CN106702525A - Material for producing fibers and fibers produced therefrom - Google Patents

Abstract

A material for producing fibers comprises a copolyester, an inorganic additive and a non-aromatic organic additive. The copolyester is composed of hard segment molecules and soft segment molecules, wherein the hard segment molecules are mainly composed of polybutylene terephthalate, and the soft segment molecules are mainly composed of polyethylene glycol. The non-aromatic organic additive has a melting point between the crystallization temperature of the hard segment molecules and the melting temperature of the soft segment molecules, and the molecular weight of the organic additive is not more than 1000. The material for producing the fiber can simultaneously improve the strength and the bidirectional temperature regulating capability of the subsequently produced fiber.

Description

Materials for the production of fibers and fibers obtained therefrom

technical field

The invention relates to a material for producing fibers, in particular to a material for producing fibers with two-way temperature regulation function.

Background technique

With the advancement of textile technology, various fabrics with different properties have appeared on the market, especially fabrics with high fiber strength and two-way temperature adjustment function, which have become a hot development direction of the textile industry.

CN 102505179A discloses that during the spinning process, polyethylene glycol acrylate (phase-change monomer) is grafted onto the polymer to prepare fibers with a temperature-regulating function, but it cannot be improved during the spinning process. The added amount of the phase change monomer is low, so the temperature adjustment effect of the subsequent obtained fiber is not obvious.

The document "Acta Polymerica, vol.41, p31-36, 1990" discloses a copolyester composed of polybutylene terephthalate (polybutylene terephthalate, PBT for short) and polyethylene glycol (polyethylene glycol, PEG for short). (PBT-PEG copolyester) is used as a material for producing fibers, and the strength of the obtained fibers is improved by increasing the crimping speed of the spinning process, but the fibers obtained by this method do not have the effect of temperature regulation , and when the PEG content in the PBT-PEG copolyester is greater than 34wt% (based on the total weight of the copolyester as 100wt%), the fiber strength cannot be effectively improved.

US 4401792 discloses that the crystallization rate of copolyester can be increased by adding alkali metal benzoic acid salt or ionic polyethylene sodium salt crystallization nucleating agent, but does not mention how to increase the heat enthalpy to enhance the temperature adjustment ability of the material.

The document "Synthetic Fiber Industry, vol.27(2), p25-26, 2004" reveals that polypropylene (PP) is used as a crystallization nucleating agent and added to PBT-PEG copolyester to improve the subsequent However, due to the high molecular weight of polypropylene and the poor dispersion uniformity after mixing with PBT-PEG copolyester, it cannot provide an effective crystallization nucleation surface for the PBT segment at high temperature (that is, the crystallization temperature of the PBT segment and crystallinity cannot be improved), and then the strength of the obtained fiber cannot be effectively improved.

CN 1051115C discloses a core-sheath fiber with two-way temperature regulation function and uses a thermoplastic polymer with a low melting temperature (20-40°C) as a phase change material. Anti-crystallization agent to prevent the phenomenon of overheating melting or supercooling crystallization of the phase change material, so as to achieve better temperature adjustment effect. However, the types and addition ratios of part of the anti-superheating melting agent and the anti-supercooling crystallization agent disclosed in this patent (for example, only adding a single anti-superheating melting agent and anti-supercooling crystallization agent, or adding a phenyl-containing anti-superheating melting agent and anti-supercooled crystallization agent), after experiments, it was found that it could not effectively improve the two-way temperature regulation ability as expected.

Therefore, how to find a material that can be used to produce fibers, which can effectively improve the strength and bidirectional temperature adjustment ability of the subsequent fibers, has become the goal of current research.

Contents of the invention

The first object of the present invention is to provide a material for producing fibers, which can effectively improve the strength and bidirectional temperature regulation ability of the subsequently produced fibers at the same time.

Therefore, the material used in the present invention for producing fibers includes copolyester, inorganic additives and non-aromatic organic additives.

The copolyester is composed of hard segment molecules and soft segment molecules, wherein the hard segment molecules are mainly composed of polybutylene terephthalate (PBT), and the soft segment molecules are mainly composed of polyethylene glycol (PEG), and the weight average molecular weight of the soft segment molecule is between 2500 and 10000;

The non-aromatic organic additive has a melting point between the crystallization temperature of the hard segment molecule and the melting temperature of the soft segment molecule, and the molecular weight of the non-aromatic organic additive is not greater than 1000;

Based on 100 parts by weight of the total weight of the copolyester, the content of the inorganic additive ranges from 0.02 to 1.00 parts by weight, and the content of the non-aromatic organic additive ranges from 0.02 to 1.00 parts by weight.

The first object of the present invention is to provide a fiber produced from the aforementioned materials for producing fiber by a melt spinning machine.

