WO2009122681A1 - ハイドロタルサイト型化合物粒子粉末、該ハイドロタルサイト型化合物粒子粉末を用いた含塩素樹脂安定剤及び含塩素樹脂組成物 - Google Patents

ハイドロタルサイト型化合物粒子粉末、該ハイドロタルサイト型化合物粒子粉末を用いた含塩素樹脂安定剤及び含塩素樹脂組成物 Download PDF

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WO2009122681A1
WO2009122681A1 PCT/JP2009/001335 JP2009001335W WO2009122681A1 WO 2009122681 A1 WO2009122681 A1 WO 2009122681A1 JP 2009001335 W JP2009001335 W JP 2009001335W WO 2009122681 A1 WO2009122681 A1 WO 2009122681A1
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Prior art keywords
hydrotalcite
type compound
chlorine
resin composition
particle powder
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PCT/JP2009/001335
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English (en)
French (fr)
Japanese (ja)
Inventor
山本学武
小林斉也
本名虎之
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戸田工業株式会社
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Application filed by 戸田工業株式会社 filed Critical 戸田工業株式会社
Priority to CN200980111183.1A priority Critical patent/CN101980963B/zh
Publication of WO2009122681A1 publication Critical patent/WO2009122681A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/78—Compounds containing aluminium, with or without oxygen or hydrogen, and containing two or more other elements
    • C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/78—Compounds containing aluminium, with or without oxygen or hydrogen, and containing two or more other elements
    • C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
    • C01F7/785—Hydrotalcite
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/20—Two-dimensional structures
    • C01P2002/22—Two-dimensional structures layered hydroxide-type, e.g. of the hydrotalcite-type
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

Definitions

  • the present invention can suppress a decrease in electrical insulation derived from hydrotalcite-type compound particle powder, and has excellent thermal stability of the chlorine-containing resin, and can suppress resin coloring. It is.
  • Hydrotalcite is generally a layered compound represented by Mg 6 Al 2 (OH) 16 CO 3 .4H 2 O, and CO 3 , H 2 O, OH ⁇ are inserted between layers of Mg—Al.
  • Mg 2+ in the structure can be replaced with divalent cations such as Ni 2+ , Zn 2+ , Sr 2+ and Ca 2+
  • Al 3+ can be replaced with Fe 3+ , Cr 3+, etc. It can be replaced with a trivalent cation.
  • CO 3 2 ⁇ can also be exchanged for anions such as SO 4 2+ and Cl ⁇ .
  • the structure can be maintained even when the molar ratio of divalent and trivalent cations is changed, and a layered structure can be formed in a molar ratio of 2 to 4.
  • Layered compounds in which the composition of these constituent elements and the ratio of divalent and trivalent cations are changed are generally called hydrotalcite compounds.
  • stabilizers for wire coating applications are rapidly changing to those containing hydrotalcite type compounds.
  • hydrotalcite-type compounds are used as stabilizers for wire coating applications, the electrical resistance tends to decrease, and it can be used for low-voltage wires.
  • Pb-based stabilizers with high electrical insulation are still used.
  • Hydrotalcite-type compound particles contain trace amounts of impurity ions such as sulfate ions and sodium ions in the structure and in the vicinity of the surface, and are considered to be a cause of lowering electrical insulation. These ions are also a cause of deterioration of resin coloring and thermal stability.
  • the present invention is Mg-Al-based or Mg-Zn-Al-based hydrotalcite-type compound particle powder characterized in that the total value of soluble anions is 70 ppm or less (Invention 1).
  • a chlorine-containing resin stabilizer for stabilizing a chlorine-containing resin composition using the hydrotalcite-type compound particle powder according to the first or second aspect of the invention (Invention 3).
  • the step of washing is the production method according to the fifth aspect of the present invention, wherein the washing is performed with a dilute alkaline aqueous solution and then further washed with water (the seventh aspect of the present invention).
  • the manufacturing method according to the sixth aspect of the present invention wherein the temperature of the dilute alkaline aqueous solution and / or water used in the washing step is 30 to 90 ° C. (the present invention 8).
  • the resin can have high electrical insulation. Moreover, thermal stability and coloring can also be improved.
  • hydrotalcite-type compound particle powder according to the present invention will be described.
  • the hydrotalcite-type compound is composed of Mg, Al, Zn, etc., and is commonly used as Mg-Al type or Mg-Zn-Al. It is written as a system.
