DE2505742C3 - 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. Furthermore, the Invention a method of treating these synthetic fibers with the treating agent. That Treatment agent gives the synthetic filler fibers superior compression elasticity, smoothness, suppleness and a soft feel similar to quilted quilts and good usage time and behavior.

Cotton and feathers were the usual main filling materials for quilts or quilts and due to particularly superior compressive elasticity, smoothness, suppleness and the feel of springs Bed quilts with the use of feathers as a filling material are used as luxury items

In recent years, such fillers have been replaced by synthetic fibers such as Polyester fibers or polypropylene fibers, detached, however, have oil materials made from such synthetic fibers, compressive elasticity, smoothness and suppleness inferior to springs and grip and result in poor body conformance when used in bed quilts will.

Attempts have been made to produce luxury bed quilts with good compressive elasticity and a soft feel by the fiber arrangement of the filling using synthetic fibers was used. For example became an attempt to use synthetic fibers in the form of tow instead of staple fibers undertaken. However, this process does not result in any significant change in fiber properties and the bed quilts obtained cannot be compared with the feather quilts, although they are better Deliver compression elasticity, smoothness and better grip than bed quilts using the usual synthetic fiber fillings in stack form. Furthermore, this method has another disadvantage, by using the fibers in tow form, as common processes for the manufacture of bed quilts as such cannot be used.

Without any effective and decisive solution to the problem, current practice is Use of synthetic fiber filling materials that are compatible with a treating agent composed primarily of a surface active agent. For example, in Japanese Laid-Open So Patent application 67 592/73 specified a treatment agent which consists of 80 to 60% by weight of a potassium salt of an ethylene oxide (2 mol) added to lauryl phosphorus ether and 40 to 20% by weight of an arbitrary one Propylene glycol ethylene oxide copolymers with a "■ -, average 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 treatment agent cannot have compressive elasticity, smoothness and feel similar to feathers.

Attempts have therefore been made to treat synthetic fibers for fillings with synthetic textile fiber treatment agents that have hitherto been used in view of the Granting smoothness and suppleness similar to animal fibers such as alpaca and mohair synthetic fibers have been suggested. For example, this was disclosed in U.S. Patent 3,655,420 specified treatment agent, which is a mixture of about 0.3 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 compression elasticity to the smoothness and flexibility Synthetic fibers have given it the serious flaw that, due to its strong activity, this Mixture has poor storage stability; when left in the form of an emulsion, it shows gradually a crosslinking at room temperature and in about 2 or 3 days it is damaged if this Treatment agent is used in the circulation, there is no uniform treatment due to the Networking, which takes place at elevated temperatures during operation, is ensured and the networked Treatment agent often adheres strongly to rollers and other treatment equipment, causing it it becomes necessary to interrupt work frequently. In addition, according to US-PS 36 55 420 did not obtain entirely satisfactory results as from the experimental results given later emerges

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, pliability, soft hand, and good service life and good quality Usage behavior results and unites a method for treating the synthetic filler fibers with the Treatment agents.

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 (I)

O R,

wherein Ri is a hydrogen atom, an alkyl group having 1 to 4 carbon atoms or a phenyl group, R _{2 is} an alkylene group having 1 to 4 carbon atoms and Rj, R ₄ and R5 are independently an alkyl group having 1 to 4 carbon atoms and

(b) I to 20 parts by weight of an epoxysiloxane which has at least one structural unit of the formula

-O — Si-

(Π)

that are comparable or that exceed them.

This is also proven by the following test results.

The following experiments were carried out in order to show that the treating agents for synthetic filler fibers according to the invention are superior Provide advantage over those treated with the treatment agent according to US Pat. No. 3,655,420.

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.

