic viscosity of 0.65. It carried out similarly to Example 1.
Comparative example 2
The acid component is terephthalic acid (TPA) / isophthalic acid (IPA) / adipic acid (AA) (30/50/20, mol%) and the diol component is ethylene glycol (EG) / 1,4-butanediol (BD) (50 / 50, mol%), and the reaction was carried out in the same manner as in Example 1 except that the reaction was carried out so that the intrinsic viscosity was 0.64.
Comparative example 3
The acid component is adjusted to terephthalic acid (TPA) / isophthalic acid (IPA) (50/50, mol%) and the diol component to ethylene glycol (EG) / 1,4-butanediol (75/25, mol%) and the ultimate viscosity It carried out similarly to Example 1 except having reacted so that it may become 0.67.
Table 1 below shows copolymer composition ratios and intrinsic viscosities of polyester binder resins of Examples and Comparative Examples.
division
Extreme viscosity
※Test Methods
1.Measurement of mol% of copolymerization component
Low-melting-point poly mol% of a copolymer component to be added for the production of the binder resin is an ester of chloroform and trifluoroacetic acid (4: 1) was dissolved in a mixed solvent of a Bruker (Bruker)'s Proton nuclear magnetic resonance spectrometer (1 H- NMR, model name: AMX-300).
2. Extreme Viscosity (IV) Measurement
The copolyester prepared in Examples and Comparative Examples was melted in an Ortho-Chloro Phenol solvent at a concentration of 2.0 g / 25 ml at 110 ° C. for 30 minutes, and then incubated at 25 ° C. for 30 minutes. Measurements were made using an automatic viscometer connected to a Canon Viscometer.
3. Melting point, glass transition temperature and softening behavior
The temperature difference was measured at 20 ℃ / min using a thermal differential scanning calorimeter (Perkin Elmer, DSC-7), and the softening behavior was measured using a dynamic thermal measuring instrument (Perkin Elmer, TMA-7) if no melting point was present. Measured.
4. Adhesive Evaluation
The prepared binder fiber was cut into 6 mm fiber sheets, mixed with wood insulation materials, and subjected to workability evaluation by wet bonding under steam air conditions at 90 to 100 ° C./60 seconds. : Excellent, (triangle | delta): Normal, x: It evaluated as poor.
5. Tactile Evaluation
Sensory evaluation was conducted by comparing internal touch with internal touches, and evaluated as ◎: very good, ○: excellent, △: normal, and ×: poor.
Table 2 below shows the thermal characteristics and functional evaluation of the Examples and Comparative Examples.
(℃)
Looking at the results of Table 2, it was confirmed that the low melting point polyester resin of the present invention was measured at a softening temperature of 60 ~ 100 ℃, excellent molding processability even at low temperature below 100 ℃.
In addition, it was confirmed that the low-melting-point polyester binder fiber of the present invention can be applied to new applications, such as wood insulation, especially for building materials, in view of the excellent adhesion to wood insulation in the adhesive evaluation.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. It will be clear to those who have knowledge of.
Claims (9)
The low melting point polyester resin is a low melting point polyester binder resin having an ultimate viscosity of 0.60 ~ 0.80.
The low melting polyester binder fiber is 0.3-15 mono fineness, low melting point polyester binder fiber having a length of 1 to 100mm.
The low melting polyester binder fiber is a low melting point polyester binder fiber having a processing temperature of 80 ~ 100 ℃ by steam air (Steam Air) wet processing.
The low melting polyester binder fiber is a low melting polyester binder fiber used as a building material.
The building material is a low-melting polyester binder fiber is a wood insulation.
Acid components containing 40 to 84 mol% of terephthalic acid, 15 to 40 mol% of isophthalic acid and 1 to 20 mol% of adipic acid, and 60 to 75 mol% of ethylene glycol and 20 to 40 mol% of 1,4-butanediol and 1,4 -Mix the diol component containing 1 ~ 10 mol% cyclohexane dimethanol, and mix so that the reaction ratio of acid component and diol component 1: 1.1 ~ 1: 2 Ester reactant preparation step of esterification reaction at 200 ~ 270 ℃, 700 ~ 1500 torr;
To the ester reactant, 0.01 to 0.04 parts by weight of antimony trioxide and 0.001 to 0.01 part by weight of tetrabutyl titanate were added to 100 parts by weight of the ester reactant. Condensation polymerization step of polymerizing to form a polymer while; And
A viscosity control step of terminating the reaction when the intrinsic viscosity becomes 0.60 to 0.80 while continuing the polymerization reaction of the polycondensed polymer;
Method for producing a low melting polyester binder resin comprising a.
The low melting point polyester binder resin prepared by the method of claim 8 and the polyester resin having a melting point of 230 to 280 ° C. have a sheath-core or side-by-side type, and have fineness at an area ratio of 8: 2 to 2: 8 and an extension ratio of 2.0 to 4.5. Composite spinning step to spin to 0.3 to 15 mono denier fibers; And
Cutting the composite spun fibers to 1 ~ 100mm
Method for producing a low melting polyester binder fiber comprising a.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190013234A (en) * | 2017-08-01 | 2019-02-11 | 주식회사 휴비스 | Crystalline low melting Polyester binder resin with improved heat resistance |
| CN113957563A (en) * | 2021-12-10 | 2022-01-21 | 扬州富威尔复合材料有限公司 | Low-melt-viscosity low-melting-point polyester fiber and preparation method and application thereof |
| KR20220059050A (en) * | 2020-11-02 | 2022-05-10 | 윤준혁 | Apparatus and method of manufacturing emulsion for LMF, and emulsion for LMF manufactured thereby |
-
2011
- 2011-12-30 KR KR1020110147542A patent/KR20130078537A/en not_active Application Discontinuation
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190013234A (en) * | 2017-08-01 | 2019-02-11 | 주식회사 휴비스 | Crystalline low melting Polyester binder resin with improved heat resistance |
| KR20220059050A (en) * | 2020-11-02 | 2022-05-10 | 윤준혁 | Apparatus and method of manufacturing emulsion for LMF, and emulsion for LMF manufactured thereby |
| CN113957563A (en) * | 2021-12-10 | 2022-01-21 | 扬州富威尔复合材料有限公司 | Low-melt-viscosity low-melting-point polyester fiber and preparation method and application thereof |
| CN113957563B (en) * | 2021-12-10 | 2023-08-29 | 扬州富威尔复合材料有限公司 | Low-melt-viscosity low-melting-point polyester fiber and preparation method and application thereof |
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