  • the composition of the hydrotalcite type compound particle powder according to the present invention is not particularly limited.
  • the generally known Mg / Al molar ratio is preferably 1.0 to 3.5
  • Mg— Zinc in the Al—Zn system is preferably in a molar ratio of 0.0010 to 0.30 with respect to the total number of moles of Mg and Al, and expressed as a Zn / Al molar ratio of about 0.005 to 0.5. preferable.
  • the total value of soluble anions (soluble sulfate ion, soluble nitrate ion and soluble chloride ion) contained in the hydrotalcite-type compound particle powder according to the present invention is 70 ppm or less. If the amount of these soluble anions is large, high electrical insulation cannot be obtained. In particular, bivalent sulfate ions have a greater adverse effect on electrical insulation than monovalent ions.
  • the soluble anion is preferably 60 ppm or less, more preferably 50 ppm or less. The lower limit is usually about 5 ppm.
  • the sodium contained in the hydrotalcite-type compound particle powder according to the present invention is preferably 700 ppm or less. If there is little sodium contained, possibility that the sodium which melt
  • Preferably sodium is 600 ppm or less, and even more preferably 550 ppm or less. In addition, a lower limit is about 20 ppm normally.
  • the specific surface area of the hydrotalcite-type compound particle powder according to the present invention is 5 to 150 m 2 / g. Hydrotalcite-type compound particles of less than 5 m 2 / g are difficult to obtain industrially. Even if it exceeds 150 m 2 / g, it is difficult to obtain industrially. It is preferably 7 to 100 m 2 / g, more preferably 8 to 50 m 2 / g.
  • the hydrotalcite type compound particle powder according to the present invention may contain about 0.01 to 5 wt% of calcium.
  • the hydrotalcite-type compound particle powder according to the present invention may contain about 0.01 to 8 wt% of zinc oxide.
  • the average plate surface diameter of the hydrotalcite-type compound particle powder according to the present invention is preferably 0.05 to 0.8 ⁇ m.
  • the hydrotalcite-type compound particle powder in the present invention is prepared by mixing an alkaline aqueous solution containing anions, a magnesium salt aqueous solution and an aluminum salt aqueous solution to obtain a mixed solution having a pH value in the range of 10 to 14, and then mixing the mixed solution.
  • the magnesium added to the aqueous suspension containing the core particles at the time of forming the core particles by aging in the temperature range of 80 to 105 ° C. to form core particles of Mg—Al hydrotalcite type particles.
  • the pH value is 10 to 14.
  • a core at normal pressure that is aged in the range of 60 to 105 ° C to obtain Mg-Al hydrotalcite-type particle powder Growth and reaction (JP-2002-293535) for the child, it is desirable to use a generated by 105 ⁇ 350 ° C. using an autoclave.
  • raw materials such as sulfate metal, nitrate metal, chloride salt metal, and metal oxide, alkali such as caustic soda and potassium hydroxide, sodium carbonate, basic magnesium carbonate, carbonate What is necessary is just to produce from anion source materials, such as potassium.
  • a slurry after the target hydrotalcite-type compound particles are generated and aged, or
  • the slurry after the treatment such as the hydrophobizing surface treatment is preferably adjusted to pH 9.5 to 12, more preferably 9.8 to 11.5.
  • anions such as sulfate ions are likely to be lowered by washing (water washing). Sodium tends to fall relatively easily with water washing, but soluble anions such as soluble sulfate ions, soluble nitrate ions and soluble chloride ions are difficult to reduce simply by washing.
  • washing with a thin alkaline aqueous solution first to reduce anions such as sulfate ions, and then washing with water further reduces the anions such as sulfate ions.
  • An alkaline aqueous solution such as sodium hydroxide or sodium carbonate may be used as the thin alkaline aqueous solution used for pH adjustment of the slurry containing the hydrotalcite-type particle powder and washing before washing with water.
  • the temperature of the thin alkaline aqueous solution and / or the thin alkaline aqueous solution and / or water used for washing is preferably 30 to 90 ° C.
  • the diffusion rate of ions is improved, and the viscosity of water is further lowered to enhance the washing effect. More preferably, it is 40 to 70 ° C.