O — Si -

R, CH-

CH ₂

wherein Rg is an alkyl group having 1 to carbon atoms or the moiety

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 The skein obtained with a total denier of 400,000 denier (individual fiber denier 6 denier) was converted into a treatment agent (IH) 20 in each case from one of those listed in Table A. Approaches immersed as an aqueous solution, with a compression crimping device to an uptake of 10% squeezed off and dried at 90 ° C. for 20 minutes. The strand was then at 140 ° C. during Heat treated for 30 minutes and cut to a fiber length of 76 mm.

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

JO

- R, --CH-

-CH ₂

J5

and R9 is an alkylene group having 2 to 5 carbon atoms or a substituted or unsubstituted one Arylene group with 6 to 10 carbon atoms, the epoxysiloxane 03 to 10 % By weight of epoxy groups, based on its total weight

The method according to the invention box treatment of synthetic filler fibers is characterized in 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 having at least one structural unit of the above Formula (H) and at least two structural units of the above formula (III) where the epoxysiloxane has from 3 to 10% by weight of epoxy groups based on its total weight, is so impregnated that the total amount of adhering aminosilane and epoxysiloxane 0.1 to 3.0 wt.%, based on the dry weight of the Fibers is and then a heat treatment at a temperature of 100 to 230 ° C during 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 yields synthetic fiber fillings with superior compression elasticity, smoothness, pliability and feel Usage behavior that is similar to that of feather quilting

Table A. Treatment agent (part by weight)
I II III
(US-PS inven-
36 55 420) education
according to 0.88 0.57 composition 0.34 Hexamethylene
diamine
y-aminopropyl
triethoxysilane

45

Epoxysiloxane (l) *) 4.99 Potassium cetyl phosphate 1.17

Polyoxyethylene 0.5

(10 moles) nonylphenyl ether

Water 93.0

4.45 4.76 1.17 1.17 0.5 0.5

93.0

93.0

*) The epoxysiloxane (I) given above existed "From structural units of the following formulas:

60

L ¹ Il

\ -O- Si-f
i CH, I

and

CH,

-Si-O- (CH ₁ ), HC

CH,

and has a viscosity of 6000 centislokes at 25 C ", a Bpoxygru,) rengehält of I wt.%, with a trimethylsilyl group I-SKCH, h] on both linden trees.

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

Each of the pulps treated according to the procedure outlined above were hand-finished touched. It was found that the fibers treated with the treatment agents II and III were one had a good feel, similar to a feather quilt, while those treated with treatment agent I. Fibers 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 that with the treatment agents according to of the invention (treatment agents II and III) had treated fibers. This means that the dynamic Frictional resistance between the fibers treated with the treating agent I is high, i.e. theirs Smoothness is poor. It follows that when 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 particularly preferred as alkyl groups, 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.

Suitable aminosilanes include, for example: Aminomethyltrimethoxysilane, ß-aminoethyltrimethoxysilane, 0-Aminoäthyltriälhoxysilan, y-aminopropyltrimethoxysilane, y-aminopropyltriethoxysilane, (5-aminobutyltriethoxysilane, ß-methylaminoethyltriethoxysilane, / 3-ethylaminoethyltriethoxysilane, y-methylaminopropyltrimethoxysilane, y-Fropyiaminopropyiiriäinoxysiian, d-ethylaminobutyltriethoxysilane, y-phenylaminopropyltrimethoxysilane and y-phenylaminopropyltriethoxysilane. Of these will be y-aminopropyltriethoxysilane

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

[H ₂ NC ₃ H ₆ Si (OCH ₃ ) J, / J-Metfc / laminoethyltriethoxysilane

[CH ₃ NHC ₂ H ₄ Si (OC ₂ Hs) ₃ ] and γ-phenylaminopropyltrimethoxysilane

[Ph-NHC ₃ H ₆ Si (OCH ₃ ) J.

preferred. Of these, γ-aminopropyltriethoxysilane is particularly preferred.

in the treatment agent according to the invention there is an epoxysiloxane with the following repeating units

and

-O - Si

• ν

R »

-O — Si-R,

(Π)

CH CH ₂

(ΙΠ)

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-chain or branched and contains 2-5 carbon atoms. For example, it includes ethylene,

Propylene, butylene and pentylene groups, of which ethylene and propylene groups are particularly preferred. R9 can also be an arylene group, for example a phenylene or naphthylene group.
The group Re can also be the group

- R ₉ -CH

-CH ₂

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

O
CH-

-CH:

O - Si

(IV)

CH

-CH ₂

may contain.