The beneficial effects of the present invention are: since the material used for producing fibers in the present invention contains both the inorganic additive and the non-aromatic organic additive with a molecular weight not greater than 1000, and the melting point of the non-aromatic organic additive is between the hard The crystallization temperature of the segment molecule is between the melting temperature of the soft segment molecule, so that the material used in the production of the fiber of the present invention can effectively improve the strength and bidirectional temperature adjustment ability of the subsequent obtained fiber.

The principle of the aforementioned effects will be described in detail below:

(1) It should be explained first that the crystallization mechanism of copolyesters generally composed of hard segment molecules (mainly composed of PBT) and soft segment molecules (which produce phase change parts, mainly composed of PEG) is: when the copolyester When the polyester gradually cools down from the molten state to the crystallization temperature of the hard segment molecules, the hard segment molecules will be randomly collided by thermal disturbances to form a stable crystallization nucleus. When the hard segment molecules grow to crystals of a certain size At the same time, the soft segment molecules will be excluded from the crystallization region of the hard segment molecules, and when the copolyester continues to cool down to the crystallization temperature of the soft segment molecules, the soft segment molecules will follow the hard segment A crystal of the molecule begins to crystallize.

In the present invention, in the process of gradually cooling down the copolyester from the molten state, the inorganic additive can be used as a crystallization nucleating agent for the hard segment molecule, and the non-aromatic organic additive can be used in the crystallization process of the hard segment molecule It can also produce a lubricating effect between molecules, and then can improve the crystallinity of the hard segment molecules (that is, it can increase the crystallization enthalpy of the hard segment molecules), so that the material used to produce fibers in the present invention can improve the strength of the subsequent fibers .

In addition, when the copolyester continues to cool down to the crystallization temperature of the soft segment molecule, since the non-aromatic organic additive will first crystallize before reaching the crystallization temperature of the soft segment molecule, the non-aromatic organic additive Can be used as the crystallization nucleating agent of the soft segment molecule, and then can improve the crystallinity of the soft segment molecule [that is, it can increase the melting enthalpy of the soft segment molecule (i.e. the phase change enthalpy)], and reduce the melting temperature of the soft segment molecule The difference (ΔT) from the crystallization temperature enables the material used in the production of fibers in the present invention to simultaneously improve the bidirectional temperature regulation ability of the subsequently produced fibers.

(2) Since the molecular weight of the non-aromatic organic additive of the present invention is less than 1000, it is not easy to have uneven mixing after mixing with the copolyester, so that it can be more effective in the crystallization process of the hard segment molecules The lubricating effect between the molecules can further increase the crystallinity of the hard segment molecules (that is, the crystallization enthalpy), so that the material used in the production of fibers according to the present invention can further increase the strength of the subsequent fibers.

The content of the present invention will be described in detail below:

[copolyester]

The copolyester used in the material for producing fibers of the present invention is composed of hard segment molecules and soft segment molecules.

Preferably, based on the total weight of the copolyester as 100wt%, the proportion of the soft segment molecules is 30-80wt%. When the proportion of the soft segment molecule is less than 30wt%, the temperature adjustment ability of the fiber obtained subsequently is low; when the proportion of the soft segment molecule is greater than 80wt%, the melt strength of the copolyester is low , and then in the spinning process, it is less easy to form filaments (that is, it is easier to break filaments). More preferably, based on the total weight of the copolyester as 100wt%, the proportion of the soft segment molecules is 45-65wt%.

The weight average molecular weight of the soft segment molecule is between 2500-10000. When the weight-average molecular weight of the soft segment molecule is less than 2500, the melting point and phase change temperature are relatively low, which cannot effectively improve the temperature-regulating ability of the subsequent fibers, and is not suitable for the applicable temperature range of general temperature-regulating fabrics; when the soft segment When the weight-average molecular weight of the molecule is greater than 10,000, the melting and crystallization temperature of the soft segment molecule will be too high, and the high-temperature adjustable temperature of the subsequent fiber will be too high, so it is not suitable for fabrics. Preferably, the weight average molecular weight of the soft segment molecules is between 3000-9000. More preferably, the weight average molecular weight of the soft segment molecules is between 3400-8000. In a specific embodiment of the present invention, the weight average molecular weight of the soft segment molecule is 4000.

The hard segment molecule is mainly composed of polybutylene terephthalate. Preferably, in addition to polybutylene terephthalate, the hard segment molecule may also contain other polyesters, such as but not limited to polyethylene terephthalate (PET for short) and Polytrimethylene terephthalate (PTT for short). In a specific embodiment of the present invention, the hard segment molecule is composed of polybutylene terephthalate.

The soft segment molecule is mainly composed of polyethylene glycol. Preferably, besides polyethylene glycol, the soft segment molecule may further contain other polyethers, such as but not limited to polypropylene glycol (PPG). In a specific embodiment of the present invention, the soft segment molecule is composed of polyethylene glycol.