  • the hydrotalcite-type compound particle powder obtained as described above is preferably basically dried at 105 to 150 ° C. At a drying temperature of less than 105 ° C., the resulting hydrotalcite-type compound particle powder has a large amount of water, so that foaming is likely to occur in the resin. When the temperature exceeds 150 ° C., the function of suppressing deterioration of the resin tends to decrease as a stabilizer for soft to semi-rigid chlorine-containing resin compositions. In the use of a soft to semi-rigid chlorine-containing resin composition as a stabilizer, the drying temperature is more preferably 105 to 130 ° C. The drying time may be as long as necessary depending on the amount of drying and the drying method. Preferably, it is 3 to 24 h.
  • the hydrotalcite-type compound particle powder of the present invention 1 or 2 can be used as a chlorine-containing resin stabilizer added to a chlorine-containing resin composition.
  • the chlorine-containing resin composition according to the present invention preferably contains 0.01 to 10 parts by weight of the hydrotalcite-type compound particle powder with respect to 100 parts by weight of the resin.
  • the content of the hydrotalcite-type compound particle powder is less than 0.01 parts by weight, the effect as a stabilizer is low.
  • the amount exceeds 10 parts by weight the effect is saturated, so there is no point in adding more than necessary.
  • foaming is likely to occur, which may have adverse effects such as poor appearance and initial coloration.
  • the resin may contain a plasticizer, other stabilizers and additives.
  • plasticizer examples include trioctyl ester plasticizers such as trioctyl trimellitate (TOTM) and tri-n-octyl-n-decyl trimellitate, diirodecyl phthalate (DIDP), diisononyl phthalate (DINP), di- Preferred are phthalate plasticizers such as -2-ethylhexyl phthalate (DOP), and polyester plasticizers such as polypropylene / adipate and polypropylene / sebacate.
  • TOTM trioctyl trimellitate
  • DIDP diirodecyl phthalate
  • DINP diisononyl phthalate
  • di- Preferred are phthalate plasticizers such as -2-ethylhexyl phthalate (DOP), and polyester plasticizers such as polypropylene / adipate and polypropylene / sebacate.
  • stabilizers include zinc compounds such as zinc stearate, zinc laurate, zinc ricinoleate, ⁇ -diketones such as dibenzoylmethane, stearoylbenzoylmethane, dehydroacetic acid, alkylallyl phosphates, trialkyl phosphates, etc. Phosphites, dipentaerythritol, pentaerythritol, polyhydric alcohol compounds such as glycerin, diglycerin, trimethylolpropane, higher fatty acids such as stearic acid, lauric acid, oleic acid, epoxidized linseed oil, epoxidized soybean oil, etc. Of these, epoxy compounds are preferred.
  • additives include phenolic compounds, amine compounds, phosphoric acid compounds and other antioxidants, polyesters with OH-terminated polyester, acrylonitrile-styrene copolymers, and methyl methacrylate styrene copolymers.
  • Accelerator extenders such as calcium carbonate, silica, glass beads, mica, glass fiber, inorganic flame retardants such as antimony trioxide, aluminum hydroxide, zinc borate, bromine-containing organic flame retardants, halogen phosphate ester-based flame retardants Flame retardants such as flame retardants, lubricants such as stearic acid, polyethylene wax, calcium stearate, magnesium stearate, barium stearate, anti-fungal agents such as triclosan, orthoside, sun isol 100, sun isol 300 and the like are used.
  • inorganic flame retardants such as antimony trioxide, aluminum hydroxide, zinc borate, bromine-containing organic flame retardants, halogen phosphate ester-based flame retardants
  • Flame retardants such as flame retardants, lubricants such as stearic acid, polyethylene wax, calcium stearate, magnesium stearate, barium stearate, anti-fungal agents such as triclosan, orthoside, sun is
  • hydrotalcite-type compound according to the present invention When used as a chlorine-containing resin composition, a higher fatty acid, an anionic surfactant, a higher fatty acid phosphate, a coupling agent, and a polyhydric alcohol ester are added to the hydrotalcite-type compound. It is preferable to perform at least one surface treatment selected from By applying the surface treatment, a further stability of the chlorine-containing resin composition can be imparted.
  • Examples of the higher fatty acid include lauric acid, stearic acid, palmitic acid, oleic acid, and linoleic acid.
  • Examples of the higher fatty acid phosphate ester include stearyl ether phosphoric acid, oleyl ether phosphoric acid, and lauryl ether phosphoric acid.
  • Examples of the polyhydric alcohol ester include sorbitan monooleate, sorbitan monolaurate, and stearic acid monoglyceride.
