DE2505742B2 - Treatment agents for synthetic filler fibers - Google Patents

Description

10

The invention relates to a treatment agent for synthetic filler fibers based on an amino compound and an epoxysiloxane. The invention also relates to a method for treating these synthetic fibers with the treatment agent The treatment agent gives the synthetic filler fibers superior compression elasticity, smoothness, suppleness, soft feel similar to feather quilts and good service life and behavior.

Cotton and feathers have been the common main filling materials for bedspreads or the like and due to especially superior compressive elasticity, smoothness, flexibility and the feel of springs Bed quilts using feathers as a filling material are used as luxury items

In recent years, such filler materials have been replaced by synthetic fibers such as _J0 polyester fibers or polypropylene fibers. However, filler materials composed of such synthetic fibers have inferior compressive elasticity, smoothness, pliability and feel to springs and give poor body conformance when used in bed quilts.

Attempts have been made to produce luxury bed quilts with good compressive resilience and a soft hand by using the fiber arrangement of the filling using synthetic fibers. For example, attempts have been made to use synthetic fibers in the form of tow instead of staple fibers. However, this method does not result in any significant change in fiber properties and 4-, the resulting bed quilts are not comparable to the feather quilts, although they provide better compression elasticity, smoothness and better feel than bed quilts using the usual synthetic fiber fillings in staple form. - _{) 0} Furthermore, this method has another disadvantage in that the fibers are used in tow form, since conventional methods of making bed quilts as such cannot be used.

Without any effective and decisive solu- γ, solution to the problem is the current practice in the use of synthetic Faserfüllmaterialien treated with a mainly composed of a surfactant treatment agent. For example, there is provided a treatment agent in Japanese Laid-Open _b o Patent Application 67 592/73, which consists of 80 to 60 wt ° / o of a potassium salt of an ethylene oxide (2 mol) is added to Laurylphosphoräther and 40 to 20 wt .-% of an arbitrary Propylene glycol ethylene oxide copolymers with an _h -> mean molecular weight of 24,000, in which 5 moles of ethylene oxide are added to 1 mole of propylene glycol. Synthetic fiber fillers treated with this treating agent cannot exhibit compressive resilience, smoothness and feel similar to feathers a

It was therefore tried to use synthetic fibers for Fillings with synthetic textile fiber treatment agents to be handled, which was previously similar in terms of the granting of smoothness and suppleness .much animal fibers, such as alpaca and mohair, have been suggested to synthetic fibers. For example was the treatment agent specified in US Pat. No. 3,655,420, which is a mixture from about 03 to 20 parts by weight of a liquid Epoxysiloxane and 1 part by weight of an amine compound with at least two amino groups per molecule and represents no more than one aromatic ring bonded directly to the nitrogen atom is used

If this mixture also has superior compressive elasticity, Granted smoothness and suppleness to the synthetic fibers, it has the serious Failure that this mixture has poor storage stability due to its strong activity; if it is left to stand in the form of an emulsion, it gradually shows crosslinking at room temperature and in about 2 or 3 days it is damaged when this treatment agent is used in the circulatory system no uniform treatment due to the crosslinking, which occurs at elevated temperature during of operation takes place, ensured and the crosslinked treatment agent often adheres strongly to rollers and other treatment facilities, which makes it necessary to interrupt work frequently. In addition, according to US-PS 36 55 420 no completely satisfactory results are obtained, as can be seen from the test results presented later.

The object of the invention is therefore to provide a treatment agent for synthetic fibers which synthetic filler fibers with superior properties such as compression elasticity, smoothness, suppleness, soft handle and good service life and good usage behavior results, as well as a method for Treatment of the synthetic filler fibers with the treatment agent.

The treatment agent according to the invention for synthetic filler fibers, based on an amino compound and an epoxysiloxane is characterized by having it as active ingredients

(a) 1 part by weight of an aminosilane of the formula:

R ₃
O

R ₁ -NH-R ₂ -Si-OR ₄ (1)

O
R ₅

wherein Ri is a hydrogen atom, an alkyl group with 1 to 4 carbon atoms or a phenyl group, R2 is an alkylene group with 1 to 4 Carbon atoms and R3, R4 and R5 independently of one another an alkyl group with 1 to 4 Carbon atoms mean and

(b) 1 to 20 parts by weight of an epoxysiloxane,
at least one structural unit of the formula

R ₆

-O — Si
R.

(Π)

that are comparable or that they surpass.

This is also proven by the following test results.

The following experiments were conducted to show that the treatment agents for synthetic Filler fibers according to the invention have a superior advantage over those with the treatment agent treated according to LJS patent specification 36 55 420 provide.

