KR20140090280A - The thermoplastic cellulose derivative composite fiber and manufacturing method thereof - Google Patents

Abstract

The present invention relates to a thermoplastic cellulose derivative composite fiber and a method for preparing the same. Specifically, the thermoplastic cellulose derivative composite fiber of the present invention is harmless to humans as the fiber is prepared by melt spinning without using toxic organic solvent; rapid consolidation of the cellulose is prevented upon spinning to enhance work efficiency of the spinning and to enable high-speed spinning of 3,500 mpm or more to maximize productivity; and physical properties of the prepared thermoplastic cellulose derivative composite fiber such as strength and elongation or the like can be improved. Furthermore, by removing easy dissolution components from the thermoplastic cellulose derivative composite fiber, the fiber becomes superfine to be able to provide high-sensitive thermoplastic cellulose derivative composite superfine fiber with excellent texture.

Description

TECHNICAL FIELD The present invention relates to a thermoplastic cellulose derivative conjugated fiber,

 The present invention relates to a thermoplastic cellulose derivative conjugate fiber and a process for producing the same. More specifically, the present invention relates to a thermoplastic cellulose derivative conjugate fiber capable of melt spinning without dissolving in an organic solvent and capable of spinning at a high speed, The present invention relates to a thermoplastic cellulose derivative conjugated fiber and a process for producing the same.

Polymer synthetic resins have been extensively used for a variety of purposes because of their excellent mechanical properties, chemical resistance and durability. However, such synthetic resins have a disadvantage in that harmful substances are released when they are incinerated because they are not decomposed by themselves in nature.

Recently, environmental pollution problem has become a big social problem, and biodegradable resins that can be completely decomposed in nature have been actively studied and are attracting interest worldwide.

Although biodegradable resins such as polybutylene succinate, polyethylene succinate and polylactic acid are excellent in biodegradability, they are not economical due to their high cost, or have a low melting point, In the manufacture of products such as textile products, it is difficult to develop a product group that needs to maintain thermal stability.

Recently, products such as polylactic acid (PLA) or starch have been spotlighted in recent biomass-based products, which are supplied from nature. However, they can not be dyed at high temperature for fiberization and are susceptible to hydrolysis, It has various disadvantages such as hardening and brittle property when the tenter work is carried out, and it is difficult to carry out spinning at 4000mpm in the spinning apparatus which emits the conventional polyester.

Cellulosic materials are biodegradable resource-recycling biomass materials that can be produced in pulp and are therefore produced in the largest amount on the earth without the need for separate cultivated land and water. The use of cellulose as a fiber has been conventionally carried out by spinning short fibers such as cotton and hemp produced in the natural environment. In order to obtain a filament material other than short fibers, cellulose is dissolved in a specific solvent to effect wet spinning, cellulose is derivatized such as cellulose acetate, dissolved in an organic solvent such as methylene chloride or acetone, A dry spinning process has been carried out in which the spinning is carried out while evaporating.

However, these wet spinning or dry spinning fibers have a problem of low productivity due to a slow spinning speed, and also have problems in that organic solvents such as carbon disulfide, acetone, and methylene chloride used in the production of fibers have a bad influence on the environment and human body . Therefore, in order to obtain an environmentally friendly fiber comprising cellulose as a raw material, it is necessary to use a melt spinning method without using an organic solvent.

As a thermoplastic cellulose composition capable of melt spinning and fibers made of the same, a cellulose composition in which a large amount of a water-soluble plasticizer such as polyethylene glycol is added to cellulose acetate, and a fiber comprising the cellulose composition are known. However, since the content of the plasticizer in the composition is high, the spin rate during spinning is high, and melt spinning is difficult unless the spinning draft is low.

 In order to solve such problems, research and development of thermoplastic cellulose fibers for improving the spinning workability and improving the strength of fiber have been variously attempted. However, conventionally, the maximum Even after spinning at the critical spinning temperature, the thermoplastic cellulose rapidly solidifies immediately after spinning, resulting in a high incidence of threading, resulting in difficulty in melt spinning. Furthermore, since it is impossible to radiate at a high speed of 3,500mpm or more, the productivity is low. There is a problem that it is difficult to produce thermoplastic cellulose microfine fibers having good mechanical properties and excellent tactile sensation.

Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a method for producing cellulose fibers by melt spinning, It is an object of the present invention to provide a thermoplastic cellulose derivative conjugate fiber which can prevent rapid solidification of cellulose immediately upon spinning at the time of production, thereby improving radiation workability and improving mechanical properties such as strength and the like.

A second problem to be solved by the present invention is to provide a thermoplastic cellulose derivative microfine fiber having high sensitivity and having excellent tactile sensation by removing the easily soluble component from the thermoplastic cellulose derivative conjugate fiber.

A third problem to be solved by the present invention is to provide a method for producing a thermoplastic cellulose derivative conjugate fiber capable of spinning at a high speed during melt spinning, thereby remarkably increasing productivity.

 In order to solve the above-described problems,

A first component comprising a cellulose ester and a plasticizer; And a second component comprising a water-soluble copolymerizable polyester.

According to a preferred embodiment of the present invention, the cellulose ester is selected from the group consisting of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, cellulose acetate phthalate, cellulose acetate caproate, cellulose acetate caprylate, cellulose acetate laurethate, cellulose acetate Palmitate, cellulose acetate stearate, and cellulose acetate oleate.

According to another preferred embodiment of the present invention, the plasticizer may include at least one selected from the group consisting of polyethylene glycol, glycerin, triacetin and tributyl sebacate.

According to another preferred embodiment of the present invention, the water soluble copolymer polyester is prepared by mixing an acid component containing a polycarboxylic acid and an alkali metal sulfonate and a diol component having 2 to 10 carbon atoms, .

According to another preferred embodiment of the present invention, the acid component containing the alkali metal sulfonate may be 0.5 to 25 mol% of the total acid component.

According to another preferred embodiment of the present invention, the alkali metal sulfonic acid salt is selected from the group consisting of sulfur terephthalic acid, 5-sulfur isophthalic acid, 4-sulfur phthalic acid, 4-sulfinaphthalene-2,7-dicarboxylic acid, Xylylene glycol, and 2-sulfur-1,4-bis (hydroxyethoxy) benzene.

According to another preferred embodiment of the present invention, the composite fiber may be a sheath-core type, an island in the sea type, a side by side type, and a segmented pie ) ≪ / RTI > type.

According to another preferred embodiment of the present invention, the composite fiber may be an island-in-the-sea type fiber in which the first component is a conductive component and the second component is a sea component.

According to another preferred embodiment of the present invention, the composite fiber may be a sheath-core type fiber comprising a first component as a core component and a second component as a sheath component.

According to another preferred embodiment of the present invention, the weight ratio of the first component and the second component may be 3: 7 to 7: 3.

The present invention also provides a thermoplastic cellulose derivative fiber obtained by eluting and removing the second component from the above-mentioned thermoplastic cellulose derivative conjugate fiber.

According to a preferred embodiment of the present invention, the fibers may be microfine fibers having a fineness of 0.1 to 1 D.

According to another preferred embodiment of the present invention, the fiber may have a strength of 2.5 g / de or more and an elongation of 25% or more.

The present invention also relates to a composition comprising a first component comprising a cellulose ester and a plasticizer; And a second component comprising a water-soluble copolymerizable polyester is spin-melt-conjugated spinning at a rate of 3,500 to 5,000 mpm through a composite spinneret, thereby producing a thermoplastic cellulose derivative conjugate fiber.

According to a preferred embodiment of the present invention, the spinning temperature of the molten composite spinning may be 220 to 250 ° C.

According to another preferred embodiment of the present invention, the water soluble copolyester is prepared by esterifying and polycondensing a mixture of an acid component containing a polycarboxylic acid and an alkali metal sulfonate and a diol component having 2 to 10 carbon atoms .

According to another preferred embodiment of the present invention, the weight ratio of the first component and the second component may be 3: 7 to 7: 3.

