JPS62257465A - Antistaining nylon fiber - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

BACKGROUND OF THE INVENTION Field of the Invention The present invention relates to nylon 4M fibers having unusual and advantageous dyeing properties. In particular, the present invention is less susceptible to staining by acid dyes at ambient temperatures, but at elevated temperatures.
6. Concerning nylon fibers, which can be dyed without staining with acidic dyes at ambient temperature, ordinary nylon fibers can be used at room temperature for food, cosmetics, pharmaceuticals, food, cosmetics, pharmaceuticals, etc.
The nylon fibers of the present invention have the ability to be resistant to smearing normally caused by those colorants at room temperature. and is therefore particularly suitable for use in carpet manufacturing.

The term fiber as used herein includes fibers of very long or indefinite length (i.e., filaments) and fibers of short length! J! II <i.e. staples> 3
nothing.

The term yarn as used herein refers to a continuous thread consisting of multiple fibers.

"Stain" and "dirt" as used herein with respect to nylon fibers
The term "stain" refers to the discoloration of such fibers caused by the chemical reaction of such fibers with substances such as acid dyes.

[6゛C Prior Art] Carpets made from nylon fibers are popular floor coverings for both residential and commercial applications. Such carpets are relatively inexpensive and offer a desirable combination of properties such as durability, aesthetic appeal, comfort, safety, warmth and sound deadening. Also, it is available in a variety of attractive colors, patterns, and fabrics. However, nylon fiber is Kool-Aid.
Carpets made from nylon fibers are severely and permanently stained by certain artificial and natural colorants present in common household products such as id) and other soft drinks. Most of these colorants are acid dyes, which are easily damaged by spillage.
All of them are approved by the Food, Drug and Cosmetic Commission as acceptable for human consumption. It
is one of the commonly used acidic dyes, and the one that stains nylon most severely at room temperature is F&D.
C Red D ey N o, 40 (hereinafter referred to as Red D ey N o, 40), Red D ey N o, 40 (C, T ).

Nylon carpet melts (also known as food fleds 17) have the following flI structure: fluor.

chemical'). The fluorine compounds reduce the tendency of dirt to stick to the fibers, thereby making it much easier to remove stains from the carpet than without the fluorine compounds. This fluorine treatment also reduces the wettability of the fibers, but for spills containing acid dye colorants, it is best to remove such colorants for 5 to 7 minutes.
Very little C1 is applied to the carpet unless it is immediately removed from the carpet within minutes. In contrast to substances such as lipstick, shoelaces, and motor oil, which can be physically removed from nylon carpet by well-known cleaning methods, Red Dye No.
Acidic dyes such as No. 40 penetrate the nylon and chemically react with it, forming such dyes that they cannot be completely removed from the nylon fibers. are actually stained by these colorants within minutes and are therefore permanently stained.

Looking around the carpet replacement market, we see that more Carbela 1s are being replaced due to wear and tear. bCSo, in this field, what is l?
There is a need to provide nylon carpet fibers that can make carpets that are resistant to scratches.

[Summary of the invention]

The present invention is resistant to stain resistance to acid dye colorants at ambient temperatures, but at elevated temperatures, without losing their resistance to acid dye colorants at that temperature. Nylon 8XI tI 'r-'''J, j. The invention is characterized by having a coating on its surface comprising one or more soil barrier agents in an amount sufficient to provide the fibers with an amount of at least one soil barrier agent.

As used herein, the term "stain 3I!! remover" means that when applied as a coating to nylon fibers in an amount of 0.35% or less based on the weight of the fibers, the dye absorption test value at 25°C is 796 or less. It means a compound that gives 30% or more fiber at 100°C.

The fibers of the present invention are particularly useful in providing stain resistant nylon carpets. Such carpets can survive prolonged exposure to large spills of substances containing acid dye colorants, such as red wine and soft drinks.

According to a preferred embodiment of the invention, the coating on the surface of the fibers is such that when one or more fluorine compounds are used in the manufacture of the carpet, the fluorine compounds are used to increase the initial stain resistance of the carpet. They contain one or more fluorine compounds in a sufficient amount to provide carpet fibers that maintain to a greater extent even after being subjected to 30,000 walks than do their untreated counterparts. Contains in addition to stain blocker. The term "walking" used here
means that a case has occurred where an individual walks across the carpet. "Initial stain resistance" means the stain resistance of the new Carbella I~ before it is exposed to foot traffic or other wear. Fluorine compounds by themselves do not impart significant stain resistance to nylon fibers, and when used in conjunction with a stain blocker, they provide even better stain resistance initially (i.e., walking) than the stain blocker itself provides. However, the use of one or more fluorine-containing compounds in conjunction with a stain barrier can reduce the initial stain resistance imparted to the fiber by the stain barrier. It was completely unexpected that it would improve the maintenance of.

