DE2505742A1 - TREATMENT PRODUCTS FOR SYNTHETIC FIBERS - Google Patents

Description

PATENT LAWYERS

DR. E. WIEGAND DIPL-iNC. W. ΝΙΈΜΛΝΝ DR. M. KÖHLER DIPL-ING. C. GERNHARDT

MÖNCHEN HAMBURG

TELEPHONE = 555476 8000 MONKS 2,

TELEGRAMS: KARPATENT MATHI LDENSTRASSE 12

TELEX: 5 29 068 IC ARPD

V. 4-2 257/75 -. Wtte February 12, 1975

Teigin Limited Osaka (Japan)

Treatment agents for synthetic filler fibers

The invention relates to a treatment agent for synthetic Fibers for use as filling or cushioning material, a method of treating synthetic fibers Fibers with this treatment agent and synthetic fibers for filling obtained by treatment with the treatment agent became. In particular, the invention relates to a treatment agent for synthetic 'filler fibers, the superior Compression elasticity, smoothness, suppleness, soft feel similar to feather quilts and usability, a method of treating this synthetic fibers with the treatment agent 'and synfclietic Filler fibers obtained by treatment with the treating agent.

Cotton wool and feathers were the common main filler materials For bed quilts or the like. And. due to particularly superior compressive elasticity, smoothness and flexibility and the handle of feathers, bed quilts became

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BATH ORIGINAL

using feathers as filling material as luxury items used.

In recent years, such fillers have been replaced by synthetic fibers such as polyester fibers or polypropylene fibers. However, fillers made from such synthetic fibers have are constructed, compressive elasticity, smoothness, pliability and grip inferior to springs and result in poor ones Adapt to the body 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 was used. For example, the attempt was undertook to use synthetic fibers in the form of tow instead of staple fibers. However, this proposed method does not result in any significant change in the fiber properties and the quilts obtained are not comparable to feather quilts, although they are better Provide compression elasticity, smoothness and better feel than bed quilts using the usual synthetic ones Fiber fillings in stack form. Furthermore, this method has another disadvantage in that the fibers are in tow form is used because conventional methods of manufacturing bed quilts cannot be used as such.

Current practice is to use without any effective and decisive solution to the problem synthetic fiber fillers formed with a predominantly surfactant gown Treatment agents have been treated. For example, in Japanese Patent Application Laid-Open No. 67592/73

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a treatment agent specified, which consists of 80 to 60 wt.% of a potassium salt of an ethylene oxide (2 mol) added Laurylphosphoric ether and 40 to 20% by weight of an arbitrary one Propylene glycol .iiylene oxide CoOol viners with a medium

consists, . .. Molecular weight of 24,000 / wherein 5 moles of ethylene oxide on "~ 1 mol of propylene glycol are added. Synthetic Ifaser fillers treated with this treatment agent, cannot have compressive elasticity, smoothness and grip similar to springs.

Attempts have therefore been made to use synthetic fibers for fillings with synthetic textile fiber treatment agents. to treat that have been proposed so far with a view to imparting smoothness and suppleness similar to animal fibers, such as alpaca and mohair, to synthetic fibers. For example, this has been described in U.S. Patent. 3 655 4-20 specified treatment agent, which is a mixture of about 0.3 to 20 parts by weight of a liquid epoxysiloxane and Λ part by weight of an amine compound with at least two amino groups per molecule and no more than one aromatic ring bonded directly to the nitrogen atom, is used .

If this mixture also has superior compression elasticity, smoothness and suppleness to the synthetic fibers issued, it has a serious flaw that due to its strong activity, this mixture has poor storage stability Has; when left to stand in the form of an emulsion, it gradually shows crosslinking Room temperature and in about 2 or 3 days it is damaged. When this treatment agent is used in the circulatory system, there is no uniform treatment due to the networking, which takes place at elevated temperature during operation, ensured and the crosslinked treatment agent often adheres strongly to rollers and other hand-

609833 / 091-5

treatment facilities ah, making it necessary to work to interrupt frequently.

A main object of the invention is therefore a treatment agent for synthetic fibers, which synthetic fiber fillings with superior properties such as resilience, smoothness, pliability, softness Grip and suitability for use results.

Another object of the invention is a method for treating synthetic filling fibers using such a treating agent.

