KR102115849B1 - Method for manufacturing of a hydrophilic softner composition for Cellulose textile - Google Patents

Abstract

The present invention relates to a manufacturing method of a hydrophilic softener composition for cellulose fibers and, more specifically, to manufacturing method of a hydrophilic softener composition for eco-friendly cellulose fibers, which shows excellent flexibility, absorbency, elasticity, and washing resistance when processing highly sensitive and highly functional cellulose fibers, can be resalted, and can use water as a solvent.

Description

Method for manufacturing of a hydrophilic softner composition for Cellulose textile

The present invention relates to a method for manufacturing a hydrophilic softener composition for cellulose-based fibers, and more specifically, expresses excellent flexibility, absorbency, elasticity, wash resistance when processing high sensitivity and high-functionality of cellulose-based fibers, and can be re-salted. It relates to a method for producing an environmentally friendly hydrophilic softener composition for cellulosic fibers because water can be used as a solvent.

In recent years, as the economy has grown rapidly and the standard of living for consumers has improved, the demand for high-sensitivity and high-functional materials has increased in the textile field, as well as technical demands for products made of eco-friendly and human-friendly materials. Is in

As a processing agent for imparting an excellent tactile feel to textile products, conventionally, emulsified silicone oils such as modified amino silicone and dimethyl silicone are emulsified, but these products have disadvantages that are not environmentally friendly due to their chemical characteristics. Demands are increasing.

In addition, the silicone softener commonly used in the dyeing process is a forced high-speed dispersion and emulsification of a hydrophobic material, and a hydrophobic silicone polymer is clustered by self-migration according to chemical and physical process changes, resulting in re-dyeing and processing. Poor dyeing is a serious problem.

Furthermore, if the fabric is fabricated using a hydrophobic silicone softener, it is necessary to separately process the surface softener to remove it if re-salting is necessary due to defects. Even after the removal process, the softener is not removed to 100% and remains uneven when re-salting as it remains on the surface. , And even the removed softener is a cause of defects such as re-adhesion to the fiber due to the occurrence of gum-up left in the bath and re-adherence to the fiber.

On the other hand, hydrophilic silicone-based softeners have been developed in recent years to prevent such problems, but there are disadvantages of lowering the flexibility, absorbency, and functionality of the fibers. In addition, in order to compensate for this problem, in addition to a hydrophilic silicone softener, an emulsifier or a water-soluble urethane is mixed together, but in this case, the stability of the product decreases during processing, and gum-up and compatibility are poor. There is.

In addition, the water-soluble urethane mixed with a hydrophilic silicone softener for improving elasticity has a problem that the performance of the soft touch is not expressed while the application of the knitted fabric is dry due to the sticky wet feeling. In addition, even elastic properties are not achieved at a desired level, and shape stability is also poor.

Accordingly, it is an urgent need to develop an environmentally friendly softener because it exhibits excellent flexibility, absorbency, elasticity, and wash resistance when processing high-sensitivity and high-functionality cellulose-based fibers, and can be resalted and water can be used as a solvent.

Published Patent Publication No. 1998-0052504

The present invention has been devised in view of the above points, and exhibits excellent touch feeling, flexibility, absorbency, elasticity, wash resistance when processing high-sensitivity and high-functionality of cellulose-based fibers, and can be re-salted. It is an object of the present invention to provide a method for manufacturing a hydrophilic softener composition for a cellulose-based fiber, and a fabric treated with the hydrophilic softener composition for a cellulose-based fiber and a hydrophilic softener composition.

In order to solve the above problems, the present invention (1) diisocyanate component containing an aliphatic diisocyanate and a diol component containing polyethylene glycol having a weight average molecular weight of 2200 to 4500 reacted at a molar ratio of 1: 1.4 to 1.9. It provides a method for producing a hydrophilic softener composition for cellulose-based fibers, comprising the steps of preparing a polyurethane polymer and (2) treating the polyurethane polymer with an acidic solution to hydrophilize the polyurethane polymer.

According to an embodiment of the present invention, the aliphatic diisocyanate is 1,6-hexamethylene diisocyanate, (2,2,4) -trimethylhexamethylene diisocyanate, (2,4,4) -trimethylhexamethylene diisocyanate And it may include one or more selected from the group consisting of lysine diisocyanate.

In addition, the acidic solution of step (2) may be an acetic acid solution.