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

they uic VJi uiiucigciiaunai icu ucs L-puAjraiiuAana iii «.iit change considerably. The terminal groups can usually consist of trialkylsilyl or hydroxyalkylsilyl groups, but can also be silicon-free groups. If the molecules form a ring, the absence of terminal groups is also possible.

The epoxysiloxanes used according to the invention in the treatment agents are advantageously liquid and have a high molecular weight. It is usually advantageous to add epoxysiloxanes with viscosities at 25 ° C. of 1000 to 100,000 centistokes, preferably 3000 to 100,000 centistokes, most preferably 3000 to 20,000 centistokes use.

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 from 03 to 10% by weight, preferably from 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 soluble or in water

Water can be easily dispersible for easy use, but they can also be combined in one if desired

-, organic solvent 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

in up 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,

ii like 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 treatment agent of 1 part by weight einp «; Aminosi'ans of the above formula (I) and 1 to 20 parts by weight of an epoxysiloxane with at least one Structural unit of the above formula (II) and at least two structural units of the above

2i formula (III) and / or (IV) on synthetic fibers for Fillings are applied and then the fibers are heat treated.

The adhesion of the treatment agents according to Invention to the synthetic filling fibers can

jo 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,

J3 before or after the previous 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. The concentration of the ami.iosilane and the epoxysiloxane in such a solution or dispersion can be within a range vary. 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 goes without saying that this concentration range is not strictly critical, but depends on the method of application, the type of synthetic fibers and the like, is dependent, so that concentrations outside the above range can also be used.

The application of the treatment agent to the

Synthetic fibers can be produced according to various measures, such as dipping processes, oiling roller winding processes 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, however, using 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 wt .-%, preferably 0.2 to 1.5 wt .-%, 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 or an antisutic agent and the like may be mixed in order to facilitate dispersion of the effective ingredients. Examples of preferred emulsifiers and antistatic agents are anionic surface-active agents such as polyoxyethylene alkylaryl ethers, polyoxyethylene alkyl ethers, polyoxyethylene sorbitan alkylamides, polyvinyl alcohol or their analogues or alkyl phosphate potassium salts and cationic surface active agents such as quaternary ammonium salts, ζ. B. Stearyldimethylbenzylammoniumchlorid or Stearylamidpropyldimethyl-ji-hydroxy üthylammoniiimnitrat

After applying the treating agent of the invention to the fibers, preferably at one If the temperature does not exceed 50 ° C, the fibers are used to harden and crosslink the aminosilane and the Epoxysiloxane in the treating agent heat-treated on the surface of the fibers. This grants the Fibers significantly improved compressive elasticity, smoothness, pliability, grip and usability. These 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 not sufficient. On the other hand, if it is too high, the properties will the fibers deteriorate. Therefore, in general, the heat treatment temperature is at least 100 ° C, but less than the melting point (or softening point) of the synthetic fibers and Temperatures from 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 use heat treatment within a short period of time that does not cause deterioration in the properties of the fibers cancel. If polyethylene terephthalate fibers are used, the period is about 10 minutes up to 2 hours at a temperature of 110 to 170 ° C suitable and a period of 1 second to 10 minutes is particularly suitable when the temperature 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 setting of the treatment agent and heat setting of the crimps at the same time can be done.