  • anionic surfactant examples include salts such as sodium lauryl sulfate, sodium dodecylbenzenesulfonate, sodium stearate, potassium oleate, and potassium castor oil.
  • a silane-based, aluminum-based, titanium-based, zirconium-based coupling agent or the like can be used as the coupling agent.
  • the treatment method of the surface treatment agent is not particularly limited, but may be performed on the surface of the hydrotalcite type compound particles by a wet reaction.
  • the surface of the hydrotalcite compound particles may be subjected to a dry surface treatment using a Henschel mixer or the like.
  • the hydrotalcite type compound particles and the surface treatment agent may be simply mixed.
  • the hydrotalcite according to the present invention is a chlorine-containing resin composition having the following composition:
  • the type compound is used, 0.8 parts by weight of zinc stearate has a level 3 time of 65 minutes or more and a level 5 time of 100 minutes or more at the coloring level described later.
  • Chlorine-containing resin degree of polymerization 1000: Taiyo PVC TH1000 manufactured by Taiyo PVC Co., Ltd. 100 parts by weight Di-2-ethylhexyl phthalate (DOP manufactured by Daihachi Chemical) 0 to 25 parts by weight Hydrotalcite type compound particle powder 3.5 parts by weight Zinc stearate (general reagent) 0.6 to 0.9 parts by weight
  • the level 3 time is 65 minutes at the coloring level described later.
  • the level 5 time is 100 minutes or longer.
  • Chlorine-containing resin degree of polymerization 1000
  • Taiyo PVC TH1000 manufactured by Taiyo PVC Co., Ltd. 100 parts by weight Di-2-ethylhexyl phthalate (DOP manufactured by Daihachi Chemical) 40-80 parts by weight
  • Hydrotalcite compound of the present invention 3.0 parts by weight
  • Zinc stearate (general reagent) 0.6 parts by weight
  • the chlorine-containing resin composition according to the present invention preferably has a volume resistivity value of 2.0 ⁇ 10 14 ⁇ ⁇ cm or more, although it varies depending on the application.
  • the chlorine-containing resin composition according to the present invention can be obtained by an ordinary production method. For example, when obtaining a kneaded sheet, the resin, the hydrotalcite-type compound particle powder and the above various stabilizers and additives are added. It is obtained by mixing a predetermined amount, kneading the mixture with a hot roll to obtain a kneaded sheet, and then pressurizing with a hot press.
  • the kneading temperature of the hot roll varies depending on the resin and resin composition used, but is preferably 140 to 300 ° C.
  • the press temperature of the hot press is preferably 145 to 320 ° C.
  • the hydrotalcite-type compound particle powder according to the present invention was used as a resin stabilizer because it has a low content of soluble anions such as soluble sulfate ions, soluble nitrate ions and soluble chloride ions having electrical conductivity.
  • soluble anions such as soluble sulfate ions, soluble nitrate ions and soluble chloride ions having electrical conductivity.
  • a resin composition having high electrical insulation is obtained.
  • resin burning due to salt can be suppressed, and a resin composition having high thermal stability and suppressed coloring can be obtained.
  • a higher effect will be acquired.
  • a typical embodiment of the present invention is as follows.
  • the content of elements such as sodium, magnesium, aluminum, zinc, and calcium is obtained by dissolving a sample with an acid and analyzing it with a plasma emission spectroscopic analyzer (manufactured by Thermo Electron Co., Ltd., iCAP6500) using yttrium as an internal standard. It was.
  • the method for measuring soluble anions is described below. Disperse 5 g of sample in 40 ml of ethanol, add 100 ml of ultrapure water, shake in a sealed container for 1 minute, leave it at 22 ° C. for 20 hours, filter this slurry, and replenish ultrapure water. The filtrate was boiled for 60 minutes to evaporate ethanol, cooled, and the liquid volume was adjusted to 100 ml with ultrapure water. This was analyzed with an ion chromatograph (Toa DKK, ICA-2000) to measure sulfate ion, nitrate ion, and chloride ion, respectively.
  • ion chromatograph Toa DKK, ICA-2000
  • Specific surface area value is B. using nitrogen.
  • Resin roll kneading was carried out by adjusting the temperature to 140 to 190 ° C. according to the resin composition using a 6-inch two-piece type. The kneading time was 5 minutes.
  • the roll-kneaded sheet was formed into a compression molded body of 200 ⁇ 200 ⁇ 1 to 1.5 mm.