10

wherein Re and R7 independently of one another are Denote an alkyl group having 1 to 3 carbon atoms, and at least two structural units the formula

R ₈

-O — Si -
R ₉
CH-

-CH ₂

(ΠΙ)

20th

25th

wherein Re is an alkyl group having 1 to carbon atoms or the grouping

-R ₉ -CH-

-CH ₂

Experimental procedure
1. Treatment of synthetic fibers

A polyethylene terephthalate with an intrinsic viscosity of 0.62, calculated from the measured value in O-chlorophenol at 35 ° C, was melt spun. Of the obtained strand with a total denier of 400,000 den (single fiber denier 6 denier) was in a treatment agent each dipped from one of the approaches listed in Table A as an aqueous solution, with a Upsetting curling device squeezed off to an uptake of 10% and at 90 ° C for 20 minutes dried. Then the strand was heat-treated at 140 ° C for 30 minutes and made into a fiber length cut by 7G mm.

The number of crimps was 5 per 25 mm and the percentage crimp was in all cases 18%.

30th

Table A.

35

and Rs is an alkylene group having 2 to 5 carbon atoms or a substituted or unsubstituted arylene group having 6 to 10 carbon atoms mean, wherein the epoxysiloxane 0.3 to 10 wt .-% epoxy groups, based on its Total weight, owns, contains.

The method according to the invention for treating synthetic filler fibers is characterized in that that in the synthetic fibers a treatment agent that acts as an active ingredient

(a) 1 part by weight of an aminosilane of the above formula (I),

(b) 1 to 20 parts by weight of an epoxysiloxane which has at least one structural unit of the above formula (II) and at least two structural units of the above formula (III) wherein the epoxysiloxane has 0.3 to 10% by weight of epoxy groups, based on containing its total weight, is impregnated so that the total amount of adhered aminosilane and epoxysilane 0.1 to 3.0 wt .-%, by weight based on the dry weight of the fibers, and then heat treatment at a temperature of 100 to 23O ⁰ C for performed for at least 1 second.

The above treating agent has the effect of markedly reducing the coefficient of friction of synthetic fibers for fillings and results in synthetic fiber fillings with superior compressive elasticity, Smoothness, pliability, grip and behavior in use that match those of Federsteppdek-50

55

Coalescence Treatment agent (part by weight!) 0.5 (10 moles) -nonylphenyl- 93.0 Il Ml I. ether invent invent (U.S. PS water dungs dungs 36 55 420) according to according to _ Hexamethylene 0.34 diamine 0.88 0.57 y-aminopropyl - triethoxysilane 4.45 4.76 Epoxysiloxane (l) *) 4.99 1.17 1.17 Potassium cetyl phosphate 1.17 0.5 0.5 Polyoxyethylene 93.0 93.0

*) The epoxysiloxane (l) given above consisted of structural units of the following formulas:

b0

CH, "

- O - Si -
CM,

and

CII,

--Si —ΟΙ
(CII,),

HC

CII,

and maintain a viscosity of 6,000 Cntistoccs at 25 (. a t ^: .poxy group of I (% in each case, with a trimethylsilyl group on both limes I - Si (CI1,), |.

2. Measurement of tensile strength
the treated fiber

The fibers (100 g) treated according to the above procedure were roller carded for Subjected to formation of a tape with a length of 4 to 5 m. A sample with a length of 20 cm was cut lengthways near the center of the tape and stabilized by 1.5 hours was left standing.

The tape sample was inserted vertically into a compression test device of the TOM 200 D type, so that held at each end of the specimen by a pair of vertically attached clamps for a length of 5 cm became. The lower clamp was moved downwards at a constant speed of 20 cm / min, pulled until the tape was completely broken. The maximum on the lower bracket at this point tension applied was read. The maximum tension (g) determined in this way became by divides the weight (g) of the tape per 10 cm. The quotient obtained is the tensile strength.

The results of the measurement are listed below:

Table B. Tensile strength Treatment agents 85-90 I (comparison) 70-75 II (according to the invention) 65-70 III (according to the invention) 3. Handle test

Any of those following the procedure outlined above treated pulps were touched by hand. It was found that those with the Treatment agents II and III treated fibers had a good feel similar to a feather quilt, while the fibers treated with Treatment Agent I were somewhat rough to the touch.

It is clear from the results of the foregoing experiments that the one described in US Pat 36 55 420 described treatment agent (treatment agent I) treated fibers a higher tensile strength than those treated with the treatment agents according to the invention (treatment agents II and III) Had fibers. This means that the dynamic frictional resistance between those with the treatment agent I treated fibers is high, i.e. their smoothness is poor. It follows that if such treated fibers are used for stuffing or cushioning purposes as intended by the present invention their flexibility are inferior to their grip and their usability.

To this extent, the treatment agents according to the invention bring a far superior technical advance versus the treatment agent described in US Pat. No. 3,655,420.