In addition, the diol component further comprises a polydialkylsiloxane containing a hydroxyl group at the sock end, and the polydialkylsiloxane and the polyethylene glycol may be included in a molar ratio of 1: 4 to 14.

In addition, the aliphatic diisocyanate is 1,6-hexamethylene diisocyanate, and the polyethylene glycol is a first polyethylene glycol having a weight average molecular weight of 2200 to 3100 and a second polyethylene glycol having a weight average molecular weight of 3400 to 4500 is 2.0 to 3.6. : It can be provided in a molar ratio of 1. At this time, the diol component may further include at least one alkanolamine selected from the group consisting of diethanolamine and triethanolamine. In addition, preferably, the polydialkylsiloxane containing a hydroxyl group at the sock end and the alkanolamine may be included in a molar ratio of 1: 2.5 to 6.5.

In addition, the polyurethane polymer is dispersed in water, the average particle diameter may be 120 ~ 200㎚.

Further, the aliphatic diisocyanate is 1,6-hexamethylene diisocyanate, and the diol component further includes a polydialkylsiloxane containing a hydroxyl group at the sock end and an alkanolamine that is diethanolamine, and the polydialkyl The siloxane, the polyethylene glycol and the diethanolamine are contained in a molar ratio of 1: 4 to 14: 2.5 to 6.5, and the polyethylene glycol has a weight average molecular weight of 2200 to 3100, a first polyethylene glycol and a weight average molecular weight of 3400 to 4500 The second polyethylene glycol may be provided at a molar ratio of 2.0 to 3.6: 1.

In addition, the present invention provides a hydrophilic softener composition for cellulose-based fibers produced by the manufacturing method according to the present invention.

In addition, the present invention provides a fabric having a cellulose-based fiber, and a fabric treated with a softener comprising a hydrophilic softening agent dried after the hydrophilic softener composition for cellulose-based fibers according to the present invention is treated on the fabric.

According to the present invention, the method of manufacturing a hydrophilic softener composition can produce a softener composition that can easily express excellent touch feeling, flexibility, absorbency, elasticity, and wash resistance when processing high sensitivity and high functionality of cellulose fibers. . In addition, even after the softener treatment, it can be re-salted without a separate removal process and can be widely applied to cellulose-based fibers as it is environmentally friendly with water as a solvent.

1 to 6 are graphs of FT-IR analysis results for a softener composition according to one preferred embodiment of the present invention, and FIGS. 1 to 6 are results of samples according to Examples 1 to 6, respectively.
7 is a photograph of the results of the evaluation of alkali stability and gum-up for the softener composition according to one preferred embodiment of the present invention and a comparative example.
Figure 8 is a photograph of the results of the pH stability evaluation for the softener composition according to one preferred embodiment and a comparative example of the present invention.
9 is a photograph of the fabric after re-salt evaluation for the softener composition according to one preferred embodiment and a comparative example of the present invention.

Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art to which the present invention pertains can easily practice. The present invention can be implemented in many different forms and is not limited to the embodiments described herein.

The hydrophilic softener composition for cellulose-based fibers according to the present invention comprises (1) a diisocyanate component containing an aliphatic diisocyanate and a diol component comprising polyethylene glycol having a weight average molecular weight of 2200 to 4500 at a molar ratio of 1: 1.4 to 1.9. It comprises a step of preparing a reacted polyurethane polymer, and (2) hydrophilizing the polyurethane polymer by treating the polyurethane polymer with an acidic solution.

First, as the step (1) according to the present invention, a diisocyanate component containing an aliphatic diisocyanate and a diol component comprising polyethylene glycol having a weight average molecular weight of 2200 to 4500 are reacted at a molar ratio of 1: 1.4 to 1.9. The step of preparing a urethane polymer is performed.

The aliphatic diisocyanate may be used without limitation in the case of a known aliphatic diisocyanate, but for example, 1,6-hexamethylene diisocyanate, (2,2,4) -trimethylhexamethylene diisocyanate, (2,4,4) ) -Trimethylhexamethylene diisocyanate and lysine diisocyanate. However, more preferably, it is preferable to select 1,6-hexamethylene diisocyanate in order to prevent yellowing or discoloration after treatment on a fabric having cellulose-based fibers.

On the other hand, the diisocyanate component may further include an aromatic or cycloaliphatic component, but it may be difficult to prevent discoloration of the fabric with cellulose-based fibers after softener treatment, and re-salting due to gum-up phenomenon, suspended matter having a large particle size, etc. Staining may occur, and a polyurethane polymer having a large particle size may be implemented, and thus may be unsuitable to achieve the object of the present invention, such as poor fabric penetration and thus poor processing, such as poor washing fastness.