The present invention also provides a process for producing a thermoplastic cellulose derivative microfine fiber, which comprises the steps of preparing a thermoplastic cellulose derivative conjugate fiber according to the above-mentioned production method, and eluting and removing the water soluble copolymer polyester.

 The thermoplastic cellulose derivative conjugate fiber of the present invention is produced by melt spinning without using a toxic organic solvent, so that it is not poisonous to the human body and prevents rapid solidification of cellulose immediately after spinning to improve spinning workability, It is possible to increase the productivity, and it is possible to improve the physical properties such as the strength of the produced thermoplastic cellulose derivative fiber. Further, by removing the dissolving component from the thermoplastic cellulose derivative conjugate fiber, it is possible to provide a highly sensitive thermoplastic cellulose derivative microfine fiber having a fine texture and excellent tactile sensation.

1 is a cross-sectional view of a cis-core type conjugate fiber according to a preferred embodiment of the present invention.
2 is a cross-sectional view of a sea-island type conjugate fiber according to a preferred embodiment of the present invention.
3 is a cross-sectional view of a side-by-side type composite fiber according to a preferred embodiment of the present invention.
4 is a cross-sectional view of an NP split yarn according to a preferred embodiment of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS The invention will be described in more detail with reference to the accompanying drawings.

As described above, the conventional thermoplastic cellulose derivative fibers suffer from the problem that the thermoplastic cellulose rapidly shrinks immediately after spinning even at the maximum critical spinning temperature at which the color and physical properties of the fiber can be preserved during melt spinning, High-speed spinning of 3,500mpm or more is impossible, so that productivity is low, and it is difficult to produce thermoplastic cellulose microfine fibers having good mechanical properties and excellent tactile sensation.

Accordingly, the present invention provides a composition comprising a first component comprising a cellulose ester and a plasticizer; And a second component comprising a water-soluble copolymerizable polyester. The present invention has been made to solve the above-mentioned problems by providing a thermoplastic cellulose derivative conjugate fiber. As a result, it is possible to prevent rapid solidification of cellulose immediately upon spinning during melt spinning, to improve spinning workability, to enable high-speed spinning of more than 3,500 mpm, to increase productivity, and to improve the physical properties such as strength and the like of the produced thermoplastic cellulose derivative fiber Can be improved. Further, by removing the dissolving component from the thermoplastic cellulose derivative conjugate fiber, it is possible to provide a highly sensitive thermoplastic cellulose derivative microfine fiber having a fine texture and excellent tactile sensation.

 The composite fiber of the present invention may be a sheath-core type, an island in the sea type, a side by side type, an NP split fiber or the like, and is not particularly limited thereto. Component and the second component separately from each other.

 The present invention relates to a water-soluble copolymerizable polyester which protects a loss of heat of a cellulose and blocks external air as a result of complex spinning of a second component comprising a water-soluble copolymerizable polyester together with a first component comprising a cellulose ester and a plasticizer, It is possible to prevent rapid solidification of cellulose immediately upon spinning, to prevent rapid solidification of cellulose, to improve spinning workability, to improve the strength, and to enable high-speed spinning of 3,500 mpm or more, and productivity can be remarkably increased.

FIG. 1 is a cross-sectional view of a sheath-core type conjugate fiber according to a preferred embodiment of the present invention, more preferably a sheath-core type conjugate fiber as shown in FIG. 1 , The first component may be a core component (21), and the second component may be a sheath component (20). On the other hand, when the second component is used as a core component and the first component is used as a sheath component, the solidification of cellulose due to the external air is abruptly accelerated, partial filing occurs, and high-speed spinning is not possible and product quality can not be guaranteed , There may be a problem that the strength is rather reduced when the water-soluble copolyester of the core component is removed.

 FIG. 2 is a cross-sectional view of an island-in-the-sea type composite fiber according to a preferred embodiment of the present invention. In the case of island-in-the-sea type fibers, And an island-in-the-sea type fiber in which the second component is a sea component 30. In this case, the number of the conductive components 31 is preferably 2 to 8, and the fineness of the conductive component 31 may be 0.1 to 1 D. On the other hand, when the second component is used as a conductive component and the first component is used as a sea component, the solidification of cellulose due to the external air is accelerated and partial yarn breakage occurs. And there is a problem that ultrafine fiber can not be manufactured.

