EP1131400A1 - Verfahren zur herstellung von tensidgranulaten - Google Patents
Verfahren zur herstellung von tensidgranulatenInfo
- Publication number
- EP1131400A1 EP1131400A1 EP99963299A EP99963299A EP1131400A1 EP 1131400 A1 EP1131400 A1 EP 1131400A1 EP 99963299 A EP99963299 A EP 99963299A EP 99963299 A EP99963299 A EP 99963299A EP 1131400 A1 EP1131400 A1 EP 1131400A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- aqueous
- surfactant
- anionic surfactants
- granulation
- 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
- 239000008187 granular material Substances 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 239000004094 surface-active agent Substances 0.000 claims abstract description 53
- 238000001035 drying Methods 0.000 claims abstract description 26
- 238000005469 granulation Methods 0.000 claims abstract description 16
- 230000003179 granulation Effects 0.000 claims abstract description 16
- 239000003945 anionic surfactant Substances 0.000 claims description 48
- 239000006072 paste Substances 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 33
- 238000002360 preparation method Methods 0.000 claims description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000013543 active substance Substances 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 239000012459 cleaning agent Substances 0.000 claims description 8
- 239000004435 Oxo alcohol Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000002537 cosmetic Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000000606 toothpaste Substances 0.000 claims description 3
- 229940034610 toothpaste Drugs 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- 239000003599 detergent Substances 0.000 abstract description 7
- 125000000129 anionic group Chemical group 0.000 abstract 1
- 239000002585 base Substances 0.000 description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- -1 alkyl ether sulfates Chemical class 0.000 description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 16
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 15
- 239000003513 alkali Substances 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 9
- 239000012876 carrier material Substances 0.000 description 9
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 9
- 150000001298 alcohols Chemical class 0.000 description 8
- 150000004679 hydroxides Chemical class 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000002736 nonionic surfactant Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 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 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 159000000003 magnesium salts Chemical class 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- WNWHHMBRJJOGFJ-UHFFFAOYSA-N 16-methylheptadecan-1-ol Chemical compound CC(C)CCCCCCCCCCCCCCCO WNWHHMBRJJOGFJ-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 238000005844 autocatalytic reaction Methods 0.000 description 2
- NOPFSRXAKWQILS-UHFFFAOYSA-N docosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCO NOPFSRXAKWQILS-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- 235000014593 oils and fats Nutrition 0.000 description 2
- 229940055577 oleyl alcohol Drugs 0.000 description 2
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000003760 tallow Substances 0.000 description 2
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- CFOQKXQWGLAKSK-KTKRTIGZSA-N (13Z)-docosen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCCO CFOQKXQWGLAKSK-KTKRTIGZSA-N 0.000 description 1
- DJYWKXYRGAMLRE-QXMHVHEDSA-N (z)-icos-9-en-1-ol Chemical compound CCCCCCCCCC\C=C/CCCCCCCCO DJYWKXYRGAMLRE-QXMHVHEDSA-N 0.000 description 1
- TVPWKOCQOFBNML-SEYXRHQNSA-N (z)-octadec-6-en-1-ol Chemical compound CCCCCCCCCCC\C=C/CCCCCO TVPWKOCQOFBNML-SEYXRHQNSA-N 0.000 description 1
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- XUJLWPFSUCHPQL-UHFFFAOYSA-N 11-methyldodecan-1-ol Chemical compound CC(C)CCCCCCCCCCO XUJLWPFSUCHPQL-UHFFFAOYSA-N 0.000 description 1
- CFOQKXQWGLAKSK-UHFFFAOYSA-N 13-docosen-1-ol Natural products CCCCCCCCC=CCCCCCCCCCCCCO CFOQKXQWGLAKSK-UHFFFAOYSA-N 0.000 description 1
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229920006051 Capron® Polymers 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 229910052936 alkali metal sulfate Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 229960000541 cetyl alcohol Drugs 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004851 dishwashing Methods 0.000 description 1
- 229960000735 docosanol Drugs 0.000 description 1
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 238000007046 ethoxylation reaction Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical class OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 1
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical class Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229940043348 myristyl alcohol Drugs 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- ALSTYHKOOCGGFT-MDZDMXLPSA-N oleyl alcohol Chemical compound CCCCCCCC\C=C\CCCCCCCCO ALSTYHKOOCGGFT-MDZDMXLPSA-N 0.000 description 1
- 238000006384 oligomerization reaction Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 150000003138 primary alcohols Chemical class 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/044—Hydroxides or bases
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/146—Sulfuric acid esters
-
- 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
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
Definitions
- the invention relates to a process for the preparation of anionic surfactant granules by means of granulation and simultaneous drying in the fluidized bed, which is carried out in the presence of volatile bases, and to the use thereof for the production of, in particular, pH-neutral detergents, dishwashing detergents and agents for oral hygiene.