Preferably, the crystallization enthalpy of the hard segment molecule is not less than 20 J/g, the crystallization temperature range of the hard segment molecule is 160-200°C, the melting enthalpy of the soft segment molecule is not less than 40 J/g, the soft segment molecule The melting temperature range of the segment molecule is 20-50°C, and the difference (ΔT) between the melting temperature and the crystallization temperature of the soft segment molecule is not greater than 20°C.

[Inorganic additives]

Preferably, the inorganic additive is at least one selected from the group consisting of talc, mica, zinc oxide, calcium oxide, titanium dioxide, silicon dioxide, calcium carbonate, barium sulfate and magnesium oxide. In a specific embodiment of the present invention, the inorganic additive is talcum powder or titanium dioxide.

In the material for producing fibers of the present invention, based on 100 parts by weight of the copolyester, the content of the inorganic additive is in the range of 0.02-1.00 parts by weight. When the content of the inorganic additive is greater than 1.00 parts by weight, the strength of the fiber obtained subsequently is low, and it is less likely to form filaments (that is, easier to break filaments) during the melt spinning process.

[Non-aromatic organic additives]

Preferably, the non-aromatic organic additive is selected from the group consisting of C ₁₃ -C ₂₈ straight-chain aliphatic hydrocarbons, C ₁₃ -C ₂₈ straight-chain aliphatic hydrocarbon esters, and C ₁₃ -C ₂₈ straight-chain fatty acids or their salts at least one of the group. More preferably, the non-aromatic organic additive is at least one selected from the group consisting of stearic acid or its salt, and tridecylmethacrylate. In a specific embodiment of the present invention, the non-aromatic organic additive is tridecyl methacrylate, stearic acid (stearic acid, referred to as St), manganese stearate [manganese (II) stearate, referred to as MnSt ], zinc stearate (ZnSt for short) or calcium stearate (CaSt for short).

Preferably, the melting point of the non-aromatic organic additive is between 50°C and 168°C. More preferably, the melting point of the non-aromatic organic additive is between 55°C and 160°C.

In the material for producing fibers of the present invention, based on 100 parts by weight of the copolyester, the content of the non-aromatic organic additive is in the range of 0.02-1 part by weight. When the content of the non-aromatic organic additive is greater than 1 part by weight, there will be disadvantages of smoke and odor during the subsequent process of making fibers by melt spinning.

[Materials used to produce fibers]

Preferably, the material used for producing fibers of the present invention may also contain other additives, such as but not limited to dyes, ultraviolet absorbers, flame retardants, fluorescent whitening agents, matting agents, antistatic agents or antibacterial agents.

[fiber]

The fiber of the invention has both high fiber strength and high bidirectional temperature regulation ability.

Preferably, the fiber of the present invention is composite fiber (composite fiber), the material that can be used for making this fiber is such as but not limited to polyester (pplyester), polyamide (polyamide), polyolefin (polyolefin) and polyurethane (polyurethane), and wherein at least one component is formed from the material for producing fibers of the present invention.

The fiber of the present invention can be any type of fiber, such as but not limited to sheath-core composite fiber, side by side composite fiber and sea-island composite fiber, Preferably, the fiber of the present invention is a sheath-core composite fiber, and the core layer of the sheath-core composite fiber is formed from the material for producing the fiber of the present invention.

detailed description

The present invention will be further described with reference to the following examples, but it should be understood that these examples are for illustrative purposes only and should not be construed as limitations on the implementation of the present invention.

<chemicals>

Table 1

<Measurement method of relative viscosity (Rv)>

First take 0.1g of the sample to be tested and dissolve it in 25mL of phenol/tetrachloroethane mixed solvent [3/2(v/v)], then heat it at 110°C to dissolve, then cool down to 30°C, and use Ubbelohde viscometer (Ubbelohde viscometer) ) to test the relative viscosity (Rv). It should be noted that the relative viscosity of the material used for producing fibers generally suitable for melt spinning should be between 2.6 and 3.5.

<Examples 1 to 16>

Preparation of materials for fiber production

The materials used to produce fibers in Examples 1 to 16 are based on the type and amount of inorganic additives and organic additives selected in Table 2 (based on the total weight of PBT-PEG copolyester as 100 parts by weight) and polyethylene glycol The weight average molecular weight of , and prepared according to the following steps:

Table 2

Step (1): 195.2g of dimethyl terephthalate, 138.3g of 1,4-butanediol, 285.0g of polyethylene glycol, inorganic additives and organic additives were added to a batch reactor to obtain a reaction mixture .

Step (2): First heat the reaction mixture obtained in step (1) to 155°C, wait until it is completely melted, then add 1000ppm titanium isopropoxide for esterification reaction until the amount of methanol distilled reaches 64.34g, and then obtain a polymerization precursor things.

