JP7040838B1 - Basic aluminum lactate solution for ceramics formation and its manufacturing method - Google Patents
Basic aluminum lactate solution for ceramics formation and its manufacturing method Download PDFInfo
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- VXYADVIJALMOEQ-UHFFFAOYSA-K tris(lactato)aluminium Chemical compound CC(O)C(=O)O[Al](OC(=O)C(C)O)OC(=O)C(C)O VXYADVIJALMOEQ-UHFFFAOYSA-K 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 239000000919 ceramic Substances 0.000 title claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 title description 17
- -1 aluminum lactate lactate Chemical compound 0.000 claims abstract description 50
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 41
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 21
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 19
- 150000002500 ions Chemical class 0.000 claims abstract description 19
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 14
- 229940085991 phosphate ion Drugs 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 11
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 68
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 52
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 42
- 239000004310 lactic acid Substances 0.000 claims description 34
- 235000014655 lactic acid Nutrition 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000002002 slurry Substances 0.000 claims description 17
- 239000011734 sodium Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 10
- 238000010586 diagram Methods 0.000 abstract description 7
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 93
- 230000000052 comparative effect Effects 0.000 description 31
- 239000007864 aqueous solution Substances 0.000 description 21
- 238000003756 stirring Methods 0.000 description 19
- 229940024546 aluminum hydroxide gel Drugs 0.000 description 18
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 description 18
- 238000010304 firing Methods 0.000 description 17
- 238000003786 synthesis reaction Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 13
- 239000000460 chlorine Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 10
- 150000007524 organic acids Chemical class 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 229910001388 sodium aluminate Inorganic materials 0.000 description 9
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 8
- 229940024545 aluminum hydroxide Drugs 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 239000001630 malic acid Substances 0.000 description 8
- 235000011090 malic acid Nutrition 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 229910052717 sulfur Inorganic materials 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 238000005187 foaming Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 150000007522 mineralic acids Chemical class 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 239000008399 tap water Substances 0.000 description 6
- 235000020679 tap water Nutrition 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 229910001415 sodium ion Inorganic materials 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000013081 microcrystal Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 2
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- 150000008043 acidic salts Chemical class 0.000 description 2
- 150000001339 alkali metal compounds Chemical class 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 235000012501 ammonium carbonate Nutrition 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000011151 fibre-reinforced plastic Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 241000694440 Colpidium aqueous Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
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- 239000003112 inhibitor Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
【課題】 本発明は、製造が簡単で、溶液状態でも長期間安定性が保持させることが可能なセラミックス形成用の塩基性乳酸アルミニウム溶液およびその製造方法を提供する。【解決手段】 本発明は、セラミックス形成用の塩基性乳酸アルミニウム溶液であって、塩基性乳酸アルミニウム溶液が、塩基度６７～８５％であり、Ａｌを、Ａｌ２Ｏ３に換算して、８～１３重量％、Ｆｅを０～５０ｐｐｍ、Ｃａを０～５０ｐｐｍ、Ｍｇを０～５０ｐｐｍおよびＳｉを０～５０ｐｐｍの量で含み、アルカリ金属元素イオンを０～１重量％の量、塩素イオンを０～１．０重量％の量で含み、更に炭酸イオン、硫酸イオンおよびリン酸イオンの３種を総量で０～５００ｐｐｍの量で、かつそれら３種を個別に０～２００ｐｐｍの量で含有する、ことを特徴とする塩基性乳酸アルミニウム溶液およりその製造方法を提供する。【選択図】図１PROBLEM TO BE SOLVED: To provide a basic aluminum lactate lactate solution for forming ceramics, which is easy to produce and can maintain stability for a long period of time even in a solution state, and a method for producing the same. The present invention is a basic aluminum lactate solution for forming ceramics, wherein the basic aluminum lactate solution has a basicity of 67 to 85%, and Al is converted into Al2O3 by 8 to 13 weights. %, Fe in an amount of 0 to 50 ppm, Ca in an amount of 0 to 50 ppm, Mg in an amount of 0 to 50 ppm, and Si in an amount of 0 to 50 ppm, an alkali metal element ion in an amount of 0 to 1% by weight, and a chlorine ion in an amount of 0 to 1. It is characterized by containing in an amount of 0% by weight, further containing 3 types of carbonate ion, sulfate ion and phosphate ion in a total amount of 0 to 500 ppm, and individually containing these 3 types in an amount of 0 to 200 ppm. Provided is a method for producing a basic aluminum lactate solution. [Selection diagram] Fig. 1
Description
本発明はセラミックス形成用の塩基性乳酸アルミニウム溶液およびその製造方法に関する。 The present invention relates to a basic aluminum lactate solution for forming ceramics and a method for producing the same.
塩基性乳酸アルミニウムは、耐火物用バインダーやセラミックス製品のアルミニウム原料として広く用いられている。具体的には、乳酸／Ａｌ２Ｏ３（モル比）＝１．０～２．０、リンゴ酸／Ａｌ２Ｏ３モル比）＝０．０５～０．５であることを特徴とする塩基性乳酸アルミニウム水溶液（特許文献１）、有機酸が乳酸のみ、又は、乳酸とグリコール酸の双方であり、乳酸とグリコール酸との割合がモル比で１００：０～２０：８０であり、有機酸／Ａｌ２Ｏ３（モル比）=１～３である塩基性乳酸アルミニウムと水溶性金属硫酸塩とを含有することを特徴とするセラミックス形成用組成物（特許文献２）、塩基性有機酸多価金属（アルカリ土類金属を除く）塩と有機酸とを特許文献記載式に沿って混合した溶液を乾燥してなるスレーキング抑制剤（特許文献３）、乳酸アルミニウムにアミノ酸またはアルカリ金属アミノ酸塩を使用する乳酸アルミニウムの安定化方法（特許文献４）、乳酸アルミニウムに有機酸のアルカリ金属塩（但し、乳酸のアルカリ金属塩を除く）又は有機酸とアルカリ金属の水酸化物、炭酸塩、重炭酸塩から選ばれたアルカリ金属化合物を使用することからなる乳酸アルミニウムの安定化方法（特許文献５）、Ａｌ２Ｏ３／乳酸（モル比）＝０．２～２．０の塩基性乳酸アルミニウムに対して、Ａｌ２Ｏ３／無機酸（モル比）＝１．５～２．５の範囲で無機酸、無機酸の酸性塩を存在させることからなる塩基性乳酸アルミニウムの安定化方法（特許文献６）、金属アルミニウムと乳酸より塩基性乳酸アルミニウムを製造する際に触媒として鉱酸及び又は鉱酸のアルミニウム塩を用いることを特徴とする塩基性乳酸アルミニウムの製造方法（特許文献７）等が知られている。 Basic aluminum lactate is widely used as a binder for refractories and as a raw material for aluminum in ceramic products. Specifically, a base characterized by having lactic acid / Al 2 O 3 (molar ratio) = 1.0 to 2.0 and malic acid / Al 2 O 3 molar ratio) = 0.05 to 0.5. Sexual aluminum lactate aqueous solution (Patent Document 1), the organic acid is only lactic acid, or both lactic acid and glycolic acid, and the ratio of lactic acid to glycolic acid is 100: 0 to 20:80 in molar ratio, and the organic acid. A composition for forming ceramics (Patent Document 2), which contains basic aluminum lactate having / Al 2 O 3 (molar ratio) = 1 to 3 and a water-soluble metal sulfate (Patent Document 2), and a large amount of basic organic acids. A slake inhibitor (Patent Document 3) made by drying a solution obtained by mixing a valent metal (excluding alkaline earth metal) salt and an organic acid according to the formula described in the patent document, and adding an amino acid or an alkali metal amino acid salt to aluminum lactate. Stabilization method of aluminum lactate used (Patent Document 4), alkali metal salt of organic acid (excluding alkali metal salt of lactic acid) or hydroxide, carbonate, bicarbonate of organic acid and alkali metal in aluminum lactate A method for stabilizing aluminum lactate, which comprises using an alkali metal compound selected from a salt (Patent Document 5), to a basic aluminum lactate having Al 2 O 3 / lactic acid (molar ratio) = 0.2 to 2.0. On the other hand, a method for stabilizing basic aluminum lactate, which comprises the presence of an inorganic acid and an acidic salt of the inorganic acid in the range of Al 2 O 3 / inorganic acid (molar ratio) = 1.5 to 2.5 (Patent Document). 6), a method for producing a basic aluminum lactate, which is characterized by using a mineral acid and / or an aluminum salt of the mineral acid as a catalyst when producing a basic aluminum lactate from metallic aluminum and lactic acid (Patent Document 7) is known. Has been done.
特許文献１記載の方法は粉末での使用が前提であり、リンゴ酸は塩基性領域では溶解性が低いため、溶液状態において低温では液中のリンゴ酸の溶解度が下がり、析出する課題がある。特許文献２記載の方法では、金属硫酸塩を含有するため、９００℃以上で焼成する際にアルミニウム酸化物以外の複合酸化物を形成すると同時に硫酸塩由来の残留炭素、炭化物等を形成しやすくなり、純度の高い酸化アルミニウムを得にくい課題がある。特許文献３記載の方法においては、塩基性多価金属塩と有機酸とを特定の計算式で表された時間と温度で混合・乾燥してなるスレーキング剤であるが、塩基性多価金属塩と有機酸を混合し、乾燥することを前提としており、粉末での供給を前提としており、液状態での安定性が考慮されておらず、不安定になる課題がある。 The method described in Patent Document 1 is premised on the use in powder form, and since malic acid has low solubility in the basic region, there is a problem that the solubility of malic acid in the solution decreases at a low temperature in a solution state and precipitation occurs. Since the method described in Patent Document 2 contains a metal sulfate, it becomes easy to form a composite oxide other than the aluminum oxide when firing at 900 ° C. or higher, and at the same time, it becomes easy to form residual carbon, carbides, etc. derived from the sulfate. There is a problem that it is difficult to obtain high-purity aluminum oxide. The method described in Patent Document 3 is a slaking agent obtained by mixing and drying a basic polyvalent metal salt and an organic acid at a time and temperature represented by a specific formula, but the basic polyvalent metal salt is used. It is premised that it is mixed with an organic acid and dried, and it is premised that it is supplied as a powder. Stability in a liquid state is not taken into consideration, and there is a problem of instability.