Another object of the invention is synthetic filling fibers treated with the above treating agent are treated and have superior resilience to compression, smoothness, suppleness, grip and suitability for carrying and bed quilts that are comparable to feather quilts are.

Another object of the invention is to provide bedspreads having the above superior properties.

Further objects of the invention, along with their features and advantages, will be apparent from the following description.

According to the invention, a treatment agent results for synthetic filling fibers, consisting of

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

Si-O-R ^ (I)

wherein R ^ is a hydrogen atom, an alkyl group having 1 to 4 carbon atoms or a phenyl group, dp a

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Alkylene group with 1 to 4 carbon atoms and R ₇₁ , R. and Rc- independently of one another denote an alkyl group with 1 to 4 carbon atoms,
and

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

-O-Si
R ₇

(II)

^ and Rr _7, independently of one another, have an alkyl group

Mean 1 to 3 carbon atoms,

and at least two structural units of the formula

-O -

oil-

CH - CH ₀

V ²

wherein Ro is an alkyl group having 1 to 3 carbon atoms or the group Rg-CH-CHp, Rg is an alkylene group

2 to 5 carbon atoms or a substituted or unsubstituted one Mean arylene group having 6 to 10 carbon atoms.

The foregoing treating agent has an effect of markedly reducing the coefficient of friction of synthetic fibers for fillings, and yielding synthetic fiber fillings with superior press resilience, smoothness, pliability, feel and ease of use that are comparable to or exceed those of feather quilts.

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In the aminosilanes of the formula (I), the alkyl and alkylene groups 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-butyl engrupp en. 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 used according to the invention of the formula (I) are known compounds, and new aminosilanes of the formula above can be used in completely the same way as with the method for the production of the known AriinoDilane has been manufactured.

Suitable aminosilanes include, for example:

Aminomethyltriinethoxysilane,

ß-aminoethyltrimethoxysilane,

ß-Aminoäthyltriäthoxysilan,

γ-aminopropyltrimethoxysilane,

γ-aminopropyltriethoxysilane,

^ -Aminobutyltriethoxysilane,

ß-methylaminoethyltriethoxysilane, ß-ethylaminoethyltriethoxysilane, γ-methylaminoprop2 ^ 1trimethoxy silane, γ-propylaminopropyltriethoxysilane, t ^ -ethylaminobutyltriethoxysilane, γ-phenylaminopropyltrimethoxysilane and γ-phenylaminopropyltriethoxysilane.

Of these, γ-aminopropyltriethoxy / silane

γ-aminopropyltrimethoxysilane ß-methylaminoethyltriethoxysilane Ic) -J and γ-phenylaminopropyltrimethoxysilane / Ph-IIIHC ^ H ^ Si (OCH _7. ) ^ J are preferred. Of these, γ-aminopropyltriethoxysilane is particularly preferred.

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In the treatment agent according to the invention there is an epoxysiloxane having the following repeating units

O -

ι ©

Si

R ₇

and

O - Si
? 9

(II)

O (HI)

used in combination with the aminosilane of formula (I).

In the above formulas, those with R _c , R

and R

specified alkyl groups 1 to 3 carbon atoms and can be either straight chain or branched chain. The alkyl groups include methyl, ithyl and n- or isopropyl groups, of which methyl groups are particularly suitable. The alkylene group indicated by Rq can be either straight-chain or be branched 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. Hq can also be a Arylene group, for example a phenylene or naphthylene group be. .

The group Rg can also be the group -Rn-CH-CHg

o ^y

interpret. This means that the used according to the invention Epoxysiloxane also has a structural unit of the following iormel

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CH - CH

Si

CH - CH

(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 100 to 600 such units in total contain and at least two, preferably 4 to 20 of these must be recurring units of the formula (il).

Usually, the recurring: units (II) and (III) and / or (IV) can be completely present in the epoxysiloxane, however, they can also be in block form. A small amount of other repeating units can be added be included unless they significantly change the basic properties of the epoxysiloxane. The terminal ones Groups can usually be selected from trialkylsilyl or Hydroxyalkylsilyl groups exist, but can also be silicon-free groups. If the molecules form a ring form, the absence of terminal groups is also possible.