[Preferred specific example]

What kind of nylon! a jI to the present inventionC-)＞+l
rQ You can also do it. Commercially important nylon fiber HIE
is a fiber formed from nylon 66 (polyhexamethylene adipamide) and nylon 6 (polycaprolactam).The present invention is particularly useful for providing nylon carpet yarns that can be made with stain-resistant carpet. The coating is preferably applied to the nylon fiber from a finish (spin finish) during the melt-spinning process used to produce the fiber, typically comprising appropriate amounts of soil barrier agents and fluorine compounds. l) of the fibers in a finishing agent containing lubricating oils and dispersants for such oils;

Soil barrier agents particularly useful in the practice of this invention include, by way of example, condensation polymer products consisting essentially of repeating units of the formula:

(where X is hydrogen or a cation such as sodium or potassium) These condensation products are commercially available;
fruit! It can be made using traditional methods in a laboratory. Preferred condensation products of this sideway include at least 40 to 6 of the repeating units, X groups, and at least 10% of the 11-positions of the repeating units are of : A water-soluble product containing a merging group.

The molecular weight of the S-I condensation product should be as high as possible while maintaining some water solubility, and should contain as many monosulfonated phenyl groups as possible.

Such products may contain one or more suitable phenols (or derivatives thereof) of the following formula:
and formaldehyde in an acidic or alkaline medium at elevated temperatures. Typically, in acidic media, 0.3 to 0.5 moles of formaldehyde are used per mole of phenol, and in basic media, 0.9 to 1.5 moles of formaldehyde are used per mole of phenol. It is used as 11
The solubility of the synthesis product in water is influenced by the type of end groups present in its structure, such as -CI+ 20 H and -CH,5
Hydrophilic moieties such as O3H make the product more water soluble than hydrophilic moieties such as methyl or phenyl groups. Basic condensation gives a product with a greater proportion of terminal -CII,OH groups and therefore greater water solubility.

The polymerized cotton-containing product obtained from the above-mentioned purified unit is obtained by acetylating the hydroxyl group of diphenol sulfone, then sulfonating it, and then hydrolyzing it to convert the acetylated hydroxyl group into a free hydroxyl group. It can also be produced by a method of converting it to its original state, and then reacting it with formaldehyde under alkaline or acidic conditions. In this case, reaction step f't-1 is selected to avoid or at least minimize the formation of products containing di- and/or trisulfonated phenyl groups. in general,
Condensation products in which the repeating unit contains only one -SO,X group are more effective soil barrier agents than corresponding products in which the repeating unit contains two or more -SO,X groups. Again-
Finally, one -S for a unit containing no -SO,X group
As the proportion of units containing O,X groups increases, the product becomes a more effective soil barrier.

Condensation products of formula I are commercially available; for example, mixed condensation products of phenolsulfonesulfone and formaldehyde are available from Ciba-Geigy Co., Ltd.
rp. ) to E rional P A
It is available under the trademark name Crompton or Crompton.
& Knowles, Inc. (Crossρton - an
It is available under the trade name inLraLex N from Knowles Corp.

Also useful as a stain barrier agent in the practice of this invention are mixed condensation products of naphthalene monosulfonic acid, dihydroxy diphenyl sulfone, and formaldehyde. Such a product is commercially available from Ciba Geigy under the trade name Elional NW.

Fluorine compounds useful in the practice of this invention can be applied as a coating to nylon fibers in combination with a stain barrier, and the fluorine compound and soil barrier can be combined at 0.35 parts by weight, based on the weight of the fibers. % stain barrier and 650 ppm of fluorine, and the fibers are used in the manufacture of carpet, the carpet will have a higher fluoride content than if the fluorine compounds were omitted from the coating. to a large extent,
It is a fluorine compound that maintains its initial stain resistance even after 30,000 walks. Such fluorine compounds include, by way of example, those commercially available from Minnesota Mining and Manufacturing Company under the trademark Scotchgard (Scotchgard 358 and 352), and E.

■ Includes those commercially available for use with fibers, such as those commercially available from DuPont de Numer & Company under the trademarks Zcpel and Deflon. Typically, these fluorine arsenides contain a perfluoroalkyl group <Rf) having 3 to 20 g of carbon and are a condensation product of RfOH or "RrNH2 with a suitable anhydride or incyanate, e.g.
N-ethyl perfluorooctyl-sulfonamide is the reaction product of ethanol and tolulene diisocyanate in a 2:1 molar ratio.

The coating of the nylon fibers of the present invention, preferably o, zo-0,35% by weight based on the weight of the nylon (2000~
3500ppm) stain blocker and nylon ff1f
According to four preferred embodiments of the invention, the soil barrier and the fluorine compound may be applied separately or simultaneously, including sufficient fluoride to provide 450 to 650 pp- of fluorine based on fi. For example, the stain barrier and fluoride are simultaneously applied to the nylon fiber from the finish. According to this embodiment, the soil spinner and the fluorine compound are of the same polarity, ie both anionic or cationic, to avoid the possibility of their precipitation in the finish. Sulfone-1 mentioned above
Containing soil barrier agents are anionic and therefore it is preferred to use anionic fluorine compounds when using these soil barrier agents, but do not form suitably stable finishes containing components with opposite charges. It is possible to select a suitable dispersant to do so.