The diol component includes polyethylene glycol having a weight average molecular weight of 2200 to 4500. The polyethylene glycol improves the hydrophilicity of the polyurethane polymer to enable water dispersion, and may contribute to the dispersion of the polyurethane polymer having an appropriate particle diameter. Preferably, the polyethylene glycol may include two or more types having different weight average molecular weights, and more preferably, first polyethylene glycol having a weight average molecular weight of 2200 to 3100 and second polyethylene glycol having a weight average molecular weight of 3400 to 4500. It may include, and more preferably, the first polyethylene glycol and the second polyethylene glycol may be provided in a molar ratio of 2.0 to 3.6: 1. Equipped with two types of polyethylene glycol having a weight average molecular weight as a diol component, in particular, when selecting 1,6-hexamethylene diisocyanate as a diisocyanate component, it exhibits a more elevated effect to achieve the object of the present invention. It can be advantageous. If the first polyethylene glycol is less than 2.0 times compared to the number of moles of the second polyethylene glycol, hydrophilicity may be significantly reduced and flexibility may be reduced. Furthermore, there is a concern that washing, sunlight, and friction fastness may deteriorate. Furthermore, it may be unsuitable to achieve the object of the present invention, such as the possibility of lowering the pH stability. In addition, if the first polyethylene glycol is provided in excess of 3.6 times based on the number of moles of the second polyethylene glycol, the particle diameter of the polyurethane polymer may be excessively large, and the fabric permeability may deteriorate. In addition, hydrophilicity may decrease or hydrophilicity may be insignificant. In addition, there is a possibility that washing, sunlight, and friction fastness may be deteriorated, and the possibility of yellowing is significantly increased in the fabric softly processed by phenol, etc., and a sticky float similar to gum-up is generated in the alkali solution, and due to the float having a large particle size, It may be difficult to achieve the object of the present invention, such as staining occurs during re-salting and the re-salting quality may be lowered.

Meanwhile, the first polyethylene glycol may include a third polyethylene glycol having a weight average molecular weight of 2200 to 2600 and a fourth polyethylene glycol having a weight average molecular weight of 2800 to 3100, and the third polyethylene glycol compared to the fourth polyethylene glycol is 1: It may be provided in an 8 to 13 molar ratio, through which may be more suitable to achieve the object of the present invention.

According to one preferred embodiment of the present invention, the fabric treated with a softener having a urethane-based component may have excellent elasticity, but may give a poor impression with a sticky wet feeling of touch. In order to solve this and improve a dry and soft touch feeling, the diol component may further include a polydialkylsiloxane containing a hydroxyl group at the sock end. The polydialkylsiloxane including the hydroxyl group in the sock end may be, for example, a polydimethylsiloxane including a hydroxyl group in the sock end, but is not limited thereto. In addition, preferably, the polydialkylsiloxane containing a hydroxyl group at the sock end may have a weight average molecular weight of 1700 to 2300. If the weight average molecular weight is less than 1700, it may be difficult to realize a soft touch feeling while being dry to a desired level. In addition, if the weight-average molecular weight exceeds 2300, the gum-up phenomenon may increase significantly, thereby greatly increasing the likelihood of occurrence of stains during re-salt, and significantly lowering the stability to pH, thereby achieving the object of the present invention. It can be difficult to do. More preferably, the polydialkylsiloxane and the polyethylene glycol may be included in the diol component at a ratio of 1: 4 to 14 moles, more preferably 1: 5.5 to 8 moles in terms of long-term durability security. If polyethylene glycol is provided in less than 4 times compared to the number of moles of polydialkylsiloxane, hydrophilicity may be remarkably deteriorated, and the color difference of the fabric may fluctuate compared to before the flexible processing in the case of flexible processing on the dyed fabric. It can be difficult to realize the color of the fabric. In addition, if the polyethylene glycol is provided in excess of 15 times compared to the number of moles of polydialkylsiloxane, a sticky suspension similar to gum-up is generated in the alkali solution, and staining occurs when re-salting due to a large-size suspension, and particle size analysis of the softener composition As the average particle size increases significantly, there is a possibility that the fabric permeability decreases, the possibility of non-uniform processing of the softener increases, and the washing, sunlight, and friction fastness may decrease.