  • the heating press was a 70-ton automatic press (ram area 210 cm 2 )
  • the cooling press was a 30-ton manual press (ram area 180 cm 2 ).
  • the compression molding conditions were 140-190 ° C., preheating (no pressure) for 3 minutes, pressurizing (6.3 MPa) for 2 minutes, and cooling (3.1 MPa) for 3 minutes.
  • the thermal stability test was performed with a gear aging type tester (manufactured by Yasuda Seiki Seisakusho, 102-SHF-77S).
  • the pressed sheet was cut into 30 ⁇ 30 mm squares, placed on a glass plate, tested at 190 ° C. for 200 minutes, and taken out every 2 minutes / sample for 10 minutes. Pasted on paper.
  • the coloring levels of the press sheet and the thermal stability test piece are defined as 1 to 7 as follows.
  • Example 1 (Preparation of hydrotalcite-type compound particle powder) A slurry in which 26.9 g of magnesium oxide was dispersed in pure water and an aqueous solution of 81.0 g of aluminum sulfate octahydrate crystals were mixed with stirring. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 58.3 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into a slurry obtained by mixing the above magnesium oxide and aluminum sulfate octahydrate, heated to 80 ° C., and stirred at 80 ° C. for 5 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 175 ° C. for 4 hours.
  • reaction slurry was stirred and brought to 67 ° C., and the pH was adjusted to 10.3.
  • a solution prepared by dissolving 2.3 g of sodium palmitate in hot water (80 ° C.) was added. This was aged for 0.7 hours. After filtration, it was washed with 2 L of a thin caustic soda solution having a pH of 11.5 at 40 ° C., then washed with 15 L of 40 ° C. pure water, and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 11.0 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Example 2 (Preparation of hydrotalcite-type compound particle powder) 141.0 g of magnesium sulfate heptahydrate crystals, 41.5 g of zinc sulfate heptahydrate crystals and 69.4 g of aluminum sulfate octahydrate crystals were dissolved in pure water. Separately, 30.6 g of sodium carbonate crystals were dissolved in pure water, and 152.4 ml of caustic soda (12N) and pure water were further added.
  • This alkaline solution was put into an aqueous solution in which the magnesium sulfate heptahydrate crystals, zinc sulfate heptahydrate crystals and aluminum sulfate octahydrate were mixed, heated to 85 ° C., and stirred at 85 ° C. for 6 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 185 ° C. for 6 hours.
  • reaction slurry was stirred and brought to 65 ° C. to adjust the pH to 10.1.
  • a solution prepared by dissolving 2.5 g of sodium stearate in hot water (80 ° C.) was added. This was aged for 0.6 hours. After filtration, it was washed with 2 L of a thin aqueous solution of caustic soda having a pH of 11 at 50 ° C., then washed with 15 L of pure water at 50 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 10.0 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Example 3 (Preparation of hydrotalcite-type compound particle powder) 176.3 g of magnesium sulfate heptahydrate crystals and 69.4 g of aluminum sulfate octahydrate crystals were dissolved in pure water. Separately, 30.6 g of sodium carbonate crystals were dissolved in pure water, and 152.4 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution in which the magnesium sulfate heptahydrate crystal and aluminum sulfate octahydrate were mixed, heated to 90 ° C., and stirred at 90 ° C. for 10 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 145 ° C. for 6 hours.
  • reaction slurry was stirred and brought to 65 ° C., and the pH was adjusted to 11.2.
  • a solution prepared by dissolving 1.9 g of sodium laurate in hot water (80 ° C.) was added. This was aged for 0.8 hours. After filtration, it was washed with 2 L of a thin caustic soda solution having a pH of 12.5 at 45 ° C., then washed with 15 L of pure water at 45 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 9.0 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 20 phr Zinc stearate 0.8 phr Sample above 3.5phr
  • Example 4 (Preparation of hydrotalcite-type compound particle powder) Magnesium chloride hexahydrate crystal 101.9 g, zinc chloride monohydrate crystal 26.0 g crystal and aluminum chloride hexahydrate crystal 80.5 g were dissolved in pure water. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 136.1 ml of caustic soda (12N) and pure water were added. This alkaline solution was put into an aqueous solution obtained by mixing the above magnesium chloride hexahydrate crystal, zinc chloride monohydrate crystal and aluminum chloride hexahydrate, heated to 95 ° C., and stirred at 95 ° C. for 8 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 165 ° C. for 7 hours.