From a large variety of soil barrier agents and fluorine compounds, it is possible to select the optimal combination of soil barrier agent and fluorine compound for a particular application, and to make that selection the optimum combination of soil barrier agents and fluorine compounds to be applied under the given conditions of the combination. For a given nylon fiber i
Fine tuning to give the desired result is accomplished by routine experimentation that is within the ability of one skilled in the art by simply testing various combinations of ingredients and selecting the combination that gives the best results. I can do it.

Typically, the nylon carpet yarn that is ready for tufting is a double staple or continuous monofilament yarn that is subjected to heat treatment to set the twist in the yarn. The process is referred to as heat curing. Conventionally, the heat curing operation is accomplished using a Superba device in which the yarn is exposed to steam at about 130-140°C or a Suessen device in which the yarn is exposed to hot air at about 195-205°C. 9. The adhesion of the coating to the nylon fibers of the present invention is facilitated by subjecting the coated fibers to heat curing conditions. High IfL adhesion of the coating to 1M fibers is achieved when the coating incorporates a soil barrier with end groups that can further react with the surface of the nylon during heat curing, or that can react themselves. The reaction between the end groups of the soil barrier and the nylon surface is a covalent bond.

Dirt 3j with such groups! The cutting agents include those made with alkaline strips C':i.

Preferably, the stain barrier and the fluorine compound have a fluorine content of 4% or less, most preferably 0 or substantially 0 (O 2 have a dye absorption test value of at least 30% at 100°C (no visible stains), but preferably also
Selected and applied to nylon fibers to provide fibers with a dye absorption test value of at least 60%.

The dye absorption test value obtained here is Red Dye No.
, 40 by determining the % of the dye absorbed by a fiber sample from an aqueous solution of 40, versus the temperature of the solution. The test is accomplished as follows: (1) 4 degrees of dye is 0.054 g#! Prepare an aqueous solution of Red Dye No. 40. (This is the concentration of Red Dye No. 40 in Cherry Kool-Aid when mixed with water according to the commercial package ingredients and instructions written on the package.) (2) Light absorption value of the solution (optical density) is the carry (C
ary) Type 15 spectrophotometer or equivalent device, 1/2
The measurement was carried out using an e11 cell, and the measurement was carried out at 495+a+aμ, where Red Dye No. 40 shows the maximum absorption rate (the light absorption rate is a measure of the dye concentration of the solution).

(3) Record the light absorption reading as To.

(4) Next, 0.25. Trial I! 14.8m of A-fiber T・1
ml of Red Dye No. 40 solution is placed in a container, and the pH of the 8-ml solution is adjusted to 3 by adding an appropriate amount of Universal Buffer.

(5) The two containers are then hermetically sealed, e.g. with a lid) and heated, e.g. by a motorized vibrator, at the selected temperature for 3 hours, the temperature being regulated by a thermostat. (6) The fibers are then removed from the solution and the light absorption of the solution is measured again as before.

(7) Record the reading at this time with T. (If the fiber sample was not stain-resistant, it would absorb the dye r4 from the solution and the value of T1 would be less than the value of Tll; on the other hand, if the fiber sample was not stain-resistant) Then, without taking up too much dye from the solution, T
(8) The dye absorption test value at the selected temperature is T. % of the value of
Expressed as: Calculate as follows: Dye absorption test value (%)
=(T,-T,)/T,X100 The following examples are given to further illustrate the invention.

Example 1 In this example, nylon 66 fibers of the present invention were prepared and tested to illustrate their resistance to staining.

300 single fiber, denier per piece (dpf) 6
0 nylon 66 yarn was extruded from commercial grade fiber-forming nylon 66 at a melt temperature of 282° C. down through the holes of a 300-hole spinneret into a conventional melt-spun upright cylinder approximately 1.8 m long. It was produced by forming a corresponding number of melt streams. The upright cylinder has cooling air at an ambient temperature of 27
It was used to receive cross flow at a speed of 0 m/min. The melt stream solidified in an upright cylinder to form a single fiber. The monofilaments are passed from an upright cylinder through a conventional water vapor conditioning tube about 1.8 cm long, where they
The fibers were treated with steam. The monofilament tag is sent from the Corr4 conditioner pipe to a conventional metered finish application machine where it is applied with a stain blocker and a fluorine-containing compound, each at a concentration of 3,500 ml based on the fiber base.
An aqueous finish containing 650 ppm of soil barrier and a water-based finish sufficient to provide 650 ppm of filtration was applied and the single 1 lltli was collected to form a yarn as it passed around a dynamic feed roll. Feed (450m/min), and f
f - The 0th order yarn that has been wound several times on the weave separation roll and fed is then collected on the bobbin by applying slight tension to promote the winding of the yarn onto the bobbin. It was unwound and combined with 54 similar rings to form a tow with a total denier of approximately 1,000,000. Pull the tow onto the roll, giving a nominal 18 dpf tow,
Crinkled in a traditional crimping box, 19.05cm (717
2 inch) staples. The staple is fluffed, stretched, and protected with a conventional circular spinning frame, and the number of rotations per 11A in two directions (LpIll) is approximately 177 (1i
31 with twist of rotation per n (tpi) 4.5)
/ Gave second single yarn. Two of these yarns were then twisted together with a twist of 157 Lp+@(4,0 tpi) in the S direction. A portion of the twisted yarn was heat cured at 200°C using conventional Suesen heat cure conditions.