Advantageously, those according to the invention are in the treatment agents Epoxysiloxane used liquid and Viaben a high molecular weight. Usually it is advantageous, epoxysiloxanes with viscosities at 25 ° G of 1000 to 100,000 centistokes, preferably ^ O00 to

000 centistokes, most preferably 3000 to 20,000 centistokes.

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The epoxysiloxanes used according to the invention preferably contain at least 0% by weight of epoxy groups, based on their total weight. The upper limit of the epoxy group content is not critical, but the amount of epoxy groups is usually 0.1 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 given in U.S. Patent 3,055 ΊΊ ¹ ^ and are valuable. .

The epoxysiloxanes must be water soluble or in water be easily dispersible for ease of use, but they can also be in an organic one if desired Solvent or in the absence of a solvent.

The epoxysiloxanes described above can be used in a proportion of 1 to 20 parts by weight, preferably 1 to 18 parts by weight, more preferably 10% by weight, per part by weight of the aminosilane of the formula (I).

Due to the adhesion of the treatment agent according to Invention of syntheti see filling fibers are different properties suitable for filling purposes, such as superior resiliency, smoothness, pliability, grip and The synthetic fibers are suitable for wearing. -

According to the invention there is a method for treating synthetic fibers for fillings, wherein a treatment agent composed of 1 part by weight of an aminosilane of the above formula (I) and 1 to 20 parts by weight of one Epoxysiloxane with at least one structural unit of the above formula (II) and at least two structural units of the above formula (Hl) and / or (IV) to synthetic Fibers for fillings are applied and then

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the fibers are heat treated.

The adherence of the treatment agents according to the invention to the synthetic filling fibers can take various forms known methods are effected. The time of application can be before or after the stage of stretching extruded synthetic fibers, before or after the crimping treatment step, before or after. Level of Bulking, before or after the previous heat treatment step 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, but is usually advantageously used in the form of an aqueous dispersion, in particular an aqueous emulsion is used. The concentration of the aminosilane and the epoxysiloxane in such a solution or dispersion can vary within a wide range. The right concentration is 0.5 to 20% by weight, preferably 1 to 15% by weight, based on based on the weight of the solution or dispersion. It goes without saying that this concentration range is not is strictly critical, but depends on the application method, the type of synthetic fibers and the like, so that also concentrations outside the above Area can be applied.

The application of the treatment agent to the synthetic Fibers can be processed according to various measures, such as dipping processes, roller application processes or spraying processes take place. This results in adhesion or impregnation of the treatment agent according to the invention on or, in synthetic fibers.

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

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In general, it is advisable to use them in a total amount, based on the dry weight of the irons, of at least Apply 0.1% by weight. There is no specific upper limit, but the use of too large amounts brings about no corresponding effect, but is uneconomical. Usually, the total amount of the applied aminosilane and the epoxysiloxane is expediently 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 or an antistatic agent and the like may be mixed 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 ones surfactants such as quaternary ammonium salts, e.g. B. stearyldimethylbenzylammonium chloride or stearylamide propyldimethyl-ß-hydroxyethylamoionium nitrate.

After applying the treating agent of the invention on the fibers, preferably at a temperature not above 50 ° C., the fibers are used to harden and crosslink the Aminosilane and the epoxysiloxane in the treating agent are heat-treated on the surface of the fibers. This granted the fibers considerably improved compressive elasticity, smoothness, pliability, grip and usability. This heat treatment also significantly improves wash resistance of the fibers. The treatment temp. Htnr varies depending on the treatment time and cannot be clearly determined. If the temperature is too low, are long Periods of time required to carry out the heat treatment

509833/091 p

ren and the effect obtained is not sufficient. On the other hand, if it is too high, the properties of the fibers will deteriorate. Therefore, in general, the WärmebehandlungstemperaiLir at least 100 C but less than the melting point (or softening point) of the synthetic fibers and temperatures of 100 to 2 John ⁰ C are particularly suitable. The heat treatment time is at least 1 second and can be varied over a wide range according to 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, they must Fibers are curled. The frizz treatment can be done before, be carried out during or after the treatment of the fibers according to the invention. It is preferred to be synthetic To crimp fibers to 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 setting of the crimps can occur simultaneously.

The frizz treatment can be done by several methods carried out, for example mechanical crimping methods using a filling crimping device, a gear crimping device and the like. Or latent crimps Methods in which the crimps are caused by heat

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treatment or chemical treatment.

