JP2000290827A - Production of inorganic ingredient for fiber - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing an inorganic ingredient for fiber excellent in dispersibility and dispersion stability of ingredient particles, free from the generation of coagulants even when added to a fiber dope, free from the generation of yarn cutting, and the like, during spinning into fiber, and at the same time, capable of effectively exhibiting characteristic performances of the ingredient such as excellent flame resistance, deodorant activity and antibacterial activity in a state where it is compounded in fiber. SOLUTION: This production method is characterized in that a zinc and/or magnesium-containing inorganic compound is crushed by wet milling in an aprotonic polar solvent at a concentration of 1-80 wt.% so that the volume average particle diameter (D50) is 0.1-1.0 μm, and the ratio of the particles having particle sizes of 2 μm or more is 10 vol.% or less.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an inorganic compounding agent for fibers, and more particularly, to a compounding agent which is excellent in dispersibility and dispersion stability of compounding agent particles and is compounded in a dope for fiber formation. No agglomeration occurs when the fiber is spun, and no yarn breakage occurs when spinning into fiber.
The present invention relates to a method for producing an inorganic compounding agent for fibers, which effectively exhibits the inherent performance of the compounding agent such as deodorizing performance and antibacterial performance.

[0002]

2. Description of the Related Art Although synthetic fibers have excellent physical properties as fibers, they lack flame retardant, deodorant, and antibacterial properties. It is widely practiced to mix an inorganic compounding agent into a dope for use.

[0003] Zinc silicate-based compounds have deodorizing performance and antibacterial performance, and it has been known for a long time to incorporate them into fibers. For example, JP-A-2-99606 discloses that the weight ratio of zinc oxide to silicon dioxide is 1: 5 to 5: 1.
And a substantially amorphous average particle diameter of zinc silicate having a mostly amorphous structure having an average particle diameter of 5 μm or less, and a melting point lower than 10 ° C. and a viscosity at 25 ° C. or lower of 10 poise or more. A fiber having a deodorant property and an antibacterial property, characterized in that a mixture with a liquid polyester-based compound is dispersed in a thermoplastic polymer having a melting point of 150 ° C. or higher.

Japanese Patent Application Laid-Open No. Hei 8-246334 discloses an antibacterial / deodorant cloth obtained by applying an antibacterial / deodorant porous ceramic powder processing agent to a cloth together with a resin binder for fibers.

Further, Japanese Patent Application Laid-Open No. 9-87924 discloses that
In acrylic synthetic fibers, the average particle size is 0.5 to 10 μm.
m, a deodorant and antibacterial acrylic synthetic fiber containing 0.5 to 20.0% by weight of a fine powder containing a metal silicate or aluminosilicate as an active ingredient. I have.

[0006]

However, the above-mentioned inorganic compounding agents for fibers, particularly zinc-based or magnesium-based compounding agents, still have insufficient dispersibility in a resin solution and also have a tendency to aggregate particles. For example, in molding into fibers, there is a tendency that clogging of the orifice or breakage of the yarn tends to occur, and there is a strong demand for improvement. Furthermore, flame retardant performance,
Maintaining the original performance of the compounding agent such as deodorant performance and antibacterial performance is also an important issue, and with a fine particle size suitable for blending into fibers,
There is also a tendency for these performances to be reduced or their durability to be lost.

Accordingly, an object of the present invention is to provide a compounding agent which has excellent dispersibility and dispersion stability, does not cause agglomeration even when compounded into a fiber-forming dope, and has an advantage in spinning into fibers. Also, it does not cause thread breakage, etc.
An object of the present invention is to provide a method for producing an inorganic compounding agent for fibers, in which the intrinsic performance of the compounding agent such as deodorizing performance and antibacterial performance is effectively exhibited.

[0008]

According to the present invention, a zinc-based and / or magnesium-based inorganic compound having antibacterial, deodorizing or flame-retardant properties is added to an aprotic polar solvent in an amount of 1 to 80% by weight. An inorganic compound for fibers, which is wet-pulverized so that a volume-based average particle diameter (D ₅₀ ) of 0.1 to 1.0 μm and a particle diameter of 2 μm or more is 10% by volume or less at a concentration of A method for producing an agent is provided.