特許文献４記載の方法はアミノ酸、アルカリ金属のアミノ酸塩を使用するので、高価になると同時にアルカリ金属イオンを多数含有する課題がある。特許文献５記載の方法は、乳酸アルミニウムに有機酸のアルカリ金属塩または有機酸とアルカリ金属の水酸化物、炭酸塩、重炭酸塩から選ばれるアルカリ金属化合物を使用することを特徴とする乳酸アルミニウムの安定化方法があるが、このままでは乳酸アルミニウムにアルカリ金属分が残留し、９００℃以上で焼成する際にアルカリ金属が融点低下、ｐＨ変動等を発生させる課題がある。特許文献６記載の方法はＡｌ２Ｏ３／乳酸（モル比）＝０．２～２．０の塩基性乳酸アルミニウムに対して、Ａｌ２Ｏ３／無機酸（モル比）＝１．５～２．５の範囲で無機酸、無機酸の酸性塩を存在させることが前提となっており、硫酸イオン、塩化物イオン等を多量に含む塩基性乳酸アルミニウムであり、９００℃以上で焼成した際に事前に一定量以下に除去しておかないと残留炭素、炭化物等を形成しやすくなり、純度の高い酸化アルミニウムを得にくい課題がある。特許文献７記載の方法は金属アルミニウムと乳酸より塩基性乳酸アルミニウムを製造する際に触媒として鉱酸及び鉱酸のアルミニウム塩をもちいることを特徴としており、合成に時間を非常に要する課題がある。 Since the method described in Patent Document 4 uses amino acids and amino acid salts of alkali metals, there is a problem that it is expensive and at the same time contains a large number of alkali metal ions. The method described in Patent Document 5 is characterized in that an alkali metal salt of an organic acid or an alkali metal compound selected from an organic acid and an alkali metal hydroxide, a carbonate, and a bicarbonate is used for aluminum lactate. However, there is a problem that the alkali metal component remains in aluminum lactate as it is, and the alkali metal causes a decrease in melting point, pH fluctuation, etc. when fired at 900 ° C. or higher. The method described in Patent Document 6 is Al 2 O 3 / inorganic acid (molar ratio) = 1.5 to 2.0 with respect to basic aluminum lactate having Al 2 O 3 / lactic acid (molar ratio) = 0.2 to 2.0. It is a basic aluminum lactate containing a large amount of sulfate ion, chloride ion, etc. on the premise that an inorganic acid and an acidic salt of the inorganic acid are present in the range of 2.5, and when fired at 900 ° C or higher. If it is not removed in advance to a certain amount or less, residual carbon, carbonic acid, etc. are likely to be formed, and there is a problem that it is difficult to obtain high-purity aluminum oxide. The method described in Patent Document 7 is characterized by using mineral acid and an aluminum salt of the mineral acid as a catalyst when producing basic aluminum lactate from metallic aluminum and lactic acid, and has a problem that it takes a very long time to synthesize. ..
上記の問題点を鑑みて、本発明の目的は生産性が良好で製造時にＦｅ、Ｃａ、Ｍｇ、Ｓｉ含有量及び炭酸イオン、硫酸イオンおよびリン酸イオンの３種の含有量を低く制御することにより、焼成時に酸化アルミニウム以外の結晶相の生成や残留炭素、着色等の不具合が発生せず、リンゴ酸、アミノ酸等の安定化剤成分を含有させずに溶液状態でも長期間安定性が保持させることが可能なセラミックス形成用の塩基性乳酸アルミニウム溶液およびその製造方法を提供する。 In view of the above problems, an object of the present invention is to have good productivity and to control the content of Fe, Ca, Mg, Si and the content of three kinds of carbonate ion, sulfate ion and phosphate ion to be low at the time of production. As a result, problems such as formation of crystal phases other than aluminum oxide, residual carbon, and coloring do not occur during firing, and stability is maintained for a long time even in a solution state without containing stabilizer components such as malic acid and amino acids. A basic aluminum lactate solution for forming ceramics and a method for producing the same are provided.
本発明者らは上記課題を解決すべく鋭意検討を実施した結果、以下の態様を提供する：
[１] セラミックス形成用の塩基性乳酸アルミニウム溶液であって、塩基性乳酸アルミニウム溶液が、
塩基度６７～８５％であり、
Ａｌを、Ａｌ２Ｏ３に換算して、８～１３重量％、Ｆｅを０～５０ｐｐｍ、Ｃａを０～５０ｐｐｍ、Ｍｇを０～５０ｐｐｍおよびＳｉを０～５０ｐｐｍの量で含み、
アルカリ金属元素イオンを０～１重量％の量、塩素イオンを０～１．０重量％の量で含み、
更に炭酸イオン、硫酸イオンおよびリン酸イオンの３種を総量で０～５００ｐｐｍの量で、かつそれら３種を個別に０～２００ｐｐｍの量で含有する、
ことを特徴とする塩基性乳酸アルミニウム溶液。
［２］ 塩化アルミニウム溶液とアルミン酸アルカリ金属溶液と水とを混合して、水酸化アルミニウムのゲル化物を形成し、前記ゲル化物を水洗した後、水を加えて水酸化アルミニウムスラリーを得、次に乳酸を添加して反応させることを特徴とする、
セラミックス形成用の塩基性乳酸アルミニウム溶液であって、塩基性乳酸アルミニウム溶液が、
塩基度６７～８５％であり、
Ａｌを、Ａｌ２Ｏ３に換算して、８～１３重量％、Ｆｅを０～５０ｐｐｍ、Ｃａを０～５０ｐｐｍ、Ｍｇを０～５０ｐｐｍおよびＳｉを０～５０ｐｐｍの量で含み、
アルカリ金属元素イオンを０～１重量％の量、塩素イオンを０～１．０重量％の量で含み、
更に炭酸イオン、硫酸イオンおよびリン酸イオンの３種を総量で０～５００ｐｐｍの量で、かつそれら３種を個別に０～２００ｐｐｍの量で含有する、
塩基性乳酸アルミニウム溶液の製造方法。
［３］ 乳酸と水酸化アルミニウムスラリーとの反応が、６５～１１０℃で０．５～４．０時間実施することを特徴とする［２］記載の塩基性乳酸アルミニウム溶液の製造方法。
［４］ 前記塩化アルミニウム溶液は、Ｆｅの含有量が０～５０ｐｐｍ、Ｃａの含有量が０～５０ｐｐｍ、Ｍｇの含有量が０～５０ｐｐｍおよびＳｉの含有量が０～５０ｐｐｍに制御することを特徴とする［２］または［３］記載の塩基性乳酸アルミニウム溶液の製造方法。
［５］ 前記アルミン酸アルカリ金属溶液は、Ｆｅの含有量が０～５０ｐｐｍ、Ｃａの含有量が０～５０ｐｐｍ、Ｍｇの含有量が０～５０ｐｐｍおよびＳｉの含有量が０～５０ｐｐｍに制御することを特徴とする［２］～［４］のいずれかに記載の塩基性乳酸アルミニウム溶液の製造方法。
［６］ 前記乳酸は、Ｆｅの含有量が０～５０ｐｐｍ、Ｃａの含有量が０～５０ｐｐｍ、Ｍｇの含有量が０～５０ｐｐｍおよびＳｉの含有量が０～５０ｐｐｍに制御することを特徴とする［２］～［５］のいずれかに記載の塩基性乳酸アルミニウム溶液の製造方法。
［７］ 前記アルミン酸アルカリ金属溶液のアルカリ金属はナトリウム、カリウムおよびそれらの混合からなる群から選択されることを特徴とする［２］～［６］のいずれかに記載の塩基性乳酸アルミニウム溶液の製造方法。
As a result of diligent studies to solve the above problems, the present inventors provide the following aspects:
[1] A basic aluminum lactate solution for forming ceramics, wherein the basic aluminum lactate solution is
The basicity is 67-85%,
Al is converted into Al 2 O 3 , and contains 8 to 13% by weight, Fe in an amount of 0 to 50 ppm, Ca in an amount of 0 to 50 ppm, Mg in an amount of 0 to 50 ppm, and Si in an amount of 0 to 50 ppm.
Alkali metal element ion is contained in an amount of 0 to 1% by weight, and chlorine ion is contained in an amount of 0 to 1.0% by weight.
Further, the three types of carbonate ion, sulfate ion and phosphate ion are contained in a total amount of 0 to 500 ppm, and these three types are individually contained in an amount of 0 to 200 ppm.
A basic aluminum lactate solution characterized by that.
[2] An aluminum chloride solution, an alkali metal aluminate solution and water are mixed to form a gelled product of aluminum hydroxide, the gelled product is washed with water, and then water is added to obtain an aluminum hydroxide slurry. It is characterized by adding lactic acid to and reacting with aluminum chloride.
A basic aluminum lactate solution for forming ceramics, the basic aluminum lactate solution is
The basicity is 67-85%,
Al is converted into Al 2 O 3 , and contains 8 to 13% by weight, Fe in an amount of 0 to 50 ppm, Ca in an amount of 0 to 50 ppm, Mg in an amount of 0 to 50 ppm, and Si in an amount of 0 to 50 ppm.
Alkali metal element ion is contained in an amount of 0 to 1% by weight, and chlorine ion is contained in an amount of 0 to 1.0% by weight.
Further, the three types of carbonate ion, sulfate ion and phosphate ion are contained in a total amount of 0 to 500 ppm, and these three types are individually contained in an amount of 0 to 200 ppm.
A method for producing a basic aluminum lactate solution.
[3] The method for producing a basic aluminum lactic acid solution according to [2], wherein the reaction between lactic acid and the aluminum hydroxide slurry is carried out at 65 to 110 ° C. for 0.5 to 4.0 hours.
[4] The aluminum chloride solution is characterized in that the Fe content is controlled to 0 to 50 ppm, the Ca content is controlled to 0 to 50 ppm, the Mg content is controlled to 0 to 50 ppm, and the Si content is controlled to 0 to 50 ppm. The method for producing a basic aluminum lactate solution according to [2] or [3].
[5] In the alkali metal aluminate solution, the Fe content is controlled to 0 to 50 ppm, the Ca content is controlled to 0 to 50 ppm, the Mg content is controlled to 0 to 50 ppm, and the Si content is controlled to 0 to 50 ppm. The method for producing a basic aluminum lactate lactate solution according to any one of [2] to [4].
[6] The lactic acid is characterized in that the Fe content is controlled to 0 to 50 ppm, the Ca content is controlled to 0 to 50 ppm, the Mg content is controlled to 0 to 50 ppm, and the Si content is controlled to 0 to 50 ppm. The method for producing a basic aluminum lactate solution according to any one of [2] to [5].
[7] The basic aluminum lactate lactate solution according to any one of [2] to [6], wherein the alkali metal of the alkali metal aluminate solution is selected from the group consisting of sodium, potassium and a mixture thereof. Manufacturing method.