Step (3): After adding 1000ppm of titanium isopropoxide to the polymerization precursor obtained in step (2), the polymerization reaction was carried out at 250°C in a vacuum environment until the relative viscosity (Rv) ranged from 2.6 to 3.5 (relative viscosity test The method is as described above), that is, the material for producing fibers (containing PBT-PEG copolyester; granular), wherein, based on the total weight of the PBT-PEG copolyester as 100wt%, the The proportion of soft segment molecule (PEG) is 57wt%.

<Comparative Examples 1-7, 9-13>

Preparation of materials for fiber production

The preparation method of the material (containing PBT-PEG copolyester) that is used to produce the fiber of comparative example 1～7,9～13 is similar to embodiment 1, and its difference is that comparative example 1～7,9～13 is based on Table 3 selects the type and amount of inorganic additives and organic additives (the amount added is based on the total weight of the PBT-PEG copolyester being 100 parts by weight) and the weight average molecular weight of polyethylene glycol.

table 3

<Comparative example 8>

Preparation of materials for fiber production

The material that is used to produce the fiber of comparative example 8 is to select the type and the addition amount of the inorganic additive, the addition amount of the organic additive (polypropylene) according to the above table 3 (with the total weight of PBT-PEG copolyester as 100 parts by weight ) and the weight average molecular weight of polyethylene glycol, and prepared according to the following steps:

Step (1): Mix 195.2g dimethyl terephthalate, 138.3g 1,4-butanediol, 285.0g polyethylene glycol, and inorganic additives, and prepare PBT-PEG copolyester by the above polymerization method. Step (2): Place the copolyester and polypropylene (PP) of the step (1) in the main feeding tank of the twin-screw extruder, extrude into bundles after melt mixing, and then granulate Cut into pellets by machine to obtain the material (containing PBT-PEG copolyester) for producing fibers.

<Comparative Example 14>

Preparation of materials for fiber production

The preparation method of Comparative Example 14 is similar to Comparative Example 1, and its difference is that Comparative Example 14 is to replace the polyethylene glycol of Comparative Example 1 with polytetramethylene ether glycol (PTMEG2000; weight average molecular weight is 2000) as the soft segment molecular.

<Comparative Examples 15-18>

Preparation of material for fiber production (copolyester is PET-PEG)

The materials used to produce fibers in Comparative Examples 15-18 are to select the type and amount of inorganic additives, organic additives (based on the total weight of PET-PEG copolyester as 100 parts by weight) and polyethylene glycol according to Table 4. The weight average molecular weight of , and prepared according to the following steps:

Table 4

Step (1): 221.6g of dimethyl terephthalate, 108.8g of 1,2-ethylene glycol, 285.0g of polyethylene glycol, inorganic additives and organic additives were added to a batch reactor to obtain a reaction mixture .

Step (2): First heat the reaction mixture obtained in step (1) to 155°C, wait until it is completely melted, then add 1000ppm titanium isopropoxide for esterification reaction until the amount of methanol distilled reaches 73.13g, and then obtain a polymerization precursor things.

Step (3): After adding 1000ppm of titanium isopropoxide to the polymerization precursor obtained in step (2), the polymerization reaction was carried out at 250°C in a vacuum environment until the relative viscosity (Rv) ranged from 2.6 to 3.5 (relative viscosity test The method is as described above), that is, the material for producing fibers (copolyester is PET-PEG; granular), wherein, based on the total weight of the PET-PEG copolyester as 100wt%, the The proportion of soft segment molecule (PEG) is 57wt%.

<Application example 1>

Preparation of composite fiber (core: the material of Example 2; sheath: PET)

The material used to produce fibers in Example 2 and polyethylene terephthalate [PET; Rv is 1.60 to 1.75] were respectively placed in two extruders (extruders) of a melt spinning machine. Spun to obtain a sheath-core composite fiber, wherein the core layer of the composite fiber is Example 2, the sheath layer is PET, and the weight ratio of the material of Example 2 to PET is 1:1.

<Comparative application example 1>

Preparation of composite fiber (core: the material of Comparative Example 1; sheath: PET)

The preparation method of comparative application example 1 is similar to application example 1, and its difference is that comparative application example 1 is to select the material for producing fiber of comparative example 1 as the core layer, the sheath layer is PET, and the material of comparative example 1 is the same as The weight ratio of PET is 1:1.

<Comparative application example 2>

Preparation of composite fiber (core: material of Comparative Example 12; sheath: PET)

The preparation method of comparative application example 2 is similar to application example 1, and its difference is that comparative application example 2 selects the material used for producing fibers of comparative example 12 as the core layer, the sheath layer is PET, and the material of comparative example 12 and The weight ratio of PET is 1:1.

<Application example 2>

Preparation of non-woven fabric (prepared using the composite fiber of Application Example 1)

The composite fiber obtained in Application Example 1 was made into a nonwoven fabric with a basis weight of 500 g/m ² .