The raw material inorganic compound targeted by the present invention has antibacterial properties, deodorant properties or flame retardancy, and may be any of zinc-based or magnesium-based compounds as exemplified later. Particularly effective ones include zinc-containing aluminum phyllosilicate, zinc hydroxystannate, zinc borate, magnesium borate, or a combination thereof. As the aprotic polar solvent, any of those exemplified below can be used. Particularly effective one is dimethylformamide (DMDM).
F). The concentration of the raw material inorganic compound in the wet pulverization is 1 to 80% by weight, preferably 20 to 60% by weight, more preferably 30 to 60% by weight. It is particularly preferable to carry out wet pulverization in the presence of an aprotic polar solvent in an amount of 2.0 times or more, particularly 2.0 to 7.0 times the oil absorption of the compound. The wet grinding in the present invention is performed in the presence of an oxidizing agent, particularly hydrogen peroxide, to prevent the coloring tendency of the compounding agent even if there is a long time lapse between the production and the compounding into the fiber dope. Can be.

[0010]

[Operation] The present invention relates to a zinc-based and / or zinc-based
Or magnesium-based inorganic compounds with aprotic polarity
When wet grinding at a concentration of 1 to 80% by weight in a solvent,
Product-based average particle size (D ₅₀) Is 0.1 to 1.0 μm and
One having a particle size of 2 μm or more accounts for 10% by volume or less of the whole.
It is possible to produce a slurry with a particle size distribution
And the slurry of the compounding agent having the above particle size distribution is
Excellent fiber dispersibility and dispersion stability and fiber formation
No aggregation occurs even when compounded into a dope for
Also, yarn spinning may occur during spinning into fibers.
Excellent flame retardancy when combined with fiber
Effectiveness of compounding agent's original performance such as performance, deodorant performance, antibacterial performance
It is based on the knowledge that the gene is expressed in

[0011] The aprotic polar solvent is defined as a polar solvent having no active hydrogen. In this aprotic polar solvent, a zinc-based and / or magnesium-based inorganic compounding agent for fibers is wet-ground. It was found that a relatively stable slurry of particles having an average particle diameter of submicron and having a very small content of coarse particles of 2 μm or more was obtained.

As a means for finely pulverizing an inorganic substance, wet pulverization is a well-known means. However, as shown in a comparative example described later, when a zinc-based and / or magnesium-based inorganic compounding agent for fibers is wet-pulverized in water, In addition, the average particle diameter is limited to about 2 μm, and it is difficult to reduce the particle diameter to submicron particles. Further, particles formed by wet pulverization tend to agglomerate and lack both dispersibility and dispersion stability.

On the other hand, zinc-based and / or magnesium-based inorganic compounds are replaced with dimethylformamide (DM
When wet grinding is performed in an aprotic polar solvent such as F), it is possible to finely grind into the above-mentioned submicron particles, and the formed slurry is excellent in the dispersibility and dispersion stability of the particles. Benefits are achieved. In this slurry, particles may settle with the lapse of time after the preparation of the slurry, but even in this case, the particles settled can be easily re-dispersed to the original state by slightly stirring the slurry. It can be seen that the dispersibility is excellent. In addition, an aprotic polar solvent such as DMF is a solvent for a dope for producing, for example, acrylic fibers, and a slurry obtained by wet-milling an inorganic compounding agent for fibers may be used as it is for preparing a dope for spinning. The advantage that it can be achieved is also achieved.

In the present invention, a zinc-based and / or magnesium-based inorganic compound is used at a concentration of 1 to 80% by weight, preferably 20 to 60% by weight, more preferably 30 to 6% by weight.
It is subjected to wet grinding at a concentration of 0% by weight. Concentration 80
If the content is more than 10% by weight, the advantage of the wet pulverization is lost, and it becomes difficult to obtain submicron particles. Wet pulverization is based on the principle that the destruction of fine substances is more likely to occur in a wet state than in a dry state, the efficiency is higher than in a dry state, and fine powder is easily obtained. This is because the wet state is no longer suitable for grinding.