本発明では、合成時に炭酸由来の発泡が発生しないため生産性が高く、リンゴ酸のような安定化剤を入れないため、液温変化（特に低温）由来の相溶性悪化や析出物発生といった不具合もない塩基性乳酸アルミニウム溶液を提供することができる。また、本発明の塩基性乳酸アルミニウム溶液は、系の中に炭酸イオン、硫酸イオンやリン酸イオン等が非常に少ないため、９００℃以上の焼成温度、具体的には１０００℃で焼成しても残留炭素分、硫黄分等を含むような脱脂性の悪化や焼成体の不純物をきわめて少なくすることを可能とし、１１００℃焼成においても、アルミニウムのみが供給できるので、目的の組成や結晶を持ったα-アルミナを合成できる。 In the present invention, since carbonic acid-derived foaming does not occur during synthesis, productivity is high, and since a stabilizer such as malic acid is not added, problems such as deterioration of compatibility and generation of precipitates due to changes in liquid temperature (particularly low temperature) occur. A basic aluminum lactate solution can be provided. Further, since the basic aluminum lactate solution of the present invention contains very few carbonate ions, sulfate ions, phosphate ions, etc. in the system, even if it is fired at a firing temperature of 900 ° C. or higher, specifically 1000 ° C. It is possible to deteriorate the degreasing property such as residual carbon content, sulfur content, etc. and to extremely reduce impurities in the fired body, and even in 1100 ° C. firing, only aluminum can be supplied, so that it has the desired composition and crystals. α-Alumina can be synthesized.
本発明による塩基性乳酸アルミニウム溶液を用い、意図した配合比率でＳｉ源、Ｍｇ源、Ｎ源等を添加し、所定の焼成温度、焼成雰囲気で焼成することによってムライトやスピネル、窒化アルミ等の粉体及びセラミックス合成や純度の高い耐火物の原材料、吹き付け材等への適応及び各種セラミックファイバー合成やコーティングへの応用が可能となる。 Using the basic aluminum lactate solution according to the present invention, Si source, Mg source, N source, etc. are added at the intended blending ratio, and the mixture is fired at a predetermined firing temperature and firing atmosphere to produce powders such as mullite, spinel, and aluminum nitride. It can be applied to body and ceramic synthesis, raw materials for high-purity refractories, spraying materials, etc., and to various ceramic fiber synthesis and coating.
本発明の塩基性乳酸アルミニウム溶液は、
塩基度６７～８５％であり、
Ａｌを、Ａｌ２Ｏ３に換算して、８～１３重量％、Ｆｅを０～５０ｐｐｍ、Ｃａを０～５０ｐｐｍ、Ｍｇを０～５０ｐｐｍおよびＳｉを０～５０ｐｐｍの量で含み、
アルカリ金属元素イオンを０～１重量％の量、塩素イオンを０～１．０重量％の量で含み、
更に炭酸イオン、硫酸イオンおよびリン酸イオンの３種を総量で０～５００ｐｐｍの量で、かつそれら３種を個別に０～２００ｐｐｍの量で含有する、
ことを必要とする。また、塩基性乳酸アルミニウム溶液は、塩化アルミニウム溶液とアルミン酸アルカリ金属溶液と水とを混合して、水酸化アルミニウムのゲル化物を形成し、前記ゲル化物を水洗した後、水を加えて水酸化アルミニウムスラリーを得、次に乳酸を添加して反応させることにより製造することができる。
The basic aluminum lactate solution of the present invention is
The basicity is 67-85%,
Al is converted into Al 2 O 3 , and contains 8 to 13% by weight, Fe in an amount of 0 to 50 ppm, Ca in an amount of 0 to 50 ppm, Mg in an amount of 0 to 50 ppm, and Si in an amount of 0 to 50 ppm.
Alkali metal element ion is contained in an amount of 0 to 1% by weight, and chlorine ion is contained in an amount of 0 to 1.0% by weight.
Further, the three types of carbonate ion, sulfate ion and phosphate ion are contained in a total amount of 0 to 500 ppm, and these three types are individually contained in an amount of 0 to 200 ppm.
Need that. The basic aluminum lactate solution is prepared by mixing an aluminum chloride solution, an alkali metal aluminate solution, and water to form a gelled product of aluminum hydroxide, washing the gelled product with water, and then adding water for hydroxylation. It can be produced by obtaining an aluminum slurry and then adding lactic acid to react.
本発明の塩基性乳酸アルミニウム溶液は、塩基度６７～８５％を有することを必要とする。本明細書中において、「塩基度」は塩基で置換し得る価数の何％が埋まっているかを示す値であり、アルミニウムは３価であるので、２／３（３価の内２価）が使用されれば、６６．６６％（即ち、約６７％）となる。本発明では、乳酸アルミニウムの塩基度は６７～８５％、好ましくは６８～８３％、より好ましくは６９～８０％である。６７％より少ないと、塩基性が低くなり、乳酸のアルミニウムへの付加量が増大するため、水への溶解性が低下し、保管安定性が悪化する。逆に８５％より高いと、塩基性が高くなりすぎて、液粘度が増大し、液状物としての取り扱いが難しくなる。 The basic aluminum lactate solution of the present invention needs to have a basicity of 67 to 85%. In the present specification, "basicity" is a value indicating what percentage of the valence that can be replaced with a base is filled, and since aluminum is trivalent, it is 2/3 (divalent of trivalents). If is used, it will be 66.66% (ie, about 67%). In the present invention, the basicity of aluminum lactate is 67 to 85%, preferably 68 to 83%, and more preferably 69 to 80%. If it is less than 67%, the basicity becomes low and the amount of lactic acid added to aluminum increases, so that the solubility in water decreases and the storage stability deteriorates. On the contrary, if it is higher than 85%, the basicity becomes too high, the liquid viscosity increases, and it becomes difficult to handle it as a liquid.
本発明の塩基性乳酸アルミニウム溶液は〔（ＣＨ３ＣＨ（ＯＨ）ＣＯＯ）ｎ（ＯＨ）３－ｎ Ａｌ〕（式中、ｎは０．４５≦ｎ≦１を満足する数値である。）の化学式を有する化合物の水溶液であり、Ａｌ２Ｏ３に換算してＡｌを８～１３重量％の量で含有する。Ａｌの濃度は、Ａｌ２Ｏ３の量に換算して表示する。Ａｌは種々の価数を取る金属であり、水溶液中でも種々の形態や陰イオンとの化合物として存在している。従って、この分野では、Ａｌ２Ｏ３に換算してＡｌを表示している。本発明では、Ａｌ２Ｏ３に換算してＡｌを８～１３重量％の量で存在していることを必要とする。Ａｌの量が８重量％より少ないと、Ａｌの量が不足し、Ａｌが１３重量％を超えると水への溶解性が低下し、保管安定性が悪化する。Ａｌの量は、Ａｌ２Ｏ３に換算して、好ましくは８．１～１２．０重量％、より好ましくは８．３～１１．０重量％の量で含まれる。 The basic aluminum lactic acid solution of the present invention is [(CH 3 CH (OH) COO) n (OH) 3-n Al] (in the formula, n is a numerical value satisfying 0.45 ≦ n ≦ 1). It is an aqueous solution of a compound having a chemical formula, and contains Al in an amount of 8 to 13% by weight in terms of Al 2 O 3 . The concentration of Al is converted into the amount of Al 2 O 3 and displayed. Al is a metal having various valences, and exists as a compound with various forms and anions even in an aqueous solution. Therefore, in this field, Al is displayed in terms of Al 2 O 3 . In the present invention, it is required that Al is present in an amount of 8 to 13% by weight in terms of Al 2 O 3 . If the amount of Al is less than 8% by weight, the amount of Al is insufficient, and if the amount of Al exceeds 13% by weight, the solubility in water is lowered and the storage stability is deteriorated. The amount of Al is preferably 8.1 to 12.0% by weight, more preferably 8.3 to 11.0% by weight in terms of Al 2 O 3 .
本発明の塩基性乳酸アルミニウム溶液は、合成に使用する薬剤や使用器材等から種々の不純物のイオンが存在している。本発明の塩基性乳酸アルミニウム溶液では、それらの不純物イオンを制御することにより、高い安定性や色の純粋性を確保することができる。本発明の塩基性乳酸アルミニウム溶液は、Ｆｅを０～５０ｐｐｍ、Ｃａを０～５０ｐｐｍ、Ｍｇを０～５０ｐｐｍおよびＳｉを０～５０ｐｐｍの量で含み、アルカリ金属元素イオンを０～１重量％の量、更に塩素イオンを０～１重量％の量で、炭酸イオン、硫酸イオンおよびリン酸イオンの３種を総量で０～５００ｐｐｍで、それら３種を個別に０～２００ｐｐｍの量で含むことを必要とする。陽イオンであるＦｅ、Ｃａ、ＭｇやＳｉはそれぞれが５０ｐｐｍを上限に含まれることが必要で、少なければ少ない方が良いが、基本的に反応装置などからの混入は避けられない。 In the basic aluminum lactate lactate solution of the present invention, ions of various impurities are present from the chemicals used for synthesis, the equipment used, and the like. In the basic aluminum lactate lactate solution of the present invention, high stability and color purity can be ensured by controlling these impurity ions. The basic aluminum lactate lactate solution of the present invention contains Fe in an amount of 0 to 50 ppm, Ca in an amount of 0 to 50 ppm, Mg in an amount of 0 to 50 ppm, and Si in an amount of 0 to 50 ppm, and contains alkali metal element ions in an amount of 0 to 1% by weight. Furthermore, it is necessary to contain chlorine ions in an amount of 0 to 1% by weight, carbonate ions, sulfate ions and phosphate ions in a total amount of 0 to 500 ppm, and these three types individually in an amount of 0 to 200 ppm. And. Each of the cations Fe, Ca, Mg and Si needs to be contained in the upper limit of 50 ppm, and the smaller the amount, the better, but basically, contamination from a reaction device or the like is unavoidable.
アルカリ金属元素イオンは、本発明の塩基性乳酸アルミニウム溶液の製造に使用されるアルミン酸アルカリ金属元素溶液から導入される。アルカリ金属元素は、リチウム、ナトリウム、カリウム等が一般的に例示されるが、本発明ではナトリウムイオンが一般的である。アルカリ金属元素イオンは、本発明の塩基性乳酸アルミニウム溶液中に、０～１重量％、好ましくは０～０．５重量％、より好ましくは０～０．２重量％の量で存在し得る。１重量％を超えてアルカリ金属元素イオンが存在すると焼成時に融点を下げることになり、高温焼成では異常粒成長を発生させて、セラミックスの欠陥を発生させたり、粉体の場合においては一次粒子径の増大を発生させる。 The alkali metal element ion is introduced from the alkali metal aluminate element solution used in the production of the basic aluminum lactate lactate solution of the present invention. Lithium, sodium, potassium and the like are generally exemplified as the alkali metal element, but sodium ion is generally used in the present invention. The alkali metal element ion may be present in the basic aluminum lactate lactate solution of the present invention in an amount of 0 to 1% by weight, preferably 0 to 0.5% by weight, and more preferably 0 to 0.2% by weight. If alkali metal element ions are present in excess of 1% by weight, the melting point will be lowered during firing, abnormal grain growth will occur during high-temperature firing, causing defects in ceramics, and in the case of powder, the primary particle size. Causes an increase in.
