Layered double hydroxide, additive for resin including layered double hydroxide, and resin composition including layered double hydroxide

The layered double hydroxide with optimized X-ray diffraction peaks and ultrasonic treatment, coated with fatty acids or organic derivatives, enhances resin composition filterability, addressing filter pressure issues and maintaining production efficiency.

WO2025248977A1PCT designated stage Publication Date: 2025-12-04SETOLAS HLDG INC
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Patent Information

Application Number
PCT/JP2025/014049
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-05-30
Filing Date
2025-04-08
Publication Date
2025-12-04

AI Technical Summary

Technical Problem

Existing resin compositions containing layered double hydroxides do not consider filterability, leading to issues such as increased filter pressure and frequent filter replacements during production, which affects mass productivity.

Method used

A layered double hydroxide with specific X-ray diffraction peak intensities and ultrasonic treatment to reduce particle size and improve dispersibility, coated with higher fatty acids or organic acid derivatives to enhance filterability.

Benefits of technology

The improved filterability reduces filter pressure and frequency of replacements, maintaining consistent production efficiency and productivity in resin composition manufacturing.

✦ Generated by Eureka AI based on patent content.

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Abstract

The purpose of the present disclosure is to provide a layered double hydroxide that, when mixed with a resin to produce a resin composition, makes it possible for the resin composition to pass favorably through a filter. When a layered double hydroxide according to the present invention is analyzed by x-ray diffraction, the intensity ratio I1 / I2 of the peak intensity I1 of a peak in a 2θ range of 11.6°–11.7° and the peak intensity I2 of a peak in a 2θ range of 34.8°–34.9° is at least 10.
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Description

Layered double hydroxide, resin additive containing layered double hydroxide, and resin composition containing layered double hydroxide

[0001] The present disclosure relates to a layered double hydroxide, a resin additive containing the layered double hydroxide, and a resin composition containing the layered double hydroxide.

[0002] Layered double hydroxides are widely used as additives for resins, etc. Patent Document 1 describes the following (A) to (C): (A) The lattice strain in the (003) direction measured by X-ray diffraction is 3×10 -3 (B) the average lateral width of the primary particles measured by the SEM method is 5 nm or more and 200 nm or less; (C) the monodispersity expressed by the following formula is 50% or more: Monodispersity (%) = (average lateral width of the primary particles measured by the SEM method / average lateral width of the secondary particles measured by the dynamic light scattering method) × 100, and the following formula is satisfied: (M 2+ ) 1-X (M 3+ ) X (OH) 2 (A n- ) X/n ・mH 2 O (wherein M 2+ is at least one divalent metal, M 3+ is at least one trivalent metal, A n- is an n-valent anion, n is an integer of 1 to 6, and x and m are in the ranges of 0.17≦x≦0.36 and 0≦m≦10, respectively.

[0003] International Publication No. 2018 / 169019

[0004] The resin composition can be produced by mixing a resin with additives for imparting various functions to the resin, and preferably by kneading them together. In order to prevent unexpected foreign matter from being mixed into the resin composition, the mixture may be passed through a filter during mixing.

[0005] With regard to the hydrotalcite described in Patent Document 1, when a resin composition is prepared by mixing the hydrotalcite with a resin, no consideration is given to the filterability of the resin composition when the resin composition passes through a filter.

[0006] Therefore, an object of the present disclosure is to provide a layered double hydroxide that, when mixed with a resin to prepare a resin composition, can improve the filterability of the resin composition, and a resin composition containing such a layered double hydroxide.

[0007] In the first embodiment of the present disclosure, in X-ray diffraction measurement, the peak intensity I of a peak present in the 2θ range of 11.6° or more and 11.7° or less is 1 and the peak intensity I of the peak present in the 2θ range of 34.8° or more and 34.9° or less. 2 Intensity ratio I 1 / I 2 is 10 or more.

[0008] In a second embodiment of the present disclosure, after the ultrasonic treatment described below is performed in the first embodiment, the proportion of layered double hydroxides having a particle size of 10 μm or more can be 0.90 vol% or less of the total amount of layered double hydroxide. [Ultrasonic Treatment] 0.7 g of layered double hydroxide is mixed with 70 mL of a 0.002 g / mL aqueous solution of sodium hexametaphosphate to prepare a mixed solution with a layered double hydroxide concentration of 0.01 g / mL. This mixed solution is irradiated with ultrasonic waves at an oscillation frequency of 19.5 kHz±1 kHz, an output of 70 W, and an intensity of 20 mμA for 3 minutes.

[0009] In a third embodiment of the present disclosure, in any one of the first and second embodiments, the average secondary particle size after the ultrasonic treatment can be 0.9 μm or less.

[0010] In a fourth embodiment of the present disclosure, in any one of the first to third embodiments, the layered double hydroxide is coated with a higher fatty acid.

[0011] In a fifth embodiment of the present disclosure, in any one of the first to fourth embodiments, the layered double hydroxide is coated with an organic acid or a derivative thereof.

[0012] A sixth embodiment of the present disclosure provides a resin additive comprising any one of the layered double hydroxides described in the first to fifth embodiments.

[0013] A seventh embodiment of the present disclosure provides a resin composition comprising any one of the layered double hydroxides described in the first to fifth embodiments and a resin. The content of the layered double hydroxide may be 100 ppm by mass or more and 5,000 ppm by mass or less based on the total amount of the resin composition.

[0014] In an eighth embodiment of the present disclosure, in the seventh embodiment, the resin may include a polyolefin resin.

[0015] According to the present disclosure, it is possible to provide a layered double hydroxide that, when mixed with a resin to prepare a resin composition, can improve the filterability of the resin composition.The present disclosure also provides a resin composition containing such a layered double hydroxide.

[0016] FIG. 1 is a diagram showing an example of an X-ray diffraction result of the layered double hydroxide according to the present embodiment and a comparative layered double hydroxide. FIG. 2 is another diagram showing an example of an X-ray diffraction result of the layered double hydroxide according to the present embodiment and a comparative layered double hydroxide. FIG. 3 is a diagram showing an example of particle size distribution of the layered double hydroxide according to the present embodiment and a comparative layered double hydroxide by ultrasonic treatment. FIG. 4 is another diagram showing an example of particle size distribution of the layered double hydroxide according to the present embodiment and a comparative layered double hydroxide by ultrasonic treatment. FIG. 5 is a diagram showing the filter pressure in a twin-screw kneading extruder using the layered double hydroxide according to the present embodiment and a comparative layered double hydroxide. FIG. 6 is a schematic cross-sectional view of a twin-screw kneading extruder for preparing a resin composition according to the present embodiment.