Usually the fibers so treated are cut to suitable lengths.

The curling treatment can also take place after the treatment of the fibers according to the method of the invention *. Or it is also possible to apply the treatment agent of the invention to fibers which are initially crimped synthetic fibers and then optionally cutting were obtained. .

There is no particular limitation on the type of synthetic fibers on which the treating agent is applied and the treatment method of the invention can be used and are examples of suitable synthetic fibers synthetic polyester, polyamide, polyacrylic and polyolefin fibers. The polyester fibers are particularly suitable.

Thus, according to the invention with a heat-treated Aminosilane and epoxysiloxane coated synthetic fibers product get that excellent Have compressive elasticity, smoothness and suppleness and a soft handle. When these fibers are used as filler material Used for bed quilts, they have a soft feel similar to feather quilts and make good Usability.

The synthetic treated and curled and optionally cut by the process of the invention Fibers can be used as filling materials or cushioning materials for bed quilts, pillows or other quilts and the like., Can be used. It was found, that if the synthetic fibers have the following properties, fillers are of superior quality by the beneficial interaction between the properties of the barrels and the treatment of the invention.

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1.5 = D ^ 10

10 D - £ 20 LI 10D + 60
10 ^ L

+ 10.0 i C _F ^ -3 / 4D + 15.5

where D is the denier size of the synthetic fibers, L is the length of the fibers in mm, C-vr is the number of crimps per 25 mm and Cjj is the crimp percentage (%) measured

according to the method described in JIS L-1074. .

Synthetic fibers, especially polyester fibers, with the above properties and those with the treatment agent of the invention not only provide superior compressive elasticity, smoothness, flexibility, superior Grip and superior usability, but all properties that are required for filling materials or ■ cushioning materials are required, such as the highest degree 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 bulkiness Filler material and its handling properties (for example, the appearance of nodules during processing on cards). When compliance is a consideration, the particularly preferred denier of the fibers is included 2 to 8 denier. When making a bulk, fibers can be of different denier sizes as well as the same Denier size can be used.

If the length (L mm) of the fibers is too short, the fibers will become entangled at the time of manufacture of the filler materials is reduced, and fiber breakage is easy to occur. If it is too long, the fibers will lean

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to wrap around the card cylinder and develop also knot. That is, the handling properties the pasers are deteriorated. So it becomes preferred that the length of the fibers be as follows:

1OD - 20 =. L £ 1OD + 60 10 ^ L,

particularly preferred

10D -1O = L ^ 10D + 50

30 ^ L. ■ "■.-_ .. ■

The number is a measure of the frizz properties the crimps (C ™ -, number / 25 iim) and the percentage the curl (C-η,%) is preferably within the following Range:

+ 10.0 = G ₁₁ = -3Ad + 15.5

15 = C _n + C _D ^ 32
more preferably within the following range

-3AD + 11.0 = C _n ^ -3 / 4D + 14.5 18 ^ C _n + C _D ^ 30.

When the pucker properties below the lower If the above ranges are limited, the handling properties of the filler material tend to deteriorate and if they go beyond the upper limits, the smoothness of the washing material is slightly reduced. These crimping properties can be achieved in a simple manner, for example, by customary crimping devices be granted.

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. - 16 -

The treatment agent of the invention can be applied equally to synthetic parsers are, the ~ _f or as a filler in the form of Ver - strand used v / ground.

Synthetic fibers to which the treating agent of the invention has been applied and which optionally heat treated and curled have far superior compressive resilience, smoothness, pliability and superior grip and superior usability and possess a wide range of applications as filling material or cushioning material. Venn, for example, a quilted bedspread Made using these fibers, it delivers superior grip and conformance to the body comparable to feather quilts or beyond. If a pillow or winter clothing is made using these synthetic fibers, it will fit they fit well to the body.

The treatment agent of the invention described above results in synthetic filler fibers with superior compressive elasticity, smoothness, suppleness, superior grip and superior adaptability to use, thanks to the usual synthetic could not be achieved and the fibers can not only be used for filling purposes, but also in other fields which require the above properties. Thus, the treatment agent offers d.er Invention a great technical advantage.

