JP2019525984A - 顆粒の製造方法、及び顆粒とその使用方法 - Google Patents
顆粒の製造方法、及び顆粒とその使用方法 Download PDFInfo
- Publication number
- JP2019525984A JP2019525984A JP2019501998A JP2019501998A JP2019525984A JP 2019525984 A JP2019525984 A JP 2019525984A JP 2019501998 A JP2019501998 A JP 2019501998A JP 2019501998 A JP2019501998 A JP 2019501998A JP 2019525984 A JP2019525984 A JP 2019525984A
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- JP
- Japan
- Prior art keywords
- range
- alkali metal
- acid
- present
- granules
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 239000007864 aqueous solution Substances 0.000 claims abstract description 51
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- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- NNNSKJSUQWKSAM-UHFFFAOYSA-L magnesium;dichlorate Chemical compound [Mg+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O NNNSKJSUQWKSAM-UHFFFAOYSA-L 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000002663 nebulization Methods 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000001254 oxidized starch Substances 0.000 description 1
- 235000013808 oxidized starch Nutrition 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 229960001639 penicillamine Drugs 0.000 description 1
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 108040007629 peroxidase activity proteins Proteins 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
- 229960001553 phloroglucinol Drugs 0.000 description 1
- 150000003007 phosphonic acid derivatives Chemical class 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001515 polyalkylene glycol Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 108010064470 polyaspartate Proteins 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920006306 polyurethane fiber Polymers 0.000 description 1
- SATVIFGJTRRDQU-UHFFFAOYSA-N potassium hypochlorite Chemical compound [K+].Cl[O-] SATVIFGJTRRDQU-UHFFFAOYSA-N 0.000 description 1
- IFIDXBCRSWOUSB-UHFFFAOYSA-M potassium;1,5-dichloro-4,6-dioxo-1,3,5-triazin-2-olate Chemical compound [K+].ClN1C(=O)[N-]C(=O)N(Cl)C1=O IFIDXBCRSWOUSB-UHFFFAOYSA-M 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004094 preconcentration Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000011012 sanitization Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 125000003548 sec-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- MSFGZHUJTJBYFA-UHFFFAOYSA-M sodium dichloroisocyanurate Chemical compound [Na+].ClN1C(=O)[N-]C(=O)N(Cl)C1=O MSFGZHUJTJBYFA-UHFFFAOYSA-M 0.000 description 1