In the aminosilanes of the formula (I), the Alkyl and alkylene groups can be either straight or branched chain and include, for example Methyl, ethyl, n- or isopropyl, n-, iso- or tert-butyl, methylene, ethylene, n- or isopropylene and n-, iso- or tert-butylene groups. Methyl and ethyl groups are especially used as alkyl groups preferred and ethylene and propylene groups are particularly preferred as alkylene groups.

Some of the aminosilanes of the formula (I) used according to the invention are known compounds and also new aminosilanes of the formula above can be used in completely the same manner as in the method for Production of the known aminosilanes are produced.

ίο Suitable aminosilanes include, for example:
Aminomethyltrimethoxysilane,
/) - Aminoäthyltrimethoxysilan,
jJ-Aminoäthyltriäthoxysilan,
y-aminopropyltrimethoxysilane,
y-aminopropyltriethoxysilane,
O-aminobutyltriethoxysilane,
/ S-methylaminoethyltriethoxysilane,
0-ethylaminoethyltriethoxysilane,
y-methylaminopropyltrimethoxysilane,
y-propylaminopropyltriethoxysilane,
<5-ethylaminobutyltriethoxysilane,
y-phenylaminopropyltrimethoxysilane and
y-phenylaminopropyltriethoxysilane.
Of these will be
-> 5 γ-aminopropyltriethoxysilane

[H ₂ NC ₃ H ₆ Si (OC ₂ Hs) ₃ ],
y-aminopropyltrimethoxysilane

[H ₂ NC ₃ H ₆ Si (OCH ₃ ) J,
0-methylaminoethyltriethoxysilane
j «[CH ₃ NHC ₂ H ₄ Si (OC ₂ Hs) ₃ ] and

y-phenylaminopropyltrimethoxysilane

[Ph-NHC ₃ H ₆ Si (OCH ₃ ) J.

preferred. Among them is the γ-aminopropyltriethoxysilane particularly preferred.

In the treating agent according to the invention, an epoxysiloxane having the following repetitive ones is used units

and

R ₆

-O-Si-R ₇

R ₈

-O-Si-R ₉

CH CH ₂

US)

used in combination with the aminosilane of the formula (I) In the above formulas, the _{alkyl groups indicated with R 6} , R7 and Rg have 1 to 3 carbon atoms and can be either straight-chain or branched-chain. The alkyl groups include methyl, ethyl and n- or isopropyl groups, of which methyl groups are particularly suitable. The alkylene group indicated by R9 can be either straight or branched chain and contains 2 to 5 carbon atoms. For example, it includes ethylene,

Propylene, butylene and pentylene groups, of which ethylene and propylene groups are particularly preferred. R.9 can also be an arylene group, for example a phenylene or naphthylene group.
The group Rg can also be the group

- Ro — CH

-CH ₂

mean. This means that the epoxysiloxane used according to the invention is also a structural unit of the following formula

ο Ί

CH CH ₂

-0 - Si-R ₉
CH

-CH ₂

(IV)

may contain.

The epoxysiloxanes to be used according to the invention must have at least one of the repeating units of the formulas (II) and (III), preferably at least 35 and more preferably contain 100 to 600 such units in total and at least two, preferably 4 to 20 of these must be recurring units of the formula (II).

Usually, the repeating units (II) and (III) and / or (IV) can be used indiscriminately in the epoxysiloxane are present, but they can also be present in block form. A small amount more recurring Units can be included herein as long as they do not have the basic properties of the epoxysiloxane change considerably. The terminal groups can usually be selected from trialkylsilyl or hydroxyalkylsilyl groups exist, but can also be silicon-free groups. If the molecules form a ring, is the absence of terminal groups is also possible.

The epoxysiloxanes used according to the invention in the bending agents are advantageously liquid and have a high molecular weight. Usually it is advantageous to use epoxysiloxanes with viscosities 25 ° C from 1000 to 100,000 centistokes, preferably from 3000 to 100,000 centistokes, most preferred 3,000 to 20,000 centistokes to be used.

The epoxysiloxanes used according to the invention preferably contain at least 03% by weight of epoxy groups, based on your total weight The upper limit of the epoxy group content is not critical, however, the amount of the epoxy groups is usually 3 to 10% by weight, preferably 1 to 5 % By weight, based on the total weight of the epoxysiloxanes.

Epoxysiloxanes known per se can be used according to the invention. Examples of epoxysiloxanes of this type are shown in U.S. Patent 3,055,774 and are valuable.

The epoxysiloxanes must be water soluble or easily dispersible in water for ease of use but they can also be in one if desired

5 organic solvents! or in the absence of one Solvent are brought.

The epoxysiloxanes described above can be used in a ratio of 1 to 20 parts by weight, preferably 1 to 18 parts by weight, more preferably 5

ίο to 10 parts by weight per part by weight of the aminosilane Formula (I) can be used.

Due to the adhesion of the treatment agent according to the invention to synthetic filling fibers various properties suitable for filling purposes, such as superior compressive elasticity, smoothness, suppleness, The synthetic fibers have a grip and suitability for carrying.