- Anionic surfactants such as alkyl sulfates and alkyl ether sulfates are common surfactants which, due to their high detergency, are widely used in cleaning processes of all kinds. Due to their manufacturing processes, these are usually obtained in salt form as aqueous solutions or pastes, which are converted into their powders or granules, for example, by conventional drying technology, in particular in the spray tower or in granulating devices. At the drying temperatures prevailing there, however, pH-neutral solutions or pastes of the alkyl (ether) sulfates would decompose autocatalytically into the corresponding olefinic base bodies and the corresponding salts of hydrogen sulfate, which themselves act as an acid in aqueous solution.
- such pastes are equipped with a so-called alkali reserve according to the prior art, ie such pastes are treated with an excess of free hydroxides, in particular sodium hydroxide.
- the sodium hydroxide is then able to trap the acid that may form through autocatalysis and thus stop the decomposition process.
- the alkali reserve is added in excess, usually in such amounts that, for example, a fatty alcohol sulfate paste has a pH value above 10, small residual amounts of unused sodium hydroxide always remain in the aqueous solution or paste of the alkyl (ether) sulfates.
- a process for the preparation of surfactant granules containing anionic surfactants is known from German published patent application DE-Al-43 04 062, which granules are produced from aqueous pastes by means of granulation and simultaneous drying.
- aqueous pastes of the anionic surfactants in the acid form and an aqueous alkaline solution are separately charged with a gaseous medium (air, nitrogen) and sprayed into the fluidized bed system separately or combined at a high propellant pressure.
- a gaseous medium air, nitrogen
- the object of the present invention was accordingly to provide a new process for the preparation of surfactant granules containing anionic surfactants which overcomes the disadvantages of the prior art described.
- the new process should continue to effectively prevent the autocatalytic decomposition of the anionic surfactants when they dry.
- the object was achieved if volatile bases were added to the aqueous surfactant pastes containing anionic surfactants (in salt form) before and / or during the granulation and simultaneous drying in the fluidized bed.
- the invention includes the knowledge that anionic surfactant granules are available with the method according to the invention which contain little or no residual amounts of alkaline substances, so that they do not cause any undesirable interactions with perfumes or dyes. Furthermore, the invention includes the knowledge that through the ubiquitous presence of the volatile bases in the fluidized bed even at the most distant parts of the apparatus, for example in the filter, decomposition of dried anionic surfactants already formed can be effectively reduced under thermal stress and wall caking of the decomposed product can be reduced.
- One object of the present invention therefore relates to a process for the production of surfactant granules by granulation and simultaneous drying of an aqueous surfactant preparation containing anionic surfactants in the fluidized bed, characterized in that volatile bases are added before or during the granulation and simultaneous drying.
- aqueous surfactant preparations containing anionic surfactants are used for the process.
- these are aqueous surfactant preparations that only contain anionic surfactants.
- These are preferably used in the form of aqueous pastes, in particular with an active substance content of 25 to 90% by weight, based on aqueous anionic surfactant paste.
- anionic surfactants are fatty alcohol sulfates, fatty alcohol ether sulfates, glycerol ether sulfates, hydroxy mixed ether sulfates, monoglyceride (ether) sulfates, fatty acid amide (ether) sulfates and alkyl oligoglucoside sulfates. If the anionic surfactants contain polyglycol ether chains, they can have a conventional, but preferably a narrow, homolog distribution.
- fatty alcohol sulfates and / or fatty alcohol ether sulfates are preferably used as anionic surfactants. Particularly suitable are those which follow the formula (I)
- R 1 is a linear or branched alkyl and / or alkenyl radical having 6 to 22 carbon atoms
- m is 0 or numbers from 1 to 10
- X is an alkali and / or alkaline earth metal, ammonium, alkylammonium, alkanolammonium or glucammonium.