In the wet grinding, the amount of oil absorption of the raw material inorganic compound (JIS. K.5101.19) is 2.0 times or more,
Particularly, it is most preferable to carry out the reaction in the presence of 2.0 to 7.0 times the amount of the aprotic solvent in terms of the pulverization efficiency. That is,
The efficiency of wet pulverization is also related to the oil absorption of the raw material inorganic compound. If the amount of solvent is larger than the amount of oil absorption, the raw material inorganic compound absorbs a large amount of solvent, and the efficiency of the wet grinding is lower than the amount of oil absorption. If the amount of the solvent is small, the amount of the solvent absorbed by the raw material inorganic compound becomes extremely small, and in any case, the wet state suitable for pulverization tends to be lost. In the present invention, the solvent amount a times the oil absorption amount is, for example, when the oil absorption amount of the raw material inorganic compound is bml / 100 g, the solvent amount for 100 g of the raw material inorganic compound is (a × b) ml. Means that.

[Raw material inorganic compound] The raw material inorganic compound used in the present invention is a zinc-based or magnesium-based compound having antibacterial, deodorant or flame retardant properties, and is not limited thereto. The following formula (1) having excellent flame retardancy: MSn (OH) ₆ (1) In the formula, M represents Zn or Mg; zinc or magnesium hydroxystannate represented by the formula: excellent in flame retardancy Zinc stannate represented by the following formula (2): ZnSnO ₃ (2), borates such as zinc borate and magnesium which are also excellent in flame retardancy, and further excellent in deodorant and antibacterial properties Various siliceous compounds such as aluminum-containing zinc phyllosilicate, hemimorphite-type zinc silicate, sauconite-type zinc silicate, zinc phyllosilicate,
Examples thereof include crystalline silicate compounds such as magnesium phyllosilicate, amorphous silicate compounds such as amorphous zinc silicate and magnesium silicate, and zinc oxide having deodorant properties.

In the present invention, the properties such as deodorant property, antibacterial property and flame retardancy are good, the particles have little tendency to agglomerate, and are excellent in fine dispersibility and dispersion stability. From a standpoint, zinc-containing aluminum phyllosilicate, zinc hydroxystannate, zinc borate, magnesium borate or combinations thereof are most preferably used.

The aluminum-containing zinc phyllosilicate is
Following general formula _{(3): (Zn 3-} X Al X) (Si 2-X Al X) O 5 (OH) (3) wherein, x is a number from 0.1 to 1.75, in Table Is a two-layer structure phylloaluminosilicate having the chemical structure described below, which is generally referred to as frypontite. That is, in this chemical structure, the tetrahedral layer Si of silica is substituted with Al, and in order to balance this, part of Zn in the octahedral layer of ZnO ₆ is also substituted with Al, and these are laminated in two layers. Is used as a basic skeleton, and this basic skeleton has a structure laminated in the C-axis direction in some cases.

The production of such a synthetic frypontite is described in JP-A-61-10021, 61-275128.
And (A) silica or a silicon compound capable of forming silica under the reaction conditions, (B) zinc white, zinc hydroxide or zinc hydroxide under the reaction conditions, as described in JP-A No. 61-275127. The zinc compound which can be formed, and (C) alumina hydrate, aluminum hydroxide or an aluminum compound which can form these under the reaction conditions are represented by oxides of SiO ₂ 5 to 45 in terms of a three-component composition ratio.
Mol%, ZnO 35-65 mol% and Al ₂ O ₃ 0-6
The reaction is carried out in the presence of water at a quantitative ratio corresponding to 0 mol%. The reaction can be obtained by once forming a precipitate from the reactant mixture and heating the precipitate, or by subjecting the reactant mixture to hydrothermal treatment in an autoclave. Of course, the present invention is not limited to this production method.

The above aluminum-containing zinc phyllosilicate is
It can also be used in the form of a complex with amorphous silica. This composite is composed of amorphous porous silica and an aluminum-containing zinc phyllosilicate layer formed on the surface of its primary particles, and has a three-component composition ratio of SiO ₂ : 5 to 80 mol%, as a whole. ZnO: 5 to 65 mol%, Al ₂ O ₃ :
It has a composition of 1 to 60 mol%. In this composite, a layer of aluminum-containing zinc phyllosilicate is formed in the pores of the amorphous silica or on the surface of the primary particles,
The aluminum-containing zinc phyllosilicate in the composite is characterized in that the crystal is not developed and is amorphous or low crystalline. This complex-type aluminum-containing zinc phyllosilicate is characterized in that it is easily incorporated into a resin, but is active. This complex is known as
As described in JP-A-9602, it can be easily obtained by producing aluminum-containing zinc phyllosilicate in a sol or gel dispersion of silica.