<Comparative application example 3>

Preparation of nonwoven fabric (prepared using the composite fiber of Comparative Application Example 1)

The composite fiber obtained in Comparative Application Example 1 was made into a nonwoven fabric with a basis weight of 500 g/m ² .

<Testing methods for thermal properties of materials used to produce fibers, composite fibers or nonwoven fabrics>

(a) The crystallization temperature (Tc) of the hard segment molecule and the soft segment molecule and the melting temperature (Tm) of the soft segment molecule:

The sample of the material (or composite fiber, non-woven fabric) to be tested for the production of fibers is measured by a differential scanning calorimeter (DSC for short, manufactured by TA Instrument Company of the United States, model DSC 2910) to measure its hard segment molecules and the crystallization temperature of the soft segment molecules, and the melting temperature of the soft segment molecules. The measurement method refers to the operation manual of the DSC, and the following steps are followed in sequence: the sample is in the range of -80°C to 250°C, and the temperature of the hard segment molecule and the soft segment molecule is measured at a heating rate of 10°C/min. Melting peak (ie, melting temperature) and crystallization peak (ie, crystallization temperature).

(b) Melting enthalpy of soft segment molecules and crystallization enthalpy of hard segment molecules:

The melting peak of the soft segment molecule and the crystallization peak of the hard segment molecule obtained in (a) are respectively integrated and calculated by using a DSC instrument, and the obtained melting peak area and crystallization peak area are respectively the melting enthalpy and the crystallization peak area of the soft segment molecule. The crystallization enthalpy of the hard segment molecule.

(c) The difference between the melting temperature and the crystallization temperature (ΔT) of the soft segment molecule:

The melting temperature and crystallization temperature of the soft segment molecule obtained in (a) above are calculated using the following formula I to calculate the difference (ΔT) between the melting temperature and the crystallization temperature of the soft segment molecule.

Formula I:

ΔT (°C) = melting temperature of soft segment molecules - crystallization temperature of soft segment molecules

<Comparison and Discussion of Thermal Properties of Examples 1-16 and Comparative Examples 1-18>

(a) Thermal property data of Examples 1-16:

For the materials used to produce fibers in Examples 1-16, the various thermal property data measured according to the aforementioned test method are shown in Table 5 below:

table 5

It can be seen from Table 5 above that the melting temperatures of the soft segment molecules (PEG) measured in Examples 1-16 are all in the range of 20-50°C, the melting enthalpy is not less than 40J/g, and the ΔT is also less than 20°C In addition, it can also be found that the crystallization enthalpy of the hard segment molecule (PBT) measured in Examples 1-16 is not less than 24J/g.

(b) Comparison and discussion of Examples 1～5, 11 and Comparative Examples 1～4:

The various thermal properties of the materials used to produce fibers in Comparative Examples 1-4 are shown in Table 6 below according to the aforementioned test methods.

Table 6

From Table 5 and Table 6, it can be found that organic additives (all non-aromatic, molecular weight less than 1000, and melting points all between the crystallization temperature of the hard segment molecule and the melting temperature of the soft segment molecule) and/or inorganic additives have the same additive amount, and the weight average molecular weight of the soft segment molecule (PEG) is also the same condition, the comparative example 1 without adding inorganic and organic additives, the comparative example 2 with only adding inorganic additives (without adding organic additives), or only adding non-aromatic In Comparative Examples 3-4 with organic additives (without adding inorganic additives), the enthalpy of crystallization of hard segment molecules (PBT) is less than 16 J/g, which is lower than that of Example 1 in which both inorganic additives and non-aromatic organic additives are added. ～5, 11 (not less than 25J/g) [that is, the crystallinity of the hard segment molecule (PBT) of Comparative Examples 1～4 is lower than that of Examples 1～5, 11], which means that the crystallinity of Comparative Examples 1～4 is used for production. As for the fiber material, the intensity of the fibers obtained subsequently is lower than that of the fibers obtained in Examples 1-5, 11.

In addition, the melting enthalpy of the soft segment molecule (PEG) of Comparative Examples 1-4 is less than 37 J/g, which is lower than that of Examples 1-5, 11 (not less than 46 J/g), and the ΔT of Comparative Examples 1, 3-4 Greater than 20°C (Examples 1-5, 11 are less than 20°C), which means that the materials used in the production of fibers in Comparative Examples 1-4, the two-way temperature regulation ability of the fibers obtained subsequently is lower than that obtained from Examples 1-4 5. 11. The prepared fiber.

It is confirmed from the above two paragraphs that when the material for producing fibers of the present invention contains both inorganic additives and non-aromatic organic additives, it can simultaneously improve the strength and two-way temperature regulation ability of the subsequently obtained fibers.