  • reaction slurry was stirred and brought to 70 ° C., and the pH was adjusted to 9.9.
  • a solution prepared by dissolving 2.5 g of sodium palmitate in hot water (80 ° C.) was added. This was aged for 0.7 hours. After filtration, it was washed with 2 L of an aqueous solution of thin caustic soda having a pH of 11 at 45 ° C., then washed with 16 L of pure water at 45 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 10.2 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Example 5 (Preparation of hydrotalcite-type compound particle powder) Magnesium chloride hexahydrate crystals 141.0 g and aluminum chloride hexahydrate crystals 74.3 g were dissolved in pure water. Separately, 32.9 g of sodium carbonate crystals were dissolved in pure water, and 163.5 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution in which the magnesium chloride hexahydrate crystals and aluminum chloride hexahydrate were mixed, heated to 75 ° C., and stirred at 75 ° C. for 15 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 170 ° C. for 9 hours.
  • reaction slurry was stirred and brought to 70 ° C., and the pH was adjusted to 10.9.
  • a solution prepared by dissolving 2.0 g of sodium laurate in hot water (80 ° C.) was added. This was aged for 0.9 hours. After filtration, it was washed with 2 L of an aqueous solution of thin caustic soda having a pH of 12 at 40 ° C., then washed with 15 L of pure water at 40 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 10.4 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Example 6 (Preparation of hydrotalcite-type compound particle powder) 149.8 g of magnesium nitrate hexahydrate crystals, 25.0 g of zinc nitrate hexahydrate crystals and 125.0 g of aluminum nitrate 9 hydrate crystals were dissolved in pure water. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 126.4 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution obtained by mixing the above magnesium nitrate hexahydrate crystal, zinc nitrate hexahydrate crystal and aluminum nitrate nonahydrate, heated to 90 ° C., and stirred at 90 ° C. for 10 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 175 ° C. for 8 hours.
  • reaction slurry was stirred and brought to 62 ° C., and the pH was adjusted to 10.0.
  • a solution prepared by dissolving 2.5 g of sodium stearate in hot water (80 ° C.) was added. This was aged for 0.6 hours. After filtration, it was washed with 2 L of a thin caustic soda solution having a pH of 11.5 at 45 ° C., then washed with 15 L of pure water at 45 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 9.8 m 2 / g.
  • Chlorine-containing resin composition 100phr TOTM 60phr Zinc stearate 0.7 phr Sample above 3.3 phr
  • Example 7 (Preparation of hydrotalcite-type compound particle powder) 171.2 g of magnesium nitrate hexahydrate crystals and 125.0 g of aluminum nitrate 9 hydrate crystals were dissolved in pure water. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 126.4 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution in which the magnesium nitrate hexahydrate crystal and the aluminum nitrate nonahydrate were mixed, heated to 90 ° C., and stirred at 90 ° C. for 10 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 130 ° C. for 5 hours.
  • reaction slurry was stirred and brought to 62 ° C., and the pH was adjusted to 10.0.
  • a solution prepared by dissolving 2.5 g of sodium stearate in hot water (80 ° C.) was added. This was aged for 0.6 hours. After filtration, it was washed with 3 L of a thin caustic soda solution having a pH of 11 at 60 ° C., then washed with 25 L of pure water at 60 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 19.2 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Example 8 (Preparation of hydrotalcite-type compound particle powder) 176.3 g of magnesium sulfate heptahydrate crystals and 69.4 g of aluminum sulfate octahydrate crystals were dissolved in pure water. Separately, 30.6 g of sodium carbonate crystals were dissolved in pure water, and 152.4 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution in which the magnesium sulfate heptahydrate crystal and aluminum sulfate octahydrate were mixed, heated to 90 ° C., and stirred at 90 ° C. for 10 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 145 ° C. for 6 hours.
  • reaction slurry was stirred and brought to 65 ° C., and the pH was adjusted to 11.9.