陰イオンである、塩素イオンは、後述する製造時に使用する薬剤から導入され、水洗など方法で極力除いているが、本発明では上限を１．０重量％とした。塩素イオンは極力取り除くのが、好ましく０～０．９重量％、より好ましくは０～０．８５重量％に制限される。塩素イオン以外の陰イオンである炭酸イオン、硫酸イオンおよびリン酸イオンは本発明では反応に使用する薬剤には含まれてはいないので、基本的には存在しない筈であり、０重量％にしたいが、何らかのルートで持ち込まれたとしても、炭酸イオン、硫酸イオンおよびリン酸イオンの３種を総量で０～５００ｐｐｍに制限し、それら３種の各イオン個別に（即ち、炭酸イオン、硫酸イオンおよびリン酸イオンのそれぞれ）０～２００ｐｐｍの量に制限する必要がある。これらのイオンが多いと、本発明の塩基性乳酸アルミニウム溶液の性能、即ち安定性等が悪くなり、着色などの不具合とみられる現象が生じる恐れがある。 Chloride ion, which is an anion, is introduced from a chemical used in the production described later and is removed as much as possible by a method such as washing with water, but in the present invention, the upper limit is set to 1.0% by weight. Chloride ions are preferably removed as much as possible, preferably from 0 to 0.9% by weight, more preferably from 0 to 0.85% by weight. Anions other than chlorine ions, such as carbonate ion, sulfate ion, and phosphate ion, are not included in the drug used in the reaction in the present invention, so basically they should not be present, and we want to reduce the weight to 0% by weight. However, even if it is brought in by some route, the total amount of the three types of carbonate ion, sulfate ion and phosphate ion is limited to 0 to 500 ppm, and each of these three types of ions (that is, carbonate ion, sulfate ion and It is necessary to limit the amount of phosphate ion) to 0 to 200 ppm. If these ions are abundant, the performance of the basic aluminum lactate lactate solution of the present invention, that is, stability and the like, may deteriorate, and a phenomenon that may be considered as a defect such as coloring may occur.
本発明の塩基性乳酸アルミニウム溶液は、塩化アルミニウム溶液とアルミン酸アルカリ金属溶液（特に、アルミン酸ナトリウム溶液）と水とを混合して、水酸化アルミニウムのゲル化物を形成し、前記ゲル化物を水洗した後、水を加えて水酸化アルミニウムスラリーを得、次に乳酸を添加して反応させることにより製造することができる。 In the basic aluminum lactate lactate solution of the present invention, an aluminum chloride solution, an alkali metal aluminate solution (particularly, a sodium aluminate solution) and water are mixed to form a gelled product of aluminum hydroxide, and the gelled product is washed with water. After that, water is added to obtain an aluminum hydroxide slurry, and then lactic acid is added to cause a reaction.
本発明の塩基性乳酸アルミニウム溶液は、より具体的には、以下に記載する工程で製造される：
工程（１）塩化アルミニウム溶液とアルミン酸アルカリ金属溶液（特に、アルミン酸ナトリウム溶液）と水とを、所定量計量し、５～４０℃の範囲で０．５～３.０時間攪拌する。
工程（２）工程（１）の完了後の混合液を５～３０℃にした後、沈殿した水酸化アルミニウムゲルをろ過する。
工程（３）工程（２）でろ過された水酸化アルミニウムゲルに水を加えて、攪拌を行うことで含有するアルカリ金属元素イオン（特に、ナトリウムイオン）、塩化物イオンを溶解してろ過分離する。この作業を２～１０回繰り返すことで含有するナトリウムイオン、塩化物イオンをそれぞれ１％未満に制御する。
工程（４）工程（３）で得られた水酸化アルミニウムゲルに水を加えて、１０～３０℃で、１０～６０分攪拌することでスラリー化する。
工程（５）工程（４）で得られたスラリーに乳酸を投入し、６５～１１０℃で０．５～４．０時間加熱攪拌を行う。
工程（６）工程（５）で得られた溶液を徐冷することで本発明の塩基性乳酸アルミニウム溶液を得る。
The basic aluminum lactate solution of the present invention is more specifically produced by the steps described below:
Step (1) Weigh a predetermined amount of aluminum chloride solution, alkali metal aluminate solution (particularly sodium aluminate solution), and water, and stir in the range of 5 to 40 ° C. for 0.5 to 3.0 hours.
Step (2) After the mixed solution after the completion of the step (1) is brought to 5 to 30 ° C., the precipitated aluminum hydroxide gel is filtered.
Step (3) Add water to the aluminum hydroxide gel filtered in step (2) and stir to dissolve the alkali metal element ions (particularly sodium ions) and chloride ions contained in the gel and separate by filtration. .. By repeating this operation 2 to 10 times, the sodium ion and chloride ion contained in each are controlled to less than 1%.
Step (4) Water is added to the aluminum hydroxide gel obtained in step (3), and the mixture is stirred at 10 to 30 ° C. for 10 to 60 minutes to form a slurry.
Step (5) Lactic acid is added to the slurry obtained in step (4), and the mixture is heated and stirred at 65 to 110 ° C. for 0.5 to 4.0 hours.
Step (6) The basic aluminum lactate lactate solution of the present invention is obtained by slowly cooling the solution obtained in step (5).
上記工程（１）に使用する塩化アルミニウム溶液は、Ｆｅの含有量が０～５０ｐｐｍ、Ｃａの含有量が０～５０ｐｐｍ、Ｍｇの含有量が０～５０ｐｐｍ、Ｓｉの含有量が０～５０ｐｐｍに制御したものである必要がある。製造原料にこれらのイオンが含まれていなければ、最終の塩基性乳酸アルミニウム溶液にも含まれなくなる。 The aluminum chloride solution used in the above step (1) has a Fe content of 0 to 50 ppm, a Ca content of 0 to 50 ppm, a Mg content of 0 to 50 ppm, and a Si content of 0 to 50 ppm. It needs to be something that has been done. If the raw material does not contain these ions, it will not be contained in the final basic aluminum lactate solution.
上記工程（１）に使用するアルミン酸アルカリ金属溶液（特に、アルミン酸ナトリウム溶液）も、Ｆｅの含有量が０～５０ｐｐｍ、Ｃａの含有量が０～５０ｐｐｍ、Ｍｇの含有量が０～５０ｐｐｍ、Ｓｉの含有量が０～５０ｐｐｍに制御したものである必要がある。製造原料にこれらのイオンが含まれていなければ、最終の塩基性乳酸アルミニウム溶液にも含まれなくなる。 The alkali metal aluminate solution (particularly, sodium aluminate solution) used in the above step (1) also has a Fe content of 0 to 50 ppm, a Ca content of 0 to 50 ppm, and a Mg content of 0 to 50 ppm. The Si content needs to be controlled to 0 to 50 ppm. If the raw material does not contain these ions, it will not be contained in the final basic aluminum lactate solution.
上記工程（４）に使用する乳酸は、Ｆｅの含有量が０～５０ｐｐｍ、Ｃａが０～５０ｐｐｍ、Ｍｇが０～５０ｐｐｍ、Ｓｉが０～５０ｐｐｍに制御したものである必要がある。製造原料にこれらのイオンが含まれていなければ、最終の塩基性乳酸アルミニウム溶液にも含まれなくなる。 The lactic acid used in the above step (4) needs to have a Fe content of 0 to 50 ppm, Ca of 0 to 50 ppm, Mg of 0 to 50 ppm, and Si of 0 to 50 ppm. If the raw material does not contain these ions, it will not be contained in the final basic aluminum lactate solution.
上述の塩化アルミニウム（溶液を含む）、アルミン酸アルカリ金属（特に、アルミン酸ナトリウム）（溶液を含む）、乳酸においてＦｅの含有量、Ｃａ含有量、Ｍｇ含有量、Ｓｉ含有量のいずれか１つ以上の含有量が５０ｐｐｍを超えると、９００℃以上で焼成した際に着色や酸化アルミニウム以外の結晶系の複合酸化物をつくってしまうため好ましくない。 Any one of the above-mentioned aluminum chloride (including solution), alkali metal aluminate (particularly sodium aluminate) (including solution), Fe content, Ca content, Mg content, and Si content in lactic acid. If the above content exceeds 50 ppm, it is not preferable because it forms colored or crystalline composite oxides other than aluminum oxide when fired at 900 ° C. or higher.
上記工程（１）では、塩化アルミニウムとアルミン酸アルカリ金属溶液（特に、アルミン酸ナトリウム溶液）と水とを、所定量計量し、撹拌して混合する。撹拌混合の温度範囲は、５～４０℃の範囲が好ましく、５℃未満になると液の粘度が高くなり、攪拌が難しくなる課題がある。一方で４０℃を超えると水酸化アルミニウムの微結晶ができやすくなり、次の工程で溶解が難しくなる課題がある。塩化アルミニウムとアルミン酸アルカリ金属溶液と水の量は、塩化アルミニウム水溶液濃度、アルミン酸アルカリ金属水溶液の濃度にもよるが、重量を基準として水量を１とすると塩化アルミニウム水溶液が０．８～２．０、アルミン酸アルカリ金属水溶液が０．８～２．０の比率で混合する。アルミン酸アルカリ金属水溶液添加量を一定として、塩化アルミニウム水溶液が０．８未満になるとアルミン酸アルカリ金属水溶液が過剰になるためｐＨが高くなり、アルカリ金属残留が過剰になり、所望の水酸化アルミニウムゲルが得られなくなる。一方で塩化アルミニウム水溶液が２．０を超えるとｐＨが低くなりすぎて、水酸化アルミニウムゲル析出に不具合を発生させる課題がある。そのため上記の範囲で最適な塩化アルミニウム水溶液、アルミン酸アルカリ金属水溶液量比率を選択する必要がある。 In the above step (1), aluminum chloride, an alkali metal aluminate solution (particularly, a sodium aluminate solution) and water are weighed in a predetermined amount, stirred and mixed. The temperature range of stirring and mixing is preferably in the range of 5 to 40 ° C., and if it is less than 5 ° C., the viscosity of the liquid becomes high and there is a problem that stirring becomes difficult. On the other hand, if the temperature exceeds 40 ° C., fine crystals of aluminum hydroxide are likely to be formed, and there is a problem that dissolution becomes difficult in the next step. The amount of aluminum chloride, alkali metal aluminate solution and water depends on the concentration of the aqueous solution of aluminum chloride and the concentration of the aqueous solution of alkali metal aluminate, but when the amount of water is 1 based on the weight, the aqueous solution of aluminum chloride is 0.8 to 2. 0, Aqueous alkali metal aluminate solution is mixed at a ratio of 0.8 to 2.0. When the amount of the alkali metal aluminate solution is constant and the amount of the aluminum chloride aqueous solution is less than 0.8, the pH becomes high due to the excess of the alkali metal aluminate aqueous solution, the alkali metal residue becomes excessive, and the desired aluminum hydroxide gel is obtained. Cannot be obtained. On the other hand, if the aqueous solution of aluminum chloride exceeds 2.0, the pH becomes too low, which causes a problem in the precipitation of aluminum hydroxide gel. Therefore, it is necessary to select the optimum ratio of the amount of the aluminum chloride aqueous solution and the aluminate alkali metal aqueous solution within the above range.