(c) Comparison and Discussion of Embodiments 1～5 and Comparative Examples 5～7:

The various thermal properties of the materials used to produce fibers in Comparative Examples 5-7 are shown in Table 7 below according to the aforementioned test methods.

Table 7

It can be found from Table 7 that under the condition that the organic additives (all non-aromatic and molecular weight less than 1000) and inorganic additives (all Talc) have the same addition amount, and the weight average molecular weight of the soft segment molecule (PEG) is also the same, the The melting point of the non-aromatic organic additive is not between the crystallization temperature of the hard segment molecule (PBT) and the melting temperature of the soft segment molecule (PEG) in Comparative Examples 5-7, and the crystallization enthalpy of the hard segment molecule (PBT) is less than 17J/g, which is lower than that of Examples 1-5 (not less than 25J/g) whose melting points are between the crystallization temperature of the hard segment molecule (PBT) and the melting temperature of the soft segment molecule (PEG) [i.e. comparative examples 5-7 The crystallinity of the hard segment molecule (PBT) is lower than that of Examples 1 to 5], which means that the materials used to produce fibers in Comparative Examples 5 to 7 have a lower strength than those obtained in Examples 1 to 5. The strength of the resulting fiber.

In addition, the melting enthalpy of the soft segment molecule (PEG) of Comparative Examples 5-7 is less than 38 J/g, which is lower than that of Examples 1-5 (not less than 47 J/g), and the ΔT of Comparative Examples 5-7 is also greater than 21 °C (less than 20 °C in Examples 1 to 5), which means that the materials used to produce fibers in Comparative Examples 5 to 7, the two-way temperature regulation ability of the fibers obtained subsequently is lower than that of the fibers obtained in Examples 1 to 5 of fiber.

It is confirmed by the above two paragraphs that the non-aromatic organic additives used in the material for producing fibers in the present invention can simultaneously Improve the strength and bi-directional temperature regulation ability of the fibers obtained later.

(d) Comparison and Discussion of Embodiments 1 to 5 and Comparative Example 8:

The various thermal property data of the material used to produce fibers in Comparative Example 8 measured according to the aforementioned test method are shown in Table 8 below.

Table 8

It can be found from Table 8 that the organic additives (both are non-aromatic and have melting points between the crystallization temperature of the hard segment molecule and the melting temperature of the soft segment molecule) and inorganic additives (both Talc) have the same addition amount, and the soft segment Molecule (PEG) weight average molecular weight is also under the same condition, the comparative example 8 in which the molecular weight of the organic additive is greater than 1000, the crystallization enthalpy of the hard segment molecule (PBT) is only 15.3J/g, which is lower than that of the organic additive molecular weight not greater than 1000 Examples 1 to 5 (not less than 25J/g) [that is, the crystallinity of the hard segment molecule (PBT) of Comparative Example 8 is lower than that of Examples 1 to 5], which represent the materials used to produce fibers in Comparative Example 8, which The strength of the fibers obtained subsequently is lower than that of the fibers obtained in Examples 1-5.

In addition, the melting enthalpy of the soft segment molecule (PEG) of Comparative Example 8 is only 37.1 J/g, which is lower than that of Examples 1-5 (not less than 47 J/g), and the ΔT of Comparative Example 8 is also greater than 20°C (Example 1 to 5 are less than 20°C), which means that the material used to produce fibers in Comparative Example 8 has a bidirectional temperature regulation ability of the fibers obtained subsequently that is lower than that of the fibers obtained in Examples 1 to 5. ability.

It is confirmed from the above two paragraphs that the non-aromatic organic additive used in the fiber production material of the present invention, when its molecular weight is not greater than 1000, can simultaneously improve the strength and bidirectional temperature regulation ability of the subsequent obtained fiber.

(e) Comparison and discussion of Examples 1 to 16 and Comparative Example 9:

The various thermal property data of the material used to produce fibers in Comparative Example 9 measured according to the aforementioned test method are shown in Table 9 below.

Table 9

From the above Table 5 and Table 9, it can be found that the organic additives (with molecular weights less than 1000 and melting points between the crystallization temperature of the hard segment molecule and the melting temperature of the soft segment molecule) and inorganic additives have the same addition amount, and the soft segment molecule (PEG) weight average molecular weight is also under the same condition, the organic additive contains phenyl (aryl) comparative example 9, its hard segment molecule (PBT) crystallization enthalpy is only 15.5J/g, lower than organic additive non- Aromatic Examples 1 to 16 (not less than 24J/g) [that is, the crystallinity of the hard segment molecule (PBT) in Comparative Example 9 is lower than that of Examples 1 to 16], which represent the performance of Comparative Example 9 for fiber production. material, the strength of the fibers obtained subsequently is lower than that of the fibers obtained in Examples 1-16.