According to one preferred embodiment of the present invention, the diol component may further include an alkanolamine in order to increase the hydrophilicity and increase the water absorption of the flexible processed fabric. The alkanolamine may be any one of diethanolamine and / or triethanolamine, and preferably, diethanolamine may be better in terms of improving hydrophilicity and maintaining color of the initial dyed fabric. In this case, the alkanolamine may be included in a molar ratio of 1: 2.5 to 6.2 with the polydialkylsiloxane containing the aforementioned hydroxy group at the sock end. If the polydialkylsiloxane containing the hydroxy group in the sock end is less than 2.5 times based on the number of moles of alkanolamine, hydrophilicity may be insignificant. Furthermore, fluctuations in the initial dyeing color may be caused. In addition, if the alkanolamine is provided in excess of 6.2 times, a sticky suspension similar to gum-up is generated in the alkali solution, and staining occurs when re-salting due to a large-size suspension, and the average particle size is significantly increased when analyzing the particle size of the softener composition. Accordingly, there is a possibility that the permeability of the fabric decreases, the possibility of non-uniform processing of the softener increases, and the wash, sunlight, and friction fastness may decrease. Furthermore, even in this case, fluctuations in the initial dyeing color may be caused.

In addition, according to a preferred embodiment of the present invention, the aliphatic diisocyanate is 1,6-hexamethylene diisocyanate, and the diol component is a polydialkylsiloxane containing a hydroxyl group at the sock end and an alkanolamine that is diethanolamine. Further comprising, the polydialkylsiloxane, the polyethylene glycol and the diethanolamine are contained in a molar ratio of 1: 4 ~ 14: 2.5 ~ 6.2, the polyethylene glycol is a first polyethylene glycol having a weight average molecular weight of 2200 ~ 3100 And a second polyethylene glycol having a weight average molecular weight of 3400 to 4500 in a molar ratio of 2.0 to 3.6: 1 to react. Fabrics processed with a softener composition comprising a polyurethane polymer prepared by reacting with such a composition express remarkably excellent hydrophilicity and water absorption, and can be re-salted without removing the softener, and at the same time, excellent re-salting such as no stain on the fabric when re-salting Quality can be achieved. In addition, it is possible to maintain water absorption for a long period of time due to excellent washing, sunlight, and color fastness. Furthermore, it is very environmentally friendly because it does not use harmful organic solvent because it can be dispersed. In addition, it can be very advantageous to achieve the object of the present invention, such as the flexibility and elasticity is excellent, and the touch feeling can be very excellent due to the soft and dry feeling.

Each component provided in the above-described step (1) can be reacted for 2 to 5 hours after being heated to a temperature of 80 to 110 ° C while purging nitrogen gas as an example after being introduced into the washed reactor. Thereafter, after cooling to 60 ° C. or less after a certain reaction time, F-NCO = 0, and an isocyanate peak of 2270 cm ^-1 does not appear in the FT-IR spectrum and a urethane bond peak of 1708 cm ^-1 appears as a reaction end point. It can be finished to prepare polyurethane polymer.

In the reaction of step (1) described above, a catalyst used in the polymerization reaction of polyurethane may be used, and the catalyst may be a commonly used catalyst, and the present invention is not particularly limited.

The polyurethane polymer prepared through the above-mentioned step (1) is then subjected to the step of being hydrophilized through an acidic solution as step (2).

The hydrophilization treatment may be a process for cationizing a polyurethane polymer, and the acidic solution may be acetic acid, for example. At this time, acetic acid may be an aqueous solution having a concentration of 1 to 3% by weight.

The softener composition prepared through the above-described method may be processed into a fabric having cellulosic fibers and dried to realize a flexible fabric.

The cellulose-based fibers may be known and cotton yarns, for example. Further, the fabric may be a fabric or a knitted fabric.

The softener composition may be treated at the temperature of 50 to 70 ° C for 20 minutes to 1 hour at a concentration of 25 to 50 g / L and then dried for 1 to 5 minutes at 100 to 150 ° C. Thereafter, the dried fabric may be further subjected to a solidifying process to fix it, and the solidifying process may be performed at a temperature of 160 to 200 ° C. for 30 seconds to 5 minutes to fix the softener component to the fabric. If the fastening conditions are not satisfied, there is a possibility that the fastness is significantly reduced.

The present invention will be described in more detail through the following examples, but the following examples are not intended to limit the scope of the present invention, which should be interpreted to help understand the present invention.