[0017] In X-ray diffraction measurement, the layered double hydroxide of the present disclosure has a peak intensity I of a peak present in the 2θ range of 11.6° or more and 11.7° or less. 1 and the peak intensity I of the peak present in the 2θ range of 34.8° or more and 34.9° or less. 2 Intensity ratio I 1 / I 2 is 10 or more,

[0018] According to the present disclosure, it is possible to provide a layered double hydroxide that can improve the filterability of a resin composition prepared by mixing the layered double hydroxide with a resin.

[0019] In a preferred embodiment, the layered double hydroxide and the resin can be mixed by kneading. Kneading of the layered double hydroxide and the resin is typically carried out using a twin-screw kneading extruder. As shown schematically in FIG. 6 , production of a resin composition using a twin-screw kneading extruder is initiated by introducing raw material 10 from a hopper 11 into the twin-screw kneading extruder 1. The introduced raw material 10 is heated by a heating cylinder 13 and a heater 14 and extruded by a screw 12 toward a filter 15, thereby forming a resin composition. The resin composition that reaches the filter 15 passes through the filter 15 and is extruded by a die 17. The resin composition extruded by the die 17 is then cooled in a cooling water tank 2 and molded into strands 20. The strands 20 are further drained by a drainer 21 and pelletized by a pelletizer 3.

[0020] In this embodiment, the filterability is improved, which suppresses an increase in the filter pressure on the filter 15 and reduces the frequency of filter replacement in the twin-screw kneading extruder. When replacing the filter, not only is there a time loss for the replacement, but there may also be a waste of resin due to the filter replacement. Therefore, the filterability is an important factor in the production of a resin composition.

[0021] Although the present disclosure should not be interpreted as being limited to a particular theory, the reason why the layered double hydroxide of the present disclosure can exhibit such effects is thought to be as follows. That is, a layered double hydroxide is understood to be a polycrystal containing two or more crystallites. In X-ray diffraction measurement, a peak present in the 2θ range of 11.6° or more and 11.7° or less is understood to be a peak attributable to the (003) plane of the layered double hydroxide. In X-ray diffraction, a peak present in the 2θ range of 34.8° or more and 34.9° or less is understood to be a peak attributable to the (102) plane of the layered double hydroxide. The peak intensity I of the peak attributable to the (003) plane 1 and the peak intensity I of the peak assigned to the (102) plane 2 Relative to I 1 / I 2The larger the α value, the stronger the crystal orientation and the smaller the crystal growth in the thickness direction. Therefore, it is believed that the layered double hydroxide tends to contain many crystallites with a high aspect ratio. Furthermore, it is believed that the presence of many flat crystallites makes the resin composition more susceptible to shear stress. As a result, it is believed that the filterability of the resin composition can be improved. In other words, when a resin composition containing the layered double hydroxide of this embodiment is fed to a twin-screw kneading extruder, the twin-screw kneading extruder can be operated regardless of the screw rotation speed of the twin-screw kneading extruder. For example, in the filter pressure increase evaluation method, the twin-screw kneading extruder can be operated in the same way at both a screw rotation speed of 250 Hz and a screw rotation speed of 200 Hz, thereby reducing the dependency on the screw rotation speed. In the filter pressure increase evaluation method, the mass productivity of the resin composition is evaluated by observing the filter pressure of the twin-screw kneading extruder over time. It is understood that a higher filter pressure increase rate corresponds to lower mass productivity, and a lower filter pressure increase rate corresponds to higher mass productivity.

[0022] The above intensity ratio I 1 / I 2 is preferably 10 or more and 18 or less, more preferably 11 or more and 14 or less. 1 / I 2 is preferably 10 or more, more preferably 11 or more, and is preferably 18 or less, more preferably 14 or less. 1 / I 2 If the molecular weight falls within this range, when a resin composition is prepared by mixing the layered double hydroxide with a resin, the filterability of the resin composition can be improved.

[0023] X-ray diffraction measurement of layered double hydroxides is carried out as follows: [X-ray diffraction measurement] Measurements can be performed by powder X-ray diffraction using CuKα radiation (λ=1.54 Å) as the X-ray source, with a 2θ measurement interval of 0.026°, an accumulation time of 296.565 seconds, an acceleration voltage of 45 kV, an acceleration current of 40 mA, a focal length of 12.0 mm, and a take-off angle of 6°.

[0024] The layered double hydroxide of the present disclosure preferably has a particle size of 10 μm or more of 0.90% by volume or less of the total amount of layered double hydroxide after the following ultrasonic treatment. [Ultrasonic Treatment] 0.7 g of layered double hydroxide is mixed with 70 mL of a 0.002 g / mL aqueous solution of sodium hexametaphosphate to prepare a mixture with a layered double hydroxide concentration of 0.01 g / mL. This mixture is irradiated with ultrasonic waves at an oscillation frequency of 19.5 kHz±1 kHz, an output of 70 W, and an intensity of 20 mμA for 3 minutes.

[0025] The results of the ultrasonic treatment make it possible to predict how the layered double hydroxide will be disintegrated when it is mixed with a resin and kneaded. Since the layered double hydroxide of the present disclosure has reduced residual coarse particles after the ultrasonic treatment, it is believed that the filterability of a resin composition containing the layered double hydroxide of the present disclosure and a resin will be improved.

[0026] After the layered double hydroxide of the present disclosure is subjected to the ultrasonic treatment, the proportion of layered double hydroxide having a particle size of 10 μm or more can be 0.0 vol% or more, preferably 0.90 vol% or less, more preferably 0.80 vol% or less, and even more preferably 0.50 vol% or less. If the proportion of coarse particles, for example, layered double hydroxide having a particle size of 10 μm or more, is within this range, the filterability of a resin composition containing the layered double hydroxide of the present disclosure can be improved.

[0027] After subjecting the layered double hydroxide of the present disclosure to the ultrasonic treatment, the particle size of the layered double hydroxide preferably ranges from 0.06 μm to 7 μm, and more preferably from 0.07 μm to 5 μm. By using such a particle size, it is possible to maintain good dispersibility in a resin, for example. The particle size of the layered double hydroxide preferably ranges from 7 μm or less, more preferably from 5 μm or less, and may also range from 0.06 μm or more, more preferably from 0.07 μm or more. In the present disclosure, when the particle size is distributed within a specific range, it means that the proportion of particles having particle sizes outside the specific range is preferably 10 vol% or less, more preferably 5 vol% or less, and even more preferably 1 vol% or less.

[0028] After the layered double hydroxide of the present disclosure is subjected to the ultrasonic treatment, the layered double hydroxide preferably has an average secondary particle size of 0.05 μm to 0.9 μm, more preferably 0.1 μm to 0.8 μm, and even more preferably 0.2 μm to 0.6 μm. The average secondary particle size of the layered double hydroxide is preferably 0.05 μm or more, more preferably 0.1 μm or more, and even more preferably 0.2 μm or more, and is preferably 0.9 μm or less, more preferably 0.8 μm or less, and even more preferably 0.6 μm or less. By setting the layered double hydroxide to such a particle size, it is possible to maintain good dispersibility in resin, for example.