In addition, the melting enthalpy of the soft segment molecule (PEG) of Comparative Example 9 is only 37.4 J/g, which is lower than that of Examples 1-16 (not less than 40 J/g), and the ΔT of Comparative Example 9 is also greater than 20°C (Example 1 to 16 are less than 20°C), which means that the material used to produce fibers in Comparative Example 9 has a bidirectional temperature regulation ability of the fibers obtained subsequently that is lower than that of the fibers obtained in Examples 1 to 16. ability.

It is proved from the above two paragraphs that when the organic additives in the material used for producing fibers in the present invention are non-aromatic, they can simultaneously improve the strength and bi-directional temperature regulation ability of the subsequently obtained fibers.

(f) Comparison and Discussion of Embodiment 2, 14～16 and Comparative Examples 10～11, 13～14:

The various thermal property data of the materials used to produce fibers in Comparative Examples 10-11 and 13-14 are shown in Table 10 below according to the aforementioned testing methods.

Table 10

It can be found from Table 10 that under the condition that the organic additives (both are St) and the inorganic additives (both are Talc) have the same addition amount, the soft segment molecule (PEG) weight average molecular weight of Comparative Example 10 is less than 2500, the soft segment molecule (PEG) melting enthalpy is only 33.7J/g, lower than embodiment 2, 14～16 (not less than 40J/g), and the ΔT of comparative example 10 is also greater than 21 ℃ (embodiment 2, 14～16 is less than 20° C.), which means that the material used to produce fibers in Comparative Example 10 has a bidirectional temperature regulation ability of the fibers obtained subsequently that is lower than that of the fibers obtained in Examples 2, 14-16.

And soft segment molecule (PEG) weight average molecular weight is greater than 10000 comparative example 11, its soft segment molecule (PEG) melting temperature is higher than embodiment 2, 14～16 (not more than 50 ℃), makes the adjustable Warm high temperatures are too high for use on fabrics.

It is confirmed from the above description that when the molecular weight average molecular weight of the soft segment in the material used for producing fibers in the present invention is 2,500 to 10,000, it can improve the bidirectional temperature regulation ability of the subsequent obtained fibers, and the high temperature of the temperature can be adjusted Moderate, suitable for application on fabrics.

In addition, it should be noted that the soft segment molecule used in Comparative Example 14 is PTMEG 2000. Compared with Comparative Example 13 (the soft segment molecule is PEG 2000), if the carbon number of the soft segment molecule is too long, the resulting The fiber ΔT becomes larger, which leads to poor effect of two-way temperature regulation.

(g) Comparison and discussion of embodiment 2 and comparative examples 15-18:

The various thermal property data of the materials used to produce fibers in Comparative Examples 15-18 measured according to the aforementioned test methods are shown in Table 11 below.

Table 11

It can be found from Table 11 that in Comparative Examples 15-18 where PET is used to replace PBT in the hard segment molecule, no matter whether organic or inorganic additives are added, the crystallization enthalpy of the hard segment molecule (PET) is less than 15 J/g, which is lower than that of the hard segment molecule. Example 2 (27.8J/g) in which the molecule is PBT [that is, the crystallinity of the hard segment molecule (PET) in Comparative Examples 15-18 is lower than that of Example 2], which means that the crystallinity of the hard segment molecule (PET) in Comparative Examples 15-18 is used to produce fibers. material, the strength of the fibers obtained subsequently is lower than that of the fibers obtained in Example 2.

In addition, the melting enthalpy of the soft segment molecule (PEG) of Comparative Examples 15-18 is less than 41 J/g, which is lower than that of Example 2 (48.5 J/g), and the ΔT of Comparative Examples 15-18 is also greater than 22°C (Example 2 is 19.4° C.), which means that the materials used to produce fibers in Comparative Examples 15-18 have lower bidirectional temperature regulation ability than the fibers produced in Example 2.

It is confirmed from the above two paragraphs that when the hard segment molecules in the material used for producing fibers in the present invention are composed of PBT, it can simultaneously improve the strength and bi-directional temperature adjustment ability of the subsequently obtained fibers.

<Comparison and Discussion of Thermal Properties of Application Example 1 and Comparative Application Examples 1-2>

For the composite fibers of Application Example 1 and Comparative Application Examples 1-2, the various thermal property data measured according to the aforementioned test methods are shown in Table 12 below, and the composite fibers of Application Example 1 and Comparative Application Examples 1-2 were tested. Fiber strength test, the obtained results are also shown in Table 12.

Table 12

It can be found from Table 12 that in Comparative Application Example 1 without adding organic and inorganic additives, the melting enthalpy of the soft segment molecule (PEG) is lower than that of Application Example 1 in which organic and inorganic additives are added simultaneously, and the range of ΔT in Comparative Application Example 1 is also It is wider than that of Application Example 1, which means that the bidirectional temperature regulation ability of the composite fiber of Comparative Application Example 1 is lower than that of Application Example 1. In addition, it can also be found from the fiber strength data that the fiber strength of Application Example 1 is higher than that of Comparative Application Example 1, confirming again When the material for producing fibers of the present invention contains both inorganic additives and non-aromatic organic additives, the strength and bi-directional temperature regulation ability of the subsequently obtained fibers can be improved.