FIG. 3 is a sectional view of a side by side type composite fiber according to a preferred embodiment of the present invention, FIG. 4 is a sectional view of an NP divided yarn, and the side by side type or NP divided yarn The positions where the first component and the second component are included may not be particularly limited as long as the first and second components of the present invention satisfy the preferable weight ratio.

 The first component included in such a composite fiber of the present invention includes a cellulose ester and a plasticizer.

 The cellulose ester is a cellulose derivative in which a part or all of the hydroxyl groups of cellulose are substituted by ester bonds, weakening the strong hydrogen bonding of the cellulose hydroxyl groups and allowing the plasticizer to mix well therebetween. By effectively mixing the plasticizer, strong hydrogen bonding due to cellulose hydroxyl groups can be prevented and melt spinning can be enabled.

The cellulose ester is preferably selected from the group consisting of cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, cellulose acetate phthalate, cellulose acetate caprate, cellulose acetate caprylate, cellulose acetate laurethate, cellulose acetate palmitate, cellulose acetate stearate Or cellulose acetate oleate, and the like.

The cellulose ester of the present invention may have an average degree of polymerization of 30,000 to 50,000 and a degree of substitution of 2.2 to 2.6. The substitution degree of the cellulose ester means the degree of substitution of the hydroxyl group of the cellulose by the ester bond. When the degree of substitution of the cellulose ester is less than 2.2, the fluidity may be lowered and the strength may be lowered at the time of wetting. There may be a problem of degradation.

 Next, the plasticizer is not particularly limited as long as it is mixed with the cellulose derivative to interfere with strong hydrogen bonding due to the cellulose hydroxyl group and can be melt-spun, but it is more preferable to use a low molecular weight of 1000 or less so as to promote plasticization .

Examples of the plasticizer include phthalic acid esters such as dimethyl phthalate, diethyl phthalate, dihexyl phthalate, dioctyl phthalate, dimethoxyethyl phthalate, ethyl phthalyl ethyl glycolate and butyl phthalyl butyl glycolate, tetraoctyl pyromellitate, Aromatic dicarboxylic acid esters such as dibutyl adipate, dibutyl adipate, dibutyl sebacate, dioctyl sebacate, diethyl azelate, dibutyl azelate and dioctyl azelate; and aromatic dicarboxylic acid esters such as dibutyl adipate, Aromatic polycarboxylic acid esters, lower fatty acid esters of polyhydric alcohols such as glycerin triacetate and diglycerin tetraacetate, phosphoric acid esters such as triethyl phosphate, tributyl phosphate, tributoxyethyl phosphate, tricresyl phosphate and the like Alone or in combination.

Examples of relatively high molecular weight plasticizers include aliphatic polyesters composed of glycols and dibasic acids such as polyethylene glycol, polypropylene glycol, polyethylene adipate, polybutylene adipate, polyethylene succinate, and polybutylene succinate; Aliphatic polyesters composed of oxycarboxylic acids such as glycolic acid, aliphatic polyesters composed of lactones such as polycaprolactone, polypropiolactone and polar valerolactone, vinyl polymers such as polyvinylpyrrolidone Or mixed form.

The second component included in the composite fiber of the present invention includes a water soluble copolymer polyester. The water-soluble copolyester serves to block cellulose from the outside air to prevent the loss of heat and attain a sufficient crystallization time by attaining the solidification rate. Therefore, the thermoplastic cellulose derivative composition (the first component ), It is possible to prevent rapid solidification of cellulose immediately after spinning, to improve spinning workability and strength, and to be capable of spinning at a high speed of 3,500 mpm or more. Further, after the composite fiber is produced, the second component including the water-soluble copolymerizable polyester can be easily eluted and removed, so that the thermoplastic cellulose derivative superfine fiber of 0.1 to 1 D can be produced.