Soil 31 used to produce the thermoset and non-thermoset yarns described above! Detergent (stain shielding agent A)
) consists essentially of repeating units of the following formula:

and R' is at least 50% of the units -S O3N
m, and hydrogen in the remaining units. The fluorine 16 compound used to form these yarns and fAs was a mixture of anionic fluorine compounds based on N-ethyl-perfluorooctyl-sulponamide ethanol.

Dye absorption test values for trial t1 of heat-set yarn (Yarn E) and non-heat-set yarn (Yarn D) were determined at various temperatures shown in Table I below.

(f!!, the cured yarn is represented by curve E in Figure 1, and the non-thermoset yarn is represented by the curve.) Both Yarn E and Yarn D are within the scope of this invention. It is thought to be yarn. In another experiment, thermoset yarns and non-thermoset yarns (control) were
A sample of the control yarn (Yarn A) was prepared in the same manner as described above, except that in this case the stain barrier and the fluorinated compound "r1" were omitted from the finish. Dye f: [Absorption test (direction was determined and is shown in Table I. (This yarn is represented by curve fi A in Figure 1.) Heat-cured control yarn (conventional nylon carpet yarn) ) samples from US Ti Special Fraud No. 3 and 11
8,72:1, 2ffi% acetic acid and 0
．． Aqueous Rakuchu including 26 5-star Elional NW:
A1'''l obsess, then evacuate the bath for 320 minutes; maintain the boiling bath for a further hour;
The yarn was removed from the bath and then processed by washing and drying the yarn. The dye absorption test values of this yarn (Yarn B) were determined and are also shown in Table 1. (
This treatment of the yarn (this yarn is represented by curve B in Figure 1) was carried out by adding Elional NW to the dye bath as a dye adjuvant (equalizer or preservative) during beak dyeing of the carpet. Similar to carpet treatment.

A second sample of non-thermoset control yarn was also treated in the manner just described according to the teachings of U.S. Pat. No. 3,118,723 (Example 2 thereof).
Heat curing was achieved by heating the sample in an air atmosphere for 1 minute, then cooling to ambient temperature.

This place is FI! Dye absorption test values for the heat-cured yarn (Yarn C) were determined and are also shown in Table I below.

(This yarn is represented by the curve FiC in FIG. 1.) Yarn C is considered to be a yarn within the scope of the present invention. The processing of this sample is steam treated in that in this case sample f:l is treated and then heat cured whereas in the above example the sample is heat cured and then heat cured.
It is different from the conventional method.

FIG. 1 is a plot of the data given in Table I. Curves A, B, and C in FIG. 1 each end at a point defined by the intersection of the coordinates 100° C. and 100%.

"Shishi" - Dye bath "L suction" (Value Yui υ-゛Temperature -■ Contrast Conventional ("C)
Yarn yarn yarn yarn yarn CDF,
No＼ B25
6.4 0.0 0.0 75.3 18.1
'30 9.6. 1.6 0.0 100.
0 30.935 14.1 1.6 0.0
54.940 20.2 4.3
0.0 79.5i5 31.9
6.6 1.6 93.150
53.2 10.1 2.7 100.
055 76.1 14.9 3.260 8B
, 2 16.2 3.765 90.4 17.6
4.370 95.7 20.7 4.375
99.2 23.9 4.880 100.0
31.4 6.185 37.8 1
1.790 52.1 18.095
59.0 29.8100 100.0
67.0 34.8 100.0 100.0 The data shown in Table I and shown in FIG. lt dramatically demonstrates the unusual stain-resistant properties of the nylon fibers of the present invention. The u1 fibers represented by curves A and B with respect to FIG.
The fiber represented by the 0 curve C (invention) stains to a light pink color at 25°C and lacks significant stain resistance properties, staining to a light pink color at 25°C, which is barely acceptable for some carpet yarn applications. It is worth noting that the fibers represented by curves aD and E did not stain at all at 25°C, although they were nevertheless significantly less stained than the fibers represented by curves A and B. be.

Example 2 This example uses nylon AaH1 with a fluorine compound and a stain blocker.
1 illustrates the unexpected benefits obtained by coating This example demonstrates that carpets made from these fibers maintain their initial stain resistance to a greater extent after walking than corresponding carpets made from nylon fibers coated with only a stain barrier. It shows.

68 single fiber with denier per sheep fiber (dpf) of 6
0 nylon 66 yarn 13 wood was produced. Each yarn is prepared by extruding commercial grade fiber-forming nylon 66 at a melt temperature of 274°C downward through three holes in a 68-hole spinneret into a conventional melt-spun upright cylinder approximately 1.8 rings long. was produced by forming several melt streams.