It should be noted that the material used for producing fibers in Comparative Example 12 has a relatively high addition amount of inorganic additives (more than 1 part by weight when the total weight of the copolyester is 100 parts by weight), so in the following During the process of melt-spinning to produce composite fibers (that is, Comparative Application Example 2), filaments were easily broken and subsequent processing was impossible, so data could not be obtained.

<Comparison of thermal regulation factor (TRF) between application example 2 and comparative application example 3>

The nonwoven fabrics of Application Example 2 and Comparative Application Example 3 were tested for their TRF according to ASTM D7024-2004, and the results are shown in Table 13 below. It should be noted that when the external temperature changes, the smaller the value of TRF, the smaller the temperature change of the fiber surface with time, so the better the two-way temperature regulation ability of the fiber.

Table 13

Non-woven composite fiber Materials used to make fibers TRF Application example 2 Application example 1 Example 2 0.54 Comparative application example 3 Comparative application example 1 Comparative example 1 0.82

It can be seen from Table 13 that the TRF value of Comparative Application Example 3 without adding organic and inorganic additives is higher than that of Application Example 2 with simultaneous addition of organic and inorganic additives, indicating that Comparative Application Example 3 has a lower two-way temperature regulation ability, which further proves the present invention When the material for producing fibers contains both inorganic additives and non-aromatic organic additives, it can improve the bidirectional temperature regulation ability of the subsequently prepared fibers.

To sum up, since the material used for producing fibers of the present invention contains both the inorganic additive and the non-aromatic organic additive with a molecular weight not greater than 1000, and the melting point of the non-aromatic organic additive is between that of the hard segment molecule Between the crystallization temperature of the soft segment molecule and the melting temperature of the soft segment molecule, the material used for the production of fibers in the present invention can effectively improve the strength and bidirectional temperature adjustment ability of the subsequently obtained fibers at the same time, so the purpose of the present invention can indeed be achieved.

The above are only embodiments of the present invention, and should not limit the scope of the present invention with this, that is, all simple equivalent changes and modifications made according to the claims of the present invention and the contents of the description still belong to the present invention. scope of the invention.

Claims (10)

1. A material for producing fibers, characterized in that: the material for producing fibers comprises: Copolyester is composed of hard segment molecules and soft segment molecules, the hard segment molecules are mainly composed of polybutylene terephthalate, the soft segment molecules are mainly composed of polyethylene glycol, and the The weight average molecular weight of the soft segment molecules is between 2500 and 10000; inorganic additives; and A non-aromatic organic additive, the melting point of which is between the crystallization temperature of the hard segment molecule and the melting temperature of the soft segment molecule, and the molecular weight of the non-aromatic organic additive is not greater than 1000; Based on 100 parts by weight of the total weight of the copolyester, the content of the inorganic additive ranges from 0.02 to 1.00 parts by weight, and the content of the non-aromatic organic additive ranges from 0.02 to 1.00 parts by weight. 2 . The material for producing fibers according to claim 1 , wherein, based on the total weight of the copolyester as 100 wt %, the proportion of the soft segment molecules is 30-80 wt %. 3. The material for producing fibers according to claim 1, wherein the weight average molecular weight of the soft segment molecules is between 3000-9000. 4. The material for producing fibers according to claim 3, wherein the weight average molecular weight of the soft segment molecules is between 3400-8000. 5. The material for producing fibers according to claim 1, characterized in that: the non-aromatic organic additive is selected from C ₁₃ -C ₂₈ straight chain aliphatic hydrocarbons, C ₁₃ -C ₂₈ straight chain aliphatic hydrocarbon esters , and at least one of the group consisting of C ₁₃ -C ₂₈ straight chain fatty acids or salts thereof. 6. The material for producing fibers according to claim 5, wherein the non-aromatic organic additive is selected from the group consisting of stearic acid or its salt, and tridecyl methacrylate at least one of the . 7 . The material for producing fibers according to claim 1 , wherein the melting point of the non-aromatic organic additive is between 50° C. and 168° C. 8 . The material for producing fibers according to claim 7 , wherein the melting point of the non-aromatic organic additive is between 55°C and 160° C. 9. The material for producing fibers according to claim 1, characterized in that: the inorganic additive is selected from talcum powder, mica, zinc oxide, calcium oxide, titanium dioxide, silicon dioxide, calcium carbonate, barium sulfate and oxide At least one of the group consisting of magnesium. 10. A fiber, characterized in that: said fiber is made from the material for producing fiber according to any one of claims 1 to 9 through a melt-spinning mechanical device.