[0029] In the present disclosure, the particle size after ultrasonic treatment can be measured by a laser diffraction / scattering method.

[0030] The layered double hydroxide is represented by the following formula (I): [M1 2+ ] 1-x [M2 3+ ] x (OH) 2 ](A n- ) x/n ・mH 2 O (I) In formula (I), M1 2+ represents one or more divalent metal ions. 3+represents one or more trivalent metal ions. n- represents one or more n-valent anions. m is 0 or more and less than 2. n is 1 or more and 5 or less. x is more than 0 and 0.6 or less.

[0031] M1 2+ represents one or more divalent metal ions. 2+ is Mg 2+ , Zn 2+ , Ca 2+ , Sr 2+ , Cu 2+ , Fe 2+ , Mn 2+ , Co 2+ , Ni 2+ , Sn 2+ , Pb 2+ , Cd 2+ and Ba 2+ Preferably, the material contains one or more selected from the group consisting of Mg 2+ , Zn 2+ , Cu 2+ , Fe 2+ , Mn 2+ , Co 2+ , Ni 2+ , and Cd 2+ More preferably, the composition contains one or more selected from the group consisting of Mg 2+ and Zn 2+ It is more preferable that the compound contains one or more selected from the group consisting of: 2+ However, the above metal ions, especially Mg 2+ and Zn 2+ By including one or more selected from the group consisting of: 2+ may contain two or more metal ions. 2+ consists of one type of metal ion.

[0032] M2 3+ represents one or more trivalent metal ions. 3+ is Al 3+ , Fe 3+ , Sc3+ , Y 3+ , Ti 3+ , Cr 3+ , Fe 3+ , Al 3+ , Ga 3+ , In 3+ and La 3+ Preferably, the compound contains one or more selected from the group consisting of Al 3+ and Fe 3+ It is more preferable that the compound contains one or more selected from the group consisting of Al 3+ It is more preferable that M2 3+ However, the above metal ions, especially Al 3+ and Fe 3+ By including one or more selected from the group consisting of: 3+ may contain two or more metal ions. 3+ consists of one type of metal ion.

[0033] Above A n- represents one or more n-valent anions, where n is 1 or more and 5 or less, preferably 1 or more and 3 or less, and more preferably 1 or more and 2 or less. x is more preferably greater than 0.15 and less than 0.35.

[0034] The n-valent anion preferably includes one or more selected from the group consisting of carbonate ion, chloride ion, nitrate ion, sulfate ion, phosphate ion, and bicarbonate ion, and more preferably includes one or more selected from carbonate ion, chloride ion, nitrate ion, and sulfate ion. In one embodiment, the n-valent anion may include carbonate ion.

[0035] The layered double hydroxide of the present disclosure is preferably coated with a higher fatty acid, which can improve the dispersibility of the layered double hydroxide in resins.

[0036] The higher fatty acid may be a saturated higher fatty acid or an unsaturated higher fatty acid. Examples of the higher fatty acid include saturated higher fatty acids such as lauric acid, myristic acid, palmitic acid, erucic acid, stearic acid, arachic acid, and behenic acid, and unsaturated higher fatty acids such as palmitoleic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, erucic acid, and ricinoleic acid. In one aspect, the higher fatty acid is preferably a saturated higher fatty acid, and more preferably stearic acid, erucic acid, palmitic acid, lauric acid, and behenic acid. As the saturated higher fatty acid, stearic acid is even more preferred. The higher fatty acid preferably includes a plant-derived higher fatty acid.

[0037] The proportion of the higher fatty acid is preferably 0.1% by mass or more and 10.0% by mass or less, more preferably 0.5% by mass or more and 8.0% by mass or less, and even more preferably 1.0% by mass or more and 5.0% by mass or less, based on 100% by mass of the total layered double hydroxide that has been surface-treated with the higher fatty acid. The proportion of the higher fatty acid is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, and even more preferably 1.0% by mass or more, based on 100% by mass of the total layered double hydroxide that has been surface-treated with the higher fatty acid, and is preferably 10.0% by mass or less, more preferably 8.0% by mass or less, and even more preferably 5.0% by mass or less.

[0038] The layered double hydroxide of the present disclosure is preferably coated with an organic acid or a derivative thereof. The organic acid or a derivative thereof can function as a crystal nucleating agent. By coating the layered double hydroxide with an organic acid or a derivative thereof, when the layered double hydroxide is mixed with a resin, the layered double hydroxide coated with the organic acid or a derivative thereof can have crystal nucleation ability. However, the higher fatty acid is different from the organic acid or a derivative thereof.

[0039] In the present disclosure, organic acid derivatives may include organic acids and / or derivatives of organic acids, and salts of organic acid derivatives may include salts of organic acids and / or salts of organic acid derivatives.

[0040] The organic acid derivative or its salt may be an N-substituted isocyanurate or a compound represented by the following formula (II): [In formula (II), A represents one selected from the group consisting of an alicyclic hydrocarbon group, an aromatic group, and a heteroaromatic group, and L represents a single bond or NR 12 represents -, R 1 represents a hydroxyl group, a carboxyl group, R 10 -OCO-, R 11 -CO-NR 12 -, NR 12 2 -, NR 12 2 -CO-, C 1-6 R represents one or more groups selected from the group consisting of an alkyl group, a hydroxyphosphoryl group, a heterocyclic group, and an aryl group; 2 represents one atom selected from the group consisting of a carbon atom, a phosphorus atom, and a sulfur atom; R 3 represents a hydroxy group when L is a single bond, and represents C when L is -NH-. 1-6 represents an alkyl group, R 4 is R 2 is a phosphorus atom, a hydroxy group or C 1-6 represents an alkyl group, and R 1 When is a sulfur atom, R 2 represents an oxygen atom forming a double bond with R 10 is C 1-6 represents an alkyl group, R 11 represents an aryl group; R 12 is C 1-6 represents an alkyl group or a hydrogen atom, n1 represents an integer of 0 to 5, n2 is 0 or 1, and n3 represents an integer of 1 to 3.], derivatives thereof, and salts thereof.

[0041] The above formula (II) is preferably the following formula (III): [In formula (III), R 1 , R 2 , R 4 , A, n1 and n2 are as defined above.]

[0042] The above A represents one selected from the group consisting of an alicyclic hydrocarbon group, an aromatic group, and a heterocyclic group. A is an n1+n3-valent group, preferably a monovalent to tetravalent group, and more preferably a monovalent to trivalent group.