The upright cylinder was used to receive 18.3°C cooling air flowing crosswise at a flow rate of 11.2 m'/min.

The 'lFJ melt solidified in the upright cylinder to form single fibers.

The filaments were passed from an upright cylinder through a conventional steam conditioning tube approximately 1.8 mm in length, where they were treated with steam. The single fiber is from the adjustment tube to the conventional light n1L
- sent to a top applicator where an aqueous finish containing a stain barrier (or) fluorine compound was applied; The stain blocker used in this example was Elional PA, and the fluorine
The drug was Scotchgard FC358. The contents of the soil blocking agent and the fluorine compound were varied for each yarn as shown in Table 3.

Two of these yarns were twisted together as described in the Examples and then passed through a draw loom to produce fibers of approximately 18 dpf. The resulting double yarns were heat cured (200° C. for 1 minute) in a Suesen thermosetting apparatus and the yarns were used to make two similar samples.

Each of the samples contained 13 bands, each band being tufted with a different yarn. The obtained 26 wood strips are 2.5ffi amount% [about the weight of the product (owg):
1 of CalHon and 1.0% by weight of 011
11 alkanol (A 1kanol) N B and 2
．． The fabric was dyed using a solution of 0% by weight of itM ammonium at a 40:1 liquid-to-liquid weight ratio.The strips and the solution were then heated for 55 minutes to incubate, without stirring. The mixture was maintained at boiling point for an additional 60 minutes while stirring. The strip was rinsed with water and rolled three times to ensure 200% water uptake with each rinse, and finally dried at ambient conditions for 48 hours.

A set of fabric-dyed strips was tested to determine the stain resistance of different strips. That test is red die no.
, 40 at a concentration of 0.054 g/l on the surface of each strip.

(0,054 g/l is the concentration of Red Dye No. 40 in Cherry Kool-Aid.) The solution was applied to the strip by applying pressure with a spatula. A red dot formed on each band. (10 to 20 strokes of the spatula are usually sufficient to ensure that the fibers are penetrated with the solution.) Each strip was then treated as follows. Seven more drops of the solution were applied to the spot, rubbed in with a spatula and left for 10 minutes. After 10 minutes, blot the spot with an absorbent paper towel until no more solution can be absorbed.
Let dry for an hour.

Each strip was then cleaned using the following steps. 4#+1 of carpet cleaning solution was applied to the wick.

Cleaning solution is prepared using 28.4g of Steel 11.
Clean (S RealICI+41111) 300P
G (70 Cutter and Gamble Co. (ProcL)
(commercially available from Gamble Co., Ltd.) fi:473aal was prepared by adding it to deionized water. The cleaning solution was allowed to sit on the stain for 30 seconds and then blotted dry with an absorbent paper towel. Then 4 ml of vinegar (5% acetic acid in deionized water) was applied to the stain and left in contact with the stain for 30 seconds. I left it behind. After 30 seconds, the stain was absorbed and dried. Then apply 4ml of carpet cleaner to the stain,
It was left for 30 seconds and then blotted off. Finally 10
Apply 1 m of deionized water to the stain and blot the stain until dry 1) Then clean the area without staining 1)
A comparison was made with six strips pre-stained with Red Dye No. 40 to various degrees of soiling ranging from fully soiled (6). In this case, the color difference between adjacent stain levels was substantially the same. I attached it to the strip and the board, matched the test strip to the strip on the board, and determined its number. For numbers less than 2, decimal scale was used to indicate the value of the rm tree of 1 and 2.

Bands rated 2 or higher were judged to have no meaningful stain resistance and therefore failed the test. 30,000 for the second set of selected bands
Subject the floor test to the first gait and then the stain resistance test described above to determine what influence, if any, gait (I; 粍) can have on the initial stain resistance of the belt. The test blooming results before and after one walk are shown in the 21st page.

Mu'eyan Dirt Fluorine - Five Pressure Moxa l Moxibustion---Sample 3I! Abstinence Compound = 1 2^1 beans
0.08 5 (fail) No test 2^2
200 4 (failed) No test 2^3
0.08 200 3 (Fail) 428
1 0.1 [+ 4 (Fail) Not tested 282 400 2 (Fail) Not tested 283 0.16 400 1.2
32C10,241,84 2C213001,54 2C30,246001,12 2010, J2 1.2 4202
800 1.4 42D3
0. :J2 800 1.0 1.6 Control 6 (Fail) Not tested Figure 2 is a plot of the data shown in Table 2. In Figure 2, the dirt grade numbers not in parentheses are before walking (
*), and those in parentheses are those determined after walking <**>.

The results given in Table 2 and shown in Figure 2 are based on nylon fibers (e.g. 2D
3) is the corresponding 41 fiber (2D1>
This shows that after walking, their initial lη resistance remains to a greater extent. These results indicate that the concentration of stain blocker and fluorine compound is the 4th factor in stain resistance.
It shows the impact that

Example 3 In this example, nylon fibers were coated with a fluorine compound or a stain blocker or a combination thereof and then tested for stain resistance.

A twisted yarn was prepared as described in Example 1. However, in one case it contains both stain blocker A and a fluorine compound (control yarn); in the case of ponds, the finishing agent contains stain blocker A.
In the case of ponds, the finish contains fluorine compounds but no stain blockers (F, C, yarns); In the example, the finish contained both stain blocker A and a fluorine compound (S
, I3. + F, C.

The fluorine compound used in this step was the same as in Example 1.
It was the same as that used to make the yarn described in .

The stain blocker and fluorine compound, if present in the finish, are present in amounts sufficient to provide the yarn with 3500 ppm stain blocker and 650 ppm fluorine based on the weight of the yarn. Ta. All yarns were heat cured at 200° C. using regular Suesen heat cure conditions. The dye absorption test values of each yarn sample were determined at 30°C and 100°C and are shown in the following table.

Jξ and dye J yield value (%) Yarn 30” 100°
Teru 85' 10
0S, 8. 5
68S, [l -F, C563 F, C73100 The results in Table 3 show that the fluorine compound itself is nylon lJ!
This shows that it does not impart any significant stain resistance to H.

These results further demonstrate that the use of fluorine compounds together with the stain blocker did not improve the stain resistance of the stain blocker, thereby limiting the value of the combination to the initial stain of Shaohang Ling. The results given in Example 2 can be confirmed in terms of maintenance of resistance to dirt, that is, durability of resistance to staining.

Example 4 Two 3172 count single yarns were made as described in Example 1, except that the soil barrier was Intratex N and the yarns were not individually heat cured. No fluorine compounds were used. The yarn is 118 tpn (3 tpi) in the S direction using a conventional circular twisting machine.
Twisted together with a twist.

The resulting twisted yarn was then heat cured at 200°C using a Suesen thermoset f'lZ. A cut pile tufted carpet sample f1 was made from twisted stable yarns that had been heat set and dyed a bright gold color. A bright gold color was chosen as it contrasts well with most stains.

A 1"l carpet sample was soaked in the common household liquid substances listed in the table below to determine the resistance of the samples to staining by the colorants present in these substances.

Each substance is applied to a carpet sample, rubbed into the carpet, left on the sample overnight, and finally removed on the next day by washing the sample first with a dilute aqueous solution of a commercially available detergent and then with water. Removed. For comparison purposes, a carpet sample (control)
was made in the manner described above.

However, in this case the yarns from which the samples were made were not treated with Intratex N. In other words, Intratex N
was excluded from the finishing agent.

-Table 4-1 Coffee/Cream/Sugar Removal Contaminated Red Wine Removal Contaminated Soft Drink/Red Gui No. 40 Car Removal Contaminated Cola Removal Removal Water Color Removal Removal Mustard W/'No Turmeric Removal Removal Mustard W
/Turmeric Contamination Contaminated vehicle soft drinks were prepared by dissolving the Cherry Kool-Aid premix ingredients in the indicated amount of water.

The results presented in the table clearly show that the nylon fibers treated according to the invention have excellent stain resistance3, whereas the corresponding m41, which was not so treated, lacks stain resistance. ing.

The exposed cut edges of the pile fibers of the carpet samples made from the fibers of the present invention were stain resistant, indicating that the stain barrier agent not only coated the surface of the fibers but also impregnated into the GI fibers. There is.

Example 5 Of the staining substances tested in Example 4, the substance that most severely soiled the untreated carpet (control) was Red Dye No. 40 Min Soft Drink, Cherry Kool-Aid. 0th nylon 6 of the present invention
Another test was conducted to determine the effect of a large spill of this soft drink on a carpet sample made from 61a fiber. In this test, 3785 ml (1 gallon) of the soft drink was poured from a 1 gallon milk container onto a suitable carpet sample, the container being held at a height of 1 meter above the front surface of the carpet sample. The concentration of dye r1 in the soft drink was 0.054 g/l. Carpet sample n was given one coat in the manner described in Example 2.

(Half of the n L samples were made from yarns with fibers treated with Intratex N, and the other half (controls) were made from corresponding yarns with fibers not treated with Intratex N. The soft drink was poured onto both halves of the carpet sample from a distance of approximately 1 meter above the carpet sample, attempting to ensure that the same amount was poured onto each half. The soft drink was left on the sample overnight, but no steps were taken to clean the carpet or remove the soft drink until the next day.The next day, carpet sample F1 was cleaned in the manner described above. . Surprisingly, after cleaning, there was no sign of soft drink (Red Dye No. 40) remaining on half of the carpet samples made from the fibers of the invention, whereas on the other half of the carpet samples. Half of it was very dirty.

Similar results were obtained using the soil barrier used in Examples 1 and 2 in place of the soil 34'B agent used in this example.

In the example, two nylon carpet yarns were produced, one according to the invention (stain barrier yarn) and one according to the state of the art (control yarn). were similarly treated and each made into cut piles, both carpets were the same but one was made using dirt blocking yarn and the other was made using pair 1 (((((((((()). was tested for dirt resistance before and after walking.