<Example 1>

As a diol component, 0.8 mol of the first polyethylene glycol containing 2.0 mol of the third polyethylene glycol having a weight average molecular weight of 2500 and 0.2 mol of the fourth polyethylene glycol having a weight average molecular weight of 3000, and the second polyethylene glycol having a weight average molecular weight of 3500 The containing polyethylene glycol was introduced into the reactor. Thereafter, the weight average molecular weight was 2200, and 0.5 moles of polydimethylsiloxane having hydroxyl groups at both ends and 1.5 moles of diethanolamine, alkanolamine, were introduced into the reactor. Thereafter, 3 mol of 1,6-hexadimethylenediocyanate was added as a diisocyanate component, and then the temperature was raised to 100 ° C. while purging nitrogen gas in the reactor to react. F-NCO was added every 10 minutes after 2 hours. When the measurement reached 0, the mixture was cooled to 40 ° C, treated with an aqueous 1.5% by weight acetic acid solution, and stirred for 30 minutes to prepare a softener composition according to Example 1 in which 30% by weight of the polyurethane polymer was dispersed / dissolved.

On the other hand, F-NCO was measured based on the method for measuring the isocyanate group content through the ASTM D2572 standard test.

<Examples 2 to 13>

Prepared in the same manner as in Example 1, but by changing the composition as shown in Table 1 to prepare a softener composition as shown in Table 1.

At this time, in Example 7, xylene diisocyanate (XDI) was used as the diisocyanate.

<Comparative Example 1>

A commercially available silicone-based softener composition was prepared.

<Experimental Example>

The following physical properties were evaluated for the softener composition according to Example and Comparative Example 1, and the results are shown in Table 1.

1. Average particle size analysis

The average particle size was measured using a particle size analyzer.

2. Evaluation of gum-up and alkali stability

In order to check the gum-up and alkali stability, 100 g / l of NaOH 50% solution and 100 g / l solution of softener were treated at 100 ° C. for 30 minutes, and the stability was visually observed.

3. pH stability

To confirm the pH stability, the softener composition was prepared with a 100 g / l solution of pH 8, 9, 10, 11, 12, and then maintained at 25 ° C. for 1 hour to observe stability.

At this time, when there was no problem, it was judged to be stable, and when there was an abnormality, an abnormal pH was described.

4. Remineralization evaluation

In order to confirm the re-staining property, a fabric of 30% Cotton 100% CI Blue 1% owf, bath ratio 1: 10 was prepared by first dyeing at 60 ° C for 40 minutes and then washing at 80 ° C for 20 minutes. Thereafter, the prepared fabric was treated with a softener composition 50g / l at 60 ° C for 30 minutes, and then dried at 120 ° C for 2 minutes. Subsequently, it was observed with the naked eye whether re-staining (secondary dyeing) and surface contamination occurred under the same conditions as primary staining.

When there was no abnormality in the evaluation results, it was marked as good, and when there was an abnormality such as a stain.

5. Evaluation of changes in dyeing quality due to softener treatment

Cotton 100% 30 number of fabrics were prepared by CI Blue 1% owf, bath ratio 1: 10, and the first dyeing at 60 ° C for 40 minutes followed by washing at 80 ° C for 20 minutes. Thereafter, the prepared fabric was treated with a softener composition 50g / l at 60 ° C for 30 minutes, and then dried at 120 ° C for 2 minutes. Subsequently, a softener-treated sample and an untreated sample were measured using a CCM (Computer Color Matching) System (Macbeth Color i7), and the color difference (E) change was measured based on the untreated sample.

Here, the larger the amount of color difference, the greater the variation in dyeing quality compared to when not processed due to the processing of the softener.

6. Fastness

Cotton 100% 30 number of fabrics were prepared by CI Blue 1% owf, bath ratio 1: 10, and the first dyeing at 60 ° C for 40 minutes followed by washing at 80 ° C for 20 minutes. Thereafter, the prepared fabric was treated with a softener composition 50g / l at 60 ° C for 30 minutes, and then dried at 120 ° C for 2 minutes. Then, the fastness was evaluated according to the following standardized method for the fabric.