[0043] The alicyclic hydrocarbon group represented by A is preferably C 3-8 Alicyclic hydrocarbon groups are preferred. Specific examples of the alicyclic hydrocarbon groups include a norbornane ring group, a norbornene ring group, a cyclobutane ring group, a cyclopentane ring group, a cyclohexane ring group, and a cycloheptane ring group.

[0044] The aromatic group represented by A is C 6-20 Aromatic groups are preferred, C 6-10 Aromatic groups are more preferred. Specific examples of the aromatic groups include benzene ring groups and naphthalene ring groups.

[0045] The heterocyclic group represented by A includes C 3-10 Heterocyclic groups are preferred, and C 3-5 Heterocyclic groups are more preferred. Examples of the heterocyclic groups include a tetrahydrofuran ring group, a tetrahydrothiophene ring group, an azole ring group, a furan ring group, a thiophene ring group, a piperidine ring group, and a pyridine ring group.

[0046] A is preferably an alicyclic hydrocarbon group, and C 3-8 Alicyclic hydrocarbon groups are more preferred.

[0047] L is a single bond or NR 12 In one embodiment, L is a single bond. In another embodiment, L is -NR 12 - is.

[0048] R 1 represents a hydroxyl group, a carboxyl group, R 10 -OCO-, R 10 -COO-, R 11 -CO-NR 12 -, NR 12 2 -, NR 12 2 -CO-, C 1-6It represents one or more groups selected from the group consisting of an alkyl group, a hydroxyphosphoryl group, a heterocyclic group and an aryl group, and may preferably be a carboxy group.

[0049] R 2 represents one or more atoms selected from the group consisting of carbon atoms, phosphorus atoms and sulfur atoms, and may preferably be carbon atoms.

[0050] R 3 represents a hydroxy group when L is a single bond, and represents C when L is -NH-. 1-6 In one embodiment, R 3 is a hydroxy group. 3 is C 1-6 It is an alkyl group.

[0051] R 4 is R 2 is a phosphorus atom, a hydroxy group or C 1-6 represents an alkyl group, and R 1 When is a sulfur atom, R 2 represents an oxygen atom forming a double bond with R. 2 is a carbon atom, R 4 is not present. In some embodiments, R 4 is a hydroxy group or C 1-6 In another embodiment, R 4 is R 2 represents an oxygen atom forming a double bond with

[0052] The above R 1 , R 3 , R 4 , R 10 , R 12 C represented by 1-6 The alkyl group is preferably C 1-3 It may be an alkyl group.

[0053] The above R 11 The aryl group represented by the formula: 6-20 An aryl group is preferred, and C 6-10 An aryl group is more preferred. Specific examples of the aryl group include a phenyl group and a naphthyl group.

[0054] R 12 is C 1-6 represents an alkyl group or a hydrogen atom. 12 is C 1-6 In another embodiment, R 12 is a hydrogen atom.

[0055] n1 represents an integer of 0 to 5, preferably an integer of 0 to 2.

[0056] n2 is 0 or 1. In some embodiments, n2 is 0. In other embodiments, n2 is 1.

[0057] n3 represents an integer of 1 to 3, preferably 1.

[0058] The N-substituted isocyanurate may include 1,3,5-triazine-2,4,6-triol.

[0059] As the organic acid derivative, a compound represented by the formula (II) is preferred, a compound represented by the formula (III) is more preferred, and C 1-12 Aliphatic monocarboxylic acids, C 1-12 Aliphatic dicarboxylic acids, C 1-12 Aromatic monocarboxylic acids, C 1-12 Aromatic dicarboxylic acids, C 1-12 Alkyl sulfonyl hydroxide, C 1-12 Alkylphosphonic acid, C 1-12 Alkylphosphonates, C 3-8 Cycloalkane monocarboxylic acid, C 3-8 Cycloalkanedicarboxylic acids and C 3-8 More preferably, the carboxylic acid is one or more selected from the group consisting of cycloalkanetricarboxylic acids, 1-12 Aliphatic dicarboxylic acids, C 1-12 Aromatic dicarboxylic acids and C 3-8 Cycloalkanedicarboxylic acids are even more preferred, C 3-8 Cycloalkanedicarboxylic acids are particularly preferred.

[0060] That is, the organic acid derivative or salt thereof may be one or more selected from an organic acid, a counter anion of the organic acid (i.e., a deprotonated anion of the organic acid), an amide, an ester, a thioester, a phosphate, and an anhydride. The organic acid derivative or salt thereof may further be a salt of the counter anion, amide, ester, or thioester. The salt may be preferably an alkali metal salt, more preferably a sodium salt.

[0061] The organic acid or its derivative is preferably bicyclo[2.2.1]heptane-2,3-dicarboxylic acid, cis-1,2-cyclohexanedicarboxylic acid, (1R,2S)-2-methoxycarbonylcyclohexanecarboxylic acid, 1,3,5-tris(2,2-dimethylpropionylamino)benzene, 2,6-naphthalenedicarboxylic acid, benzoic acid, pimelic acid, phenylphosphonic acid, 2,6-dihydroxypyrimidine-4-carboxylic acid, 4-pyridinecarboxylic acid, benzene-1,3,5-tricarboxylic acid, 4-(benzoylamino) Examples of the organic acid or its derivative include benzoic acid, disodium malonate, sodium acetate, 1-octanesulfonic acid, 2,3-pyridinedicarboxylic acid, 2-carboxyethyl(phenyl)phosphinic acid, 2-naphthalenecarboxylic acid, 2-tert-butylbenzoic acid, 4-aminobenzoic acid, 4-biphenylcarboxylic acid, 4-toluenesulfonic acid, bis(2-ethylhexyl)hydrogenphosphate, butylphosphonic acid, 4-phthalimidobenzoic acid, 4-tert-butylbenzoic acid, 1,4-cyclohexanedicarboxylic acid, and / or 4-propylcyclohexanecarboxylic acid. More preferred examples of the organic acid or its derivative include bicyclo[2.2.1]heptane-2,3-dicarboxylic acid, cis-1,2-cyclohexanedicarboxylic acid, pimelic acid, phenylphosphonic acid, 2,6-naphthalenedicarboxylic acid, and 1,4-cyclohexanedicarboxylic acid and / or 4-propylcyclohexanecarboxylic acid. As the organic acid or its derivative, cis-1,2-cyclohexanedicarboxylic acid is particularly preferred.

[0062] By including the above-mentioned compound, particularly cis-1,2-cyclohexanedicarboxylic acid, as the organic acid or its derivative, it is believed that the compound is more likely to be present on the surface of the base layer of the metal hydroxide. As a result, it is believed that the functionality of the layered double hydroxide, such as its anion-trapping ability, is more likely to be maintained. This point can also be confirmed by the fact that, in X-ray diffraction measurements, there is no difference in the peak positions observed in the 2θ range of 22° to 24° when comparing layered double hydroxides coated with an organic acid or its derivative and uncoated layered double hydroxide.