 The water-soluble copolyester may be prepared by esterifying and polycondensing a mixture of an acid component containing a polycarboxylic acid and an alkali metal sulfonate and a diol component having 2 to 10 carbon atoms.

Examples of the polyvalent carboxylic acid component used in the production of the water soluble copolyester include terephthalic acid, isophthalic acid, adipic acid, 2,5-dimethytereterephthalic acid, 1,4-naphthalenedicarboxylic acid, 2,6-naphthalenedicarboxylic acid Acid, bisphenyldicarboxylic acid, 1,2-bis (phenoxy) ethane-P-P'-dicarboxylic acid or an ester-forming derivative thereof may be used, more preferably terephthalic acid or isoproparic acid Lt; / RTI >

Examples of the polycarboxylic acid containing an alkali metal sulfonate include sulfuric acid such as sulfuric terephthalic acid, 5-sulfoisophthalic acid, 4-sulfurphthalic acid, 4-sulfinaphthalene-2,7- dicarboxylic acid, sulfur- Sulfo-1,4-bis (hydroxyethoxy) benzene, or an ester-forming derivative thereof, more preferably 5-sulfoisophthalic acid, a sodium salt of sulfur terephthalic acid or an ester-forming derivative thereof have.

The sulfonic acid alkali metal salt derivative compound may be used in an amount of 0.5 to 25 mol%, more preferably 7 to 15 mol%, based on the entire polycarboxylic acid component used in the polyester polymerization. When the amount of the polyvalent carboxylic acid containing the alkali metal sulfonate is less than 0.5 mol%, the water solubility is decreased and the post-spinning elution is impossible or the energy required for the elution step is excessive. When the amount exceeds 25 mol% And the degree of polymerization is reduced. In the case of spinning, there is a problem that the increase of the pack pressure is increased and the spinning is impossible.

Examples of the polyhydric alcohol component include ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 2,4-dimethyl-2-ethylbenzene-1,3-diol, neopentyl glycol, Pentanediol, 1,6-hexanediol, 1,8-octanediol, p-xylylene glycol, 1,2-cyclohexanedimethanol, and the like. More preferred are ethylene glycol, Diol, 1,4-butanediol.

Such a water-soluble copolymerizable polyester resin can be purchased and used commercially, and Korean Patent Publication Nos. 1992-0000825, 1993-0004353, and 10-2005-0033262 are incorporated by reference.

When the water-soluble polyester other than the water-soluble copolyester produced as described above is used as the second component, the spinning operation may be deteriorated when spinning at a high speed of more than 3,500 mpm, the effect of improving the strength is insufficient, There may be a problem that spots may occur in the process of making the fibers microfine, and the fibers may be stuck and adhered to each other.

In the composite fiber of the present invention, the weight ratio of the first component and the second component may be 3: 7 to 7: 3. If the amount of the second component is less than the above range, loss of heat of the cellulose can not be blocked and rapid solidification occurs. Therefore, there may be a problem that high-speed spinning is impossible. If the second component is contained in an excessively large amount, There may be a problem in maintaining the uniformity of the division plane. In addition, the fineness of the conjugate fiber may be 0.5 to 6.0 D, and if it is less than 0.5 D, the cross-sectional formation and workability may be deteriorated. If it exceeds 6.0 D, the fiber touch is not uniform, .

 Such a conjugate fiber of the present invention comprises a first component comprising a cellulose ester and a plasticizer; And a water-soluble copolymerizable polyester by rapid spin-melt spinning at a rate of 3,500 to 5,000 mpm through a combined spinneret such as a sheath-core type, a sea-island type, and a side-by-side type.

The water-soluble copolymer polyester of the second component may be prepared by esterifying and polycondensing a mixture of an acid component containing a polycarboxylic acid and an alkali metal sulfonate and a diol component having 2 to 10 carbon atoms, Thereby preventing the loss of heat and attaining a sufficient crystallization by attaining a sufficient crystallization speed. Thus, it is possible to prevent rapid solidification of the cellulose immediately after spinning, improve the spinning workability, And may emit at a radiation temperature of from 220 to 250 캜.