* Light fastness: KS K ISO 105-B02: 2014 xenon arc (water cooling, method 3, standard blue dyeing)

* Washing fastness: KS K ISO 105-C06: 2014 A2S ((40 ± 2) ℃, 30 minutes, ECE detergent)

* Friction fastness: KS K ISO 105-X12: 2016 Croquet method

7. Yellowing

Cotton 100% 30 number of fabrics were prepared by CI Blue 1% owf, bath ratio 1: 10, and the first dyeing at 60 ° C for 40 minutes followed by washing at 80 ° C for 20 minutes. Thereafter, the prepared fabric was treated with a softener composition 50g / l at 60 ° C for 30 minutes, and then dried at 120 ° C for 2 minutes. Thereafter, in order to confirm the potential for yellowing of phenol, the fabric was evaluated according to KS K ISO 105-X18: 2007 standard.

8. Absorbency

Cotton 100% 30 number of fabrics were prepared by CI Blue 1% owf, bath ratio 1: 10, and the first dyeing at 60 ° C for 40 minutes followed by washing at 80 ° C for 20 minutes. Thereafter, the prepared fabric was treated with a softener composition 50g / l at 60 ° C for 30 minutes, and then dried at 120 ° C for 2 minutes. Thereafter, in order to confirm the degree of hydrophilicity to the fabrics produced, the absorption rate was measured by the dropping method of KS K 0642,8.26.2.1: 2016.

Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative Example 1 U
year
My
article
castle
water Diisocyanate
(Type / Number of moles) HDI / 3.0 HDI / 3.0 HDI / 3.0 HDI / 3.0 HDI / 3.0 HDI / 3.0 A commercial item D
Come
castle
minute 2PEG
(Mw, confiscation) 3500 / 0.8 3500 / 0.8 3500/1 3500 / 0.8 3500 / 0.55 3500 / 0.65 1PEG
(Mw, confiscation) 4PEG 3000 / 0.2 3000 / 0.2 3000/0 3000 / 0.2 3000 / 0.45 3000 / 0.35 3PEG 2500/2 2500 / 2.5 2500 / 2.5 2500 / 2.5 2500 / 2.5 2500 / 2.3 1PEG: 2PEG molar ratio 2.75: 1 3.38: 1 2.5: 1 3.38: 1 5.36: 1 4.08: 1 PEG total moles 3.0 3.5 3.5 3.5 3.5 3.3 Alkanolamine
(Type / Number of moles) Diethanolamine / 1.5 Diethanolamine / 1.5 Diethanolamine / 1.5 Diethanolamine / 1.5 Diethanolamine / 1.5 Diethanolamine / 1.6 PDMS (confiscation) 0.5 0.5 0.25 0.25 0.21 0.22 PDMS: PEG molar ratio 1: 6 1: 7 1:14 1:14 1: 16.7 1:15 PDMS: Alkanolamine Molar Ratio 1: 3 1: 3 1: 6 1: 6 1: 7.1 1: 7.3 Total Dior 5 5.5 5.25 5.25 5.21 5.12 water
castle Average particle diameter (nm) 158 157 154 154 1236 1145 - Sword-up none none none none none none Occur Alkali stability Microparticle suspension Microparticle suspension Microparticle suspension Microparticle suspension Coarse particle floating material Coarse particle floating material Microparticle suspension pH stability stability stability stability stability pH12 pH12 pH11 Remineralization Good Good Good Good Bad Bad Bad Light fastness (class) 4-5 4-5 4-5 4-5 3-4 3-4 4-5 Washing fastness (class) 4-5 4-5 4-5 4-5 3-4 3-4 4-5 Friction fastness (case) (class) 4-5 4-5 4-5 4-5 2-3 2-3 4-5 Friction fastness (humidity) (class) 4-5 4-5 4-5 4-5 2-3 2-3 4-5