- Particularly preferred is the use of sulfates based on technical C 12 / ⁇ 4 - or C 12/18 -Alkoholfr hopeen based seed oil on natural oils and fats such as coconut oil, palm oil, tallow or Palstearin or bwz also based on Ziegler alcohols.
- oxo alcohols in the range from C8 to C15 (or their mixtures of the aforementioned linear alcohols made from natural oils and fats or Ziegleral alcohols with oxo alcohols) in the form of their sodium, potassium and / or magnesium salts.
- Typical examples of ether sulfates of alcohols ethoxylated with an average of 1 to 10 and in particular 2 to 5 moles of ethylene oxide are selected from the group capron alcohol, caprylic alcohol, 2-ethylhexyl alcohol, capric alcohol, lauryl alcohol, isotridecyl alcohol, myristyl alcohol, cetyl alcohol, palmoleyl alcohol, stearyl alcohol Isostearyl alcohol, oleyl alcohol, elaidyl alcohol, petroselinyl alcohol, arachyl alcohol, gadoleyl alcohol, behenyl alcohol, erucyl alcohol and brassidyl alcohol and their technical mixtures, in the form of their sodium and / or magnesium salts.
- the ether sulfates can have both a conventional and a narrow homolog distribution.
- aqueous surfactant preparations to be used in accordance with the invention can optionally contain further surfactants or also additives, which are preferably ingredients of detergents and cleaning agents.
- the aqueous surfactant preparations preferably contain nonionic surfactants as further surfactants.
- Suitable nonionic surfactants are liquid alkoxylated, advantageously ethoxylated, in particular primary alcohols with preferably 9 to 18 carbon atoms and an average of 1 to 12 moles of ethylene oxide (EO) per mole of alcohol, the underlying alcohols being linear or methyl-branched in the 2-position, or contain linear and methyl-branched radicals in the mixture, as are usually present in oxo alcohol radicals.
- the nonionic surfactants of the type described are derived from linear alcohols of native origin with 12 to 18 carbon atoms, such as coconut, tallow or oleyl alcohol.
- the degrees of ethoxylation given represent statistical averages, which can be an integer or a fraction for a specific product.
- Preferred alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, nre).
- alcohol ethoxylates are preferred which have an average of 2 to 8 ethylene oxide groups.
- the preferred ethoxylated alcohols include, for example, C -C -oxoalcohol with 7 EO, C ljC 15 -oxoalcohol with 3 EO, 5 EO or 7 EO and in particular C 1 -C 1 4 -
- nonionic surfactants are present in the aqueous surfactant preparations with the anionic surfactants, the amount used can vary widely. As a rule, the nonionic surfactants are present in the aqueous surfactant preparations in amounts of up to 50% by weight, calculated as the active substance and based on the active substance of the surfactants.
- the aqueous surfactant preparation can contain additives, which are preferably ingredients of detergents and cleaning agents, as further constituents, preferably in amounts of 0.001 to 80% by weight, based on the active substance of the aqueous surfactant preparation.
- additives are inorganic builder substances such as zeolite, SKS6, sodium carbonate, sodium sulfate, Aerosil and / or organic builder substances such as starch, cellulose, cellulose ether, microcrystalline cellulose and the like.
- aqueous pastes are preferred as aqueous surfactant preparations which contain exclusively anionic surfactants, in particular fatty alcohol sulfates and / or fatty alcohol ether sulfates in the form of their sodium, potassium and / or magnesium salts.
- Such pastes are commercially available and currently have an addition of aqueous hydroxides as an alkali reserve.
- the aqueous hydroxides according to the prior art are usually added in such amounts that, for example, fatty alcohol sulfate pastes (measured as a 1% by weight aqueous solution) have a pH above 10 have.
- the aqueous hydroxides are added during the production of the fatty alcohol sulfates by means of continuous neutralization.
- the anionic surfactant pastes have such an amount of alkali reserves that the pH is between 7 and 9.5.
- Such pH values of the anionic surfactant pastes can be adjusted during the preparation of the sulfates in the neutralization step after sulfonation of the alcohols by adding the calculated amount of hydroxides, in particular sodium hydroxide. This is particularly recommended for highly viscous anionic surfactant pastes, especially those that have active substance contents of 60 to 90% by weight. The same procedure can be followed for low-viscosity anionic surfactant pastes with active substance contents below 30% by weight.