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 by heat treatment or

■ j chemical treatment will 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

done in. 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

ii the type of synthetic fibers to which the Treatment agents and the treatment method of the invention can be applied and examples suitable synthetic fibers are synthetic polyester, polyamide, polyacrylic and polyolefin fibers.

The polyester fibers are particularly suitable.

Thus, according to the invention with a heat-treated product of the aminosilane and the Epoxysiloxani coated synthetic fibers are obtained which have excellent compressive elasticity, smoothness and

»■> Have suppleness and a soft handle. When these fibers are used as a filling material for bed quilts, they exhibit a soft hand similar to feather quilts and result in good usability.

jn Those treated and curled and optionally cut according to the method 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

It has been found that when the synthetic fibers have the following properties, fillers of superior quality due to the beneficial interaction between the properties of the fibers and the Treatment of the invention.

1,5SDS10

10D-20SLS10D + 60
lOSZ.

15.5

wherein

D is the denier size of the synthetic fibers,

L is the length of the fibers in mm,

C _{n 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 the 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 in processing on cards). When suppleness is considered, that is particularly preferred

Donating size of the fibers at 2 to 8 denier. When a When producing fullness, fibers of different denier sizes as well as the same denier size can be used will.

If the length (L mm) of the fibers is too short, the entanglement of the fibers at the time of making 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-20SLS10D + 60

particularly preferred

10D-10 <L <10D + 50
3OS L

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

-3 / 4D +

-3 / 4D + 15.5

more preferably within the following range -3 / 4D + 11, OSO / S -3 / 4D + 14.5

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 go beyond the upper limits, the smoothness of the filler material is slightly reduced. These curling 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 provide a more detailed explanation the invention. In the examples, all parts relate to parts by weight and all Viscosity values are expressed in centistokes at 25 ° C. The compressive elasticity, smoothness and suppleness were evaluated by the following methods.

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 compression elasticity is evaluated as follows: A web is made by processing raw fibers on a card and it becomes a sample of cylindrical shape with a diameter of 10 cm

/ U UIIU CIIICHI VJCWIlIfI VUII i \ f g HCI rock. L-.III 31.111.ILrWIIaI - term 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 the heavy Weight is removed and the sample is allowed to 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 is applied and the height (h ₂ ) 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

If customization results in similar feather quilts, 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 frs) 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 humidity of 65% are measured, evaluated The lower the με and μό values, the better the smoothness. Both the, ws and the μά value are preferably not more than 0.25.

15th

handle

A feel test is carried out on the handle of the filler material of the invention of 2.0 kg of Poh fibers distributed on a card are distributed evenly in a sack made of a quilted bedcloth with a size of 140 cm χ 200 cm brought the handle 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. Of the obtained strand having a total denier of 000 (having a single fiber denier of 6) was turned into a Dipped treatment agent of the recipes given in Table I as an aqueous emulsion a filler curling device squeezed to an uptake of 10% and at 90 ° C for 20 minutes

Table I.

dried ίο Then the strand was at 140 ° C for 30

Heat-treated minutes and to a fiber length of

76 mm cut. The properties of the fibers obtained are in

Table II reproduced. The number of crimps was 7 per 25 mm and the percentage of crimp was 18% in all cases.

composition

Treatment center! (Parts) ABCD

y-aminopropyltriethoxysilane y-aminopropyltrimethoxysilane

jff-methylaminoethyltriethoxysilane

y-phenylaminopropyltrimethoxysilane

Epoxysiloxane (1) *) cetyl phosphate potassium salt

Polyoxyethylene {10 MoD nonylphenol ether

Water too

0.5

P5

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

93.0 93.0 93.0 93.0

• »The epoxysiloxar (MI) used above consisted of Structural units of the following formulas:

CH,

CH,

and

and had a viscosity of 6000 centistokes at 25 ° C., an epoxy content of 1% by weight, with both ends consisting of trimethylsilyl groups I-SKCH ₁ ) I ₁ ].