上記工程（２）では、温度を整えるために冷却し、その後ろ過するが、冷却温度は、５～３０℃が好ましい。５℃未満になると沈殿している水酸化アルミニウムゲルが固くなり、ろ過に時間がかかる。３０℃を超えると沈殿している水酸化アルミニウムゲルがろ布等に張り付き、ろ布等の目詰まりを起こしやすくなり、ろ過が悪くなる課題がある。本発明の塩基性乳酸アルミニウム溶液の製造で使用するろ過はフィルタープレス、遠心脱水機、吸引ろ過等から選択することができ、不純物濃度を高める方法や生産性を著しく劣化させる方法でなければ、制約されるものではない。 In the above step (2), cooling is performed to adjust the temperature, and then filtration is performed. The cooling temperature is preferably 5 to 30 ° C. When the temperature is lower than 5 ° C., the precipitated aluminum hydroxide gel becomes hard and it takes time to filter. If the temperature exceeds 30 ° C., the precipitated aluminum hydroxide gel sticks to the filter cloth or the like, which tends to cause clogging of the filter cloth or the like, resulting in poor filtration. The filtration used in the production of the basic aluminum lactate lactate solution of the present invention can be selected from a filter press, a centrifugal dehydrator, suction filtration, etc., and is restricted unless it is a method for increasing the impurity concentration or a method for significantly deteriorating productivity. It is not something that will be done.
上記工程（３）のろ過および洗浄工程はアルカリ金属元素イオン（具体的には、ナトリウムイオン）、塩化物イオン濃度が１％未満になる回数を実施すればよく、特に制約されるものではない。陰イオンである炭酸イオン、硫酸イオンおよびリン酸イオンは本発明では反応に使用する薬剤には含まれてはいないので量的に問題は通常ないが、意図せず何らかのルートで持ち込まれたとしても、工程（３）のろ過分離工程において、水に溶解してろ過分離できるため、炭酸イオン、硫酸イオンおよびリン酸イオンの３種を総量で０～５００ｐｐｍに制限し、それら３種の各イオン個別に（即ち、炭酸イオン、硫酸イオンおよびリン酸イオンのそれぞれ）０～２００ｐｐｍの量に制御することが可能である。 The filtration and cleaning steps of the above step (3) may be carried out as many times as the alkali metal element ion (specifically, sodium ion) and chloride ion concentrations become less than 1%, and are not particularly limited. Since the anions such as carbonate ion, sulfate ion and phosphate ion are not contained in the agent used in the reaction in the present invention, there is usually no problem in quantity, but even if they are unintentionally brought in by some route. In the filtration separation step of step (3), since it can be dissolved in water and filtered and separated, the total amount of 3 types of carbonate ion, sulfate ion and phosphate ion is limited to 0 to 500 ppm, and each of these 3 types of ions is individually used. It is possible to control the amount to 0-200 ppm (ie, each of carbonate ion, sulfate ion and phosphate ion).
上記工程（４）では、得られた混合物に水を加えてスラリー化するが、１０～３０℃で１０～６０分攪拌することになっているが、特にこの温度や時間に限定しているのではなく、結果的にスラリーができればよい。 In the above step (4), water is added to the obtained mixture to form a slurry, which is to be stirred at 10 to 30 ° C. for 10 to 60 minutes, but the temperature and time are particularly limited. Instead, it is only necessary to form a slurry as a result.
上記工程（５）では、工程（４）で得られたスラリーに乳酸を投入し、６５～１１０℃で０．５～４．０時間加熱攪拌を行うが、温度が６５℃未満になると反応が十分起こらない可能性があり、１１０℃を超えると反応と同時に部分的な変性が起こり、所望の塩基性乳酸アルミニウム溶液が得られなくなることがある。反応時間に関しては、０．５時間未満になると反応が十分進まなくなり、４．０時間を超えると生産性が悪化することがある。 In the above step (5), lactic acid is added to the slurry obtained in the step (4) and heated and stirred at 65 to 110 ° C. for 0.5 to 4.0 hours, but when the temperature becomes less than 65 ° C., the reaction occurs. It may not occur sufficiently, and if the temperature exceeds 110 ° C., partial denaturation may occur at the same time as the reaction, and the desired basic aluminum lactate lactate solution may not be obtained. Regarding the reaction time, if it is less than 0.5 hours, the reaction does not proceed sufficiently, and if it exceeds 4.0 hours, the productivity may deteriorate.
最後の工程（６）では、工程（５）の反応後、冷却（通常室温まで）することにより本発明の塩基性乳酸アルミニウム溶液が得られる。 In the final step (6), after the reaction of the step (5), the solution is cooled (usually up to room temperature) to obtain the basic aluminum lactate lactate solution of the present invention.
本発明の塩基性乳酸アルミニウム溶液の製造に使用する各種設備およびそれらの接液部（攪拌機の羽根、釜、配管、ろ過機、保管等）には、Ｆｅ、Ｓｉ、Ｃａ、Ｍｇ等が溶出しない材料を使用するのが好ましい。具体的な材料としては、ＦＲＰ（繊維強化プラスチック）、ガラスライニングしたステンレス鋼（例えば、ＳＵＳ３１６やＳＵＳ３１６L）、ハステロイ、耐熱塩化ビニル、棚内壁をガラスライニングした耐熱塩化ビニル、ポリフッ化ビニリデン、ポリフルオロテトラエチレン等から選定することが好ましい。 Fe, Si, Ca, Mg, etc. do not elute in various equipment used for producing the basic aluminum lactate lactate solution of the present invention and their wetted parts (stirring blades, kettles, pipes, filters, storage, etc.). It is preferable to use the material. Specific materials include FRP (fiber reinforced plastic), glass-lined stainless steel (for example, SUS316 and SUS316L), Hastelloy, heat-resistant vinyl chloride, heat-resistant vinyl chloride with glass-lined shelf inner wall, polyvinylidene fluoride, and polyfluorotetra. It is preferable to select from ethylene or the like.
本発明を実施例により更に詳細に説明する。本発明は、これら実施例に限定されるものと解してはならない。 The present invention will be described in more detail by way of examples. The present invention should not be construed as being limited to these examples.
＜実施例１＞
容量１０Ｌのジャケット付きＧＬ攪拌釜を用いて、まずジャケットに５℃の冷却水循環を行う。釜内に水道水１５３１．６ｇを加えて撹拌しながら、塩化アルミニウム水溶液（Ａｌ２Ｏ３換算Ａｌ量１０．０重量％、塩基度２．４％、ＳＯ４
２－０.０１重量％）１９０９．４ｇおよびアルミン酸ナトリウム水溶液（Ａｌ２Ｏ３換算Ａｌ量２０．０重量％、Ｎａ２Ｏ換算Ｎａ量１８．９％）１５５９．０ｇを同時に添加し、水酸化アルミニウムゲル溶液５０００ｇを得た。投入から撹拌終了までの時間は２．５時間であり、このときの温度は２１～３０℃であった。
<Example 1>
Using a GL stirring pot with a jacket having a capacity of 10 L, first, the jacket is circulated with cooling water at 5 ° C. Aqueous aluminum chloride solution (Al 2 O 3 equivalent Al amount 10.0% by weight, basicity 2.4%, SO 4-2-0.01 % by weight) 1909 while adding 1531.6 g of tap water to the kettle and stirring. .4 g and an aqueous solution of sodium aluminate (Al 2 O 3 equivalent Al amount 20.0% by weight, Na 2 O equivalent Na amount 18.9%) 1559.0 g were added at the same time to obtain 5000 g of an aluminum hydroxide gel solution. The time from charging to the end of stirring was 2.5 hours, and the temperature at this time was 21 to 30 ° C.
次に、得られたゲル溶液に関して遠心脱水機を用いて脱水し、水を加水し撹拌を行う作業を７回繰り返した。得られた洗浄ゲルは１９２０ｇであった。このときのゲル溶液は８℃、洗浄水は１５℃であった。更に、マントルヒータに設置した容量１Ｌのガラス製セパラブルフラスコを用いて、得られた洗浄ゲル１０３．２ｇ、次いで水道水１５７．１ｇを加えて３０分間撹拌して２６０．３ｇのスラリーを得た。このときの温度は１５℃であった。得られたスラリーに乳酸（乳酸９０％）３９．７ｇを投入し、１００℃で３時間加熱撹拌を行ったのち、徐冷することで本発明の塩基性乳酸アルミニウム溶液３００ｇを得た（Ａｌ２Ｏ３換算Ａｌ量８．９重量％、塩基度７１．５％、ＳＯ４ ２－０.０重量％、ＰＯ４ ３－０.０重量％、ＣＯ３ ２－０．０重量％、Ｎａ＋０．０５重量％、Ｃｌー０．８重量％）。 Next, the obtained gel solution was dehydrated using a centrifugal dehydrator, water was added, and stirring was repeated 7 times. The obtained washing gel weighed 1920 g. At this time, the gel solution was 8 ° C. and the washing water was 15 ° C. Further, using a glass separable flask having a capacity of 1 L installed in the mantle heater, 103.2 g of the obtained washing gel and then 157.1 g of tap water were added and stirred for 30 minutes to obtain a slurry of 260.3 g. .. The temperature at this time was 15 ° C. 39.7 g of lactic acid (90% lactic acid) was added to the obtained slurry, and the mixture was heated and stirred at 100 ° C. for 3 hours and then slowly cooled to obtain 300 g of the basic aluminum lactate solution of the present invention (Al 2 ). O 3 conversion Al amount 8.9% by weight, basicity 71.5%, SO 4-2-0.0 % by weight, PO 4-3-0.0 % by weight , CO 3-2-0.0 % by weight, Na + 0.05% by weight, Cl - 0.8% by weight).