- low-viscosity anionic surfactant pastes with high alkali reserves, preferably initially with customary inorganic and / or organic acids, for example citric acid, phosphoric acid, lactic acid, glycolic acid. Neutralize gluconic acid or sulfuric acid, especially citric acid, preferably up to a pH between 7 and 9.5. If desired, the acids can also be used to set a low pH below 7, for example in the case of low-viscosity fatty alcohol ether sulfate pastes. In the context of the invention it is of course also possible to use neutral aqueous pastes of anionic surfactants which have not been additionally stabilized by adding hydroxides with an alkali reserve. For the purposes of the present invention, all anionic surfactants (pastes) that have a pH between 7 and 9.5 are considered to be pH-neutral anionic surfactants (pastes).
- bases are preferably to be understood as meaning those compounds which, in the Broenstedt base definition, are capable of taking up protons. This includes compounds which are in themselves bases, such as ammonia or amines, and also compounds which only release bases, such as ammonium carbonate, by decomposition. Such bases are referred to as volatile in the sense of the invention if they are preferably used in the fluidized bed plants prevailing temperatures, especially at 60 ° C and below, are gaseous.
- volatile bases are those which are volatile even at room temperature (about 20 ° C.), such as ammonia and / or mono-, di- and trialkylamines with 1 and / or 2 carbon atoms in the alkyl radical.
- Ammonia is particularly suitable. Ammonia can be used as a gas or in the form of its aqueous solutions such as concentrated ammonia.
- the volatile bases are preferably added in amounts of 0.05 to 5, in particular 0J to 1% by weight, calculated as the active substance content of base and based on the active substance content of anionic surfactants in the aqueous surfactant preparation.
- the volatile bases can be added in accordance with the surfactant pastes containing anionic surfactant directly before they are granulated and simultaneously dried.
- the volatile bases in particular ammonia
- the volatile bases are expediently added in the form of their aqueous solutions, in particular as concentrated ammonia, to the aqueous, anionic surfactants, if appropriate containing pH-neutral preparations, before they are injected into the fluidized bed apparatus and subjected to the granulation and simultaneous drying .
- the aqueous anionic surfactants may contain surfactant preparations which may have previously been adjusted to be pH-neutral and, independently of this, to inject an aqueous base solution into the fluidized bed apparatus.
- the aqueous surfactant preparations with the anionic surfactants into the fluidized bed apparatus via a nozzle and to spray the aqueous base solutions, in particular concentrated ammonia, preferably above the sieve bottom of the fluidized bed apparatus. Since there is negative pressure above the sieve bottom, the aqueous base solution is sucked into the fluidized bed in a simple manner.
- the volatile bases are added to the fluidizing air fed into the fluidized bed apparatus for the granulation and drying.
- the aqueous, optionally pH-neutral, anionic surfactant-containing surfactant preparations are injected into the fluidized bed apparatus and are only granulated and dried there in the presence of the volatile bases, preferably ammonia as gas, supplied with the fluidizing air. It is of course also possible within the scope of the invention to combine two or more of the described embodiments with one another.
- the aqueous surfactant preparations containing anionic surfactants, preferably the aqueous anionic surfactant pastes can be granulated alone or with the addition of solid carrier materials in the fluidized bed and dried at the same time.
- Fluidized bed apparatuses which are preferably used have base plates (sieve bases) with a diameter between 0.4 and 5 m, for example 1.2 m or 2.5 m.
- Perforated floor slabs a Contidur slab (commercial product from Hein & Lehmann, Federal Republic of Germany) or perforated floor slabs can be used as the floor slab, the holes (passage openings) of which are covered by a grid with mesh sizes of less than 600 ⁇ m.
- the grid can be arranged inside or above the passage openings. However, the grid preferably lies directly below the passage openings of the inflow floor.
- the metal gauze preferably consists of the same material as the inflow floor, in particular of stainless steel.
- the mesh size of said grid is preferably between 200 and 400 ⁇ m.
- the process is preferably carried out at swirl air speeds between 1 and 8 m / s and in particular between 1.5 and 5.5 m / s.
- the granules are advantageously discharged via a size classification of the granules. This classification is preferably carried out by means of an opposed air flow (classifier air), which is regulated in such a way that only particles above a certain particle size are removed from the fluidized bed and smaller particles are retained in the fluidized bed.