The above-mentioned raw material inorganic compound is generally obtained in the form of a slurry dispersed in a predetermined reaction solution, which is filtered, washed, dried, and then dry-pulverized with a pulverizer such as a jet mill to obtain a granular material. It is used in the form of (1), but contains many large-diameter particles having an average particle size of about 1.5 to 3 μm and about 6 to 8 μm. Therefore, if this is used as it is as a fiber compounding agent, problems such as yarn breakage during spinning occur. In dry pulverization, it is more difficult to pulverize into fine particles. However, by performing wet pulverization according to the present invention, pulverization into fine particles suitable for a compounding agent for fibers is performed.

These raw material inorganic compounds may be subjected to a surface treatment by mixing various organic dispersants, if necessary, prior to wet grinding by mixing with an aprotic polar solvent. Examples of such organic dispersants include polyethers having an average molecular weight of 10,000 or less, particularly 400 to 6000, such as polyethylene glycol, polypropylene glycol, polybutylene glycol, polyoxyethylene / polyoxypropylene copolymer; Examples thereof include ethylene oxide adducts to methylolpropane, pentaerythritol, dipentaerythritol, mannitol, sorbitol and the like, and polyethylene glycol is particularly preferred. The organic dispersant is generally used in the range of 0.5 to 10% by weight based on the amount of the raw material inorganic compound. Above all, the above-mentioned crystalline zinc silicate compound, in particular, aluminum-containing zinc phyllosilicate can significantly improve its dispersibility and dispersion stability by surface treatment using polyethylene glycol.

(Aprotic polar organic solvent) As the aprotic polar organic solvent, dimethylformamide (DM
F), dimethylacetamide (DMA), dimethylsulfoxide (DMS), tetrahydrofuran (TH
F), acetone and the like. These solvents are excellent in solubility of the polymer, recoverability of the solvent, and handling. Above all, DMF is used as a solvent for the dope used in the spinning step of the acrylic fiber. Therefore, DMF
When wet pulverization is carried out using the above method, there is an advantage that the obtained slurry can be directly mixed into the dope in the acrylic fiber spinning step.

(Wet milling) According to the present invention, the above-mentioned raw material inorganic compound is mixed with a predetermined amount of an aprotic polar organic solvent and wet milling is performed in a liquid having a concentration of 1 to 80% by weight. This wet pulverization is performed using a pulverizer such as a tube mill or a ball mill. As described above, the volume-based average particle diameter (D ₅₀ ) is 0.1 to 1.0 μm and the particle diameter is 2 μm or more. The process is performed until the content becomes 10% by volume or less. The grinding time is usually about 2 to 80 hours,
Room temperature is sufficient. If the compounding agent is pulverized while heating, it is not preferable because the spinnability deteriorates when spinning the fiber.

The wet grinding is preferably carried out by mixing an oxidizing agent, particularly hydrogen peroxide, in the liquid and in the presence of the oxidizing agent. In other words, a slurry in which the inorganic compound is dispersed in fine particles suitable as a compounding agent for fibers is obtained by wet pulverization. However, if this slurry (or a dried product thereof) is left for a long time, the compounding agent will become colored. Tend to. However, when the wet pulverization is performed in the presence of the oxidizing agent as described above, such a coloring tendency can be effectively prevented. The oxidizing agent is preferably used in an amount of 0.5 to 10% by weight, particularly 0.5 to 5% by weight, based on the amount of the raw material inorganic compound. When the amount is smaller than the above range, the prevention of coloring is not effectively performed, and even when used in a larger amount than the above range,
No improvement in anti-coloring properties is observed, but rather it may adversely affect various properties of the obtained inorganic compounding agent. As the oxidizing agent, in addition to hydrogen peroxide, there are various things such as potassium persulfate, salad powder, formic acid, etc., but hydrogen peroxide is dissolved in an aprotic solvent and has a high anti-coloring property. Most preferred. The same effect can be obtained by adding the oxidizing agent after the production of the inorganic compounding agent, that is, after wet-grinding the raw material inorganic compound in an aprotic polar organic solvent and then adding the oxidizing agent.

[Usage] The slurry containing the fine fiber compounding agent obtained as described above may be used as it is, or may be filtered, washed and dried to obtain a powder having the above-mentioned particle size distribution. Deodorant, blended with forming polymer
Functional fiber having antibacterial properties, flame retardancy, etc.

As the fibers, olefin fibers made of polyethylene, polypropylene, etc., polyvinyl alcohol fibers, polyvinyl chloride fibers, vinylidene chloride resin fibers,
Acrylic fiber, vinyl chloride / vinylidene chloride copolymer fiber, polyamide fiber such as nylon 6, nylon 6-6,
Examples thereof include thermoplastic polyester fibers such as polyethylene terephthalate, fluororesin fibers such as polytetrafluoroethylene, aramid fibers, liquid crystal polyester fibers, and acetate fibers.

These fibers are produced by means of melt spinning, dry spinning, wet spinning, etc., depending on the type of polymer constituting the fibers. The fiber compounding agent of the present invention is prepared prior to spinning. Are uniformly dispersed and blended in these polymers.
That is, the polymer to be melt-spun may be blended by kneading, and the polymer to be dry-spun or wet-spun may be dispersed in a spinning dope by shearing and stirring.

The compounding amount of the compounding agent with respect to the fiber-forming polymer varies depending on the application and required characteristics, but generally, 1 part per 100 parts by weight of the fiber-forming polymer.
An amount of from 30 to 30 parts by weight, particularly from 2 to 30 parts by weight, is suitable in terms of the balance between the performance such as deodorant, antibacterial properties and flame retardancy and the performance of the fiber.

The fibrous compounding agent of the present invention obtained by the wet pulverization described above is a fiber-forming dope comprising an aprotic polar organic solvent and a fiber-forming polymer soluble in an aprotic polar organic solvent. Can be applied advantageously. That is, the compounding agent for fibers of the present invention has the ability to disperse extremely easily and finely and stably in an aprotic polar organic solvent, so that not only can a fiber product without thread breakage be produced. In the form of a slurry obtained by wet pulverization, it can be directly incorporated into a dope.

A fiber-forming polymer soluble in the above solvent,
That is, an acrylonitrile-based polymer can be exemplified as a typical fiber-forming polymer in which an aprotic organic solvent (for example, DMF) is used as a solvent for the dope. Examples of the acrylonitrile-based polymer include acrylonitrile homopolymers and copolymers, and blends of these homopolymers and copolymers with other polymers. Acrylonitrile polymer is 40 per total
It is preferred to contain acrylonitrile units in an amount of at least 60% by weight, especially at least 60% by weight.

Examples of the monomer copolymerized with acrylonitrile include the following. For example, methyl (meth) acrylate, ethyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, n-amyl (meth) acrylate, etc. (Meth) acrylates. Styrene, vinyl toluene, vinyl acetate, etc. Acrylic acid, methacrylic acid, crotonic acid, maleic acid, fumaric acid, itaconic acid, citraconic acid, maleic anhydride, itaconic anhydride and the like. (Meth) acrylamide and the like. Hydroxyethyl (meth) acrylate, hydroxypropyl (meth) acrylate, propylene glycol monoacrylate acrylate, and the like. Dimethylaminoethyl (meth) acrylate, t-butylaminoethyl (meth) acrylate, vinylpyridine, 2-vinyl-5-ethylpyridine, oxazolylethyl (meth) acrylate, hydroxyethylamino (meth) acrylate Ethyl and the like. (Meth) acrylic acid glycidyl ether, allyl glycidyl ether, butane monoxide and the like. Dimethylolated (meth) acrylamide and etherified products thereof, for example, ethyl etherified product and butyl etherified product. Styrene sulfonic acid and the like.

On the other hand, examples of other polymers blended with the acrylonitrile-based polymer include cellulose derivatives such as acetylcellulose, acetylpropionylcellulose and acetylbutyrylcellulose, and vinyl chloride-based polymers.

In order to produce a dope for forming a fiber, an inorganic compounding agent slurry obtained by wet pulverization is dispersed in an aprotic polar solvent with stirring. In the slurry of the inorganic compounding agent, a small amount of an acrylonitrile-based polymer can be previously dissolved for dispersion stabilization. Separately, a dope can be formed by dissolving an acrylonitrile-based polymer for forming a fiber in an aprotic polar solvent, and mixing a compounding agent slurry with this solution immediately before spinning.

The method of preparing the dope for forming a fiber has been described above by taking an acrylonitrile-based polymer as an example. However, this preparation means can be similarly applied to polymers for other fibers. In addition, spinning means is known, and these known means can be applied to the present invention. Further, the above-mentioned dope has other dispersing agents known per se, for example, an antibacterial agent, as long as the dispersibility and the dispersion stability are good and the advantage of the present invention that yarn breakage does not occur during spinning is not impaired. , A flame retardant, a deodorant, and the like.

[0036]

The present invention will be described with reference to the following examples and comparative examples. The physical properties in the examples and comparative examples were measured by the following measurement methods.

(1) Chemical composition JIS. M. 8855. Performed according to. (2) Using the particle size distribution (volume basis average particle volume percent of the diameter D ₅₀ and 2μm or more coarse) Coulter Co. Particle Size Analyzer Model LS230, were measured an average particle size. (3) Oil absorption JIS. K. It was measured according to 5101.19. (4) Coloring of compounding agent The coloring (yellowing) in the production of the compounding agent was visually evaluated as follows. ：: no coloring △: slight coloring ×: considerable coloring

In each of the examples and comparative examples, the following were used as inorganic compounds for pulverization. Sample A: Aluminum-containing zinc phyllosilicate (Mizukanite manufactured by Mizusawa Chemical Co.) Chemical composition: 5.1 SiO ₂ .Al ₂ O ₃ .7.6 ZnO.nH ₂ O Average particle size: 8.484 μm (99.8 volumes if 2 μm or more) %) Oil absorption: 70 ml / 100 g Sample B: zinc hydroxystannate (commercial product) Chemical composition: ZnSn (OH) ₆ Average particle size: 1.595 μm (64.5 vol% for 2 μm or more) Oil absorption: 40 ml / 100 g sample C: zinc borate (commercially available) chemical _{composition: 2ZnO · 3B 2 O 3 ·} nH 2 O average particle size: 3.994μm (2μm above 81.6% by volume) oil absorption: 35 ml / 100 g

Example 1 500 g of sample A (containing aluminum zinc phyllosilicate) and dimethylformamide (D
MF) (1160 g) was placed in a 5 L pot mill (sample concentration: 30% by weight), and wet pulverized at room temperature for 12 hours.
The particle size distribution of the sample A in the resulting slurry (vol% of the volume-based average particle size D ₅₀ and 2μm or more coarse) were measured. Table 1 shows the results.

(Example 2) 5 L of 664 g of sample A (containing aluminum zinc phyllosilicate) and 996 g of DMF were used.
(Sample concentration: 40% by weight), and wet-pulverized at room temperature for 12 hours. The particle size distribution of Sample A in the obtained slurry was measured in the same manner as in Example 1, and the results are shown in Table 1.

Example 3 500 g of sample B (zinc hydroxystannate) and 1160 g of DMF were placed in a 5 L pot mill (sample concentration: 30% by weight), and wet pulverized at room temperature for 12 hours. The particle size distribution of Sample B in the obtained slurry was measured in the same manner as in Example 1, and the results are shown in Table 1.

Example 4 664 g of sample B (zinc hydroxystannate) and 996 g of DMF were placed in a 5 L pot mill (sample concentration: 40% by weight), and wet pulverized at room temperature for 6 hours. The particle size distribution of Sample B in the obtained slurry was measured in the same manner as in Example 1, and the results are shown in Table 1.

Example 5 Sample C (zinc borate) 500
g and 1160 g of DMF were placed in a 5 L pot mill (sample concentration: 30% by weight), and wet pulverized at room temperature for 64 hours. The particle size distribution of Sample C in the obtained slurry was measured in the same manner as in Example 1, and the results are shown in Table 1.

(Example 6) Sample C (zinc borate) 664
g and DMF996g were placed in a 5 L pot mill (sample concentration: 40% by weight), and wet pulverized at room temperature for 12 hours. Example 1 shows the particle size distribution of sample C in the obtained slurry.
And the results are shown in Table 1.

Example 7 415 g of sample B (zinc hydroxystannate) and 1245 g of DMF were placed in a 5 L pot mill (sample concentration: 25% by weight), and wet-pulverized at room temperature for 12 hours. The particle size distribution of Sample B in the obtained slurry was measured in the same manner as in Example 1, and the results are shown in Table 1.

Example 8 Sample C (Zinc borate) 332
g and 1328 g of DMF were placed in a 5 L pot mill (sample concentration: 20% by weight), and wet milled at room temperature for 20 hours. The particle size distribution of Sample C in the obtained slurry was measured in the same manner as in Example 1, and the results are shown in Table 2.

Example 9 500 g of sample A (containing aluminum zinc phyllosilicate) and dimethylformamide (D
MF) was placed in a 5 L pot mill (sample concentration: 30% by weight), and 10.2 g of hydrogen peroxide (2% by weight per sample) was added, followed by wet grinding at room temperature for 12 hours. Example 1 shows the particle size distribution of sample A in the obtained slurry.
And the results are shown in Table 1.

Example 10 A slurry obtained by wet pulverization of Example 4 (using zinc hydroxystannate as sample B) was allowed to stand for 7 days. The slurry after standing for 7 days was considerably colored. 20.5 g of hydrogen peroxide (3% by weight per sample) was added to the slurry after standing for 7 days.
Was added and wet pulverization was performed at room temperature for 1 hour. As a result, coloring was improved. Table 1 shows the results.

Example 11 A slurry obtained by wet grinding of Example 5 (using zinc borate as sample C as a sample) was allowed to stand for 7 days. The slurry after standing for 7 days was considerably colored. 26.3 g of hydrogen peroxide (5% by weight per sample) was added to the slurry after standing for 7 days, and the mixture was stirred at room temperature for 1 hour.
Coloring was improved after wet milling for hours. Table 1 shows the results.

Example 12 An experiment was performed in the same manner as in Example 11, except that salad powder was used instead of hydrogen peroxide. Table 1 shows the results.

(Comparative Example 1) 500 g of sample A (containing aluminum zinc phyllosilicate) and 1160 g of water were put into a 5 L pot mill (sample concentration: 30% by weight).
Time wet grinding was performed. The particle size distribution of Sample A in the obtained slurry was measured in the same manner as in Example 1, and the results are shown in Table 2.

Comparative Example 2 5 L of Sample A (containing aluminum zinc phyllosilicate) (1411 g) and DMF (249 g) were used.
(Sample concentration: 85% by weight), and tried to disperse the sample for wet pulverization at room temperature, but the viscosity was too high to disperse.

[0053]

[Table 1]

[0054]

[Table 2] * The amount of solvent was shown as a multiple of the oil absorption of the sample.

[0055]

According to the present invention, zinc-based and magnesium-based compounds having properties such as deodorant, antibacterial properties and flame retardancy are wet-pulverized in a predetermined amount of an aprotic polar solvent. Fine particles containing almost no coarse particles of 2 μm or more and suitable as a compounding agent for fibers having an extremely small average particle diameter could be obtained. Fibers obtained by blending the resulting fiber blending agent not only have sustained properties such as deodorant properties, antibacterial properties and flame retardancy, but also due to the use of these blending ingredients. Problems such as yarn breakage during spinning could be effectively prevented. In addition, by performing the wet pulverization in the presence of hydrogen peroxide, the coloring can be effectively prevented even when the obtained fiber compounding agent is stored for a long period of time.

Claims (9)

[Claims] 1. An antibacterial, deodorant or flame-retardant zinc-based and / or magnesium-based inorganic compound in an aprotic polar solvent at a concentration of 1 to 80% by weight, and a volume-based average particle size ( D ₅₀ ) is 0.1 to 1.0 μm and 2
A process for producing an inorganic compounding agent for fibers, which comprises wet pulverization so that particles having a particle size of μm or more become 10% by volume or less. 2. The method according to claim 1, wherein the inorganic compound is aluminum-containing zinc phyllosilicate. 3. The method according to claim 1, wherein the inorganic compound is zinc hydroxystannate. 4. The method according to claim 1, wherein the inorganic compound is zinc borate. 5. The method according to claim 1, wherein the inorganic compound is magnesium borate. 6. The method according to claim 1, wherein the wet grinding of the inorganic compound is performed in the presence of an aprotic polar solvent in an amount of 2.0 times or more the oil absorption of the inorganic compound. 7. The production method according to claim 1, wherein the aprotic polar solvent is dimethylformamide. 8. The method according to claim 1, wherein the wet pulverization is performed in the presence of an oxidizing agent. 9. The method according to claim 8, wherein the oxidizing agent is hydrogen peroxide.