[0063] The adhesion ratio of the organic acid or its derivative to the layered double hydroxide is preferably 1% by mass or more, more preferably 1.3% by mass or more, even more preferably 1.6% by mass or more, and preferably 20% by mass or less, more preferably 15% by mass or less, and even more preferably 10% by mass or less. The adhesion ratio of the organic acid or its derivative to the layered double hydroxide is preferably 1% by mass or more and 20% by mass or less, more preferably 1.3% by mass or more and 15% by mass or less, and even more preferably 1.6% by mass or more and 10% by mass or less. When the adhesion ratio of the organic acid or its derivative to the layered double hydroxide is within this range, stability and crystal nucleation ability can be improved. The adhesion ratio of the organic acid or its derivative to the layered double hydroxide can be understood as the amount of the organic acid derivative or its salt attached to the layered double hydroxide in the composite. The organic acid derivative or its salt may form a salt with an element in the layered double hydroxide. For example, an organic acid derivative may form a salt with a metal element dissolved from the layered double hydroxide, and the salt may be attached to the layered double hydroxide. Such an embodiment is also included in the technical scope of the present disclosure.

[0064] The adhesion rate can be measured by the following method. [Method for measuring adhesion rate] 5 mL of 1 mol / L hydrochloric acid is added to 0.1 g of layered double hydroxide coated with an organic acid or its derivative, and the mixture is stirred at 60°C for 4 hours. 5 mL of methanol is added to the stirred solution. This solution is diluted with phosphate buffer (pH 2). The diluted solution is subjected to high performance liquid chromatography (HPLC) under the following conditions to determine the amount of organic acid derivative adhesion, m 1The amount of treatment m is determined from an external calibration curve created using an organic acid derivative solution of known concentration. 1 The amount of layered double hydroxide in the composite, m 0 Based on this, adhesion rate = m 1 / m 0 Column: C18 reverse phase column Column temperature: 35°C Mobile phase: 20% acetonitrile, 80% phosphate buffer (pH 2), flow rate 1.0 mL / min Detector: UV (225 nm)

[0065] The BET specific surface area of ​​the layered double hydroxide is preferably 3 m 2 / g or more 50m 2 / g or less, more preferably 4m 2 / g or more 45m 2 / g or less, more preferably 5m 2 / g or more 30m 2 The BET specific surface area of ​​the layered double hydroxide is preferably 3 m / g or less. 2 / g or more, more preferably 4m 2 / g or more, more preferably 5m 2 / g or more, preferably 50m 2 / g or less, more preferably 45m 2 / g or less, more preferably 30m 2 / g or less. When the BET specific surface area is within the above range, it is believed that the acid-accepting effect can be improved compared to when it is lower than the above range. Furthermore, when the BET specific surface area is within the above range, it is believed that the reaction of an antioxidant that may be contained in the resin is suppressed, and coloration is more likely to be suppressed during kneading and molding compared to when it is higher than the above range. In the present disclosure, the BET specific surface area can be measured by the BET method using nitrogen gas as the adsorbate.

[0066] The layered double hydroxide of the present disclosure is preferably in the form of particles, and more preferably in the form of flat particles. The average secondary particle diameter of the layered double hydroxide of the present disclosure is preferably 0.05 μm or more and 5 μm or less, more preferably 0.1 μm or more and 2 μm or less, and even more preferably 0.2 μm or more and 1.5 μm or less. The average secondary particle diameter of the layered double hydroxide is preferably 0.05 μm or more, more preferably 0.1 μm or more, even more preferably 0.2 μm or more, and preferably 5 μm or less, more preferably 2 μm or less, and even more preferably 1.5 μm or less. When the average secondary particle diameter of the layered double hydroxide is within this range, the layered double hydroxide of the present disclosure can have good dispersibility when mixed with a resin. The average secondary particle diameter of the layered double hydroxide means the cumulative 50% volume diameter, i.e., D50, and can be measured by a laser diffraction / scattering method. The average secondary particle size of the layered double hydroxide is preferably measured after dispersing the layered double hydroxide in an aqueous sodium hexametaphosphate solution and irradiating it with ultrasonic waves at an intensity of 40 mμA for 3 minutes.

[0067] The average aspect ratio of the layered double hydroxide of the present disclosure may be preferably 1.5 or more and 15 or less, more preferably 2 or more and 10 or less, and even more preferably 2 or more and 7 or less. The average aspect ratio of the layered double hydroxide is preferably 1.5 or more, more preferably 2 or more, and preferably 15 or less, more preferably 10 or less, and even more preferably 7 or less. When the average aspect ratio of the layered double hydroxide is within this range, it is believed that the layered double hydroxide will have good dispersibility in the resin and good orientation in the resin.

[0068] In the present disclosure, the average aspect ratio refers to the average value of the aspect ratios of layered double hydroxides. By evaluating the average aspect ratio rather than the aspect ratio of a single layered double hydroxide, it becomes easier to more accurately evaluate the properties of the layered double hydroxide as an aggregate.

[0069] The average diameter of the layered double hydroxide of the present disclosure may be preferably 0.05 μm or more and 5 μm or less, more preferably 0.1 μm or more and 3 μm or less, and even more preferably 0.2 μm or more and 2 μm or less. The average diameter of the layered double hydroxide is preferably 0.05 μm or more, more preferably 0.1 μm or more, and even more preferably 0.2 μm or more, and preferably 5 μm or less, more preferably 3 μm or less, and even more preferably 2 μm or less. It is believed that when the average diameter of the layered double hydroxide is within this range, it will have good dispersibility in the resin and good orientation in the resin.

[0070] The average thickness of the layered double hydroxide of the present disclosure is preferably 10 nm or more and 500 nm or less, more preferably 20 nm or more and 400 nm or less, and even more preferably 50 nm or more and 300 nm or less. The average thickness of the layered double hydroxide is preferably 10 nm or more, more preferably 20 nm or more, and even more preferably 50 nm or more, and is preferably 500 nm or less, more preferably 400 nm or less, and even more preferably 300 nm or less. It is believed that when the average thickness of the layered double hydroxide is within this range, it will have good dispersibility in the resin and good orientation in the resin.

[0071] The average aspect ratio, average diameter, and average thickness can be observed using a scanning electron microscope. In a specific embodiment, they can be measured, for example, by the following method. [Method for Measuring Average Aspect Ratio, Average Diameter, and Average Thickness] Layered double hydroxide is ultrasonicated in alcohol for 1 minute. The structure of the layered double hydroxide primary particles is then observed using a scanning electron microscope (SEM) or a transmission electron microscope (TEM), and the diameter and thickness are measured. The diameter is calculated as the average of the longest diameters of the layered double hydroxide primary particles observed at a magnification of 5,000x or 10,000x. The average diameter is calculated as the arithmetic mean of the diameters measured for 20 randomly selected layered double hydroxide primary particles. The thickness is calculated by observing the particles at a magnification of 100,000x and measuring the thicknesses of 14 randomly selected layered double hydroxide primary particles, and the arithmetic mean of the measured values ​​is calculated as the average thickness. The average aspect ratio is calculated by dividing the average diameter by the average thickness.