  • a solution prepared by dissolving 1.9 g of sodium laurate in hot water (80 ° C.) was added. This was aged for 0.8 hours. After filtration, it was washed with 2 L of a thin caustic soda solution having a pH of 13 at 40 ° C., then washed with 15 L of pure water at 45 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 9.3 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 20 phr Zinc stearate 0.8 phr Sample above 3.5phr
  • Example 9 (Preparation of hydrotalcite-type compound particle powder) Magnesium chloride hexahydrate crystal 101.9 g, zinc chloride monohydrate crystal 26.0 g crystal and aluminum chloride hexahydrate crystal 80.5 g were dissolved in pure water. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 136.1 ml of caustic soda (12N) and pure water were added. This alkaline solution was put into an aqueous solution obtained by mixing the above magnesium chloride hexahydrate crystal, zinc chloride monohydrate crystal and aluminum chloride hexahydrate, heated to 95 ° C., and stirred at 95 ° C. for 8 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 165 ° C. for 7 hours.
  • reaction slurry was stirred and brought to 70 ° C., and the pH was adjusted to 11.7.
  • a solution prepared by dissolving 2.5 g of sodium palmitate in hot water (80 ° C.) was added. This was aged for 0.7 hours. After filtration, it was washed with 2 L of a thin caustic soda solution having a pH of 13 at 55 ° C., then washed with 16 L of pure water at 45 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 10.1 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Example 10 (Preparation of hydrotalcite-type compound particle powder) Magnesium chloride hexahydrate crystals 141.0 g and aluminum chloride hexahydrate crystals 74.3 g were dissolved in pure water. Separately, 32.9 g of sodium carbonate crystals were dissolved in pure water, and 203.5 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution in which magnesium chloride hexahydrate crystals and aluminum chloride hexahydrate were mixed, and then an aqueous solution in which 4.50 g of calcium chloride dihydrate crystals were dissolved was added, and the temperature was raised to 75 ° C. did. Stir at 75 ° C. for 15 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 170 ° C. for 9 hours.
  • reaction slurry was stirred and brought to 70 ° C., and the pH was adjusted to 10.9.
  • a solution prepared by dissolving 2.0 g of sodium laurate in hot water (80 ° C.) was added. This was aged for 0.9 hours. After filtration, it was washed with 2 L of an aqueous solution of thin caustic soda having a pH of 12 at 40 ° C., then washed with 15 L of pure water at 40 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 10.0 m 2 / g.
  • the molar ratio of Mg / Ca / Al was 2.40 / 0.10 / 1.00.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Example 11 (Preparation of hydrotalcite-type compound particle powder) 101.9 g of magnesium chloride hexahydrate crystals, 23.4 g of zinc chloride monohydrate crystals and 80.5 g of aluminum chloride hexahydrate crystals were dissolved in pure water. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 136.1 ml of caustic soda (12N) and pure water were added. This alkaline solution was put into an aqueous solution obtained by mixing the above magnesium chloride hexahydrate crystal, zinc chloride monohydrate crystal and aluminum chloride hexahydrate, heated to 95 ° C., and stirred at 95 ° C. for 8 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 165 ° C. for 7 hours. Thereafter, 1.4 g of zinc oxide was added and mixed.
  • reaction slurry was stirred and brought to 70 ° C., and the pH was adjusted to 11.7.
  • a solution prepared by dissolving 2.5 g of sodium palmitate in hot water (80 ° C.) was added. This was aged for 0.7 hours. After filtration, it was washed with 2 L of a thin aqueous solution of caustic soda having a pH of 12.5 at 45 ° C., then washed with 16 L of pure water at 45 ° C., and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 10.7 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Comparative Example 1 (Preparation of hydrotalcite-type compound particle powder) A slurry in which 26.9 g of magnesium oxide was dispersed in pure water and an aqueous solution of 81.0 g of aluminum sulfate octahydrate crystals were mixed with stirring. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 58.3 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into a slurry obtained by mixing the above magnesium oxide and aluminum sulfate octahydrate, heated to 80 ° C., and stirred at 80 ° C. for 5 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 175 ° C. for 4 hours.
  • reaction slurry was stirred and brought to 72 ° C., and the pH was adjusted to 8.9.
  • a solution prepared by dissolving 2.3 g of sodium palmitate in hot water (80 ° C.) was added. This was aged for 0.7 hours. After filtration, it was washed with 15 L of 40 ° C. pure water and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 11.3 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Comparative Example 2 (Preparation of hydrotalcite-type compound particle powder) 176.3 g of magnesium sulfate heptahydrate crystals and 69.4 g of aluminum sulfate octahydrate crystals were dissolved in pure water. Separately, 30.6 g of sodium carbonate crystals were dissolved in pure water, and 152.4 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution in which the magnesium sulfate heptahydrate crystal and aluminum sulfate octahydrate were mixed, heated to 90 ° C., and stirred at 90 ° C. for 10 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 145 ° C. for 6 hours.