Comparative Example 2 Example 7 Example 8 Example 9 Example 11 Example 12 Example 13 U
year
My
article
castle
water Diisocyanate
(Type / Number of moles) XDI / 3.0 HDI / 3.0 HDI / 3.0 HDI / 3.0 HDI / 3.0 HDI / 3.0 HDI / 3.0 D
Come
castle
minute 2PEG
(Mw, confiscation) 3500 / 0.8 3500 / 1.0 3500 / 1.2 3500 / 0.8 3500 / 0.8 3500 / 3.0 0 1PEG
(Mw, confiscation) 4PEG 3000 / 0.2 3000 / 0.2 3000 / 0.2 3000 / 0.2 3000 / 0.2 0 0 3PEG 2500/2 2500 / 2.0 2500 / 1.6 2500/2 2500 / 2.0 0 2500 / 3.0 1PEG: 2PEG molar ratio 2.75: 1 2.2: 1 1.5: 1 2.75: 1 2.75: 1 2.75: 1 2.75: 1 PEG total moles 3.0 3.2 3.0 3.0 3.0 3.0 3.0 Alkanolamine
(Type / Number of moles) Diethanolamine / 1.5 Diethanolamine / 1.5 Diethanolamine / 1.5 Diethanolamine / 1.0 Triethanolamine / 1.5 Diethanolamine / 1.5 Diethanolamine / 1.5 PDMS (confiscation) 0.5 0.55 0.5 0.5 0.5 0.5 0.5 PDMS: PEG molar ratio 1: 6 1: 5.8 1: 6 1:14 1: 6 1: 6 1: 6 PDMS: Alkanolamine Molar Ratio 1: 3 1: 2.7 1: 3 1: 2.0 1: 3 1: 3 1: 3 Total Dior 5 5.25 5 4.5 5 5 5 Properties Average particle diameter (nm) 385 169 245 154 161 229 230 Sword-up none none none none none none none Alkali stability Microparticle suspension Microparticle suspension Microparticle suspension Microparticle suspension Microparticle suspension Microparticle suspension Microparticle suspension pH stability stability stability pH12 stability stability pH12 pH12 Remineralization Bad Good Good Good Good Good Good Light fastness (class) 4-5 4-5 4-5 4-5 4-5 3-4 3-4 Washing fastness (class) 3-4 4-5 3-4 4-5 4-5 3-4 3-4 Friction fastness (case) (class) 3-4 4-5 4-5 4-5 4-5 3-4 3-4 Friction fastness (humidity) (class) 3-4 4-5 2-3 4-5 4-5 3-4 3-4

As can be seen from Table 1 and Table 2,

In the case of Comparative Example 2 using an aromatic diisocyanate component, it can be seen that even though a combination of diol components embodied to have excellent effects in the present invention was applied, physical properties were significantly poor compared to Example 1.

In addition, the softener having a commercially available silicone-based component as in Comparative Example 1 has poor re-salting properties, poor pH stability, and can be found to be particularly poorly absorbent.

Although one embodiment of the present invention has been described above, the spirit of the present invention is not limited to the embodiments presented herein, and those skilled in the art to understand the spirit of the present invention can add elements within the scope of the same spirit. However, other embodiments may be easily proposed by changing, deleting, adding, or the like, but it will also be considered to be within the scope of the present invention.

Claims (11)

(1) A diisocyanate component composed of an aliphatic diisocyanate containing 1,6-hexamethylene diisocyanate, a polydialkylsiloxane containing a hydroxyl group at the sock end, an alkanolamine as diethanolamine, and a weight average molecular weight of 2200 Preparing a polyurethane polymer in which a diol component containing polyethylene glycol of ~ 4500 is reacted at a molar ratio of 1: 1.4 to 1.9; And
(2) hydrophilizing the polyurethane polymer by treating the polyurethane polymer with an acidic solution;
The polydialkylsiloxane, the polyethylene glycol and the diethanolamine are contained in a molar ratio of 1: 4 to 14: 2.5 to 6.2, and the polyethylene glycol is a first polyethylene glycol and a weight average molecular weight having a weight average molecular weight of 2200 to 3100. Method for producing a hydrophilic softener composition for cellulose fibers, characterized in that the second polyethylene glycol of 3400 ~ 4500 is provided in a molar ratio of 2.0 ~ 3.6: 1. According to claim 1,
The aliphatic diisocyanate further comprises at least one selected from the group consisting of (2,2,4) -trimethylhexamethylene diisocyanate, (2,4,4) -trimethylhexamethylene diisocyanate and lysine diisocyanate. A method for producing a hydrophilic softener composition for cellulose fibers. According to claim 1,
Method of producing a hydrophilic softener composition for a cellulose-based fiber, characterized in that the acidic solution of step (2) is an acetic acid solution. delete delete According to claim 1,
The alkanolamine method of manufacturing a hydrophilic softener composition for cellulose fibers, characterized in that it further comprises a triethanolamine. delete delete delete A hydrophilic softener composition for cellulose-based fibers, characterized in that it is prepared according to any one of claims 1 to 3 and 6. Fabric with cellulose-based fibers; And
A softener-treated fabric comprising; a hydrophilic softener for cellulose-based fibers according to claim 10, dried after being treated on the fabric.

Images