＜実施例２＞
容量１０Ｌのジャケット付きＧＬ攪拌釜を用いて、まずジャケットに５℃の冷却水循環を行う。次に、釜内に水道水１４２９．８ｇを加えて撹拌しながら、塩化アルミニウム水溶液（Ａｌ２Ｏ３換算Ａｌ量１０．０重量％、塩基度２．４％、ＳＯ４
２－０.０１重量％）１９０９．４ｇとアルミン酸ナトリウム水溶液（Ａｌ２Ｏ３換算Ａｌ量２３．０重量％、Ｎａ２Ｏ換算Ｎａ量１８．０％）１６６０．８ｇを同時に添加し、水酸化アルミニウムゲル溶液５０００ｇを得た。投入から撹拌終了までの時間は２．５時間であり、このときの温度は２１～３０℃であった。
<Example 2>
Using a GL stirring pot with a jacket having a capacity of 10 L, first, the jacket is circulated with cooling water at 5 ° C. Next, while adding 1429.8 g of tap water to the kettle and stirring, the aluminum chloride aqueous solution (Al 2 O 3 equivalent Al amount 10.0% by weight, basicity 2.4%, SO 4-2-0.01 weight) %) 1909.4 g and 1660.8 g of sodium aluminate aqueous solution (Al 2 O 3 equivalent Al amount 23.0% by weight, Na 2 O equivalent Na amount 18.0%) are added at the same time, and 5000 g of aluminum hydroxide gel solution is added. Obtained. The time from charging to the end of stirring was 2.5 hours, and the temperature at this time was 21 to 30 ° C.
次に、得られたゲル溶液に関して遠心脱水機を用いて脱水し、水を加水し撹拌を行う作業を７回繰り返した。得られた洗浄ゲルは２１９０ｇであった。このときのゲル溶液は８℃、洗浄水は１５℃であった。次に、マントルヒータに設置した容量1Ｌのガラス製セパラブルフラスコを用いて、得られた洗浄ゲル１０３．２ｇ、次いで水道水１５７．１ｇを加えて３０分間撹拌して２６０．３ｇのスラリーを得た。このときの温度は１５℃であった。次に、得られたスラリーに乳酸（乳酸９０％）３９．７ｇを投入し、１００℃で３時間加熱撹拌を行ったのち、徐冷することで本発明の塩基性乳酸アルミニウム溶液３００ｇを得た（Ａｌ２Ｏ３換算Ａｌ量８．８重量％、塩基度７０．２％、ＳＯ４ ２－０.０重量％、ＰＯ４ ３－０.０重量％、ＣＯ３ ２－０．０重量％、Ｎａ＋０．０１重量％、Ｃｌー０．８重量％）。 Next, the obtained gel solution was dehydrated using a centrifugal dehydrator, water was added, and stirring was repeated 7 times. The obtained washing gel weighed 2190 g. At this time, the gel solution was 8 ° C. and the washing water was 15 ° C. Next, using a glass separable flask having a capacity of 1 L installed in a mantle heater, 103.2 g of the obtained washing gel and then 157.1 g of tap water were added and stirred for 30 minutes to obtain a slurry of 260.3 g. rice field. The temperature at this time was 15 ° C. Next, 39.7 g of lactic acid (90% lactic acid) was added to the obtained slurry, heated and stirred at 100 ° C. for 3 hours, and then slowly cooled to obtain 300 g of the basic aluminum lactate lactate solution of the present invention. (Al 2 O 3 converted Al amount 8.8% by weight, basicity 70.2%, SO 4 2-0.0 % by weight, PO 4 3-0.0 % by weight, CO 3 2-0.0 % by weight , Na + 0.01% by weight, Cl - 0.8% by weight).
＜実施例３＞
容量１Ｌのジャケット付きＧＬ攪拌釜を用いて、まずジャケットに５℃の冷却水循環を行う。次に、釜内に水道水１５３.１ｇを加えて撹拌しながら、塩化アルミニウム水溶液（Ａｌ２Ｏ３換算Ａｌ量１０．０重量％、塩基度２．４％、ＳＯ４
２－０.０１重量％）１９０．４ｇとアルミン酸ナトリウム水溶液（Ａｌ２Ｏ３換算Ａｌ量２０．０重量％、Ｎａ２Ｏ換算Ｎａ量１８．９重量％）１５５．９ｇを同時に添加し、水酸化アルミニウムゲル溶液５００ｇを得た。投入から撹拌終了までの時間は１．５時間であり、このときの温度は２０～３０℃であった。次に得られたゲル溶液に関してろ紙Ｎｏ.５を用いて吸引ろ過し、ろ紙上に残ったケーキに更に水を加水しろ過・洗浄作業を５回繰り返した。得られた洗浄ゲルは１９０ｇであった。このときのゲル溶液は１０℃、洗浄水は１７℃であった。
<Example 3>
Using a GL stirring pot with a jacket having a capacity of 1 L, first, the jacket is circulated with cooling water at 5 ° C. Next, while adding 153.1 g of tap water to the kettle and stirring, the aluminum chloride aqueous solution (Al 2 O 3 equivalent Al amount 10.0% by weight, basicity 2.4%, SO 4-2-0.01 weight) %) 190.4 g and 155.9 g of sodium aluminate aqueous solution (Al 2 O 3 equivalent Al amount 20.0% by weight, Na 2 O equivalent Na amount 18.9% by weight) were added at the same time, and 500 g of aluminum hydroxide gel solution was added. Got The time from charging to the end of stirring was 1.5 hours, and the temperature at this time was 20 to 30 ° C. Next, the obtained gel solution was suction-filtered using filter paper No. 5, water was further added to the cake remaining on the filter paper, and the filtering / washing operation was repeated 5 times. The obtained washing gel weighed 190 g. At this time, the gel solution was 10 ° C. and the washing water was 17 ° C.
次に、マントルヒータに設置した容量１Ｌのガラス製セパラブルフラスコを用いて、得られた洗浄ゲル１０３．７ｇ、次いで水道水１５６．６ｇを加えて３０分間撹拌して２６０．３ｇのスラリーを得た。このときの温度は１３℃であった。次に、得られたスラリーに乳酸（９０重量％）３９．７ｇを投入し、１００℃で１．５時間加熱撹拌を行ったのち、徐冷することで本発明の塩基性乳酸アルミニウム溶液２９８ｇを得た（Ａｌ２Ｏ３換算Ａｌ量８．６重量％、塩基度 ７２．４％、ＳＯ４ ２－０.０重量％、ＰＯ４ ３－０.０重量％、ＣＯ３ ２－０．０重量％、Ｎａ＋０．０２重量％、Ｃｌー０．５重量％）。 Next, using a glass separable flask having a capacity of 1 L installed in a mantle heater, 103.7 g of the obtained washing gel and then 156.6 g of tap water were added and stirred for 30 minutes to obtain a slurry of 260.3 g. rice field. The temperature at this time was 13 ° C. Next, 39.7 g of lactic acid (90% by weight) was added to the obtained slurry, heated and stirred at 100 ° C. for 1.5 hours, and then slowly cooled to obtain 298 g of the basic aluminum lactate lactate solution of the present invention. Obtained (Al 2 O 3 converted Al amount 8.6% by weight, basicity 72.4%, SO 4 2-0.0 % by weight, PO 4 3-0.0 % by weight, CO 3 2-0.0 %% by weight, Na + 0.02% by weight, Cl - 0.5% by weight).
＜比較例１＞
炭酸アンモニウム水溶液(ＮＨ３２．７重量％)を１００ｇに塩化アルミニウム水溶液（Ｃｌ１０．２重量％）５３gを撹拌機で攪拌しながら、徐々に添加し、反応温度３０℃を目標としながら、水酸化アルミニウムゲルを製造した。この生成した水酸化アルミニウムゲルに関して遠心分離機を用いてろ過し、更に水を投入して繰り返し洗浄することで、Ａｌ2Ｏ3＝１１．４重量％、ＮＨ3＝０．０６重量％、Ｃｌ＝０．０１重量％の水酸化アルミニウムゲルを得た。ついで、この水酸化アルミニウムゲル１００ｇと乳酸（７５重量％）３６gとを４５～５０℃で反応させ、Ａｌ２Ｏ３＝８．８重量％、Ａｌ２Ｏ３／乳酸（モル比）０．３７とし、更に当該塩基性乳酸アルミニウム１００gに塩酸（３５重量％）を１ｇ混合した塩基性乳酸アルミニウム溶液を得た。塩基性乳酸アルミニウム溶液はＡｌ２Ｏ３換算Ａｌ量８．８重量％、塩基度７２．４％、ＳＯ４
２－０.０重量％、ＰＯ４
３－０.０重量％、ＣＯ３
２－１．１重量％、Ｎａ＋０．０重量％、Ｃｌ－０．３６重量％であった。
<Comparative Example 1>
Add 53 g of an aqueous solution of aluminum chloride (Cl 10.2% by weight) to 100 g of an aqueous solution of ammonium carbonate ( NH 32.7% by weight) gradually while stirring with a stirrer, and hydroxide while aiming for a reaction temperature of 30 ° C. Manufactured an aluminum gel. The produced aluminum hydroxide gel is filtered using a centrifuge, and water is added to repeatedly wash the gel. As a result, Al 2 O 3 = 11.4% by weight, NH 3 = 0.06% by weight, Cl. = 0.01% by weight aluminum hydroxide gel was obtained. Then, 100 g of this aluminum hydroxide gel and 36 g of lactic acid (75% by weight) were reacted at 45 to 50 ° C., Al 2 O 3 = 8.8% by weight, Al 2 O 3 / lactic acid (molar ratio) 0.37. Further, a basic aluminum lactate solution was obtained by mixing 100 g of the basic aluminum lactate with 1 g of hydrochloric acid (35% by weight). The basic aluminum lactate solution has an Al 2 O 3 equivalent Al amount of 8.8% by weight, a basicity of 72.4%, SO 4-2-0.0 % by weight, PO 4-3-0.0 % by weight , and CO 3-2- . It was 1.1% by weight, Na + 0.0% by weight, and Cl − 0.36% by weight.
＜比較例２＞
炭酸アンモニウム水溶液(ＮＨ3２．７重量％)１００ｇに塩化アルミニウム水溶液（Ｃｌ １０．２重量％）５３gを撹拌機で攪拌しながら、徐々に添加し、反応温度３０℃を目標としながら、水酸化アルミニウムゲルを製造した。この生成した水酸化アルミニウムゲルに関して遠心分離機を用いてろ過し、更に水を投入して繰り返し洗浄することで、Ａｌ２Ｏ３＝１１．４重量％、ＮＨ3＝０．０６重量％、Ｃｌ＝０．０１重量％の水酸化アルミニウムゲルを得た。ついで、この水酸化アルミニウムゲル１００gと乳酸（７５重量％）２５gとを４５～５０℃で反応させ、Ａｌ２Ｏ３＝８．９％、Ａｌ２Ｏ３／乳酸（モル比）０．５２の塩基性乳酸アルミニウム溶液を作製し、保管安定性向上のためにリンゴ酸／Ａｌ２Ｏ３＝０．３になるようにリンゴ酸を加えた塩基性乳酸アルミニウム溶液を得た。塩基性乳酸アルミニウム溶液はＡｌ２Ｏ３換算Ａｌ量８．９重量％、塩基度５２．０％、ＳＯ４
２－０.０重量％、ＰＯ４
３－０.０重量％、ＣＯ３
２－１．２重量％、Ｎａ＋０．０重量％、Ｃｌ－０．０１重量％であった。
<Comparative Example 2>
Add 53 g of aluminum chloride aqueous solution (Cl 10.2% by weight) to 100 g of ammonium carbonate aqueous solution (NH 3 2.7% by weight) gradually while stirring with a stirrer, and hydroxylate while aiming at a reaction temperature of 30 ° C. Manufactured an aluminum gel. The produced aluminum hydroxide gel is filtered using a centrifuge, and water is further added to repeatedly wash the gel. As a result, Al 2 O 3 = 11.4% by weight, NH 3 = 0.06% by weight, Cl. = 0.01% by weight aluminum hydroxide gel was obtained. Then, 100 g of this aluminum hydroxide gel and 25 g of lactic acid (75% by weight) were reacted at 45 to 50 ° C., and Al 2 O 3 = 8.9%, Al 2 O 3 / lactic acid (molar ratio) 0.52. A basic aluminum lactic acid solution was prepared, and a basic aluminum lactic acid solution was obtained by adding malic acid so that malic acid / Al 2 O 3 = 0.3 in order to improve storage stability. The basic aluminum lactate solution has an Al 2 O 3 equivalent Al amount of 8.9% by weight, basicity of 52.0%, SO 4 2-0.0 % by weight, PO 4 3-0.0 % by weight, CO 3 2- . It was 1.2% by weight, Na + 0.0% by weight, and Cl − 0.01% by weight.