- 229940073490 sodium glutamate Drugs 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 235000019351 sodium silicates Nutrition 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- ZTWTYVWXUKTLCP-UHFFFAOYSA-N vinylphosphonic acid Chemical compound OP(O)(=O)C=C ZTWTYVWXUKTLCP-UHFFFAOYSA-N 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- SRWMQSFFRFWREA-UHFFFAOYSA-M zinc formate Chemical compound [Zn+2].[O-]C=O SRWMQSFFRFWREA-UHFFFAOYSA-M 0.000 description 1
- 239000011670 zinc gluconate Substances 0.000 description 1
- 235000011478 zinc gluconate Nutrition 0.000 description 1
- 229960000306 zinc gluconate Drugs 0.000 description 1
- 239000011576 zinc lactate Substances 0.000 description 1
- 235000000193 zinc lactate Nutrition 0.000 description 1
- 229940050168 zinc lactate Drugs 0.000 description 1
- JDLYKQWJXAQNNS-UHFFFAOYSA-L zinc;dibenzoate Chemical compound [Zn+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 JDLYKQWJXAQNNS-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0047—Detergents in the form of bars or tablets
- C11D17/0065—Solid detergents containing builders
- C11D17/0073—Tablets
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/36—Racemisation of optical isomers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/02—Preparation in the form of powder by spray drying
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3245—Aminoacids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
(a)
(A1)メチルグリシン二酢酸(MGDA)のL−及びD−鏡像体の混合物であって、5〜95%の範囲の鏡像体過剰率(ee)を有するそれぞれのL−異性体を主に含有する混合物の少なくとも1種のアルカリ金属塩、
(A2)グルタミン酸二酢酸(GLDA)のL−及びD−鏡像体又は鏡像異性的に純粋なL−GLDAの少なくとも1種のアルカリ金属塩、
の水溶液であって、
(A1)及び(A2)の質量比が1:9〜9:1の範囲にある、
水溶液を提供する工程、
(b)前記溶液を少なくとも125℃のガス入口温度で噴霧造粒する工程
を含む方法に関する。
(A1)メチルグリシン二酢酸(MGDA)のL−及びD−鏡像体の混合物であって、5〜95%の範囲の鏡像体過剰率(ee)を有するそれぞれのL−異性体を主に含有する混合物の少なくとも1種のアルカリ金属塩、
(A2)グルタミン酸二酢酸(GLDA)のL−及びD−鏡像体又は鏡像異性的に純粋なL−GLDAの少なくとも1種のアルカリ金属塩、
を分子分散の形態で含有し、
(A1)及び(A2)の質量比は1:9〜9:1の範囲にある。
