JPS5941345A - Preparation of dyeable polypropylene composition - Google Patents

Abstract

PURPOSE:To prepare the titled composition having high dyeability and spinnability, by compounding a polypropylene with a copolymer of ethylene and an aminoalkyl acrylate compound, and a higher fatty acid alkali metal salt containing a specific amount of water. CONSTITUTION:The objective composition is prepared by compounding 99- 80pts.wt. of polypropylene with 1-20pts.wt. of a copolymer of ethylene and an aminoalkyl acrylate compound of formula (R1 is H or methyl; R2 and R3 are H or 1-4C alkyl; n is 1-4) (especially dimethylaminoethyl methacrylate, etc.) and 0.2-5.0pts.wt. of a 8-22C higher fatty acid alkali metal salt (usually in the form of flake) containing >=0.5wt%, based on the metal salt, and <=0.2wt%, based on the polypropylene composition, of water, under melting and kneading. Preferably, the three components are mixed beforehand, and molten and kneaded. Water may be added in the premixing of the components dividedly or at a time by spraying or dripping.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing dyeable polypropylene compositions.

Crystalline polypropylene fiber has many characteristics such as being light, strong, and warm, and when it was first developed, it was expected to be a ``dream fiber''. Because it is a natural and chemically inert material, it is difficult to apply normal dyeing methods, and it has the disadvantage that it cannot be dyed, so it cannot be colored with uncolored cotton or inorganic pigments. Used only in limited areas such as carpet pile yarn.
Not yet. Because of the dyeability of polypropylene fibers, it has long been desired to improve the dyeability of polypropylene fibers, and many methods have been proposed to date.

For example, it is realistic and attracts attention because it does not have any disadvantages in terms of dyeing capacity, easy spinnability, or yarn strength for anionic dyes. Among them, Special Public Interest Publication No. 42-22528
As described in the above publication, a dyeable polypropylene composition obtained by kneading a copolymer of ethylene and an aminoacrylate compound with polypropylene is an industrially feasible and inexpensive method. This is something that can be expected. JP-A-52-16188 discloses the effect of improving dyeability by adding metal salts of various organic carboxylic acids to the above composition.

However, when the present inventors conducted a practical trial, it was found that such a polypropylene composition also impairs the physical properties of the polypropylene fiber due to an increase in the amount of basic polymer and organic carboxylic acid metal salt added. It has been discovered that reducing the amount added reduces the dyeability of anionic dyes, and that there is an appropriate range for each amount added.

If the dispersion state in the polypropylene composition is poor, the spinnability, stretchability, t3ζ, and other processability of the polypropylene composition will be impaired. (It has been found that it not only reduces yarn strength, but also has an adverse effect on various fastness properties such as washing resistance, light resistance, and abrasion resistance after dyeing with anionic dyes.)

In order to solve this problem, the present inventors have conducted extensive research into the dispersion state of oral carboxylic acid metal salts, particularly alkali metal salts of higher fatty acids, in polypropylene compositions. It has been found that the dispersibility of the alkali metal salts of higher fatty acids in the polypropylene composition is improved by pre-containing an appropriate amount of water when melting and kneading the alkali metal salts of higher fatty acids. That's it.

That is, the present invention provides (~polypropylene 99-80 polypropylene), (uniform ethylene and general formula (1) (in the formula, R, l,
hydrogen or a methyl group, R,, R, is hydrogen or an alkyl group having 1 to 4 carbon atoms, and n is an integer of 1 to 4). Copolymer with the above aminoalkyl acrylate compound 1 to 20 nail portion, and 01 type or 2 or more types having 8 to 22 carbon atoms
A method for producing a dyeable polypropylene composition by melt-kneading 0.2 to 5.0 parts by weight of an alkali metal salt of a higher fatty acid, the method comprising:
A 5J dyeable polypropylene composition, which is melt-kneaded after containing water in an amount of 0.5% by weight or more and not exceeding 0.2% by weight based on the polypropylene composition. It is a fabrication method.

The J'L (A) polypropylene used in the present invention may be of a type commercially available for fiber use and is not particularly limited, but examples include propylene homopolymer, propylene and ethylene and/or butene, 4-methyl Examples include copolymers with other α-olefins such as -1-pentene. The shape may be pellets or powder.

The ethylene copolymer (B) used in the present invention is described in Japanese Patent Publication No. 42-22528, Japanese Patent Publication No. 49-45307, and Japanese Patent Publication No. 58-6194. Examples include copolymers of ethylene and various aminoalkyl acrylate comonomers, particularly dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, dimethylaminoethyl acrylate', and the like. The amount of the ethylene copolymer added is 1 to 99 to 80 parts by weight of polypropylene.
~20 parts by weight, preferably 5 to 10 parts by weight are suitable. If the amount added is less than this range, the dyeing properties will be insufficient, and
Addition of more than 'L' has the disadvantage of impairing spinnability and yarn properties.

Examples of the alkali metal salts of higher fatty acids having less than 722 carbon atoms used in the present invention include sodium salts of stearic acid, lauric acid, oleic acid, valmitic acid, myristic acid, capric acid, etc. Examples include potassium salts. Furthermore, a mixture of two or more of these may be used.

The calorific value of the alkali metal added to these iA class 7j acids is in the range of 1.2 to 5.0, preferably 0. .5 to 20 parts.From this, even if the amount of additives F and +H1 is increased, not only will the spinning effect not increase accordingly, but the spinnability and physical properties of the yarn will be deteriorated. Become.

In addition, the amount of water contained during the production of the polypropylene (7) must be less than 0.5 Hlt% based on the alkali gold scrap salt of higher fatty acids, and must not exceed 0.2% based on the polypropylene composition. .

If the water content is less than 0.5% by weight based on the alkali metal salt of higher fatty acid, the alkali metal salt of higher fatty acid will not be sufficiently dispersed in the polypropylene composition, resulting in poor spinnability of the composition. is damaged and yarn breakage occurs frequently during spinning. In addition, even if spinning is possible, the yarn strength is low,
The uniformity of the dyeing is poor, and furthermore, the fastness of the dyeing, such as light fastness and abrasion resistance after dyeing, is poor.

Furthermore, if the amount of water added during the production of the polypropylene composition exceeds 0.2% by weight based on the polypropylene composition, it will vaporize during melt mixing and cause foaming, which will impede kneading. Furthermore, during spinning, air bubbles in the molten cross-wire composition generated by the moisture and foaming may cause yarn breakage, which is undesirable.

As the melt-kneading method, general melt-kneading n8!4 for thermoplastic resins can be used. For example, there are screw-type kneading mixers, screw-type extruders, and the like.

The polypropylene (A) is generally in the form of pellets or powder, the ethylene copolymer is also in the form of pellets or powder, and the alkali metal salt of higher fatty acid (0) is generally in the form of flakes or powder.

These 1 t may be fed separately to the melt-kneading machine, but it is better to mix 8 of them in advance and then feed 1 t of them to the melt-kneading machine.

Also, at this time, stabilizers such as antioxidants, ultraviolet absorbers, and antistatic agents for polypropylene may be added at the same time.

As a method of adding water, it is also possible to pre-include a predetermined amount in the alkali metal salt of higher fatty acid 0.
When pre-mixing the eight ingredients listed above, there is a method of adding them all at once or in portions by spraying or dropping.

The polypropylene mHlt obtained by spinning the composition obtained according to the present invention was homogeneous and the color fastness of the polypropylene film was at a level that caused no practical problems.

The present invention will be explained below with reference to Examples, but the present invention is not limited to these Examples.

Example 1 ■ Powdered Noblen FL800 (manufactured by Sumitomo Chemical, polypropylene homograde, Melt Index Iryo ISK,
Copolymer pellets (melt index 100, JISK-67 (melt index 100, 30 compliant) and a mixture of 65/8015 weight ratio of sulfur and lithium stearate, sodium balmitate, and sodium myristate (moisture content; 0.2 parts by weight for the mixture)
1 part by weight of a mixture prepared by absorbing water and adjusting the moisture content to 15.0% by weight, further adding stabilizer ■ and 17 Irganox 1010 (manufactured by Ciba Geigy).
Add 0.5 parts by weight of Sumiso ■ Ichibu 800 (manufactured by Sumitomo Chemical) as a UV absorber to the 0.1 heavy nail part at 200°C.
At a temperature of 80 gates φ screw type extruder (L/D
:20) to obtain composition pellets. Using a spinning machine equipped with an extruder (L/D = 15), the pellets were heated in a hidden manner at a resin temperature of 240°C, 1 kg of extrusion claw, and a 71ζ tensile speed of 23Q.
rn/m1n1 The nozzle was a 12-hole nozzle with a hole diameter of 0.8 mm, and melt spinning was performed, followed by drawing 8 times at 110°C to obtain a multifilament of 16 denier/filament. Ren ml.

After running for hours, the thread trimmer tL became completely straight. The obtained fibers were treated with acidic 14L8 material C, I, acid blue 1291.1.
%owfsFormic acid 2%owf dye bath with bath ratio 1:6
Stained at 0.100°C for 60 minutes. Next, wash with water, and then soak in a soaping bath containing 2 f/l of Monogen (manufactured by Dai-Kogyo Seiyaku) with a trowel at 60"C for 5 minutes at 60°C.
, 5 molecule ft + soaping, washing with water and drying to finish. The object to be dyed was dyed in a rich old color.The dyeing rate was determined by color comparison of the dyeing residue and the soaping residue, and the result was 8.
It shows a final dyeing rate of 9% and has a photoresistance rating (JIS L-
0842) Class 6, Mmm prison rating (J I 5L-0
849 mm1%>5 grade was shown.

In addition, the yarn quality and dye uniformity of Mff6 are
The surface and cross section of 1,'4 #fA were examined using an optical microscope, and it was found that the fiber quality and dyeing state were uniform.

Comparative Example 1 A mixture of sodium stearate, sodium palmitate, and sodium myristate in a 65/8015 weight ratio with a moisture content of 0.2% (water content 0.2%)
The pellets produced in the same manner as in Example 1 were further subjected to spinning, stretching, and dyeing in the same manner, except that the pellets (% by weight) were used as they were without adjusting the moisture content. During continuous spinning operation for 1 hour, thread breakage occurred 8 times, and as a result of dyeing, the final dyeing rate was only 80%, the light fastness was grade 4, the abrasion fastness was grade 4, and the abrasion fastness was grade 4. It did not show grade 4 and was not too hard.

Example 2 ■ Copolymer pellets of ethylene and dimethylaminoethyl methacrylate in a weight ratio of 72/28 (Melt Intex 100), 7-fold ffl bunch 1
and sodium laurate, sodium myristate,
Absorb a mixture of sodium caprate with a 70/l 5/15 weight α ratio (moisture content 0.11 %) + U. Adjust the moisture content to 14.0 weight 7y%. 1 nail polish. Add 0.1 part of Irganox 1010 to the molding part, and add 0.5 parts of Sumisorb 80 (+) to the part using a seal mixer.
The mixture was melted and mixed at 00°C for 65 minutes using a φ extrusion tl (L/D=20) to obtain pellets.

The pellets thus obtained were processed using a spinning machine equipped with the same 25 mm diameter extruder (L/D-15) as described in Example 1, at a resin temperature of 240' C1 and an extrusion rate of 1 k (j A
, tensile speed a o o m /rni+i /glu CD
Bath melt spinning was performed using an 82-hole nozzle with hole diameter Q of 5 mm, followed by 3x stretching at 110°C, and melt spinning using a 25 denier/filament multifilament and a 12-hole nozzle, followed by 3x stretching at IIO'C. Obtain a stretched 16 denier/), f-lament multifilament! child.

These filaments were dyed in the same manner as in Example 1,
Dyeability and various fastnesses were evaluated. The results are shown in Table 1.
100. Shows good spinnability and dyeability.

Fruit 1rI'i (!111 B A mixture of sodium laurate, sodium myristate, and capricin 9-storium in a 70/15/15 weight ratio as the alkali metal 4fi of Takasa fatty acid C content moisture content 01 weight q%) is used as it is. Example 2
Same as! Henschl mixer using the IN No. 4 composition ratio.
If the moisture content is 11' when mixing the total tookg using
2.0 M M% for alkali metal salt of primary fatty acid
Water was added in 3 portions from 1 to 1 portion so as to make the surface visible. Further, the same operations as in Example 2 were carried out to obtain multifilaments of 2.5 denier/filament and 16 denier/filament. Table 1 shows the results of staining and evaluating the strained rice in the same manner as in Example 1.

Comparative Example 2 A mixture of sulfur and lithium laurate, sodium myristate, and strium caprate in a weight ratio of 70/15/15 (moisture content 0.1) as an alkali metal salt of a higher fatty acid.
Granulation, spinning and stretching were carried out in the same manner as in Example 2, except that the same raw materials as in Example 2 were mixed at the same composition ratio in a Henschel mixer without any moisture adjustment. I did it.

The cisternal filament of 2.5 denier/filament had many thread breaks and could not be spun.

Moreover, the multifilament of 16 denier/filament was somehow able to be spun. One piece of this 2'L was dyed in the same manner as in Example 1 and evaluated. The results are shown in Table 1.

Comparative Example 8 As a composition, water was added from one spray so that the moisture content was 0.4% by weight based on the polypropylene composition. A mixture having the same composition as in Example 2, except for using a 651111≠screw type extrusion box, was melt-kneaded at t7J fat temperature 2o0°C, and granulation was attempted. There was no slippage between the wires and the composition, and crosstalk occurred smoothly.

Example 4 Potassium stearate, potassium balmitate, potassium myridate 6 as alkali metal salts of higher fatty acids
A mixture with a weight ratio of 5/80/5 (moisture content 0.2%) was absorbed to reduce the moisture content to 15.7ttFt.
Spinning, drawing, and dyeing were carried out in the same manner as in Example 1, except for using a material adjusted to %. As shown in Table 1, the results showed good spinnability and dyeability.

Example 5 Alkali metal salts of higher fatty acids, potassium laurate, potassium myridate, potassium caprate 95
/ 8 / 2 weight ratio mixture (moisture content 0.1% by weight) was absorbed and the moisture content was adjusted to 15% by weight. Do it. As shown in Table 1, the results showed good spinnability and dyeability.

Claims (1)

[Claims] (5) Polypropylene 99-80]'tjlit[in,
(g) Ethylene and the general formula■? . (In the formula, R is hydrogen or a methyl group, R1 and R1 are hydrogen or an alkyl group having 1 to 4 carbon atoms, and 11 is an integer of 1 to 4.) 1 to 20 parts by weight of a copolymer with an alkyl acrylate compound, and (0
In a method for preparing a dyeable polypropylene composition by melt-kneading 0.2 to 5.0 parts by weight of one or more alkali metal salts of higher fatty acids having 8 to 22 carbon atoms, the higher 0.5 weight percent or more based on the alkali metal salt of fatty acid, and 0.5 weight percent or more based on the polypropylene composition.
A dyeable lipropylene composition characterized in that the composition is pre-contained with water in an amount not exceeding 2% by weight and then melt-kneaded. ! ! Construction method.