The yarn of the present invention (dirt blocking yarn) has 6300 yarns made by the following method. Denier per tree (dpf) at Jll fiber
60 nylon 66 yarn? , commercial grade fiber-forming nylon 66 iii! It was produced by extruding it downward through the holes of a 300-hole spinneret into a 12-inch snow-covered upright melt-spinning cylinder of about 1.8 m at 282°C to form a corresponding number of melt streams. The upright cylinder was used to receive ambient temperature cooling air flowing crosswise at a rate of 270+A/min. The melt stream solidifies in an upright cylinder II
i fiber was formed. These monotIII fibers pass through a conventional water vapor regulating C of about 1.2 mm in length from an upright cylinder;
Therefore, these single fibers were treated with steam. Monofilament:
The A-coat tube passes the aqueous finish application machine to a conventional metered finish application machine where the aqueous solution contains a soil barrier and a fluorine compound in amounts sufficient to provide 3500 ppm soil barrier and 650 ppm fluorine, respectively, based on the weight of the fibers. The finishing agent was applied and the filaments were collected to form a yarn.The yarn was then fed around a driven feed roll (450a/min), followed by several wraps around a separating roll. The yarn is then unwound from the bobbin with the zero order yarn collected on the bobbin under slight tension to encourage winding of the yarn onto the bobbin, and combined with 54 similar yarns; Tow 3 was formed with a total denier of approximately 1.000.000. The tow was laid on a roll giving a nominal tow of 18d (If
Crinkled in a conventional crimping tube, 19.05cm (71/2
It was cut into stable pieces (inches). The staple is fluffed, stretched, protected with a conventional annular spinning frame, and subjected to twisting in the Z direction at approximately 177 revolutions per 1a (Lp+a) (4.5 revolutions per inch (TPI))31
/ Gave second single yarn. Two of these yarns were then twisted together with a 157 tpm (4,0 tpi) twist in the S direction. The soil barrier and fluorine compounds used to make this yarn were the same as those used to make the yarn described in Example 1.

A control yarn was made in the same manner as fully described.

However, dirt 7! The binder and fluorine compound were removed from the finish and both yarns were heat cured at 200° C. using conventional Suesen heat cure conditions. A Saxony carpet was made from each yarn. Each yarn was tufted with a 5/32 gauge cut pile tufting process to the primary backing using 27.6 stitches per 10 cm (7 stitches per inch). The pile height was 2.2c+++ (778 inches) and 32 ounces of yarn was used per square yard of carpet. Each carpet was dyed in Beck to a light burgundy color. The secondary backing was applied to the primary backing with adhesive. Each carpet was subjected to the following tests.

Each Carvey I.:icf:4 was tested to determine its resistance to Red Dye No. 40 prior to walking. An aqueous solution of the dye was prepared at a concentration of 0.054 g/l and used for testing the carpet samples. Five cylinders with an inner diameter of 2.54 cm and a length of 10 cm + sieve end opening were placed vertically onto each carpet sample. 20 ml of Red Dye No. 40 solution was soaked into each cylinder for the times shown below: LO (starting time), cylinder 1 to +2 hours, cylinder 2 to 4 hours, cylinder 3 to L6+ () hours. Cylinder 4 [0 MOA Between B, F, Cylinder 5 At the end of 8 hours (L, +8), all cylinders were removed from the carpet sample and the stain was blotted with a paper towel to remove excess solution from each carpet. The smudges on the sample f'l were marked on a plate equally on a scale from 1 to S. 1 is a heavily soiled carpet and 8 is a case where there is no visible dirt on the carpet. Each carpet sample was contacted with Red Dye No. 40 solution for 1.2.4.6 and 8 hours. Each time corresponds to one of the stains on the carpet sample.

The test results are shown in Table 5.

1 hour 8.0 3.02 hours
8.0 2.54 hours
8.0 2.06 hours 8.0
1.08 hours s, o
i.

Average 8.0 1.9 1 indicates heavily soiled 8 indicates no visible soiling A second sample of each carpet was subjected to 128,000 walks and then run in the manner just described. Tested. The results of this test are shown in Table 6.

Shishi”L Dan! L Main 1Lu' Ji
5-1 hours 8.0 3.02 hours 7.0 2.04 hours
6.0 1.06 hours 5
．． 0 1.08 o'clock I? SI5.0
1. Q average 6.2 1.6
Kyo1 indicates that it is very dirty. 8 indicates that there is no visible dirt. Figure 3 is before walking and after the dirt test is 3! ! Figure 2 is a photograph of a carpet made from cut yarn (invention). Figure 4 is a photograph of a carpet made from the control yarn before walking and after being subjected to the soil test. FIG. 5 is a photograph of a carpet made from the soil barrier yarn (invention) after it was first subjected to 128,000 walks and then subjected to a soil test. Figure 6 is a photograph of the control yarn after it was first subjected to 128,000 walks and then subjected to the soil test.

Each photograph is of the cut pile carpet sample described above. Each tuft of the carpet was made from nylon yarn. Each carpet was exposed to Red Dye No. 40 for a period of 1.2.4.6 and 8 hours.