[0072] The layered double hydroxide can be produced by a production method including the steps of: mixing an aqueous solution of a water-soluble metal salt of a divalent metal, an aqueous solution of a water-soluble metal salt of a trivalent metal, and an alkali metal hydroxide in a dispersion medium to form a mixed solution; coprecipitating the mixed solution to obtain a coprecipitate; mixing the coprecipitate with an aqueous solution of an alkali metal carbonate to obtain a slurry containing a layered double hydroxide precursor; and aging the slurry containing the layered double hydroxide precursor.

[0073] The water-soluble metal salt of the divalent metal may be used as a water-soluble metal salt or as a hydrate. The divalent metal in the water-soluble metal salt of the divalent metal preferably contains one or more selected from the group consisting of Mg, Zn, Ca, Sr, Cu, Fe, Mn, Co, Ni, Sn, Pb, Cd, and Ba, more preferably contains one or more selected from the group consisting of Mg, Zn, Cu, Fe, Mn, Co, Ni, and Cd, and even more preferably contains one or more selected from the group consisting of Mg and Zn. The water-soluble metal salt of the divalent metal preferably contains a chloride of the divalent metal.

[0074] As the water-soluble metal salt of the divalent metal, for example, magnesium chloride can be used.

[0075] The trivalent metal in the water-soluble metal salt of a trivalent metal preferably contains one or more selected from the group consisting of Al, Fe, Sc, Y, Ti, Cr, Fe, Al, Ga, In, and La, more preferably contains one or more selected from the group consisting of Al and Fe, and even more preferably contains Al. The water-soluble metal salt of a trivalent metal may be in either an acidic or alkaline solution.

[0076] As the water-soluble metal salt of the trivalent metal, for example, aluminum sulfate can be used.

[0077] As the alkali metal hydroxide, for example, sodium hydroxide can be used.

[0078] As the alkali metal carbonate, for example, sodium carbonate can be used.

[0079] The dispersion medium includes water and hydrophilic organic solvents, such as alcohol solvents such as methanol, ethanol, propanol, and ethylene glycol.

[0080] The method for mixing the aqueous solution of a water-soluble metal salt of a divalent metal, the aqueous solution of a water-soluble metal salt of a trivalent metal, or the alkali metal hydroxide with the dispersion medium is not particularly limited, and can typically be carried out by stirring.

[0081] The layered double hydroxide precursor may be washed with water before being subjected to the aging treatment. This is thought to remove by-products such as salts and impurities such as residual sodium carbonate, making it easier to obtain the layered double hydroxide of the present disclosure by the aging treatment. If water washing is performed, the mixture of water and the layered double hydroxide precursor after water washing can be used as a slurry in the subsequent step.

[0082] The aging treatment promotes crystal growth of the layered double hydroxide precursor, allowing the layered double hydroxide to be obtained. The aging treatment is typically carried out by hydrothermal treatment using an autoclave. The temperature of the hydrothermal treatment is preferably 100°C or higher, more preferably 120 to 200°C, and the time of the hydrothermal treatment is preferably 1 hour or longer, more preferably 1 to 20 hours, and even more preferably 5 to 15 hours.

[0083] After the aging treatment, dehydration, drying, pulverization and classification may be carried out as necessary.

[0084] The layered double hydroxides can be preferably used as additives for resins. In a preferred embodiment, the layered double hydroxides can be preferably used as acid acceptors and thermal stabilizers. Because the layered double hydroxides are easily crushed when kneaded with resins, resin compositions containing the layered double hydroxides have good filterability. Therefore, resin additives containing the layered double hydroxides of the present disclosure are also within the technical scope of the present disclosure.

[0085] The technical scope of the present disclosure also includes a resin composition containing the layered double hydroxide and a resin, and a method for producing a resin composition by mixing the layered double hydroxide and a resin.

[0086] Examples of the resin include polyolefin resin, polyvinyl chloride resin, polyvinyl alcohol, polylactic acid, and polyphenylene sulfide resin, and the polyolefin resin is preferably used. Examples of the polyolefin resin include polypropylene and polyethylene. Examples of the polyethylene include HDPE, LDPE, and LLDPE.

[0087] The content of the layered double hydroxide of the present disclosure in the resin composition is preferably 1 ppm by mass or more, more preferably 1 ppm by mass or more and 10,000 ppm by mass or less, even more preferably 50 ppm by mass or more and 5,000 ppm by mass or less, even more preferably 100 ppm by mass or more and 5,000 ppm by mass or less, and even more preferably 100 ppm by mass or more and 3,000 ppm by mass or less, based on the total amount of the resin composition. The content of the composite of the present disclosure in the resin composition is preferably 1 ppm by mass or more, more preferably 50 ppm by mass or more, even more preferably 100 ppm by mass or more, and is preferably 10,000 ppm by mass or less, more preferably 5,000 ppm by mass or less, and even more preferably 3,000 ppm by mass or less, based on the total amount of the resin composition. The content of the layered compound in the resin precursor is also referred to as concentration. When the concentration of the layered double hydroxide in the resin composition is within this range, the resin composition has good filterability.

[0088] The resin composition may further contain a solvent. Examples of such a solvent include water, an alcohol solvent, and an ester solvent. Examples of the alcohol solvent include ethanol and propanol. Examples of the ester solvent include ethyl acetate.

[0089] The resin composition of the present disclosure can be prepared by mixing a resin and a layered double hydroxide. The mixing method is not particularly limited, and a mixing method appropriate for the properties of the resin can be used. A method may be used in which a resin and a high-concentration layered double hydroxide are first mixed to prepare a masterbatch, and then the masterbatch and resin are further mixed.

[0090] The layered double hydroxide, the resin additive containing the layered double hydroxide, and the method for producing the layered double hydroxide in one embodiment of the present disclosure have been described in detail above, but various modifications are possible. Note that the layered double hydroxide in the present disclosure may be produced by a method different from the production method in the above embodiment, and the method for producing the layered double hydroxide in the present disclosure is not limited to only those that provide the layered double hydroxide in the above embodiment.

[0091] When the layered double hydroxide of the present disclosure is mixed with a resin to form a resin composition, it can provide a resin composition with good filterability, and can be used as an additive for resins, preferably as an acid acceptor and a heat stabilizer.

[0092] The present invention will be explained in more detail with reference to the following examples, but the present invention is not limited to these examples.