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

This is an essential property as a filler

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material. In the case of quilts in particular, this becomes Compression amount a measure of the adaptability to the ■ body. It pushes the deformability of the fibers into tension on the bedding. The higher the amount of compression, the more deformable the fibers are in a quilt. the Compression elasticity is provided as follows: A web is made by processing fiber optics on a card and it is a sample of cylindrical shape with a diameter of 10 cm and a weight of 20 g. A disk-like one light weight (0.5 g / cm) and a disk-like heavy one Weight (9 »5 g / cm) are placed on the sample and Pressed for 10 minutes, after which the light and heavy weights are removed and the sample is left for 2 hours stand. 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 (h ·) of the sample at this point it is measured. Then the light and heavy weights are brought back to the sample and they are left to stand for 17 hours. The height (h ^) of the sample at this point it is measured. Then the light and heavy weights are removed. Subject expiration of 7 hours only the light weight is applied and the height (ho) of the sample is measured.

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

h - H ₁ amount of compression (%) = τ- χ 100 '

h ₂ - tu -

Compression recovery (%) = <? ? - χ 1Ό0

^a o * ⁿ 1 -.

509833/09 15

- 13 -

In order for the filling material to give a soft feel and ease of use similar to 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 (las) between fiber and fiber and the dynamic coefficient of friction (ud) between fiber and fiber at a speed of 3 m / Hin., Which according to the Roeder method at a temperature of 20 C and a relative Humidity of 65 % can be measured. The lower the las and tid values, the better the smoothness. Both the us and the / Ud values are preferably not more than 0.25 · "-..--

A feel test is carried out on the feel of the filler material of the invention. 2.0 kg from a card Distributed raw fibers are equally »-. casually into a sack brought a bed quilt with a size of 140 cm 200 cm. The handle is made by hand as well valued by use.

example 1

Polyethylene terephthalate with an inherent viscosity of 0.62, calculated from the measured value in o-chlorophenol at Z3 C, was melt-spun. The obtained strand mix; a total denierxv'ert of 400,000 (with a Linzelfaserdenier of 6) was immersed in a treatment agent of the recipes given in Table I as an aqueous emulsion, squeezed by a filler crimper to an absorption of 10% and at 90 ° G for 20 minutes dried.

509833/09 15

The strand was then heat-treated at 140 ° C. for 30 minutes and cut to a fiber length of 76 mm.

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

Table I.

composition

Treatment agents (parts) A BG D

γ-aminopropyltriethoxysilane

γ-aniinopropyltrimethoxysilane

ß-methylaminoethyltriethoxy? ilane

0.5

0.5

0.5

γ-phenylaminopropyltri-
methoxysilane 1 , 9 4.9 4th , 9 0.5 Epoxysiloxane - (1) * 0 1.1 1 ,1 4.9 Cetyl phosphate potassium salt 93 , 5 0.5 O , 5 1.1 Polyoxyethylene (10 moles)
Donyl phenol ethers , 0 93.0 93 , 0 0.5 Water too 93.0

The epoxysiloxane - (1) * used above consisted of structural units of the following formulas:

-Themselves

and

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and had a viscosity of 6000 centistokes at 25 ° C, an epoxy content of 1% by weight, with both ends consisting of trimethylsilyl groups Zr-Si (CH ^) ^ 7 .

Treatment agents

smoothness

Compression elasticity Compression amount Compression recovery

Tabel II 17th C. D. A. B. 17th 0.18 0.19 0.17 ο, 0.17 0.20 0.16 ο, 77 75 79 78 97 95 99 99

handle

Very similar to feather quilts

Comparative example 1

A mixture of 60% by weight of a potassium salt of ethylene oxide (2 moles) 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 were added to 1 mole of propylene glycol, became a 2% ir: en, w- ^; issripen Lr-u

terenntnalatstrang processed. The same polyethylene / as in Example 1 used, was immersed in this treating agent through a filler curling device to a receptacle squeezed off by 10%, heat-treated at 140 ° G for 2 hours and then cut to a length of 76 mm. The number of crimps of the obtained fibers was 7 25 mm each and the percentage crimp was 18; 3.

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The fibers treated in this way had the following properties:

Smoothness ias 0 _T 36

lid O ₁ JO ■ - '

Compression elasticity "

Compression amount 64- %

Compression recovery 88%
Handle ·

worse than feather quilts (hard handle),

Example 2 . ■ ".." .- "."

The same procedure as in Example 1 v, ^T urde repeated except that the viscosity of the treatment agent A of Example 1 used epoxy siloxane as indicated in Table III, varied Wurd of the in. The results obtained are also shown in Table III.

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Table III

Try-Mr.

Viscosity of the epoxysiloxane

smoothness

Compression elasticity

Amount of compression (%)

Compression recovery (%)

2-1 2-2 2-3 2-4 2-5

2-6

68 88

2-7

500 1000 3000 8000 10 000 100 000 150 000

0.23 0.19 0.17 0.18 0.19 0.19 0.25 0.19 0.19 0.19 0.20 0.21

80
97

78

98

77

97

73

92

0.24 0.26

68
87

handle

Cover worse than quilted feather (hard)

equal to feather quilts

ο chi more real like quilted quilts (hard)

From Table III it can be seen that epoxysiloxanes with a viscosity of 100 to 10 000 'particularly good results delivered.

Example 3

The same procedure as in Example 1 was repeated except that the epoxy group content of the epoxy used in treating agent A in Example 1 siloxane was varied as indicated in Table IV, üie Results are also shown in Table IV.

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Table IV

Experiment no.

3-1 3-2

3-3

Epoxy group content (wt.%)

Smoothness as yd

Compression elasticity Compression amount

Compression achievement (%)

handle

0.5 1.0

0.24 0.16
0.25 0.16

3.0

0.17

0.16

66 80 79 87 98.97: Bad
ter like
i'eder-
quilting
cover
(hard) same feather quilt
cover Example 4-

The same procedure as in Example 1 was followed using the exception repeats that the 'relationship between the γ-aminopropyltriethoxysilane used in the treating agent of Example 1 and the epoxysiloxane as indicated in Table V was changed. The results are reproduced in Table V.

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Table V

Experiment no.

4-1

4-2

4-3

4-4

4-5

4-6.

Relationship*
smoothness

Aid

0.5

0.24 0.25

0.18
0.19

0.18
0.17

10

0.16
0.16

20th

0.18
0.19

0.25 0.26

Compression elasticity
Compression Extent 65 Compression Recovery 87

73

93

79
98

80
97

75

94

68 88

handle

Cover worse than quilted feather (hard)

equal to feather quilts

* The weight in T
γ-aminopropyltri-

Worse than F eel first epp blankets (hard)

en des Epoxysiloxans ^ e part by weight of

oxysilane. The other components of the treating agent were the same as in Example 1.

Good results have been obtained when the amount of the epoxysiioxane is 1 to 20 parts by weight per part by weight of the γ-aminopropyltrisethoxysilane was.

Example 5

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

509833/0915

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

CH, Si ^- CH,

and

CH- CH ₀

with a viscosity of 5000 centistokes at 25 C and an epoxy group content of 1.8% by weight, with both ends Trimethylsilyl groups Zr-SiCCH ^) - ^ represent.

Epoxysiloxane (3), built up from structural units of the following formulas: "" .. "· -

/ ⁰ X

CH - CH

CH _Z t 3

Si
CH-,

and

(CH ₂ ) ₃ CH-CH.

with a viscosity of 10 QOO CerfcLstokes at 25 ° C and an epoxy group content of / f Gevx.%, both ends being trimethylsilyl groups ^ Si (CH _x ), J? represent"

The results are given in Table TI below.

50 9 8 33/0915

Tabel Tempter. VI ■ ■ ^: . "■ Treatment agents 5-1 . 5-2 γ-aminopropyltriethoxy-
silane Epoxysiloxane (2) 0.5 0.9 Epoxysiloxane (3) 4.9 Cetyl phosphate potassium salt 4.5. Polyoxyethylene (10 moles)
Nonyl phenol ethers 1.1 1.1. water 0.5. 0.5 smoothness 93.0 . 93.0 ud 0.18 0.16 Compression elasticity 0.19 0.17 Compression extent Comoression recovery 75 79 94 96

handle

same .ie the quilt cover

Example 6

Polyethylene terephthalate with 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 with a total denier of 500 (single fiber denier 3). The tow was immersed in an emulsion of the recipe listed below, squeezed off by a detergent crimping device to an absorption of 6% , at 90 ° C. for 20 minutes

509833/0915

dried, then heat-treated at 140 C for JO minutes and cut to a length of 56 mm.

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

Treatment agent recipe

γ-aminopropyltriethoxysilane 1.0 parts by weight Epoxysilane (the same as in Example 1) 6.6 » Cetyl phosphate potassium salt 1.6 ^Ir Polyoxyethylene (10 mol) nonyl phenol ether 0.8 water 90 Properties of the fibers smoothness / s 0.17 yä 0.17 Compression elasticity Compression amount 82 Compression recovery 92 Handle-like feather quilts Example 7

Polyethylene terephthalate with an inherent viscosity, calculated from that measured in o-chlorophenol at 35 ° C Value, of 0.62 was melt spun and formed a tow with a total value of 400,000, consisting of hollow fibers of 7 denier each and one 13% cavity drawn. The cable obtained was with treated the treating agent A in Example 1 in the same manner as in Example 1. The number of crimps of the fibers obtained was 8 per 25 mn and the percentage

5098 33/0915

tual curl was 1A%. The fibers treated in this way had the following properties:
smoothness

Axs 0.16

ud 0.16
Compression elasticity

Compression amount 78 Compression recovery 98 grip is equal to feather quilts

Example 8

Polyethylene terephthalate with an inherent viscosity calculated from the value of 0.65 measured in o-chlorophenol at 35 ° C and polyethylene terephthalate isophthalate (10% isophthalic acid copolymerized therein) were spun at the same time at a weight ratio of 1: 1 using a spinneret with a side-by-side arrangement and stretched to 3> 3fsiclie of the original length in warm water kept 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 immersed in the treatment agent A of Example 1. It was then squeezed by a filler crimper to pick up 12 % and dried at 80 ° C for 30 minutes. It was then heat-treated in a relaxed state at 160 ° C. for 30 minutes to develop crimps at the same time as heat-setting them, and then the tow was cut to a fiber length of mm.

The number of crimps of the obtained fibers was

509833/091 5

12 per 25 mm and the percentage curl was 19%. The fibers "had the following properties: smoothness

ns 0.18

^ d 0.17 -Ζ-: ■■ -. ■■■ "'.

Compression elasticity.

Compression amount 76- ·

Compression recovery 98
Handle is the same as feather quilts

Example 9

Modified polyalkylene terephthalate with an inherent viscosity calculated from that in o-chlorophenol at 35 ° C measured value of 0.55 and that 14% by weight of a flame retardant of the following formula: ■

Br

HIGH ₀ CH ₀ O- ^{2 2}

was melt-blown and drawn to form a tow having a total denier of 400,000 (single fiber denier equal to 5.5). The resulting tow was immersed in the treatment agent A of Example 1, squeezed off by a filling material crimping device to an absorption of 8% , then subjected to the same treatment as in Example 1.

The obtained fibers gave filler fibers sir soft feel similar to that of feather quilts and one high degree of flame retardancy.

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smoothness

ns 0.18

/ id 0.19.

Compression elasticity Compression extent 74-Compression recovery 98

509833/0915

Claims (1)

Claims (1. Treatment agent for synthetic filler fibers, characterized in that the treatment agent (a) Λ part by weight of an aminosilane of the formula _: - MH -. IU - ? 5 Si O -O-R ^ wherein R ^ is a hydrogen atom, an alkyl group with Tbis. M carbon atoms or a phenyl group, Sp an alkyl ^. and R- lengruppe with 1 to A carbon atoms and independently of one another an alkyl group having 1 to 4 carbon atoms mean and (b) Λ to 20 parts by weight of an epoxysiloxane which contains at least one structural unit of the formula: 0 - Si Marg wherein Rg and R ^ independently of one another niit an alkyl group Ί mean up to 3 carbon atoms and at least two structural units of the formula 509833/0915 7. O -O —Si CH - CH. contains, wherein Eg is an alkyl group having 1 to 3 carbon atoms or the grouping -E _Q -CH - CH ₀ and E _{0 is} an alkylene group 2 to 5 carbon atoms or a substituted or unsubstituted arylene group with 6 to 10 carbon atoms,
having. 2. Treatment agent according to claim 1, characterized in that that the aminosilane from γ-aminopropyltriethoxysilane, γ-aminopropyltrinetiioxysilane, ß-ilethylaniinoäthyltriethoxysilan and / or γ-phenylaminopropyltrimethoxysilane consists. 3. Treatment agent according to claim 1 or 2, characterized characterized in that the epoxysiloxane has a viscosity of 1,000 to 100,000 centistokes at 25 ° C. 4. Treatment agent according to claim 1 to 3, characterized in that the epoxysiloxane 0.3 to 10 wt.% Contains epoxy groups based on its total weight. 5. Treatment agent according to claim 1 to 4, characterized in that the proportion of the epoxysiloxane is 1 to 18 parts by weight per part by weight of the aminosilane. 6. Treatment agent according to claim 1 to 5 »thereby characterized in that it is in the form of an aqueous emulsion. 7 procedures for the treatment of synthetic filler fibers, characterized in that on the synthetic Fesern 5 0 9833/0915 a treatment agent is applied that (a) 1 part by weight of an aminosilane of the formula: ' R ₁ -ITH-R ₂ -Si-OR ₄ where R ^ is a hydrogen atom, an alkyl group with 1 to 4 carbon atoms or a phenyl group, R ^ is an alkylene group with Λ to 4 carbon atoms and R ^, R ₂ , and R ₁ - independently of one another are an alkyl group with 1 to 4 carbon atoms and (b) 1 to 20 parts by weight of an epoxysiloxane containing at least a structural unit of iOrmel: Si * 7 wherein R ^ and Rr-, independently of one another, have an alkyl group 1 to 3 carbon atoms and at least two structural units of the formula: Si CH - contains, 509833/091 where En is an alkyl group with 1 to 3 carbon atoms or the grouping -IU-CH-CH ₂ and R "is an alkylene group O with 2 to 5 carbon atoms or a substituted or unsubstituted arylene group with 6 to 10 carbon atoms,
and then heat-treated v / grounding the fibers. 8. The method according to claim 7, characterized in that that the treatment agent is so impregnated into the synthetic fibers that the total amount of the adhering Aaiinosilans and epoxysiloxane 0.1 to 3 »0% by weight, based on is the dry weight of the fibers. 9. The method according to claim 7 or 8, characterized in that that the heat treatment is carried out at a temperature of 100 to 230 ° C for at least 1 second will. 10. The method according to claim 7 to 9j, characterized in that that the synthetic fibers are subjected to a curling treatment before the heat treatment. 11. The method according to claim 7 to 10, characterized in that the synthetic I ^! 'Asern synthetic polyester fibers are used. 12. Synthetic filler fibers coated with a heat-treated product of a treatment agent, the (a) 1 part by weight of an aminosilane of the formula: ? 3 0 · - HH - H ₂ - Si - 0
0 509833/0915 25057Λ2 wherein E ^ is a hydrogen atom, an alkyl group with 1 to 4 carbon atoms or a phenyl group, Rp an alkylene group with 1 to 4 carbon atoms and and Re independently of one another an alkyl group with 1 to 4 carbons substance atoms mean and (b) 1 to 20 parts by weight of an epoxysiloxane which at least one structural unit of the formula: O - Si wherein R ^ and R ₁ -, independently of one another, denote an alkyl group having 1 to 3 carbon atoms. and at least two structural units of the formula: O - Si CH - CH. wherein R _{Q is} an alkyl group with 1 to 3 carbon atoms or the grouping -Rq-CH - CHp, where Rq is an alkyl represents lengruppe with 2 to 5 carbon atoms or a substituted or unsubstituted arylene group with 6 to 10 carbon atoms,
on v / ei st. 13. Synthetic filler fibers according to claim 12 :, characterized characterized in that the fibers fulfill the following relationship: 509833/091 5 1.5 = D = 10
IOD -2O = L = IOP + 60 10 = L + 10.0 ^ Cjj ^ -JA D + 15.5 15 ^ C _w + Ο _π < 32, v>'orin D the denier size of the synthetic fibers, L the length of the fibers in rr.:r_, C- _T the number of crimps 25 £ i ™ ^ nd Cp the percentage crimp (; 6) mean. 14-. Filling material made up of the synthetic j? Üll- fibers according to claim 12 or IJ. 509833/0915