Each photo was taken under similar conditions and at a reduction of 1/2.67.

The yarns in each carpet are similar, except that the fibers of the yarn used to make the carpets shown in Figures 3 and 5 were coated in accordance with the present invention;
This is not the case with the yarn used to make the carpet shown in Figures and Figure 6 (control).

The results shown in Tables 5 and 6 and illustrated in Figures 3-6 clearly illustrate the unusual and advantageous stain-resistance properties of the fibers of the present invention. There is.

In Figures 3 and 4, the word "first" means before walking, and in Figures 5 and 6, the word "dirty" means before walking. Those results are in accordance with the present invention!
The treated fibers are virtually stain resistant with respect to Red Dye No. 40, even after 128,000 walks, whereas when that coating is removed from the fibers, the fibers become virtually stain resistant. 6 Carbellas made from the fibers of the present invention show no staining before walking and very little staining even after walking, even when the dye is left in contact with the carpet for up to 8 hours. It is remarkable that it is not contaminated. This would be the case, for example, if a child spilled a soft drink, or if the child did not notice the spill for a long time.

Such events are not uncommon in a typical household.

[Brief explanation of drawings]

Figure 1 shows the nylon fiber of the present invention and the conventional nylon fiber t1.
Figure 2 is a plot showing the effect of temperature on dye absorption test values. Figure 2 (2I) is a plot showing the influence of stain blocking agents and fluorine compounds on the stain resistance of nylon fibers before and after walking. No change in content) Carpet (ffl) made from cut-off yarn (invention)
This is a photograph of the fiber shape. - Figure 4 is a photograph of a carpet (g, fiber shape) made from the control yarn before walking and after being subjected to the stain test. FIG. 5 is a photograph of a carpet (fiber form) made from the soil barrier yarn (invention) after it has been subjected to an initial 128,000 walks and then a soil test. , Figure 6 shows that after the first 128,000 steps,
Next is a photograph of the control yarn (fiber form) after being subjected to the soil test.

Claims (23)

[Claims] (1) Dye absorption test value of 7% or less at 25℃ and 100℃
1. A stain-resistant nylon fiber characterized in that it has a coating on its surface comprising one or more stain blocking agents in an amount sufficient to provide the fiber with a dye absorption value of 30% or more. (2) The fiber according to item 1 above, wherein the nylon is nylon 66. (3) the first fiber whose denier is in the range of 8 to 24;
Fibers listed in section. (4) The fiber according to item 3 above, which is in the form of a staple. (5) The fiber according to item 3 above, which is in the form of a continuous filament. (6) A yarn comprising the fiber according to item 4 above. (7) A yarn comprising the fiber according to item 5 above. (8) The fiber according to item 1, further characterized in that it is not dyed. (9) The fiber according to item 1 above, which has a dye absorption value of substantially 0 at 25°C. (10) When made into carpets, they provide fibers with the ability to retain their initial stain resistance even after walking to a greater extent than if the fluorine compounds were removed from the coating. 2. The fiber of claim 1, wherein the coating includes one or more fluorine compounds in sufficient amounts. (11) one or more soil barrier agents in an amount sufficient to provide a fiber having a dye absorption test value below but within the range represented by the area above curve C in FIG. 1; A nylon fiber characterized in that it has a coating on its surface. (12) one or more soil blockers in an amount sufficient to provide a fiber with a dye absorption test value that is below curve D but within the range given by the area above curve E in FIG. A nylon fiber characterized in that it has a coating containing an agent on its surface. (13) A method for improving the ability of nylon fibers to be resistant to staining by acid dyes at room temperature while retaining the ability to be dyed by acid dyes at elevated temperatures by 6% or less at 25°C. said fiber is prepared by a spin finish characterized in that said fiber contains one or more soil barrier agents in an amount sufficient to provide a nylon fiber having a dye absorption value of 30% or more at 100°C. A method for improving the stain resistance of nylon fibers, which method comprises applying the stain resistance to the fibers during a melt polymerization process. (14) The method according to item 13, wherein the nylon is nylon 66. (15) The method according to item 13 above, wherein the finish contains one or more fluorine compounds in addition to the one or more soil blocking agents. (16) the soil barrier and the fluorine compound are 0.20 to 0.35% by weight of the soil barrier based on the weight of the nylon;
16. The method of claim 15, wherein the fluorine is present in an amount sufficient to provide fibers coated with 50 to 650 ppm fluorine. (17) A carpet having a pile consisting essentially of the fibers according to item 1 above. (18) The carpet according to item 17, wherein the carpet has a cut pile structure. (19) The carpet according to item 18 above, wherein the fibers are nylon 66 fibers. (20) A carpet having a pile consisting essentially of the fibers according to item 11 above. (21) The carpet according to item 20 above, wherein the fibers are nylon 66 fibers. (22) A carpet having a pile consisting essentially of the fibers described in item 12 above. (23) The carpet according to item 22 above, wherein the fibers are nylon 66 fibers.