Table II

Treatment agents AB C D

smoothness

Compression elasticity Compression amount Compression recovery

handle

0.17 0.17 0.18 0.19 0.16 0.17 0.17 0.20

79 78 77 75 99 99 97 95 very similar to feather quilts

130 209/181

Comparative example 1

smoothness

_ A mixture of 60 wt .-% of a potassium salt of Ethylene oxide (2 mol), added to lauryl phosphorus ether and 40% by weight of an arbitrary copolymer Propylene glycol and ethylene oxide with an average molecular weight of 24,000, in which 5 moles of ethylene oxide were added to 1 mol of propylene glycol, was processed to a 2% aqueous emulsion. The same Polyethylene terephthalate strand as used in Example 1 was immersed in this treating agent through a filler curling device to a Absorption of 10% squeezed for 2 hours heat-treated at 140 ° C and then cut to a length of 76 mm. The number of crimps of the fibers obtained was 7 per 25 mm and the percentage crimp was 18%.

The fibers treated in this way had the following properties:

! 0

με 036 μά 030

Compression elasticity Compression amount 64% Compression recovery 88%

handle worse than feather quilts (haner 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, if necessary, in Table III reproduced.

Table UI Attempt no 2-2 2-3 8000 2-5 2-6 2-7 2-1 1000 3000 10,000 100,000 150,000 500 Viscosity of the 0.18 Epoxysiloxane 0.19 0.17 0.19 0.19 0.19 0.24 smoothness 0.23 0.19 0.19 0.20 0.21 0.26 ys 0.25 78 Compression 74 80 77 73 68 elasticity 68 98 Compression 93 97 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 IH it can be seen that epoxysuoxanes having a viscosity of 1000 to 10,000 centistokes gave particularly 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 50 became. The results are also shown in Table IV Represented in the treatment agent A used in Example 1.

Table IV Attempt no. 3-2 3-3 3-1 1.0 3.0 0.5 Epoxy group content (wt .-%) 0.16 0.17 Olalte 0.24 0.16 0.16 0.25 80 79 Compression elasticity 66 98 97 Compression amount (%) 87 same Feather quilts Compression recovery (%) Worse handle as feather quilting cover (hard)

Example 4

20th

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 The results used in the treating agent of Example 1 are presented in Table V.

Table V Attempt no. 65 4-2 4-3 same 4-4 4-5 4-6 4-1 1 5 10 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 / « 0.25 as a feather
quilts Vd Compression elasticity (hard) 73 79 80 75 68 Compression extent 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 y-aminopropyltrietho>: ysilane. The other components of the treating agent were the same as in Example 1.

Good results have been obtained when the amount has an epoxy group content of 1.8% by weight, the epoxysiloxane being 1 to 20 G-iw.-Τβώ per part by weight of the two ends of trimethylsilyl groups [- Si (CH ₃ J ₃ ] darstely aminopropyltriethoxysuans var. 35 len.

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

Example 5

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

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

CH ₃ "
-O-SI

CH,

and

55

60

CH ₃

-O-Si - CH ₃

/ CH

-CH ₁

(CH ₂ ), -O-Si

(CH;),

HC

CH ₂

with a viscosity of 5000 centistokes at 25'C and

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

The results are given in Table VI below.

Table VI

Attempt no. 5-2 5-1 Treatment agents 0.9 y-arainopropyltriethoxysilane 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 Smooth fc 0.16 με 0.18 0.17 Ud 0.19

Compression elasticity Amount of compression Compression recovery

handle

measured value, of 0.62 was soft spun and to form a tow with a total denier of 400,000 consisting of hollow fibers of 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%. Treated like that th fibers had the following properties:

Smooth με 0.16 (id 0.16 compression elasticity

Compression amount 78 Compression recovery 98 handle

equal to feather quilts

equal to feather quilts

Example 6

Polyethylene terephthalate having an inherent viscosity of 0.62, calculated from the value measured in o-chlorophenol at 35 ° C, was melt spun and drawn to form a tow having a total denier of 500,000 (single fiber denier 3). The tow was immersed in an emulsion of the recipe listed below, squeezed by a Füllmittelkräuselvorrichtung to a pickup of 6%, dried at 90 ° C for 20 minutes, then heat treated at 140 ⁰ C for 30 minutes and cut mm to a length of 56th

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

Treatment agent prescription

γ- aminopropyltriethoxysilane 1.0 part by weight

Epoxysilane (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

/ ts 0.17

/u/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

Example 8

Pc iyäthylenterephthalat with an inherent viscosity, calculated from the value of 0.65 measured in o-chlorophenol at 35 ° C and polyethylene terephthalate isophthalate (10 mol% iso- phthalic acid) were spun simultaneously at a weight ratio of 1: 1 using a side-by-side spinneret and onto the ' 33 times the original length in warm water held at 75 ° C to form a Tow with a total denier of 80,000 (single fiber denier equal to 6.8). The tow was heat-treated in the relaxed state in air at 80 ° C and in the treatment agent A of Example 1 immersed It then became du.ch a Füllmittelkräuselvorrichtung squeezed to a pickup of 12% and dried at 8O ⁰ C for 30 minutes. It was then in a relaxed state at 160 ° C. for 30 minutes to develop crimps at the same time as they were heat-strengthened heat-treated 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 ßs 0.18 μά 0.17

Compression elasticity Compression amount 76 Compression recovery 98

handle equal to f-ders 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

2Ϊ

a flame retardant of the following formula: 24

HIGH ₂ CH ₂ O

Br

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, CH ₂ OH

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

smoothness

µ-s 0.18

μά 0.19
Compression elasticity Compression amount Compression recovery

Claims (7)

Patent claims: 1. Treatment agent for synthetic filler fibers, based on an amino compound and an epoxysuoxane, characterized in that that 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, O Rs wherein Ri is a hydrogen atom, an alkyl group having 1 to 4 carbon atoms or a Phenyl group, R2 is an alkyl group with 1 to 4 Carbon atoms and R * R * 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 epoxysuoxane which contains at least one structural unit of the formula: -0 — Si ! 0 15th 20th 25th 30th J5 wherein R «and R7 independently of one another Mean alkyl group with 1 to 3 carbon atoms, and at least two structural units of the formula R. O —Si- R,
CH- CHj 45 50 55 wherein Ri is an alkyl group with I to 3 Carbon atoms or the grouping R ₉ -CH-
\ CH ₂ 60 and R9 is a Alkyiengruppe having 2 to 5 carbon atoms or a substituted or unsubstituted arylene group having _h5 6 to 10 carbon atoms, wherein the epoxy polysiloxane 0.3 to 10 wt .-% F.poxygruppen, based on its total weight, contains 2. Treatment agent according to claim I, characterized in that the epoxy uroxane has a viscosity of 1000 to 100,000 centistokes at 25 "C. 3. Treatment agent according to claim 1 or 2, characterized in that the proportion of the Epoxysüoxans 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 it is present in ^c orm an aqueous emulsion. 5. A method for treating synthetic filler fibers, characterized in that a treatment agent in the synthetic fibers as Active ingredients (a) 1 part by weight of an aminosilane of the formula: R ₁ -NH-R ₂ -Si-OR ₄ O Rs wherein Rt to Rs are those given in claim 1 Have meaning, and (b) 1 to 20 parts by weight of an epoxysuoxane which contains at least one structural unit of the formula: R ₆ -O-Si- R7 and at least two structural units of the formula: wherein R ₄ to R _{9 have} the meaning given in claim I, wherein the Epoxysuoxan has 0.3 to 10 wt .-% epoxy groups, based on its total weight, is so impregnated that the total amount of the adhering aminosilane and Epoxysüoxans 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 polyester fibers are used as synthetic fibers.