(a)少なくとも2種のアミノポリカルボン酸の塩(A)の水溶液を提供する
ことから開始する。
[CH3−CH(COO)−N(CH2−COO)2]M3−xHx (Ia)
(式中、
Mは、同一又は異なるアルカリ金属カチオン、例えば、リチウム、ナトリウム、カリウム、ルビジウム、セシウムのカチオン、及び前述のうち少なくとも2つの組み合わせから選択される。アルカリ金属カチオンの好ましい例は、ナトリウム及びカリウム並びにナトリウム及びカリウムの組み合わせである)
による化合物から選択される。
[OOC−CH2CH2C−CH(COO)−N(CH2−COO)2]M4−xHx (Ib)
(式中、
Mは、上記で定義したように、同一又は異なるアルカリ金属カチオンから選択され、
式(Ib)中のxは、0〜2.0の範囲であり、好ましくは0〜0.5である。特に好ましい実施形態では、xは0である)
による化合物から選択される。
(A2)グルタミン酸二酢酸(GLDA)のL−及びD−鏡像体又は鏡像異性的に純粋なL−GLDAの少なくとも1種のアルカリ金属塩、
を含有し、(A1)及び(A2)の質量比が1:9〜9:1の範囲にある、
水溶液が得られる。
(A1)メチルグリシン二酢酸(MGDA)のL−及びD−鏡像体の混合物であって、5〜95%の範囲の鏡像体過剰率(ee)を有するそれぞれのL−異性体を主に含有する混合物の少なくとも1種のアルカリ金属塩、
(A2)グルタミン酸二酢酸(GLDA)のL−及びD−鏡像体又は鏡像異性的に純粋なL−GLDAの少なくとも1種のアルカリ金属塩
を分子分散の形態で含有し、
(A1)及び(A2)の質量比が1:9〜9:1の範囲にある顆粒に関する。モルはアニオンに関する。
R2は、同一又は異なり、水素及び直鎖C1〜C10−アルキルから選択され、好ましくは各場合において同一であり、エチル、特に好ましくは水素又はメチルであり、
R3は、分岐又は直鎖のC8〜C22−アルキルから選択され、例えば、n−C8H17、n−C10H21、n−C12H25、n−C14H29、n−C16H33又はn−C18H37であり、
R4は、C1〜C10−アルキル、メチル、エチル、n−プロピル、イソプロピル、n−ブチル、イソブチル、sec−ブチル、tert−ブチル、n−ペンチル、イソペンチル、sec−ペンチル、ネオペンチル、1,2−ジメチルプロピル、イソアミル、n−ヘキシル、イソヘキシル、sec−ヘキシル、n−ヘプチル、n−オクチル、2−エチルヘキシル、n−ノニル、n−デシル又はイソデシルから選択される)
の化合物である。
R2は、同一又は異なり、水素及び直鎖C1〜C0−アルキルから選択され、好ましくは各場合とも同一であり、エチル、特に好ましくは水素又はメチルであり、
R5は、分岐又は直鎖のC6〜C20−アルキルから選択され、特に、n−C8H17、n−C10H21、n−C12H25、n−C13H27、n−C15H31、n−C14H29、n−C16H33、n−C18H37であり、
aは、0〜10の、好ましくは1〜6の範囲の数字であり、
bは、1〜80の、好ましくは4〜20の範囲の数字であり、
dは、0〜50の、好ましくは4〜25の範囲の数字である)
の化合物である。
R2は、同一又は異なり、水素及び直鎖C1〜C10−アルキルから選択され、好ましくは各場合とも同一であり、エチル、特に好ましくは水素又はメチルであり、
R3は、分岐又は直鎖のC8〜C22−アルキルから選択され、例えば、イソ−C11H23、イソ−C13H27、n−C8H17、n−C10H21、n−C12H25、n−C14H29、n−C16H33又はn−C18H37であり、
R5は、C6〜C20−アルキル、例えばn−ヘキシル、イソヘキシル、sec−ヘキシル、n−ヘプチル、n−オクチル、2−エチルヘキシル、n−ノニル、n−デシル、イソデシル、n−ドデシル、n−テトラデシル、n−ヘキサデシル、及びn−オクタデシルから選択される)
の化合物である。
R6は、C1〜C4−アルキル、特にエチル、n−プロピル又はイソプロピルであり、
R7は、−(CH2)2−R6であり、
G1は、4個〜6個の炭素原子を有する単糖から、特にグルコース及びキシロースから選択され、
yは、1.1〜4の範囲にあり、yは平均数である)
の化合物が、同様に好適である。
AOは、エチレンオキシド、プロピレンオキシド及びブチレンオキシドから選択され、
EOは、エチレンオキシド、CH2CH2−Oであり、
R8は、分岐又は直鎖のC8〜C18−アルキルから選択され、R5は、上記のように定義され、
A3Oは、プロピレンオキシド及びブチレンオキシドから選択され、
wは、15〜70の、好ましくは30〜50の範囲の数字であり、
w1及びw3は、1〜5の範囲の数字であり、
w2は、13〜35の範囲の数字である)
の化合物である。
R9R10R11N→O (IX)
(式中、R9、R10及びR11は、脂肪族、脂環式又はC2〜C4−アルキレンC10〜C20−アルキルアミド部分から互いに独立して選択される。好ましくは、R9はC8〜C20−アルキル又はC2〜C4−アルキレンC10〜C20−アルキルアミドから選択され、R10及びR11は両方ともメチルである)の化合物である。