 The composite fiber of the present invention thus produced can produce thermoplastic cellulose derivative microfine fibers through a step of eluting and removing the second component comprising the water soluble copolymer polyester.

 The step of eluting and removing the water soluble copolyester may be carried out in the usual saponification process of the thermoplastic cellulose derivative fiber, more preferably in the hot water at 50 to 90 ° C for 30 to 120 minutes to remove the remaining water- To less than 0.1% by weight. In the production of the thermoplastic cellulose derivative superfine fiber by eluting and removing the water-soluble copolyester, the form of the cis-core type or sea-island type composite fiber may be more preferable.

The fineness of the thermoplastic cellulose derivative superfine fiber obtained after removing the second component including the water soluble copolymer polyester may be 0.1 to 1 D, the strength may be 2.5 g / de or more, and the elongation may be 25% or more.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples should not be construed as limiting the scope of the present invention, and should be construed to facilitate understanding of the present invention.

≪ Example 1 >

85% by weight of cellulose acetate having an average degree of substitution of cellulose hydroxyl group of 2.4, an average molecular weight of 40,000 (Eastman) and 15% by weight of environmentally friendly plasticizer polyethylene glycol were prepared. (3,5-di-t-butyl-4-hydroxyhydrocinnamate) methane (Anox 20, manufactured by Tosoh Corporation), which is a primary antioxidant, is added to prevent thermolysis when thermally- Tetris (2,4-di-t-butylphenyl) phosphate (Alcanox 240, Chemtura Corporation), a secondary antioxidant, was used to prevent thermal decomposition in the plasticizer- Was added in an amount of 0.1 part by weight based on 100 parts by weight of the composition containing cellulose acetate and a plasticizer, followed by mixing with a supermixer for 2 minutes. The mixed mixture was dried in a hot air drier for 12 hours, fixed at 25 kg / hr of a circle feeder and 270 rpm of a kneader motor speed using a kneader equipped with a twin-screw extruder, and then kneaded at a kneader die (DIE) A thermoplastic cellulose acetate resin (first component) was obtained by blending for 5 minutes while applying a temperature to a final terminal temperature of 200 占 폚.

In addition, dimethyl 5-sodium sulfoisophthalic acid and ethylene glycol were added to initiate the reaction, and bis-β-hydroxyethyl terephthalate, terephthalic acid, isophthalic acid and dimethyl glycol were added to initiate the esterification reaction.

In this case, dimethyl 5-sodium sulfoisophthalic acid has a molecular weight of about 300 and is added in an amount of 10 mol% of the acid component. Terephthalic acid has a molecular weight of about 150 and is added to 70 mol% of the acid component. Isophthalic acid has a molecular weight of about 150, which was added in an amount of 20 mol% in the acid component. Ethylene glycol had a molecular weight of 60, which was 70 mol% based on the diol and 30 mol% of diethylene glycol with a molecular weight of 110.

After that, polyethylene glycol was added for condensation polymerization, and a defoaming agent, an antioxidant and a heat stabilizer were added. The polyethylene glycol was added in an amount of 7 weight% in the total composition with a molecular weight of 300, other defoaming agents were added in an amount of 0.02 wt%, antioxidants in an amount of 500 ppm, and heat stabilizers in an amount of 200 ppm to obtain a water soluble copolyester (second component).

The thermoplastic cellulose acetate resin (first component) and the water-soluble copolymer polyester (second component) prepared above were mixed in a melt emitter equipped with a 36Hole Sheath / Core kneader in a core portion of 70 wt% And 30% by weight of the component, and spinning was conducted at 75D / 36F to obtain a cis-core type conjugate fiber.

Thereafter, the film was washed with hot water at 60 ° C for 1 hour and dried in a hot air drier at 80 ° C for 24 hours to remove the water-soluble copolyester to prepare a thermoplastic cellulose derivative microfine fiber of 0.5D.

≪ Example 2 >

The procedure of Example 1 was repeated, except that the first component was used as a conductive component and the second component was used as a sea component to prepare a sea-island complex fiber.

≪ Example 3 >

Was prepared in the same manner as in Example 1, except that 16 divided NP dividing yarns including the first component and the second component were produced.

<Example 4>

Was prepared in the same manner as in Example 1, except that the side-by-side-type conjugated fiber was prepared containing the first component and the second component.

&Lt; Example 5 >

Was prepared in the same manner as in Example 1 except that the first component and the second component were contained in a weight ratio of 9: 1.

&Lt; Example 6 >

The procedure of Example 1 was repeated except that the first component and the second component were contained in a weight ratio of 1: 9.

&Lt; Example 7 >

The procedure of Example 1 was repeated except that the first component was used as a sea component and the second component was used as a bead component to prepare a chart-type composite fiber.

&Lt; Example 8 >

30 mol% of dimethyl 5-sodium sulfur isophthalic acid, 60 mol% of terephthalic acid and 10 mol% of isophthalic acid as acid components and 30 mol% of diethylene glycol, 0.1 mol% of polyethylene glycol, 1.9 mol% of CHDM, 68 mol of ethylene glycol % Of a water-soluble polyester prepared by copolymerization.

&Lt; Example 9 >

Except that the second component was removed by washing in hot water at 40 캜 for 30 minutes.

&Lt; Example 10 >

Except that the second component was removed by washing in boiling water at 100 캜 for one hour.

<Comparative Example>

Except that 85% by weight of cellulose acetate having an average degree of substitution of 2.4 and an average molecular weight of 40,000 (Eastman Co.) and 15% by weight of plasticizer alone were spun.

<Experimental Example>

1. Measurement of River and Shinto

Steel fiber and elongation of the fiber were measured using an automatic tensile tester (Textechno) at a speed of 50 cm / m and a grip distance of 50 cm.

The strength and elongation are the strength (g / de) divided by the denier (de) when the fiber is stretched until a given force is given, the strength, the percentage of the initial length as a percentage of the elongation (% ) Were defined as extension.

2. Radiation workability evaluation

To evaluate the possibility of high - speed radiation, the radiation workability was determined as follows.

X: Not spinning,?: Five minutes inside,?: Ten minutes inside,?: Good

3. Tactile evaluation

Based on sensory test results by 10 experts. ⊚ indicates that 8 or more people feel good, △ indicates that 5 to 7 people think it is good, and X indicates that 8 or more people feel bad.

Spinning speed
(mpm) Radiation workability burglar
(g / de) Shindo
(%) Fineness
(De) Touch evaluation Example 1 4000 ◎ 3.5 32 0.75 ◎ Example 2 4000 ◎ 3.4 30 0.76 ◎ Example 3 4000 ◎ 3.1 28 0.78 ◎ Example 4 4000 ◎ 2.7 26 0.77 ◎ Example 5 4000 △ - - - × 2500 ○ 2.3 25 0.74 △ Example 6 4000 △ - - - × 2500 ○ 2.4 22 0.75 △ Example 7 4000 × - - - - 2500 × - - - - Example 8 4000 × - - - - 2500 ○ 1.9 20 0.76 × Example 9 4000 ◎ 2.5 23 1.2 △ Example 10 4000 ◎ 1.8 19 0.68 △ Comparative Example 4000 ○ 2.1 23 0.75 △ 2500 ◎ 2.3 24 0.77 △

As can be seen from Table 1, Examples 1 to 4, in which the water-soluble copolyester was used as a second component, were excellent in spinning workability at a high speed of 4,000 mpm as compared with Comparative Examples. De or less microfine fibers can be produced, the strength is improved, and the feeling is also remarkably excellent. However, in the case of Examples 5 and 6 in which the water-soluble copolyester polyester was contained in an excessively small amount or in an excess amount, spinnability at 2,500 mpm was lower than that in Examples 1 to 4, Physical properties such as tactile sensation deteriorated. In addition, even in the case of composite spinning including a water-soluble copolymer polyester, Example 7 in which the solution / reverse component was spun reversely was almost impossible to spin, and the effect of the present invention was hardly realized, Example 8 using a water-soluble polyester other than the water-soluble copolyester produced according to the Example was not capable of spinning at a high speed of 4,000mpm, and the spinning workability at 2,500mpm was remarkably reduced. Also, 4. In Example 9, 0.1% by weight or more of the water-soluble copolymer polyester remained, and ultrafine fibers having a diameter of 1D or less could not be produced. In Example 10, not only the water-soluble copolymerized polyester but also the plasticizer was eluted during the saponification process, and the fibers were damaged and the feel of the fibers was reduced.

Claims (18)

A first component comprising a cellulose ester and a plasticizer; And
And a second component comprising a water-soluble copolymerizable polyester. The method according to claim 1,
The cellulose esters include cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate, cellulose acetate phthalate, cellulose acetate caprate, cellulose acetate caprylate, cellulose acetate laurethate, cellulose acetate palmitate, cellulose acetate stearate and cellulose acetate And an oleate. The thermoplastic cellulose derivative conjugate fiber of any one of claims 1 to 3, The method according to claim 1,
Wherein the plasticizer comprises at least one selected from the group consisting of polyethylene glycol, glycerin, triacetin and tributyl sebacate. The method according to claim 1,
Wherein the water soluble copolymer polyester is produced by mixing and esterifying and polycondensing a mixture of an acid component containing a polyvalent carboxylic acid and an alkali metal sulfonate and a diol component having 2 to 10 carbon atoms. 5. The method of claim 4,
Wherein the acidic component containing the alkali metal sulfonic acid salt is 0.5 to 25 mol% of the total acidic component. 5. The method of claim 4,
The alkali metal sulfonic acid salt may be at least one selected from the group consisting of sulfur terephthalic acid, 5-sulfur isophthalic acid, 4-sulfur phthalic acid, 4-sulfinaphthalene-2,7-dicarboxylic acid, Bis (hydroxyethoxy) benzene. The thermoplastic cellulose derivative conjugate fiber according to claim 1, wherein the thermoplastic cellulose derivative conjugate fiber is at least one selected from the group consisting of bis (hydroxyethoxy) benzene. The method according to claim 1,
Wherein the composite fiber is selected from the group consisting of a sheath-core type, an island in the sea type, a side by side type, and a segmented pie type. Thermoplastic Cellulose Derivative Composite Fiber. The method according to claim 1,
Wherein the composite fiber is an island-in-the-sea type fiber in which the first component is a conductive component and the second component is a sea component. The method according to claim 1,
Wherein the composite fiber is a sheath-core type fiber comprising a first component as a core component and a second component as a sheath component. The method according to claim 1,
Wherein the weight ratio of the first component to the second component is 3: 7 to 7: 3. A thermoplastic cellulose derivative fiber obtained by eluting and removing a second component from the thermoplastic cellulose derivative conjugate fiber according to any one of claims 1 to 10. 12. The method of claim 11,
Wherein the fiber is a microfine fiber having a fineness of 0.1 to 1 D. 2. The thermoplastic cellulose derivative fiber according to claim 1, 12. The method of claim 11,
Wherein the fiber has a strength of at least 2.5 g / de and an elongation of at least 25%. A first component comprising a cellulose ester and a plasticizer; And
And the second component comprising the water-soluble copolymer polyester is spin-melt-combined spinning at a rate of 3,500 to 5,000 mpm through a composite spinneret. 15. The method of claim 14,
Wherein the spinning temperature of the melt-spinning composite yarn is 220 to 250 ° C. 15. The method of claim 14,
Wherein the water soluble copolyester is prepared by mixing an acid component containing a polyvalent carboxylic acid and an alkali metal sulfonate and a diol component having 2 to 10 carbon atoms and then esterifying and polycondensing the resultant mixture to produce a thermoplastic cellulose derivative conjugate fiber. Way. 15. The method of claim 14,
Wherein the weight ratio of the first component to the second component is from 3: 7 to 7: 3. A process for producing a thermoplastic cellulose derivative microfine fiber, which further comprises the steps of: preparing a thermoplastic cellulose derivative conjugate fiber according to any one of claims 14 to 17, and eluting and removing the water soluble copolyester polyester.

Images