＜比較例３＞
硫酸アルミニウム溶液（Ａｌ２Ｏ３＝２．６％、ＳＯ４
２－／Ａｌ２Ｏ３（モル比）３．０５を３００gにアルミン酸ナトリウム溶液（Ａｌ２Ｏ３換算Ａｌ量３．０重量％、Ｎａ２Ｏ／Ａｌ２Ｏ３（モル比）１．４３）５００gを添加して、攪拌を実施した後、遠心分離機を用いてろ過を行い、更に水を投入して繰り返し洗浄することで、Ａｌ2 Ｏ3 ＝１１．５重量％、ＳＯ４
２－＝１．８重量％、Ｎａ２Ｏ＝０．１３重量％の水酸化アルミニウムゲルを得た。次にこの水酸化アルミニウムゲル１００gと乳酸（７５重量％）５６gを６０～６５℃で反応させ、Ａｌ２Ｏ３＝７．４重量％、Ａｌ２Ｏ３／乳酸（モル比）０．２４、ＳＯ４
２－／Ａｌ２Ｏ３モル比）０．２の塩基性乳酸アルミニウム水溶液を得た。塩基性乳酸アルミニウム溶液はＡｌ２Ｏ３換算 Ａｌ量７．４重量％、塩基度７６．０％、ＳＯ４
２－ １．５重量％、ＰＯ４
３－０.０重量％、ＣＯ３
２－ ０．０重量％、Ｎａ＋０．０５重量％、Ｃｌ－０．０重量％であった。
<Comparative Example 3>
Aluminum sulfate solution (Al 2 O 3 = 2.6%, SO 4-2 / Al 2 O 3 (molar ratio) 3.05 to 300 g Sodium aluminate solution (Al 2 O 3 equivalent Al amount 3.0 % by weight) , Na 2 O / Al 2 O 3 (molar ratio) 1.43) 500 g is added, and after stirring, filtration is performed using a centrifuge, and water is further added for repeated washing. , Al 2 O 3 = 11.5% by weight, SO 4 2- = 1.8% by weight, Na 2 O = 0.13% by weight aluminum hydroxide gel was obtained. Next, with 100 g of this aluminum hydroxide gel. 56 g of lactic acid (75% by weight) was reacted at 60 to 65 ° C., Al 2 O 3 = 7.4% by weight, Al 2 O 3 / lactic acid (molar ratio) 0.24 , SO 4-2 / Al 2 O 3 A basic aluminum lactate aqueous solution having a molar ratio of 0.2 was obtained. The basic aluminum lactate solution has an Al 2 O 3 equivalent Al amount of 7.4% by weight, basicity of 76.0%, SO 4-2-1.5 % by weight, PO 4-3-0.0 % by weight , CO 3-2- . It was 0.0% by weight, Na + 0.05% by weight, and Cl − 0.0% by weight.
上記実施例１～３および比較例１～３の合成時における高塩基性塩化アルミニウム溶液の合成時の発泡状態、合成された塩基性乳酸アルミニウム溶液の合成直後の外観、３０℃で１か月経過後の外観、１０℃で１か月経過における液の外観を表１に示す。発泡は、合成時に発砲が生じるかどうかを、目視で判断したもので、表１には「有り」または「無し」と記載した。外観は目視で判断し、透明であれば〇、濁りが見える時は△、析出物が確認できた時は×と記載した。 Foaming state at the time of synthesis of the highly basic aluminum chloride solution at the time of synthesis of Examples 1 to 3 and Comparative Examples 1 to 3, appearance immediately after synthesis of the synthesized basic aluminum lactate lactate solution, one month passed at 30 ° C. Table 1 shows the appearance of the liquid after 1 month at 10 ° C. Foaming is a visual judgment as to whether or not firing occurs during synthesis, and is described as "yes" or "no" in Table 1. The appearance was visually judged, and if it was transparent, it was described as ◯, if turbidity was visible, it was described as Δ, and if a precipitate was confirmed, it was described as ×.
実施例１～３、比較例１および比較例３によって得られた高塩基性塩化アルミニウム溶液を、アルミナ製坩堝に入れ、１００℃/時で昇温し、９００℃、１０００℃、１１００℃で１時間焼成して得られた焼成粉の外観色をＴＥＳ－３２５０カラーメーター（株式会社佐藤商事製）にて測定した結果を表１に示す。 The highly basic aluminum chloride solutions obtained in Examples 1 to 3, Comparative Example 1 and Comparative Example 3 were placed in an alumina crucible, heated at 100 ° C./hour, and heated at 900 ° C., 1000 ° C. and 1100 ° C. 1 Table 1 shows the results of measuring the appearance color of the fired powder obtained by time-baking with a TES-3250 color meter (manufactured by Sato Shoji Co., Ltd.).
実施例１～３、比較例１および比較例３によって得られた高塩基性塩化アルミニウム溶液を９００℃、１０００℃、１１００℃で焼成し、それぞれの焼成で得られた焼成粉をＥＤＸ（ＴＭ３０３０ｐｌｕｓ：日立ハイテクノロジーズ株式会社製）のエネルギー分散型蛍光Ｘ線で元素分析し、Ａｌ、ＣａおよびＳの存在量を表３に示す。表３には、実施例および比較例の番号と焼成温度で特定できるようにし、存在量は％で表した。表３中、ｎ．ｄ．は検出されなかったことを示す。 The highly basic aluminum chloride solutions obtained in Examples 1 to 3, Comparative Example 1 and Comparative Example 3 were fired at 900 ° C., 1000 ° C. and 1100 ° C., and the fired powder obtained by each firing was EDX (TM3030plus: Elemental analysis was performed with energy dispersive X-rays manufactured by Hitachi High-Technologies Corporation), and the abundances of Al, Ca and S are shown in Table 3. In Table 3, the numbers of Examples and Comparative Examples and the firing temperature can be specified, and the abundance is expressed in%. In Table 3, n. d. Indicates that it was not detected.
実施例１の９００℃、１０００℃、１１００℃で焼成した試料のＸ線回折装置（ＳｍａｒｔＬａｂ９ｋＷ：ＲＩＧＡＫＵ株式会社製）で測定したＸ線回折図を、それぞれ図１、図２および図３として示す。同じく、比較例３の焼成した試料も同じく９００℃、１０００℃、１１００℃で焼成した試料のＸ線回折装置（ＳｍａｒｔＬａｂ９ｋＷ：ＲＩＧＡＫＵ株式会社製）で測定したＸ線回折図を、それぞれ図４、図５および図６として示す。 The X-ray diffraction patterns of the sample fired at 900 ° C., 1000 ° C., and 1100 ° C. of Example 1 measured by an X-ray diffractometer (SmartLab 9kW: manufactured by RIGAKU Co., Ltd.) are shown as FIGS. 1, 2, and 3, respectively. Similarly, the X-ray diffraction patterns of the samples fired in Comparative Example 3 also measured at 900 ° C., 1000 ° C., and 1100 ° C. with an X-ray diffractometer (SmartLab9kW: manufactured by RIGAKU Co., Ltd.) are shown in FIGS. 4 and 4, respectively. 5 and FIG. 6 are shown.
上記表１に示すように、実施例１～実施例３、比較例３においては、炭酸源になるものを配合系に含まないため、比較例１、比較例２に見られるように液合成時に炭酸由来の泡立ちが合成時に発生せず、生産性の悪化を招くことはなかった。一方で比較例１、比較例２においては炭酸由来の発泡が合成時に発生するため、発泡が終わるまで次原料が投入できない等の不具合があり、生産性を悪化させることが明確になった。 As shown in Table 1 above, in Examples 1 to 3 and Comparative Example 3, since the compounding system does not contain a carbonic acid source, as seen in Comparative Example 1 and Comparative Example 2, during liquid synthesis. Carbonic acid-derived foaming did not occur during synthesis, and productivity did not deteriorate. On the other hand, in Comparative Examples 1 and 2, since carbonic acid-derived foaming occurs at the time of synthesis, there is a problem that the next raw material cannot be added until the foaming is completed, and it is clarified that the productivity is deteriorated.
また、表１に示すように実施例１～実施例３、比較例１においては、液合成直後、３０℃で１か月経過後および１０℃で１か月経過後において液の濁り等は発生しないが、比較例２においては、合成直後においてもわずかに濁りが発生し、３０℃で１か月経過後も濁りは改善しない。更に、比較例２を１０℃で１か月経過すると微結晶のようなものが析出し、液の濁りが強くなる。これはリンゴ酸が塩基性乳酸アルミニウム溶液との相溶性があまりよくなく、特に低温にすることにより、相溶性が悪化することで微結晶の析出及び濁りの悪化が顕著になると考えられる。比較例３は液合成直後及び１０℃で１か月経過後には問題ないが、３０℃で１か月経過すると白濁が生じた。理由としては、硫酸イオンが多く含まれるために水酸化アルミニウム微結晶が析出し、白濁を発生させていると推測される。 Further, as shown in Table 1, in Examples 1 to 3 and Comparative Example 1, turbidity of the liquid occurred immediately after the liquid synthesis, after 1 month at 30 ° C. and after 1 month at 10 ° C. However, in Comparative Example 2, turbidity was slightly generated immediately after the synthesis, and the turbidity did not improve even after 1 month at 30 ° C. Further, when Comparative Example 2 is allowed to pass at 10 ° C. for 1 month, something like microcrystals is precipitated and the liquid becomes more turbid. This is because malic acid is not very compatible with the basic aluminum lactate solution, and it is considered that the compatibility is deteriorated by lowering the temperature, and the precipitation of microcrystals and the deterioration of turbidity become remarkable. In Comparative Example 3, there was no problem immediately after the liquid synthesis and after 1 month at 10 ° C., but cloudiness occurred after 1 month at 30 ° C. It is presumed that the reason is that aluminum hydroxide microcrystals are precipitated due to the large amount of sulfate ions, causing cloudiness.