  • reaction slurry was stirred and brought to 65 ° C., and the pH was adjusted to 9.0.
  • a solution prepared by dissolving 1.9 g of sodium laurate in hot water (80 ° C.) was added. This was aged for 0.8 hours. After filtration, it was washed with 15 L of pure water at 45 ° C. and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 9.5 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 20 phr Zinc stearate 0.8 phr Sample above 3.5phr
  • Comparative Example 3 (Preparation of hydrotalcite-type compound particle powder) Magnesium chloride hexahydrate crystal 101.9 g, zinc chloride monohydrate crystal 26.0 g crystal and aluminum chloride hexahydrate crystal 80.5 g were dissolved in pure water. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 136.1 ml of caustic soda (12N) and pure water were added. This alkaline solution was put into an aqueous solution obtained by mixing the above magnesium chloride hexahydrate crystal, zinc chloride monohydrate crystal and aluminum chloride hexahydrate, heated to 95 ° C., and stirred at 95 ° C. for 8 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 165 ° C. for 7 hours.
  • reaction slurry was stirred and brought to 70 ° C., and the pH was adjusted to 9.1.
  • a solution prepared by dissolving 2.5 g of sodium palmitate in hot water (80 ° C.) was added. This was aged for 0.7 hours. After filtration, it was washed with 16 L of pure water at 45 ° C. and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 9.5 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Comparative Example 4 (Preparation of hydrotalcite-type compound particle powder) 171.2 g of magnesium nitrate hexahydrate crystals and 125.0 g of aluminum nitrate 9 hydrate crystals were dissolved in pure water. Separately, 35.7 g of sodium carbonate crystals were dissolved in pure water, and 126.4 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution in which the magnesium nitrate hexahydrate crystal and the aluminum nitrate nonahydrate were mixed, heated to 90 ° C., and stirred at 90 ° C. for 10 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 130 ° C. for 5 hours.
  • reaction slurry was stirred and brought to 62 ° C., and the pH was adjusted to 8.6.
  • a solution prepared by dissolving 2.5 g of sodium stearate in hot water (80 ° C.) was added. This was aged for 0.6 hours. After filtration, it was washed with 25 L of pure water at 60 ° C. and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 18.9 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 55 phr Zinc stearate 0.6 phr Sample above 3.0 phr
  • Comparative Example 5 (Preparation of hydrotalcite-type compound particle powder) 176.3 g of magnesium sulfate heptahydrate crystals and 69.4 g of aluminum sulfate octahydrate crystals were dissolved in pure water. Separately, 30.6 g of sodium carbonate crystals were dissolved in pure water, and 122.4 ml of caustic soda (12N) and pure water were further added. This alkaline solution was put into an aqueous solution in which the magnesium sulfate heptahydrate crystal and aluminum sulfate octahydrate were mixed, heated to 90 ° C., and stirred at 90 ° C. for 10 hours. The total amount was 1 L, which was transferred to an autoclave and aged with stirring at 145 ° C. for 6 hours.
  • reaction slurry was stirred and brought to 65 ° C., and the pH was adjusted to 7.4.
  • a solution prepared by dissolving 1.9 g of sodium laurate in hot water (80 ° C.) was added. This was aged for 0.8 hours. After filtration, it was washed with 15 L of pure water at 45 ° C. and dried at 125 ° C. for 8 hours.
  • the specific surface area of the obtained sample was 9.7 m 2 / g.
  • Chlorine-containing resin composition 100phr DOP 20 phr Zinc stearate 0.8 phr Sample above 3.5phr
  • the electrical insulation, coloring and thermal stability of the resin composition can be improved by using the hydrotalcite particle powder according to the present invention. For this reason, the expansion to more applications becomes possible.

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  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
PCT/JP2009/001335 2008-03-31 2009-03-25 ハイドロタルサイト型化合物粒子粉末、該ハイドロタルサイト型化合物粒子粉末を用いた含塩素樹脂安定剤及び含塩素樹脂組成物 WO2009122681A1 (ja)

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WO2018168496A1 (ja) * 2017-03-17 2018-09-20 堺化学工業株式会社 ハイドロタルサイト類組成物、および、該組成物を含む樹脂添加剤

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