[0093] Example 1 First, magnesium chloride hexahydrate and aluminum sulfate are dissolved in deionized water. This yields a composite metal salt aqueous solution with magnesium 0.753 mol / L and aluminum 0.35 mol / L. Meanwhile, sodium hydroxide is dissolved in deionized water to a concentration of 3.3 mol / L to prepare an alkali metal hydroxide aqueous solution. Furthermore, sodium carbonate is dissolved in deionized water to a concentration of 0.7 mol / L to prepare a sodium carbonate solution.

[0094] Next, the flow rates of the composite metal salt aqueous solution were set to 8 mL / min, the alkali metal hydroxide aqueous solution to 5.3 mL / min, and the sodium carbonate solution to 1.4 mL / min, and each was poured into a cylindrical reaction vessel with an overflow capacity of 215 mL. The reaction proceeded continuously to obtain a layered double hydroxide precursor. The suspension that overflowed the reaction vessel was collected as the overflow, and the flow rate of the alkali metal hydroxide aqueous solution was adjusted so that the pH was 9.35 to 9.45. During the reaction, the temperatures of the raw materials and the reaction vessel were adjusted so that the reaction temperature was 35°C.

[0095] The suspension is then dehydrated by suction filtration using a circular nutsche filter and a suction filter bottle to obtain a cake, and an aqueous solution of sodium carbonate in an amount of 0.7 equivalents relative to the aluminum of the layered double hydroxide precursor contained in the cake is then poured into the cake to carry out ion exchange.

[0096] Next, the ion-exchanged cake is washed with deionized water in an amount 30 times by mass the layered double hydroxide precursor in order to remove by-products such as salts and impurities such as residual sodium carbonate.

[0097] The cake after washing with water is resuspended in deionized water, and deionized water is added to adjust the concentration to 50 g / L. The suspension after the concentration adjustment is subjected to hydrothermal treatment at 170°C for 13 hours to obtain a layered double hydroxide.

[0098] A 1 mol / L aqueous solution of sodium hydroxide is added to stearic acid in an amount of 1 molar equivalent to the stearic acid to obtain a sodium stearate solution. The concentration of the sodium stearate solution is adjusted using deionized water so that the stearic acid concentration is 5 g / L.

[0099] The temperature of the suspension after the hydrothermal treatment is adjusted to 80°C, and the aqueous sodium stearate solution is poured into the suspension so that the amount of stearic acid is 3% by mass of the final product. After the addition of the aqueous sodium stearate solution, the mixture is stirred and maintained at 80°C for 30 minutes to perform a surface treatment of the layered double hydroxide, yielding a compound in which the layered double hydroxide is coated with stearic acid.

[0100] After the surface treatment of the layered double hydroxide, the suspension is cooled to room temperature and dehydrated using a circular nutsche filter and a suction filter bottle to obtain a cake. To remove impurities such as residual salts contained in the surface-treated cake, the cake is washed with deionized water in an amount 20 times the solid content of the reactants, and then dried in an oven at 105°C for 12 hours. This yields the layered double hydroxide of this embodiment.

[0101] Example 2

[0102] First, magnesium chloride hexahydrate is dissolved in deionized water. This results in a magnesium salt solution with a magnesium concentration of 1.025 mol / L. Sodium hydroxide is then dissolved in deionized water to a concentration of 3.3 mol / L to prepare an alkali metal hydroxide solution. Sodium carbonate is then dissolved in deionized water to a concentration of 0.7 mol / L to prepare a sodium carbonate solution. Sodium aluminate is then dissolved to obtain an aluminum salt solution with an aluminum concentration of 0.6 mol / L.

[0103] Next, the flow rates of the magnesium salt aqueous solution were set to 5.9 mL / min, the alkali metal hydroxide aqueous solution to 1.4 mL / min, the sodium carbonate solution to 2.8 mL / min, and the aluminum salt aqueous solution to 4.7 mL / min, and each was poured into a cylindrical reaction vessel with an overflow capacity of 215 mL. The reaction was carried out continuously to obtain a layered double hydroxide precursor. The suspension that overflowed from the reaction vessel was collected as the overflow, and the flow rate of the alkali metal hydroxide aqueous solution was adjusted so that the pH was 9.25 to 9.35. During the reaction, the temperatures of the raw materials and the reaction vessel were adjusted so that the reaction temperature was 35°C.

[0104] The suspension is then dehydrated by suction filtration using a circular nutsche filter and a suction filter bottle to obtain a cake, which is then washed with deionized water in an amount 30 times the mass of the layered double hydroxide precursor in order to remove impurities such as by-products, including salts.

[0105] The cake after washing with water is resuspended in deionized water, and deionized water is added to adjust the concentration to 50 g / L. The suspension after the concentration adjustment is subjected to hydrothermal treatment at 170°C for 13 hours to obtain a layered double hydroxide.

[0106] A 1 mol / L aqueous solution of sodium hydroxide is added to stearic acid in an amount of 1 molar equivalent to the stearic acid to obtain a sodium stearate solution. The concentration of the sodium stearate solution is adjusted using deionized water so that the stearic acid concentration is 5 g / L.

[0107] The temperature of the suspension after the hydrothermal treatment is adjusted to 80°C, and the above aqueous sodium stearate solution is poured into the suspension so that the amount of stearic acid becomes 3% by mass based on the final product. After pouring the aqueous sodium stearate solution, the suspension is kept at 80°C for 30 minutes with stirring.

[0108] After the surface treatment of the layered double hydroxide, the suspension is cooled to room temperature and dehydrated using a circular nutsche filter and a suction filter bottle to obtain a cake. To remove impurities such as residual salts contained in the surface-treated cake, the cake is washed with deionized water in an amount 20 times the solid content of the reactants, and then dried in an oven at 105°C for 12 hours. This produces the layered double hydroxide of this embodiment.

[0109] Comparative Example: 36.3 g of aluminum hydroxide was added to 0.7 mol of sodium hydroxide and heated to a solution, to which 40.3 g of magnesium oxide and 1.9 mol of sodium bicarbonate were added, followed by hydrothermal treatment at 170°C for 10 hours. The resulting suspension was dehydrated and washed, and dried in an oven at 105°C for 12 hours to obtain a white powder. A stearic acid ethanol solution was sprayed onto this white powder in an amount such that the stearic acid content was 3% by mass relative to the white powder, and the mixture was heated, dried, and then pulverized to obtain a layered double hydroxide.

[0110] [X-ray diffraction measurement] The layered double hydroxides obtained in the examples and comparative examples are wet-pulverized to a particle size of 0.5 μm to several μm. The wet-pulverized sample is then pressed against a sample spinner holder to harden it, and the sample is loaded from the back of the measurement surface. A back plate is then fitted into the sample spinner holder, and the sample is compressed using a sample adjustment jig. This yields a measurement sample. This allows for a measurement sample with a uniform sample surface height to be obtained. The measurement sample can be molded using a powder sample molding machine TK750 manufactured by Tokyo Chemical Industry Co., Ltd. as the XRD sample molding machine.

[0111] X-ray diffraction measurement was performed by powder X-ray diffraction using an X-ray diffractometer (EMPYREAN, manufactured by Malvern Panalytical). The results of the X-ray diffraction measurement are shown in Figures 1 and 2. The measurement conditions were as follows: X-ray source: CuKα radiation (λ = 1.54 Å), 2θ measurement interval: 0.026°, accumulation time: 296.565 seconds, acceleration voltage: 45 kV, acceleration current: 40 mA, focal length: 12.0 mm, take-off angle: 6°.

[0112] Next, the peak intensity I of the peak present in the 2θ range of 11.6° to 11.7° 1 and the peak intensity I of the peak present in the 2θ range of 34.8° or more and 34.9° or less. 2 and I 1 I 2 By dividing by the ratio I 1 / I 2 The results of the X-ray diffraction measurement are shown in Table 1.

[0113]

[0114] [Ultrasonic Treatment] 0.7 g of layered double hydroxide was mixed with 70 mL of a 0.002 g / mL aqueous solution of sodium hexametaphosphate to prepare a mixed solution with a layered double hydroxide concentration of 0.01 g / mL. This mixed solution was irradiated with ultrasound at an oscillation frequency of 19.5 kHz ± 1 kHz, an output of 70 W, and an intensity of 15 μmA or 20 mμA for 3 minutes.

[0115] [Measurement of particle size distribution after ultrasonic treatment] Using a laser diffraction / scattering particle size distribution measuring device MT3300EXII manufactured by Microtrac Bell Co., Ltd., the particle size distribution of the measurement sample after ultrasonic treatment is measured by the Microtrac method.

[0116] FIG. 3 shows the particle size distribution when ultrasonic treatment is performed at an intensity of 15 μmA, and FIG. 4 shows the particle size distribution when ultrasonic treatment is performed at an intensity of 20 mμA. As shown in FIG. 3, when the ultrasonic intensity is 15 μmA, there is no significant difference in the particle size distribution of the layered double hydroxides of Examples 1 and 2 and the Comparative Example. From FIG. 3, it appears that there is a peak of secondary particles near 0.5 μm in particle size, and a peak of undisintegrated secondary particles near 5 to 7 μm. On the other hand, as shown in FIG. 4, when the ultrasonic intensity is 20 mμA, the particle size of the layered double hydroxide of the Comparative Example is distributed in the range of 10 μm or more, while the particle size of the layered double hydroxides of Examples 1 and 2 is distributed in the range of 0.7 to 4 μm. This suggests that the disintegration behavior of each layered double hydroxide in response to different magnitudes of stress is unique to that layered double hydroxide. It can be said that the layered double hydroxide of the present disclosure is shown to be disintegrated into fine particles even when subjected to ultrasonic treatment at the minimum intensity at which secondary particles of the layered double hydroxide can be disintegrated.

[0117] Table 2 shows the results of measuring the particle size distribution when ultrasonic waves with an intensity of 20 mμA were irradiated.

[0118]

[0119] (Measurement of Filter Pressure) The resin composition was prepared by mixing a layered double hydroxide and a polypropylene resin in a twin-screw kneading extruder ("KZW15TW-45" manufactured by Nisshin Kikai Co., Ltd.) with an L / D ratio of 45 at a processing temperature of 250°C and a screw rotation speed of 200 Hz. As shown schematically in FIG. 6 , the layered double hydroxide and the polypropylene resin were fed into the twin-screw kneading extruder as raw material 10 from a hopper 11. The raw material 10 was heated by a heating cylinder 13 and a heater 14 and extruded by a screw 12 toward a filter 15. This resulted in the formation of a resin composition. The temperature at the extrusion port was 215°C, and the extrusion rate was 1.5 kg / h. A 1,400-mesh filter was used as the filter 15. The filter pressure was measured using a pressure sensor 16 attached to the twin-screw kneading extruder 1. The resin composition was prepared so that the layered double hydroxide was 500 ppm by mass relative to the total amount of resin. FIG. 5 shows the results of the filter pressure measurements.

[0120] Examples 1 and 2 correspond to examples of the present disclosure. In these examples, it was confirmed that the increase in filter pressure was suppressed and that the filter permeability was good.

[0121] The comparative example has an intensity ratio I 1 / I 2 is an example where the value is less than 10. In the comparative example, the increase in filter pressure is not sufficiently suppressed, and the filter permeability is not fully satisfactory.

[0122] When the layered double hydroxide of the present disclosure is mixed with a resin to form a resin composition, it can provide a resin composition with good filterability, and can be used as an additive for resins, preferably as an acid acceptor and a heat stabilizer.

[0123] REFERENCE SIGNS LIST 1 Twin-screw kneading extruder 10 Raw material 11 Hopper 12 Screw 13 Heating cylinder 14 Heater 15 Filter 16 Pressure sensor 17 Die 2 Cooling water tank 20 Strand 21 Drainer 3 Pelletizer

Claims

1. In X-ray diffraction measurement, the peak intensity I of the peak present in the 2θ range of 11.6° to 11.7° 1 and the peak intensity I of the peak present in the 2θ range of 34.8° or more and 34.9° or less. 2 Intensity ratio I 1 / I 2 is 10 or more.

2. The layered double hydroxide according to claim 1, wherein the proportion of layered double hydroxide having a particle size of 10 μm or more is 0.90 volume% or less of the total amount of layered double hydroxide after the following ultrasonic treatment: [Ultrasonic Treatment] 0.7 g of layered double hydroxide is mixed with 70 mL of a 0.002 g / mL aqueous solution of sodium hexametaphosphate to prepare a mixture so that the concentration of layered double hydroxide is 0.01 g / mL. This mixture is irradiated with ultrasonic waves at an oscillation frequency of 19.5 kHz ± 1 kHz, an output of 70 W, and an intensity of 20 mμA for 3 minutes.

3. The layered double hydroxide according to claim 2, wherein the average secondary particle size after the ultrasonic treatment is 0.9 μm or less.

4. The layered double hydroxide according to claim 1, which is coated with a higher fatty acid.

5. The layered double hydroxide according to claim 1, which is coated with an organic acid or a derivative thereof.

6. A resin additive comprising the layered double hydroxide according to any one of claims 1 to 5.

7. A resin composition comprising the layered double hydroxide according to any one of claims 1 to 5 and a resin, wherein the content of the layered double hydroxide is 100 ppm by mass or more and 5,000 ppm by mass or less based on the total amount of the resin composition.

8. The resin composition according to claim 7, wherein the resin comprises a polyolefin resin.

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