上記表２に示すように、粉の色状態をＬ＊ａ＊ｂ＊表色系で表示した。実施例１、比較例１をそれぞれ９００℃、１０００℃、１１００℃で焼成したもの、実施例２、実施例３を１０００℃で焼成したものについては、Ｌ＊値が１０前後と高く、ａ＊が負の値をとり、ｂ＊値が０に近い値をとっているため、明るいやや緑味を帯びた白色の粉である事を裏付けている。一方で比較例３を９００℃、１０００℃で焼成した試料はＬ＊が低く、ａ＊及びｂ＊の値が±１程度になっている事より、黒色を呈する粉になっていることがわかる。また比較例３を１１００℃で焼成するとＬ＊値が１０前後と高く、ａ＊が負の値をとり、ｂ＊値が０に近い値をとり、明るいやや緑味を帯びた白色の粉である事が確認された。これにより比較例３においては１０００℃以下では焼成によって熱分解しにくい残渣（例えば炭素分、硫黄分、窒素分等）が粉表面に残っており、１１００℃焼成において残渣が飛散することにより、粉が白色となることから、比較例３には系の中に残渣になりやすいものが含まれていることが考えられる。 As shown in Table 2 above, the color state of the powder is indicated by the L * a * b * color system. Examples 1 and 1 were fired at 900 ° C., 1000 ° C. and 1100 ° C., respectively, and Examples 2 and 3 were fired at 1000 ° C. had a high L * value of around 10 and a *. Has a negative value and the b * value is close to 0, which confirms that it is a bright, slightly greenish white powder. On the other hand, the sample obtained by firing Comparative Example 3 at 900 ° C. and 1000 ° C. has a low L *, and the values of a * and b * are about ± 1, indicating that the powder exhibits a black color. .. Further, when Comparative Example 3 is fired at 1100 ° C., the L * value is as high as around 10, a * takes a negative value, the b * value takes a value close to 0, and it is a bright, slightly greenish white powder. It was confirmed that there was. As a result, in Comparative Example 3, a residue (for example, carbon content, sulfur content, nitrogen content, etc.) that is difficult to be thermally decomposed by firing at 1000 ° C. or lower remains on the powder surface, and the residue is scattered at 1100 ° C. Since is white, it is considered that Comparative Example 3 contains a substance that tends to be a residue in the system.
上記表３のＥＤＸ結果に示すように、比較例３の９００℃、１０００℃、１１００℃焼成においては、実施例１～３、比較例１には確認できない硫黄分が検出される。またＥＤＸでは検出限界により判断できないが、９００℃、１０００℃焼成において、黒色を示していたのは、系内に含まれる炭素要因の残渣であると推定される。硫黄分に関しては原料で使用されている硫酸イオン由来の硫黄が残っているものと推測される。また炭素分に関しては、硫黄分等と乳酸等の反応により、１０００℃以下の焼成において熱分解しづらい炭素源となり、実施例１～３及び比較例１には見られない残渣として残ったものと推定される。即ち、硫酸イオンが何らかの塩基性乳酸アルミニウムの熱分解阻害の要因であると推測される。 As shown in the EDX results in Table 3 above, in the firing at 900 ° C., 1000 ° C. and 1100 ° C. of Comparative Example 3, sulfur content which cannot be confirmed in Examples 1 to 3 and Comparative Example 1 is detected. Although it cannot be determined by the detection limit in EDX, it is presumed that the black color in the firing at 900 ° C. and 1000 ° C. is the residue of the carbon factor contained in the system. Regarding the sulfur content, it is presumed that the sulfur derived from the sulfate ion used in the raw material remains. Regarding the carbon content, due to the reaction between sulfur content and the like and lactic acid and the like, it became a carbon source that was difficult to be thermally decomposed by firing at 1000 ° C. or lower, and remained as a residue not found in Examples 1 to 3 and Comparative Example 1. Presumed. That is, it is presumed that sulfate ion is a factor of some kind of inhibition of thermal decomposition of basic aluminum lactate.
図１と図４、図２と図５を比較すると、各９００℃、１０００℃で焼成した試料のＸ線回折図を示したものであるが、いずれも主にγ-アルミナに帰属されるピークを示しているが、実施例１を基に焼成した図１、図２のほうが、比較例３を基に焼成した図４、図５よりもピークが鮮明且つ強度が高くでており、実施例１を基にしたほうが、比較例３を基にしたものより、焼結が進んでいることが確認できる。これは表３の説明でも述べたように、熱分解残渣が焼結阻害を起こしているためと推測される。 Comparing FIGS. 1 and 4 and FIGS. 2 and 5, the X-ray diffraction patterns of the samples calcined at 900 ° C and 1000 ° C are shown, both of which are peaks mainly attributed to γ-alumina. However, FIGS. 1 and 2 fired based on Example 1 have clearer peaks and higher intensity than FIGS. 4 and 5 fired based on Comparative Example 3, and the example shows. It can be confirmed that the sintering is more advanced in the case based on 1 than in the case based on Comparative Example 3. It is presumed that this is because the pyrolysis residue causes sintering inhibition as described in the explanation of Table 3.
図３と図６を比較すると、図３はα－アルミナに帰属されるピークが強度高く検出されており、１１００℃でα－アルミナに転移していることが確認された。一方で図６ではα－アルミナに帰属されるピークも見られるが、Ａｌ４Ｏ４Ｃと予測されるピークも見られる。これは上の段落でも記載した残渣が焼結阻害を起こし、１１００℃でα－アルミナになり切れないものを成分として残していることを裏付けるものである。 Comparing FIGS. 3 and 6, it was confirmed that the peak attributed to α-alumina was detected with high intensity and that the peak was transferred to α-alumina at 1100 ° C. On the other hand, in FIG. 6, a peak attributed to α-alumina can be seen, but a peak predicted to be Al 4 O 4 C can also be seen. This confirms that the residue described in the above paragraph causes sintering inhibition and leaves a component that cannot be completely converted to α-alumina at 1100 ° C.
比較例３の内容記載したような残渣による焼結阻害を起こすものを残したり、狙いの結晶相への転移が十分できないとその部分が欠陥となり、セラミックスの破壊起点や熱伝導させた際のムラを発生させる原因等になるため、実施例１のように焼成時に残渣が少なく、目的とする温度で目的とする結晶系に転移をさせることは、セラミック形成用バインダーの果たす役割としては、非常に重要である。 If something that causes sintering inhibition due to the residue as described in Comparative Example 3 is left, or if the transition to the target crystal phase is not sufficient, that part becomes a defect, and the starting point of fracture of the ceramics and unevenness when heat is conducted. As in Example 1, there is little residue during firing, and it is very important for the ceramic forming binder to transfer to the target crystal system at the target temperature. is important.
本発明による塩基性乳酸アルミニウム溶液は、アルミナ粉体合成、アルミナコーティ
ング用途だけではなく、純度の高いアルミニウム源として化粧品原料、医薬品原料、電子材料等の各種用途にも使用可能である。
The basic aluminum lactate solution according to the present invention can be used not only for alumina powder synthesis and alumina coating, but also for various uses such as cosmetic raw materials, pharmaceutical raw materials, and electronic materials as a high-purity aluminum source.
Claims (6)
セラミックス形成用の塩基性乳酸アルミニウム溶液であって、塩基性乳酸アルミニウム溶液が、
塩基度６７～８５％であり、
Ａｌを、Ａｌ２Ｏ３に換算して、８～１３重量％、Ｆｅを０～５０ｐｐｍ、Ｃａを０～５０ｐｐｍ、Ｍｇを０～５０ｐｐｍおよびＳｉを０～５０ｐｐｍの量で含み、
アルカリ金属元素イオンを０～１重量％の量、塩素イオンを０～１．０重量％の量で含み、
更に炭酸イオン、硫酸イオンおよびリン酸イオンの３種を総量で０～５００ｐｐｍの量で、かつそれら３種を個別に０～２００ｐｐｍの量で含有する、
塩基性乳酸アルミニウム溶液の製造方法。 An aluminum chloride solution, an alkali metal aluminate solution, and water are mixed to form a gelled product of aluminum hydroxide. After washing the gelled product with water, water is added to obtain an aluminum hydroxide slurry, and then lactic acid is added. Characterized by adding and reacting,
A basic aluminum lactate solution for forming ceramics, the basic aluminum lactate solution is
The basicity is 67-85%,
Al is converted into Al 2 O 3 , and contains 8 to 13% by weight, Fe in an amount of 0 to 50 ppm, Ca in an amount of 0 to 50 ppm, Mg in an amount of 0 to 50 ppm, and Si in an amount of 0 to 50 ppm.
Alkali metal element ion is contained in an amount of 0 to 1% by weight, and chlorine ion is contained in an amount of 0 to 1.0% by weight.
Further, the three types of carbonate ion, sulfate ion and phosphate ion are contained in a total amount of 0 to 500 ppm, and these three types are individually contained in an amount of 0 to 200 ppm.
A method for producing a basic aluminum lactate solution.
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| JPS5780340A (en) * | 1980-11-05 | 1982-05-19 | Taki Chem Co Ltd | Preparation of basic aluminum lactate |
| JPS5863770A (en) * | 1981-10-09 | 1983-04-15 | Taki Chem Co Ltd | Binder |
| JPS61172847A (en) * | 1985-01-28 | 1986-08-04 | Musashino Kagaku Kenkyusho:Kk | Production of basic aluminum lactate |
| JPH092999A (en) * | 1995-06-16 | 1997-01-07 | Taki Chem Co Ltd | Production of aluminum lactate crystal |
| JP2012131744A (en) * | 2010-12-22 | 2012-07-12 | Taki Chem Co Ltd | Basic aluminum lactate aqueous solution and production method of the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5780340A (en) * | 1980-11-05 | 1982-05-19 | Taki Chem Co Ltd | Preparation of basic aluminum lactate |
| JPS5863770A (en) * | 1981-10-09 | 1983-04-15 | Taki Chem Co Ltd | Binder |
| JPS61172847A (en) * | 1985-01-28 | 1986-08-04 | Musashino Kagaku Kenkyusho:Kk | Production of basic aluminum lactate |
| JPH092999A (en) * | 1995-06-16 | 1997-01-07 | Taki Chem Co Ltd | Production of aluminum lactate crystal |
| JP2012131744A (en) * | 2010-12-22 | 2012-07-12 | Taki Chem Co Ltd | Basic aluminum lactate aqueous solution and production method of the same |
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |