JP7148772B2 - Highly oriented metal complex salt - Google Patents

Description

TECHNICAL FIELD The present invention relates to a novel highly oriented metal complex salt containing Mg as a main component. More specifically, a novel highly oriented metal in which a part of the OH of Mg(OH) ₂ is substituted with an organic ligand, the width of the primary particles is large, the thickness is extremely thin, and the metal is easily oriented in the width direction. Regarding complex salts.

Magnesium hydroxide belongs to the Cd(OH) ₂ type structure of the hexagonal crystal system, and since the crystal growth in the c-axis direction (thickness) is worse than that in the a-axis direction (width), it exhibits a plate-like crystal outline. There are many. It is characterized by its low specific gravity of 2.37, its non-toxicity, and its basicity. It has a long history of use as a gastric acid neutralizer and a laxative, but there are few industrial uses other than flue gas desulfurization, and there has been little demand.

However, according to the present inventor, the width of the primary particle (single crystal) is about 0.8 to 1 μm, the thickness is about 0.2 μm, and there is almost no secondary aggregation (primary particle diameter = secondary particle diameter) Nearly monodispersed magnesium hydroxide (trade name: Kisuma 5) was developed (Patent Document 1), opening up a large market as a non-halogen flame retardant for resins. Magnesium hydroxide before that had a primary particle width of about 0.2 μm or less, and the secondary particles (particles formed by agglomeration of the primary particles, measured by the particle size distribution) were as large as 5 μm or more due to strong agglomeration. rice field.

In order to further expand the use of magnesium hydroxide-based compounds, the present inventors have the following formula (2)

（式中、Ｍ^２＋はＭｎ，Ｆｅ，Ｃｏ，Ｎｉ，ＣｕおよびＺｎから選ばれた少なくとも１種以上の２価金属を示し、ｘは０．０１≦ｘ＜０．５の範囲を示す）で表され、平均横幅が１～１０μｍ、厚さが０．０１～０．５μｍで、アスペクト比が１０以上の高アスペクト比の六角板状水酸化マグネシウム系固溶体を開発した。この固溶体は式（２）で表される水酸化物を焼成して得られる酸化物を水媒体中、モノカルボン酸および／またはオキシモノカルボン酸の共存下、水和反応させる方法で製造する。高アスペクト比化することにより、樹脂の強化剤等の新用途が開けた。（特許文献２）

(Wherein, M2 ⁺ represents at least one divalent metal selected from Mn, Fe, Co, Ni, Cu and Zn, and x represents the range of 0.01 ≤ x < 0.5) A high aspect ratio hexagonal plate-like magnesium hydroxide solid solution having an average width of 1 to 10 μm, a thickness of 0.01 to 0.5 μm, and an aspect ratio of 10 or more was developed. This solid solution is produced by hydrating an oxide obtained by calcining the hydroxide represented by the formula (2) in an aqueous medium in the presence of a monocarboxylic acid and/or an oxymonocarboxylic acid. By increasing the aspect ratio, new applications such as reinforcing agents for resins have opened up. (Patent document 2)

As a result of further research on magnesium hydroxide with a high aspect ratio, the present inventors have found that (A) an alkali is added to a mixed aqueous solution of a water-soluble magnesium salt and an alkali metal salt and/or ammonium salt of a monovalent organic acid. After precipitation, or (B) after coprecipitation by adding alkali to an aqueous solution of a water-soluble magnesium salt, an alkali metal salt and/or ammonium salt of a monovalent organic acid is added, and (C) the obtained co-precipitation By hydrothermally treating the sediment slurry at 100° C. or higher, magnesium hydroxide having a width of 0.5 μm or more, a thickness of 0.2 μm or less, and an aspect ratio of 10 or more was developed. (Patent document 3)

Furthermore, the present inventors have developed a method capable of producing a high aspect ratio magnesium hydroxide-based solid solution represented by formula (2) at reduced cost. The method comprises (A) a mixed aqueous solution of a water-soluble Mg salt and (B) a water-soluble divalent metal salt (M ²⁺ ) or a metal complex thereof and (C) an alkaline aqueous solution such as sodium hydroxide, and (D) (D) and (E) one or more chlorides selected from sodium chloride, potassium chloride, ammonium chloride, magnesium chloride and calcium chloride after coprecipitation in the presence or absence of monocarboxylic acid ions; It is a production method in which heat aging is performed at 60 to 300 ° C. in the coexistence of (Patent Document 4)

On the other hand, for the purpose of developing fine particle magnesium hydroxide, a portion of the hydroxyl group OH is substituted with a monovalent organic acid, the following formula (3)

（但し、式中Ｒは１価の有機酸を、ｘは０＜ｘ＜１の範囲を示す）で表される、平均２次粒子径が３００ｎｍ以下の水酸化マグネシウム系固溶体が開発されている。この微粒子の固溶体の製造は、（Ａ）水溶性マグネシウム塩と１価有機酸もしくはその塩との混合水溶液に、ほぼＭｇと当量のアルカリを加え共沈させ、その後水熱処理する方法、又は（Ｂ）水溶性マグネシウム塩の水溶液に、アルカリの水溶液を加え共沈させた水酸化マグネシウムに、１価有機酸またはその塩を添加し、その後水熱処理する方法で行われる。（特許文献５）

(wherein R represents a monovalent organic acid and x represents a range of 0<x<1), and a magnesium hydroxide-based solid solution having an average secondary particle size of 300 nm or less has been developed. . The solid solution of fine particles can be produced by (A) adding an alkali equivalent to about Mg to a mixed aqueous solution of a water-soluble magnesium salt and a monovalent organic acid or a salt thereof, coprecipitating it, and then hydrothermally treating it, or (B) ) A monovalent organic acid or a salt thereof is added to magnesium hydroxide obtained by adding an aqueous alkali solution to an aqueous solution of a water-soluble magnesium salt to coprecipitate, followed by hydrothermal treatment. (Patent Document 5)

JP-A-52-11579 Japanese Patent Application Laid-Open No. 8-259235 WO2012/050222 Japanese Patent Application Laid-Open No. 2020-152626 WO2016/031803

The higher the aspect ratio, the higher the reinforceability of the resin and the wider the range of applications. Therefore, the first object of the present invention is to provide a magnesium hydroxide compound having a high aspect ratio of more than 50.

In the conventional method for producing magnesium hydroxide with a high aspect ratio, the aspect ratio tends to increase as the monovalent organic acid or its salt is increased with respect to Mg. should be used for The conventional production method requiring a large amount of monovalent organic acid, which is more expensive than the Mg raw material, is difficult to separate the monovalent organic acid from water, resulting in high raw material costs. At the same time, since the waste water contains a large amount of monovalent organic acid, additional expenses are required for waste water treatment, resulting in high running costs. Therefore, a second object of the present invention is to provide an inexpensive manufacturing method.

As a result of intensive research to solve the above problems, the present inventors have found the following formula (1)

(Mg) _1-x (M ²⁺ ) _x (OH) _2-ny A _y (1)
(Wherein, M ²⁺ represents at least one type of divalent metal other than Mg, A represents at least one type of organic ligand, and x and y are each within the following range, 0≦x< 0.2 , preferably 0.001<x<0.02 , 0<y<0.05, n is an integer in the range of 1 to 4), and ) plane X-ray diffraction intensity ratio (orientation H) is 30% or less, and a highly oriented metal complex salt having a hexagonal Cd(OH) ₂ type crystal structure has been successfully developed.
In addition, the present inventors added (A) an aqueous solution of a water-soluble salt of a divalent metal containing at least Mg to (B) an organic A ligand is added, (C) a coprecipitation reaction is performed with an alkali of at least 0.95 equivalent or less with respect to the total equivalent of the divalent metal containing at least Mg, and then hydrothermal treatment is performed at 100 ° C. or higher. We succeeded in developing a method for producing the highly oriented metal complex salt.

The highly oriented metal complex salt is produced by adding about 0.01 mol of (B) an organic ligand capable of forming a metal complex to Mg to (A) a water-soluble magnesium salt aqueous solution, (C) and an alkali is supplied in an amount of at least 0.95 equivalents or less, preferably 0.9 equivalents or less, with respect to Mg for a coprecipitation reaction, and then (D) is hydrothermally treated at 100 ° C. or higher to provide high orientation (high aspect ratio) of magnesium hydroxide can be produced at reduced production costs. The required amount of the organic ligand may be an extremely small amount corresponding to about 1/100 of the amount of the monovalent organic acid or its salt required in the prior art. Even if the amount is increased or decreased, the orientation (aspect ratio) will rather decrease sharply. This is a new discovery that cannot be assumed at all from the conventional way of thinking that the aspect ratio increases as the amount of the monovalent organic acid increases.

The second important production condition in the present invention is the alkali addition equivalent to Mg, which is at least 0.95 equivalents or less, preferably 0.9 equivalents or less, and particularly preferably 0.85 equivalents or less to 0.6 equivalents or more. There is a need to. By suppressing the amount of alkali to be added to less than the equivalent amount, the function of the organic ligand can be exhibited.

The highly oriented composite metal salt of the present invention has a primary particle (crystallite) with a thinner thickness (minimum of about 5 nm) and a wider width compared to the conventional technology using a monovalent organic acid or its salt. It can be much larger (up to about 40 μm) and less agglomerated, resulting in much higher orientation and thus higher aspect ratios (up to about 200 for the present invention versus up to about 40 for the prior art). Therefore, the effect of reinforcing resin is higher than that of conventional products, and since it can be reinforced with a smaller amount, it further contributes to the weight reduction of automobiles and widens the range of applications such as door trims, bumpers, and instrument panels.

In addition to being used in automobiles, it can be used in resins as flame retardants, smoke suppressants, heat conductors, gas barrier materials, and the like. Furthermore, it can be used as a rust preventive agent for paints, a dyeing agent for fibers, a flame retardant agent for paper, and the like. Since the amount of the organic ligand required for the production of the highly oriented metal complex salt of the present invention is extremely small at about 0.01 mol per 1 mol of Mg, raw material costs can be greatly reduced compared to conventional techniques. . In addition, it is possible to omit equipment and processes for recovering organic matter, and further reduce costs.

XRD patterns of the products of Example 1, Example 4 and Comparative Example 5 SEM photographs of Examples 1 and 4

In the present invention, an organic ligand capable of forming a metal complex is used instead of the conventional monovalent carboxylic acid, and an alkali is used in an amount of 0.95 equivalents or less, preferably 0.9 equivalents or less, particularly preferably 0.9 equivalents or less, relative to Mg. is coprecipitated at 0.8 equivalents or less to 0.6 equivalents or more, and then hydrothermally treated at 100° C. or higher, preferably 120° C. or higher, particularly preferably 180° C. or higher.

The present invention was obtained as a result of intensive research based on the following idea. By creating conditions that facilitate complex formation between Mg ions and organic ligands, it is possible to add two new functions not found in conventional techniques. One is that the organic ligand binds to the Mg ion at two or more sites, so compared to the conventional technique using a monovalent organic acid that can only bond at one site, a small amount of primary particles can be effectively used. should be able to suppress growth in the thickness direction. Secondly, since the complex with Mg has some degree of water-solubility, which is a characteristic of metal complexes, it can be expected to improve the solubility. improves.

The highly oriented metal complex salt represented by formula (1) of the present invention has the following characteristics.
(1) The powder X-ray diffraction pattern has the same hexagonal Cd(OH) ₂ type crystal structure as magnesium hydroxide. Although some of the OH groups of Mg(OH) ₂ are replaced with organic ligands, the crystal structure is the same as Mg(OH) ₂ .
(2) The X-ray diffraction intensity ratio H (orientation) of the (101) plane to the (001) plane is at least 30% or less, preferably 6% or less, and particularly preferably 3% or less.
A higher orientation H means a higher aspect ratio of the primary particles and less aggregation. As a result of repeating the example of Patent Document 5 of the same solid solution as the present invention, H of the glycolic acid solid solution (Example 2) and the lactic acid solid solution (Example 3) were 143% and 147%, respectively. The difference from the complex metal salt is obvious.
(3) The average width of primary particles is 0.4 μm or more, preferably 2 μm or more, and particularly preferably 4 μm to 50 μm. The average thickness of the primary particles is in the range from 5 nm to 100 nm, preferably from 5 nm to 60 nm, particularly preferably from 5 nm to 40 nm. The aspect ratio obtained by dividing the arithmetic mean of the width by the arithmetic mean of the thickness is 20 or more, preferably 50 or more, and particularly preferably 100 or more.
(4) The average secondary particle size is the same as or slightly larger than the primary particle size.