According to the invention there is a method for treating synthetic fibers for fillings, wherein a treating agent of 1 part by weight of an aminosilane of the above formula (I) and 1 to 20 Parts by weight of an epoxysiloxane having at least one structural unit of the above formula (II) and at least two structural units of the above formula (III) and / or (IV) on synthetic fibers for Fillings are applied and then the fibers are heat treated.

The adhesion of the treatment agent according to the invention to the synthetic filling fibers can be effected by various known methods. The time of application can be before or after the step of stretching the extruded synthetic fibers, before or after the step of crimping treatment, before or after the bulking stage, before or after the above heat treatment stage or before or after a stage of the stack formation (cutting).

The treating agent can be used in the form of a solution in an organic solvent, however, it is usually advantageous in the form of an aqueous dispersion, especially an aqueous one Emulsion, used The concentration of the aminosilane and the epoxysiloxane in such a solution or dispersion can vary over a wide range. The suitable concentration is 0.5 to 20% by weight, preferably 1 to 15% by weight, based on the weight of the solution or dispersion. It is it goes without saying that this concentration range is not strictly critical, but depends on the application process, the type of synthetic fibers and the like, so that concentrations outside of the above range can be applied.

The application of the treatment agent to the

synthetic fibers can be made to various dimensions

took, such as dipping method, oil roller winding method or spray processes. This results in adhesion or impregnation of the Treatment agent according to the invention on or in the synthetic fibers.

The amounts of the aminosilane and epoxysiloxane to be applied to the fibers can be over a can be varied over a wide range according to the particular effect desired.

In general, it is advantageous to use them in a total amount based on the dry weight of the Fibers, of at least 0.1% by weight. It is no specific upper limit is set, but the use of too large amounts does not bring any corresponding

Effect, but is uneconomical. Usually the total amount of aminosilane and Epoxysiloxane suitably not more than 3% by weight, preferably 0.2 to 1.5% by weight, more preferably 0.3 to 1.0% by weight based on the dry weight of the fibers.

When the treating agent of the invention is used in the form of an emulsion, an emulsifier can be used or an antistatic agent and the like may be mixed to aid dispersion of the effective ingredients facilitate. Examples of preferred emulsifiers and antistatic agents are anionic surface-active agents Agents such as polyoxyethylene alkylaryl ethers, polyoxyethylene alkyl ethers, polyoxyethylene sorbitan alkylamides, Polyvinyl alcohol or its analogues or alkyl phosphate potassium salts and kaiionic surface-active Agents such as quaternary ammonium salts, e.g. B. stearyldimethylbenzylammonium chloride or stearylamide propyldimethyl-jJ-hydroxyethylammonium nitrate.

After the treatment agent of the invention has been applied to the fibers, preferably at a temperature not exceeding 50 ° C, the fibers are heat-treated to harden and crosslink the aminosilane and the epoxysiloxane in the treatment agent on the surface of the fibers. This gives the fibers significantly improved compressive elasticity, smoothness, pliability, grip and usability. This heat treatment also significantly improves the wash resistance of the fibers. The treatment temperature varies depending on the treatment time and cannot be clearly determined. If the temperature is too low, long periods of time are required to carry out the heat treatment and the effect obtained is insufficient. On the other hand, if it is too high, the properties of the fibers are deteriorated. Therefore, the heat treatment temperature is generally at least 10O ⁰ C, but less ali the melting point (or softening point) of the synthetic fibers and temperatures of 100 to 230 ° C are particularly suitable. The heat treatment time is at least 1 second and can be varied over a wide range depending on the heat treatment temperature. If relatively high temperatures are used, it is advantageous to discontinue the heat treatment within a short period of time which does not cause deterioration in the properties of the fibers. When polyethylene terephthalate fibers are used, a period of about 10 minutes to 2 hours at a temperature of 110 to 170 ° C is suitable, and a period of 1 second to 10 minutes is particularly suitable when the temperature is 170 to 230 ° C.

If the synthetic fibers treated according to the invention are used from filling materials, the fibers must be curled. The frizz treatment can be done before, during or after the treatment of the fibers according to the invention. It is preferred to curl synthetic fibers which the treating agent of the invention has been applied before the heat treatment of the invention is carried out. This has the advantage that both the heat curing of the treatment agent and the Heat consolidation of the crimps can take place at the same time.

The curling treatment can be carried out by various methods, such as mechanical ones Shirring methods using a stuffing shirring device, a gear curling device and the like, or latent curling methods in which the curls are formed by heat treatment or chemical treatment to be developed.

Usually the fibers so treated are cut to suitable lengths.