25℃及び50%の相対湿度で24時間の期間にわたって貯蔵することにより、吸湿性を判定した。別の方法において、いわゆる熱帯条件は、35℃及び70〜90%の相対湿度で24時間の期間にわたる貯蔵である。グレード:ゼロ(自由に流動する顆粒/粉末)から4(顆粒/粉末が溶解している)。
I.1 L−アラニン及びL−グルタミン酸の部分的に中和された溶液の提供
撹拌反応器中で、400.9g(4.46モル)のL−アラニン、234.0g(2.93モル)の50%水溶液としての水酸化ナトリウム、及び832.2gの水を70℃で混合した。次いで、665.2g(3.55モル)のL−グルタミン酸塩ナトリウム一水和物を添加した。混合物を、完全に透明になるまで60〜70℃で撹拌した。
上記の供給溶液を、3つの攪拌タンク反応器のカスケードで行われたストレッカー合成に使用した。
(c2.1−1)低温鹸化:
低温鹸化を2つの攪拌タンク反応器と管状反応器のカスケードで行った。全ての反応器において温度は約55℃であった。
高温鹸化は、180℃及び24バールで、管状プラグ流反応器中30分の滞留時間で行った。定常状態条件下で得られた溶液を970ミリバール、97℃で撹拌反応器中で処理した。次いでそれをワイプ式フィルム蒸発器中110℃及び900mbarでストリッピングしてさらにアンモニアを蒸発させた。次に、全錯化剤(A.1)の濃度を約40質量%に調整した(鉄結合能に基づく)。
L−アラニン:0.56
L−グルタミン酸ナトリウム一水和物:0.44
部分的中和に使用した水酸化ナトリウム:0.36
ホルムアルデヒド=1.97
HCN=1.99
NaOH(部分的中和と低温鹸化で追加したNaOHの合計):3.04
8,941gのMGDA−Na3(39.6質量%水溶液、ee=35%、回転値=0.76)及び9,010gのGLDA−Na4(39.4質量%水溶液、ee=95%、回転値=2.74)の混合物を、それぞれの溶液を混合して製造した。得られた溶液は、MGDA/GLDA1:1(39.5質量%水溶液、全体の回転値=1.75)の混合物であった。
(A1.2)及び(A2.2)の水溶液(I.を参照)、全固形分40.6%、温度20℃、を提供した。
Claims (12)
- 少なくとも2種のアミノポリカルボン酸の塩(A)の顆粒を製造する方法に関し、以下の工程、
(a)
(A1)メチルグリシン二酢酸(MGDA)のL−及びD−鏡像体の混合物であって、5〜95%の範囲の鏡像体過剰率(ee)を有するそれぞれのL−異性体を主に含有する混合物の少なくとも1種のアルカリ金属塩、
(A2)グルタミン酸二酢酸(GLDA)のL−及びD−鏡像体又は鏡像異性的に純粋なL−GLDAの少なくとも1種のアルカリ金属塩、
の水溶液であって、
(A1)及び(A2)の質量比が1:9〜9:1の範囲にある、
水溶液を提供する工程、
(b)前記溶液を少なくとも125℃のガス入口温度で噴霧造粒する工程
を含む方法。 - 工程(a)で提供される前記水溶液が、45〜65質量%の範囲の(A)の濃度を有する、請求項1に記載の方法。
- 工程(b)を流動床又は噴流床で行う請求項1又は2に記載の方法。
- アミノポリカルボン酸のアルカリ金属塩(A)が、メチルグリシン二酢酸及びグルタミン酸二酢酸のナトリウム塩及びカリウム塩から選択され、各場合とも完全に中和される、請求項1〜3のいずれか一項に記載の方法。
- 前記流動床中の粒子が100〜800μmの範囲の平均直径(D50)を有する、請求項1から4のいずれか一項に記載の方法。
- 工程(b)で噴霧造粒に供された前記水溶液が、シリカ、ケイ酸塩及び有機(コ)ポリマーから選択される少なくとも1種の添加剤をさらに含有する、請求項1から5のいずれか一項に記載の方法。
- アミノポリカルボン酸のアルカリ金属塩(A1)が、一般式(I)
[CH3−CH(COO)−N(CH2−COO)2]M3−xHx (I)
(式中、
Mは、同一又は異なるアルカリ金属カチオンから選択され、
xは、0〜1.0の範囲である)
による化合物から選択される、請求項1〜6のいずれか一項に記載の方法。 - 5〜15質量%の範囲の残留水分含量を有する顆粒であって、
(A1)メチルグリシン二酢酸(MGDA)のL−及びD−鏡像体の混合物であって、10〜95%の範囲の鏡像体過剰率(ee)を有するそれぞれのL−異性体を主に含有する混合物の少なくとも1種のアルカリ金属塩、及び
(A2)グルタミン酸二酢酸(GLDA)のL−及びD−鏡像体又は鏡像異性的に純粋なL−GLDAの少なくとも1種のアルカリ金属塩、
を分子分散の形態で含有し、
(A1)及び(A2)の質量比が1:9〜9:1の範囲にある顆粒。 - 350〜900μmの範囲の平均粒径(D50)を有する請求項8に記載の顆粒。
- 硬質表面洗浄剤又は洗濯洗剤の製造のための請求項8又は9に記載の顆粒の使用方法。
- 前記硬質表面洗浄剤が自動食器洗浄機洗剤である請求項10に記載の使用方法。
- 請求項8又は9に記載の顆粒から選択される顆粒から、自動食器洗浄機用の錠剤を製造する方法。
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