The organic ligand constituting the highly oriented metal complex salt of the present invention is preferably bidentate and slightly larger than the OH group. Preferred organic ligands include oxycarboxylic acids such as glycolic acid, lactic acid, glyceric acid, hydroxybutyric pantoic acid, quinic acid, salicylic acid, vanillic acid, syringic acid, orceric acid, gallic acid, mandelic acid, benzilic acid ( hydroxycarboxylic acids ) , amines such as diethanolamine, triethanolamine, ethylenediamine, putrescine, cadaverine, ethambutol, phenylenediamine, amino acids such as glycine, tryptophan, histidine, glutamic acid, aspartic acid, proline, propylene glycol, ethylene Glycol, glycerin, polyhydric alcohols such as sorbitol , aminocarboxylic acids such as glycine , and the like can be mentioned.
The amount y of the organic ligand is in the range 0<y<0.05, preferably 0.0001<y<0.03, particularly preferably 0.005<y<0.02.

In the metal complex salt of the present invention, in addition to pure magnesium hydroxide, part of Mg in Mg(OH) ₂ is replaced with another divalent metal M ²⁺ , preferably Ca ²⁺ , Mn ²⁺ , Fe ²⁺ , Co ²⁺ , Ni ²⁺ , It contains a solid solution substituted with at least one of Cu ²⁺ and Zn, particularly preferably Ca ²⁺ , Ni ²⁺ and Zn ²⁺ . The solid solubility range x of M ²⁺ is 0≦x<0.3, preferably 0≦x≦0.2, particularly preferably 0≦x≦0.1. Ca ²⁺ enhances basicity, Ni ²⁺ and Zn ²⁺ improve flame retardancy, and Ni ²⁺ improves acid resistance.

By firing the highly oriented metal complex salt of the present invention at 400 to 1000 ° C., it is possible to produce a thin, highly oriented magnesium oxide and a magnesium oxide solid solution in which a part of Mg is substituted with M 2 ⁺ . . Therefore, it can be used as an annealing separation material for electromagnetic steel sheets, a heat dissipation material for resin or rubber, a vulcanization accelerator for rubber, etc., taking advantage of its characteristics.

<Manufacturing method>
First step (coprecipitation reaction)
(A) a mixed aqueous solution of a water-soluble magnesium salt and an organic ligand, or a mixed solution of a water-soluble magnesium salt, a water-soluble divalent metal (M ²⁺ ) salt, and an organic ligand; , at least 0.95 equivalents or less, preferably 0.9 equivalents or less, and particularly preferably 0.8 equivalents or less to 0.6 equivalents or more of alkali are added to coprecipitate.
Second step (hydrothermal treatment)
The coprecipitate obtained in the first step is hydrothermally treated at 100° C. or higher, preferably 120° C. or higher, particularly preferably 180° C. to 250° C. for 1 hour or longer, preferably 2 to 10 hours. By changing the hydrothermal treatment temperature, the width of the primary particles can be adjusted to the range of 0.4 to 40 μm.

<Surface treatment>
Various functions can be added to the metal complex salt of the present invention by surface treatment. For example, in order to improve compatibility with resins and acid resistance, (a) higher fatty acids such as stearic acid and lauric acid, (b) alkali metal salts of the higher fatty acids, (c) sodium dialkylsulfosuccinate, anionic surfactants such as alkyl ether sulfate, 2-ethylhexyl alkyl sulfate, sodium salt, sodium acylmethyl taurate, sodium alkylbenzene sulfonate, and oleoyl sarcosine ; (d) orthophosphoric acid and stearyl alcohol; (e) silane coupling agents such as vinylethoxysilane and γ-aminopropyltrimethoxysilane ; (f) isopropyl trimethoxysilane; (g) aluminum coupling agents such as acetoalkoxyaluminum diisopropylate ; (h) fatty acid esters of polyhydric alcohols such as sorbitan monostearate; ) polycarboxylic acids such as sodium polyacrylate and sodium polystyrene sulfonate ; and (j) alkali metal salts of polysulfonic acid. In order to increase the acid resistance, silica coating is performed by chemical adsorption of water glass followed by addition of acid, silica coating is performed by hydrolysis of methyl silicate, ethyl silicate, etc., and silicone coating is performed with silicone oil. Coatings with particulates such as titanium oxide, zinc oxide, cerium oxide, etc. are available to enhance UV absorption and/or scattering. A pearl pigment can be produced by a method of uniformly coating the surface of a highly oriented metal complex salt dispersed in water by adding fine particles of a metal oxide such as titanium oxide or iron oxide. Examples of the surface treatment agent used as a flame retardant for paper include carboxymethyl cellulose and sodium alginate.

The surface treatment method is preferably wet or dry. The wet method is a method of dispersing a metal complex salt in a solvent such as water or alcohol and adding a surface treatment agent while stirring. The dry method is a method of adding a surface treatment agent to a powdery highly oriented metal complex salt under stirring with a high-speed stirrer such as a Henschel mixer. The amount of the surface treatment agent is appropriately selected and determined according to the purpose, but generally the preferable range is 0.5 to 20% by weight based on the weight of the highly oriented metal complex salt.

<Resin composition>
The resin composition of the present invention contains 0.01 to 300 parts by weight, preferably 0.5 to 200 parts by weight, and particularly preferably 1 to 150 parts by weight of a highly oriented metal complex salt per 100 parts by weight of the resin. . The optimum blending amount varies depending on the purpose. For example, if the purpose is to strengthen the flexural modulus, flexural strength, Izod strength, etc. of the resin, 1 to 40 parts by weight, as a rubber receiver, 1 to 20 parts by weight, as a flame retardant or gas barrier agent for the resin. is 50 to 200 parts by weight, and the acid acceptor for the resin is 0.01 to 5 parts by weight.

<Processing method>
There are no particular restrictions on the method of mixing and kneading with the resin, and any method that allows uniform mixing of the two may be used. For example, they are mixed and kneaded using a single-screw or twin-screw extruder, an open roll, a Banbury mixer, or the like. There are no particular restrictions on the molding method, and any molding means known per se can be arbitrarily adopted according to the type of resin and rubber, the type of desired molded product, and the like. Examples of molding means include injection molding, rotational molding, calendar molding, sheet forming molding, transfer molding, laminate molding, and vacuum molding.

<Resin type>
The resin used in the present invention means resin and/or rubber, and (A) for example, polyethylene, copolymer of ethylene and other α-olefin, ethylene and vinyl acetate, ethyl acrylate or methyl acrylate. Copolymers, polybutene-1, poly4-methylpentene-1, polystyrene, styrene and acrylonitrile, copolymers of ethylene and propylene diene rubber or butadiene, polyvinyl acetate, polyvinyl alcohol, polyacrylate, polymethacrylate, polyurethane, polyester , thermoplastic resins such as polyether, polyamide, ABS, polycarbonate, and polyphenylene sulfide, (B) thermosetting resins such as phenol resin, melamine resin, epoxy resin, unsaturated polyester resin, and alkyd resin, ( C) Rubbers such as EPDM, SBR, NBR, butyl rubber, chloroprene rubber, isoprene rubber, chlorosulfonated polyethylene rubber, silicon rubber, fluororubber, chlorinated butyl rubber, epichlorohydrin rubber, and chlorinated polyethylene rubber.

Examples of preferred resins are polypropylene, mixtures of polypropylene and olefinic rubber, polyethylene, polyamide, EPDM, butyl rubber, and chloroprene rubber.

In the resin composition of the present invention, conventionally known reinforcing agents such as talc, mica, glass fiber, basic magnesium sulfate fiber, etc. may be used in combination with the highly oriented metal complex salt. The blending amount of these reinforcing agents is 1 to 50 parts by weight, preferably 1 to 20 parts by weight, per 100 parts by weight of the resin.

In addition to reinforcing agents, other commonly used additives such as antioxidants, ultraviolet absorbers, lubricants, pigments such as carbon black, brominated or phosphoric ester flame retardants, zinc stannate, alkali metal stannate, carbon Flame retardant aids such as powders and fillers such as calcium carbonate, zeolite and kaolin can be appropriately selected and blended.

EXAMPLES The present invention will be described in more detail below with reference to examples, but the present invention is not limited only to these examples.

A mixed aqueous solution (approximately 20° C.) was placed in a 1 L container, and 320 mL of a 4 mol/L sodium hydroxide aqueous solution (about 20° C.), which corresponds to 0.8 equivalent to Mg, was added with stirring to cause coprecipitation. This coprecipitate was transferred to a 1 L autoclave and hydrothermally treated at 200° C. for 4 hours. The hydrothermally treated product was filtered, vortexed, washed with water, dried and sieved (100 mesh). The XRD (powder X-ray diffraction method) (Fig. 1) of the sieved sample was measured, and the diffraction intensity ratio H (%) of the (101) plane to the (001) plane was measured.
After sonicating the sieved sample in an aqueous medium for 5 minutes, SEM was measured (Fig. 2), the maximum width and thickness of the primary particles were measured with five primary particles, and their average obtained as a value. Also, the contents of lactic acid and Mg were measured by absorptiometric method and chelate titration method, respectively. Table 1 shows the above measurement results. The XRD pattern is the same as that of magnesium hydroxide and this sample has the same Cd(OH) ₂ type crystal structure as magnesium hydroxide. Since the interplanar spacing d=4.67 Å of the (001) plane is shorter than d=4.77 Å of magnesium hydroxide (POWDER DIFFRACTION FILE 7-239), lactate ions replace part of the OH groups and form a solid solution. It supports that Whether the valence n of lactic acid is 1 or 2 cannot be determined because it is a complex.
The orientation H of the sieved sample was 1%, and the orientation of the FILE was calculated to be 111%, indicating that the orientation of the product of the present invention is extremely high.

The procedure of Example 1 was repeated except that the amount of sodium lactate aqueous solution added to Mg was changed to 2.5 mol %. Table 1 shows the results. The XRD pattern is the same as magnesium hydroxide.

The procedure of Example 1 was repeated except that the amount of sodium lactate aqueous solution added to Mg was changed to 0.5 mol %. Table 1 shows the results. The XRD pattern is the same as magnesium hydroxide.

[Comparative Example 1]
In Example 1, the same procedure as in Example 1 was carried out, except that the amount of sodium lactate aqueous solution added to Mg was changed to 10 mol %. Table 1 shows the results.

[Comparative Example 2]
In Example 1, the procedure was carried out in the same manner as in Example 1, except that the amount of the 4 mol/L sodium hydroxide aqueous solution added was changed to 400 mL corresponding to 1.0 equivalent to Mg. Table 1 shows the results.

[Comparative Example 3]
In Example 1, the procedure was carried out in the same manner as in Example 1, except that the addition of sodium lactate was omitted. Table 1 shows the results.

[Comparative Example 4]
In Example 1, instead of sodium lactate as an organic ligand, sodium acetate is added in an amount of 150 mol % to Mg according to the conventional method for producing high aspect ratio magnesium hydroxide (Patent Document 3, Example 1). Except for this, the same procedure as in Example 1 was carried out. Table 1 shows the results.

In Example 1, it carried out in the same manner as in Example 1, except that the hydrothermal treatment temperature was changed from 200°C to 120°C. Table 1 shows the results. XRD is shown in FIG. 1, and SEM photograph is shown in FIG. The XRD pattern is the same as magnesium hydroxide.

[Comparative Example 5]
In Example 4, the procedure was carried out in the same manner as in Example 4 except that the amount of sodium hydroxide added was changed to 400 mL corresponding to 1.0 equivalent to Mg. (Corresponding to Patent Document 4, Example 3) Table 1 shows the results. XRD is shown in FIG.

The procedure of Example 1 was repeated except that the reagent ethylenediamine was used in an amount of 0.5 mol % based on Mg instead of sodium lactate. Table 1 shows the results. The XRD pattern is the same as magnesium hydroxide.

Example 1 was carried out in the same manner as in Example 1, except that 1.5 mol % of glycolic acid as a reagent was added to Mg instead of sodium lactate. Table 1 shows the results. The XRD pattern is the same as magnesium hydroxide.

In Example 1, the procedure was carried out in the same manner as in Example 1, except that 1 mol % of glycine as a reagent was added to Mg instead of sodium lactate. Table 1 shows the results. The XRD pattern is the same as magnesium hydroxide.

The procedure of Example 1 was repeated except that the reagent triethanolamine was added in an amount of 4 mol % based on Mg instead of sodium lactate. Table 1 shows the results. The XRD pattern is the same as magnesium hydroxide.

Example 1 was carried out in the same manner as in Example 1, except that zinc chloride as a reagent was mixed in an aqueous solution of magnesium chloride in an amount of 2 mol % based on Mg, and the hydrothermal treatment temperature was changed to 250°C. Table 1 shows the results. The XRD pattern is the same as magnesium hydroxide.

In Example 1, the same procedure as in Example 1 was repeated, except that the reagent nickel chloride was mixed with the magnesium chloride aqueous solution at 2 mol% relative to Mg, and triethanolamine was added at 5 mol% relative to Mg instead of sodium lactate. went. Table 1 shows the results. The XRD pattern is the same as magnesium hydroxide.

<Resin composition>
Add 500 g of the highly oriented metal complex salt powder prepared by the method of Example 1 to 5 L of water and disperse it with a chemistirrer, heat to 80° C., add 10 g of sodium stearate while stirring, surface treated. After filtering, washing with water and drying, 12 parts by weight (equivalent to about 20% by weight of the total) was mixed with 0.2 parts by weight of an antioxidant (IRGANOX 1010) with 100 parts by weight of polypropylene. This mixture was kneaded at about 190° C. using a twin-screw extruder to prepare pellets. After drying the pellets under vacuum, they were injection molded at about 230° C. by an injection molding machine to prepare test pieces. Using this test piece, the flexural modulus and Izod impact strength were measured, and the melt flow index (MFR) was measured using pellets. Those results are shown in Table 2.

[Comparative Example 6]
In Example 11, instead of the highly oriented metal complex salt produced by the method of Example 1, the high aspect ratio magnesium hydroxide produced by the method of Comparative Example 4 (Patent Document 3) was used. Table 2 shows the results of evaluation performed in the same manner as in No. 11.

[Comparative Example 7]
In Example 11, talc (primary particle size: 5 µm, thickness: 0.2 µm, aspect ratio: 20), which is often used as a resin reinforcing agent for automobiles, was added to the highly oriented metal complex salt of Example 11. Table 2 shows the results of evaluation performed in the same manner as in Example 11, except that it was used instead.

Claims (10)

Formula (1) below
(Mg) _1-x (M ²⁺ ) _x (OH) _2-ny A _y (1)
(Wherein, M ²⁺ represents at least one type of divalent metal other than Mg, A represents at least one type of organic ligand, and x and y are each within the following range, 0≦x<0.2,0<y<0.05, n is an integer in the range of 1 to 4), and the X-ray diffraction intensity ratio of the (101) plane to the (001) plane (orientation H ) is 30% or less, a highly oriented metal complex salt having a hexagonal Cd(OH) ₂ -type structure. 2. The highly oriented metal complex salt according to claim 1, wherein the average width of primary particles of said highly oriented metal complex salt is 0.4 μm or more and 50 μm or less . 2. The highly oriented metal complex salt according to claim 1, wherein the orientation H is 6% or less and the average width of the primary particles of the highly oriented metal complex salt is 2 μm or more and 50 μm or less . Any one of claims 1 to 3, wherein in the formula (1), the organic ligand A is at least one selected from oxycarboxylic acids , amines, amino acids, polyhydric alcohols and aminocarboxylic acids . 2. The highly oriented metal complex salt according to item 1. 4. The highly oriented metal composite salt according to any one of claims 1 to 3, wherein in formula (1), M ²⁺ is at least one selected from Ca ²⁺ , Ni ²⁺ , Cu ²⁺ and Zn ²⁺ . The highly oriented metal complex salt according to any one of claims 1 to 4, wherein in formula (1), the range of x is 0.001<x<0.02. Higher fatty acids, alkali metal salts , anionic surfactants, phosphate esters , silane coupling agents , titanium coupling agents and aluminum coupling agents, fatty acid esters, polycarboxylic acids, alkali metal salts, water Claims 1-, surface-treated with at least one selected from glass , methyl silicate, ethyl silicate, silicone oil, titanium oxide, zinc oxide and cerium oxide, metal oxide fine particles, and carboxymethyl cellulose and sodium alginate . 7. The highly oriented metal complex salt according to any one of 6. A resin composition containing 0.01 to 300 parts by weight of the highly oriented metal complex salt according to any one of claims 1 to 7 with respect to 100 parts by weight of the resin. (A) to an aqueous solution of a water-soluble salt of a divalent metal containing at least Mg, (B) an organic ligand of less than 10 mol% with respect to the total number of moles of the divalent metal containing at least Mg; C) Coprecipitation with an alkali of at least 0.95 equivalents or less with respect to the total equivalent of the divalent metals containing at least Mg, followed by hydrothermal treatment at 100 ° C. or higher , A method for producing a highly oriented metal complex salt according to any one of the above items. 10. The production method according to claim 9, wherein the divalent metal other than Mg is at least one selected from Mn2 ⁺ , Fe2 ⁺ , Co2 ⁺ , Ni2 ⁺ , Cu2 ⁺ and Zn2 ⁺ .

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