The curling treatment can also be carried out after treating the fibers according to the method of the invention

ίο take place. Or it is also possible to apply the treatment agent of the invention to fibers which have first been obtained by crimping synthetic fibers and then optionally cutting.
There is no particular limitation on the kind of synthetic fibers to which the treating agent and the treating method of the invention can be applied, and examples of suitable synthetic fibers are polyester, polyamide, acrylic and polyolefin synthetic fibers.

The polyester fibers are particularly suitable.

Thus, according to the invention with a heat-treated product of the aminosilane and the Epoxysiloxane coated synthetic fibers are obtained which have excellent compressive elasticity, smoothness and Have suppleness and a soft handle. When these fibers are used as filling material for bed quilts used, they have a soft feel similar to feather quilts and make good Usability.

Those treated and curled and optionally cut by the process of the invention Synthetic fibers can be used as filling materials or cushioning materials for bed quilts, pillows or other quilts and the like can be used. It has been found that when the synthetic fibers the have the following properties, filling materials of superior quality due to the favorable interaction between the properties of the fibers and the treatment of the invention.

1.5 <D <10

10D-20 <L <10D + 60

10 <L

-3 / 4D-I-IO ₁ OSCW ^ -3 / 4D + 15.5
15 <Gv + C _D <32

wherein

D is the denier size of the synthetic fibers,

L is the length of the fibers in mm,

Gv is the number of crimps per 25 mm and

Cd is the percentage of crimps (%) measured

using the method described in JIS L-1074,
mean.

Synthetic fibers, especially polyester fibers, with the above properties and those with the Treatment agents of the invention not only provide superior compressive resilience, Smoothness, flexibility, superior grip and superior serviceability, but all properties those required for filling materials or cushioning materials are such as the highest level of handling properties due to the above synergistic effect.

The denier (D) of the fibers is preferably 1.5 to 10 denier in view of the bulkiness of the filler material and its handling properties (for example, the occurrence of pebbles when processed on cards). When suppleness is considered, that is particularly preferred

Denier size of the fibers at 2 to 8 denier. When a fullness is made, fibers can be of different types Denier size as well as the same denier size can be used.

If the length (L mm) of the fibers is too short, the entanglement of the fibers at the time of manufacturing the filling materials is reduced and the web breakage is easy to occur. If it is too long, the fibers tend to wrap around the card cylinders and also develop knots. That is, the handling properties of the fibers are deteriorated. Thus it is preferred that the length of the fibers be as follows:

10D-20 <L <10D + 60
10 <L,

particularly preferred

10D-10 <L <10D + 50
30 <L

As a measure of the crimp properties, the number of crimps (Cn, number / 25 mr) and the percentage of crimp (Ca %) are preferably within the following range:

-3 / 4D + 10.0 < C _N < -3 / 4D + 15.5
15 <Gv + C _D < 32

more preferably within the following range

-3 / 4D + 11.0 <Qv <-3 / 4D + 14.5
18 <Gv + Cd <30.

When the curling properties are below the lower limits of the ranges given above the handling properties of the filler material tend to deteriorate and when they are over going beyond the upper limits, the smoothness of the filler material is slightly reduced. These curl properties can be given in a simple manner, for example, by conventional filling crimping devices.

The treating agent of the invention can be applied to synthetic fibers in the same manner that are used as filling material in the form of tow or rope.

Synthetic fibers to which the treating agent of the invention has been applied, and the optionally heat-treated and crimped, have far superior compressive elasticity, smoothness, Suppleness and superior grip and superior serviceability and have a wide range of uses as filling material or cushioning material. For example, when using a bed quilt Made from these fibers, it delivers superior grip and conformance to the body comparable to feather quilts or beyond. If a pillow or winter clothes Made using these synthetic fibers, they adapt well to the body.

The treating agent of the invention described above gives synthetic filler fibers superior to Compressive elasticity, smoothness, pliability, superior Grip and superior adaptability to use that cannot be matched by conventional synthetic fibers Could be and the fibers can be applied not only for filling purposes, but also on other areas that require the above properties. Thus, the treatment agent offers the Invention a great technical advantage.

The following examples serve to explain the invention in more detail. In the examples relate all parts by weight and all viscosity values are in centistokes at 25 ° C expressed. The compressive elasticity, smoothness and conformability were determined by the following methods rated.

Compressive elasticity

This is an essential property as a filler material.

ίο In the case of quilts in particular, this will Compression extent a measure of the adaptability to the body. It expresses the deformability of the fibers to train on the bedding. The higher the amount of compression, the more deformable they are Fibers in a bed quilt.

The compressive elasticity is evaluated as follows: a web is made by processing raw fibers on a card, and a sample of cylindrical shape with a diameter of 10 cm and a weight of 20 g is made. A disk-like light weight (0.5 g / cm ² ) and a disk-like heavy weight (9.5 g / cm ² ) are placed on the sample and pressed for 10 minutes, after which the light and heavy weights are removed and left Stand for 2 hours. Again, the light and heavy weights are placed on the sample and allowed to stand for 17 hours. The light and heavy weights are then removed and after 7 hours only the light weight is placed on the sample. The height (ho) of the sample at this point is measured. Then the light and heavy weights are again placed on the sample and allowed to stand for 17 hours. The height (h \) of the sample at this point is measured.

Then the light and heavy weights are removed. After 7 hours, only the light weight applied and the height (Λ2) of the Sample is measured.

The compression amount (%) and the compression recovery (%) are obtained from the following equations calculated:

Compression amount (%) =

Compression recovery (%)

100

100

So that the filling material has a soft grip and

Adjustment for use similar to feather quilts results, it is preferred that the amount of compression is at least 70% and the compression recovery is at least 90%

smoothness

The smoothness is determined by the static coefficient of friction (με) between fiber and fiber and the dynamic coefficient of friction (μα) between fiber and fiber at a speed of 3 m / min, which according to the Roeder method at a temperature of 20 ⁰ C and a relative Moisture of 65% are measured, evaluated The lower the με and μα values, the better the smoothness. Both the με and the μά value are preferably not more than 0.25.

15th

handle

A feel test is performed with regard to the grip of the Filling material of the invention carried out 2.0 kg of raw fibers distributed by a card are evenly in brought a sack made from a quilted bedcloth with a size of 140 cm 200 cm. The handle will rated both by hand and by use

example

Polyethylene terephthalate with an inherent viscosity of 0.62, calculated from the measured value in o-chlorophenol at 35 ° C., was melt-spun. The obtained strand with a Gesamtdenierwert of 000 (with a Einzelfaserdenier of 6) was immersed in a treatment agent of the recipes given in Table I are each as an aqueous emulsion, squeezed by a Füllmaterialkräuselgerät on a take of 10% and at 9O ⁰ C for 20 minutes

Table I.

dried

Then the strand was at 140 ° C for 30 Heat treated for minutes and cut to a fiber length of 76 mm.

The properties of the fibers obtained are given in Table II. The number of crimps was 7 per 25 mm and the percent crimp was 18% in all cases.

composition

Treatment agents (parts 1
ABCD

0.5

0.5

y-aminopropyltriethoxysilane 0.5 y-A.minopropyltrimethoxysilane

jS-methylaminoethyltriethoxysilane

y-phenylaminopropyltrimethoxysilane

Epoxysiloxane (l) *)
Cetyl phosphate potassium salt

Polyoxyethylene (10 mol) nonylphenol ether

Water at 93.0 93.0 93.0 93.0

*) The epoxysiloxane (l) used above consisted of structural units of the following formulas:

-Si-O-

4.9 4.9 4.9 4.9 1.1 1.1 1.1 1.1 0.5 0.5 0.5 0.5

CH, "

-O-Si - CH,

and

-CH,

and had a viscosity of 6000 centistokes at 25 ° C., an epoxy content of 1% by weight, with both ends off Trimethylsilyl groups [—SKCHj},) passed.

Table II Treatment agents C. D. AWAY 0.18 0.19 smoothness 0.17 0.17 0.17 0.20 0.16 0.17 μά 77 75 Compression elasticity 79 78 97 95 Amount of compression 99 99 Feather- Compression recovery very similar handle Quilts

030123/191

Comparative example 1

A mixture of 60% by weight of a potassium salt of ethylene oxide (2 mol) added to lauryl phosphorus ether and 40% by weight of an arbitrary copolymer of propylene glycol and ethylene oxide with an average Molecular weight of 24,000 in which 5 moles of ethylene oxide was added to 1 mole of propylene glycol became one 2% aqueous emulsion processed The same polyethylene terephthalate strand as used in Example 1, was immersed in this treating agent by an FQU material curling device into one Uptake of 10% squeezed, heat treated for 2 hours at 140 ° C and then to a length cut by 76 mm. The number of crimps of the obtained fibers was 7 per 25 mm and that percent curl was 18%.

The fibers treated in this way had the following properties:

10

smoothness

με 036
lid 030

Compression elasticity
Compression amount 64%
Compression recovery 88%

handle
worse than feather quilts (hard handle)

Example 2

The same procedure as in Example 1 was repeated except that the viscosity of the in epoxysiloxane used in treating agent A of Example 1 as indicated in Table III became. The results obtained are also shown in Table III.

Table IH Attempt no 2-2 2-3 2-4 2-5 2-6 2-7 2-1 1000 3000 8000 10,000 100,000 150,000 500 Viscosity of the Epoxysiloxane 0.19 0.17 0.18 0.19 0.19 0.24 smoothness 0.23 0.19 0.19 0.19 0.20 0.21 0.26 us 0.25 yd Compression 74 80 78 77 73 68 elasticity 68 Compression 93 97 98 97 92 87 extent (%) 88 Compression Bad recovery (%) Bad ter than handle ter than equal to feather quilts Feather quilting Feather quilting cover cover (hard) (hard)

From Table III it can be seen that epoxysiloxanes having a viscosity of from 1,000 to 10,000 centistokes are particularly useful gave good results.

Example 3

The same procedure as in Example 1 was varied with the epoxysiloxane as indicated in Table IV Repeated exception that the epoxy group content of the became so. The results are also shown in Table IV reproduced in the treatment agent A used in Example 1.

Table IV

Attempt no. 3-2 3-3 3-1 1.0 3.0 Epoxy group content (wt .-%) 0.5 smoothness 0.16 0.17 US 0.24 0.16 0.16 lid 0.25 Compression elasticity 80 79 Compression amount (%) 66 98 97 Compression recovery (%) 87 same Quilted quilted decxes handle Worse as feather quilting cover (hard)

Example 4

The same procedure as in Example 1 was carried out with the y-aminopropyltriethoxysilane and the epoxysiloxane Repeated exception that the ratio between that shown in Table V was changed. the 5 results used in the treating agent of Example 1 are shown in Table V.

Table V Attempt no. 65 4-2 4-3 same 4-4 4-5 4-6 4-1 1 5 i0 20th 30th 0.5 87 Relationship*) 0.18 0.18 0.16 0.18 0.25 smoothness 0.24 Worse 0.19 0.17 0.16 0.19 0.26 US 0.25 as a feather
quilts Ud Compression elasticity (hard) 73 79 80 75 68 Compression austnaS 93 98 97 94 88 Compression recreation Worse handle Feather quilts as a feather
quilts (hard)

*) The weight in parts of the epoxysiloxane per part by weight of the γ-aminoprupyltriethoxysilane. The other components of the equipment were the same as in Example I.

Good results have been obtained when the amount of the epoxysiloxane is 1 to 20 parts by weight per part by weight of the was y-aminopropyltriethoxysilane. J5

Example 5

The same procedure as in Example 1 was repeated except that each of the following Epoxysiloxane was used in place of the epoxysiloxane in treatment agent A in Example 1.

Epoxysiloxane (2), built up from structural units of the following formulas:

an epoxy group content of 1.8% by weight, both ends being trimethylsilyl groups [- Si (CH3) 3].

Epoxysiloxane (3), built up from structural units of the following formulas:

CH,

α H ₃

-Βί

α H,

45

-Ο —Si -
CH ₃

CH

CH ₁

-O —Si

(CH ₂ ),

HC-

CH ₂

with a viscosity of 5000 Centistokes at 25 ⁰ C and

with a viscosity of 10,000 centistokes at 25 ° C. and an epoxy group content of 2% by weight, both ends being trimethylsilyl groups [-Si (CH ₃ ) j].

The results are given in Table VI below.

Table VI

example Attempt no. 5-2 6th 5-1 Treatment agents 0.9 y-aminopropyltriethoxysilane 0.5 Epoxysiloxane (2) 4.5 Epoxysiloxane (3) 4.9 1.1 Cetyl phosphate potassium salt 1.1 0.5 Polyoxyethylene (10 mol) 0.5 Nonylphenol ether 93.0 water 93.0 smoothness 0.16 fs 0.18 0.17 μά 0.19 Compression elasticity Amount of compression Compression recovery same feather quilt handle cover

Treatment agent prescription

y- aminopropyltriethoxysilane 1.0 part by weight

Epoxysilnn (the same as in

Example 1) 6.6 parts by weight

Cetyl phosphate potassium salt 1.6 parts by weight

Polyoxyethylene (10 mol) nonyl

phenol ether 0.8 part by weight

Water 90 parts by weight

Properties of the fibers

smoothness

με 0.17

μά 0.17
Compression elasticity

Compression amount 82

Compression recovery 92
handle

similar feather quilts

Example 7

Polyethylene terephthalate with an inherent viscosity calculated from that in o-chlorophenol at 35 ° C

45

measured value, of 0.62, was melt spun and formed a tow with a Total denier value of 400,000, consisting of hollow fiber with 7 denier each and a void of 13% drawn. The obtained cable was treated with the treating agent A in Example 1 in the same manner treated as in Example 1. The number of crimps of the fibers obtained was 8 per 25 mm and the number of crimps percent curl was 19%. The fibers treated in this way had the following properties:

smoothness

με 0.16

µα 0.16
Compression elasticity

Compression amount 78

Compression recovery 98
handle

equal to feather quilts

Polyethylene terephthalate with an inherent viscosity of 0.62, calculated from that in o-chlorophenol at 35 ° C measured value was melt spun to form a tow having a total denier value of 500,000 (single fiber denier 3) drawn. The tow was emulsified in the following listed recipe, immersed through a filler curling device squeezed to an uptake of 6%, dried at 90 ° C. for 20 minutes, then heat-treated at 140 ° C. for 30 minutes and cut to a length of 56 mm.

The number of crimps of the obtained fibers was 9 per 25 mm and the percentage of crimp was 15%. The fibers thus treated had the following properties.

Example 8

Polyethylene terephthalate with an inherent viscosity calculated from that in o-chlorophenol at 35 ° C measured value of 0.65 and polyethylene terephthalate isophthalate (10 mol% isophthalic acid copolymerized therein) were at a 1: 1 weight ratio using a side-by-side spinneret spun at the same time and spun to 3.3 times the original length in at 75 ° C held warm water to form a tow with a total denier of 80,000 (Single fiber denier equal to 6.8) drawn. The tow was relaxed in air at 80 ° C heat-treated and immersed in the treatment agent A of Example 1. It was then through a Filler crimping device squeezed to an uptake of 12% and at 80 ° C for 30 minutes dried. It was then in a relaxed state at 160 ° C for 30 minutes to develop Crimps heat-treated at the same time to their heat consolidation and then the tow cut a fiber length of 76 mm.

The number of crimps of the obtained fibers was 12 per 25 mm and the percentage crimp was 19%. The fibers had the following properties:

smoothness

με 0.18

µα 0.17
Compression elasticity

Compression amount 76

Compression recovery 98
handle
equal to feather quilts

Example 9

Modified polyethylene terephthalate with an inherent viscosity calculated from that in o-chlorophenol 35 ° C measured value of 0.55 and the 14% by weight

a flame retardant of the following formula: 24

HIGH ₂ CH ₂ O

was melt spun and drawn to form a tow having a total denier of 400,000 (single fiber denier equal to 5.5). The obtained tow was dipped in the treating agent A of Example 1, squeezed by a filler curling device to an absorption of 8%, then subjected to the same treatment as in Example 1.
The obtained fibers gave filler fibers with

OCH ₂ CH ₂ OH

soft feel similar to feather quilts and a high degree of flame retardancy.

smoothness

/ us 0.18

µα 0.19
Compression elasticity Compression amount Compression recovery

Claims (7)

10 15 claims: 1. Treatment agent for synthetic filler fibers, based on an amino compound and a Epoxysiloxane, characterized in that it is used as an active ingredient (a) 1 part by weight of an aminosilane of the formula: R ₃
O R ₁ -NH-R ₂ -Si-OR ₄
O wherein R _{1 is} a hydrogen atom, an alkyl group having 1 to 4 carbon atoms or a phenyl group, R2 is an alkylene group having 1 to 4 carbon atoms and R ₃ , R4 and Rs are independently an alkyl group having 1 to 4 carbon atoms and
(b) 1 to 20 parts by weight of an epoxysiloxane which contains at least one structural unit of the formula: -O — Si R ₇ wherein Re and R7 independently of one another are Denote an alkyl group having 1 to 3 carbon atoms, and at least two structural units the formula R ₈ -O - Si- CH-
\ -CH ₂ 4 ^r > wherein R _{8 is} an alkyl group having 1 to 3 carbon atoms or the moiety -R ₉ -CH CH ₂ and R9 is an alkylene group having 2 to 5 carbon atoms or a substituted or mean unsubstituted arylene group having 6 to 10 carbon atoms, the epoxysiloxane 0.3 to 10% by weight epoxy groups, based on its total weight, contains. 2. Treatment agent according to claim 1, characterized in that the epoxysuoxane has a viscosity from 1,000 to 100,000 centistokes at 25 ° C 3. Treatment agent according to claim 1 or 2, characterized in that the proportion of the Epoxysiloxane is 1 to 18 parts by weight per part by weight of the aminosilane 4. Treatment agent according to claim 1 to 3, characterized in that there is one in Foriu aqueous emulsion is present 5. A method for treating synthetic filler fibers, characterized in that in the synthetic Fibers a treatment agent that acts as active ingredients (a) 1 part by weight of an aminosilane of the formula:
R ₃
O R ₁ -NH-R ₂ -Si-OR ₄
O wherein Ri to R5 are those given in claim 1 Have meaning, and (b) 1 to 20 parts by weight of an epoxysiloxane which contains at least one structural unit of the formula: R ₆ -O- Si-R ₇ and at least two structural units of the formula: R ₈ -O —Si- CH -CH ₂ C) wherein R ₆ to R _{9 have} the meaning given in claim 1, the epoxysuoxane having 0.3 to 10% by weight of epoxy groups, based on its total weight, is so impregnated that the total amount of the adhering aminosilane and epoxysiloxane 0.1 to 3.0% by weight, based on the dry weight of the fibers, and then a heat treatment is carried out at a temperature of 100 to 230 ° C for at least 1 second. 6. The method according to claim 5, characterized in that the synthetic fibers before Heat treatment have been subjected to a curling treatment. 7. The method according to claim 5 or 6, characterized in that synthetic fibers are used as synthetic fibers Polyester fibers are used.