- classifier air opposed air flow
- the inflowing air is composed of the heated or unheated classifier air and the heated soil air.
- the soil air temperature is preferably between 80 and 400 ° C.
- the fluidizing air cools down through heat losses and through the heat of vaporization and is preferably approximately 5 cm above the base plate 60 to 120 ° C., preferably 65 to 90 ° C. and in particular 70 to 85 ° C.
- the air outlet temperature is preferably between 60 and 120 ° C, in particular below 80 ° C.
- a starting mass is present at the beginning of the process, which serves as an initial carrier for the sprayed-in surfactant paste.
- Suitable starting materials are the surfactant granules themselves, which may contain carrier materials, which have already been obtained in a previous process, or the carrier materials can be used as starting materials.
- surfactant granules with a grain size in the range between 0J and 1.6 mm obtained from one of the preceding process sequences are used as starting mass.
- the granules obtained from the fluidized bed are then preferably cooled in a separate fluidized bed and classified by means of a sieve into granules with grain sizes between 0J and 1.6 mm as good grain fraction and in granules over 1.6 mm as Uberkom fraction, while particles below 0.1 mm already get into an exhaust air filter during drying in the fluidized bed, separated from the exhaust air there and then fed back into the fluidized bed as germ material.
- the Uberkom fraction is ground and also returned to the fluidized bed.
- the surfactant granules are regarded as dried if the free water content is preferably below 10% by weight, in particular from 0J to 2% by weight, based in each case on the finished granules.
- Surfactant granules with a high bulk density are obtained by the process according to the invention, preferably above 500 g / 1 and in particular between 550 and 1000 g / 1.
- the active substance content fluctuates depending on the addition of carrier materials used and is in particular above 50% by weight, preferably between 85 and 98% by weight.
- the surfactant granules obtained by the process according to the invention are pH neutral, i.e. after dissolving the surfactant granules in water, the aqueous solution has a pH between 7 and 9.5. Furthermore, the surfactant granules are dust-free and free-flowing and not or hardly sticky, so that they are easy to handle and silage-compatible in big bags.
- the detergents, rinsing agents and cleaning agents can contain the granules according to the invention in customary amounts, preferably in the range from 0J to 50% by weight, based on the agent.
- the surfactant granules produced according to the invention are preferably suitable for the production of pH-neutral washing, rinsing and cleaning agents such as pH-neutral powder cleaners and pH-neutral soaps, as well as for detergents mixed with colorants such as toilet blocks.
- the pH-neutral washing, rinsing and cleaning agents can be in powder, granular or lumpy form.
- Another object of the present invention relates to the use of the granules according to the invention as surfactants for the production of cleaning cosmetics for teeth, hair and skin, in particular for the production of hair shampoos, shower baths, washing lotions, toothpaste and the like.
- These agents can contain the granules according to the invention in amounts of 0J to 30% by weight, based on the agent.
- the use for the production of agents for oral hygiene, in particular for toothpaste, is particularly preferred. Examples
- a 1% aqueous solution of the granules showed a pH of 8.8 at 25 ° C.
- 500 g of this sodium lauryl sulfate granulate were stored in a porcelain bowl in a drying cabinet at 80 ° C. for 72 hours. After this time, no gray spots were found in the product.
- Example 1 10,000 kg of an aqueous paste containing 65% by weight sodium lauryl sulfate (52% C12 / 21% C 14/10% C 16/17% C 18) with a free alkali content of 0.1% .-% sodium hydroxide continuously injected at 2,000 kg per hour at a temperature of 70 ° C into the fluidized bed system (SKET system), the drying air having a temperature of 180 ° C when entering the fluidized bed, and 90 ° C at the outlet.
- the temperature in the fluidized bed was 70 ° C. 24 kg of a 25% aq.
- Ammonia solution were operated in parallel using a positively controlled
- the multi-piston metering pump together with the aqueous surfactant paste is continuously fed into the fluidized bed of the SKET system.
- a 1% aqueous solution of the granules showed a pH of 9.5 at 25 ° C.
- 500 g of this sodium lauryl sulfate granulate were stored in a porcelain bowl in a drying cabinet at 80 ° C. for 72 hours. After this time, no gray spots were found in the product.
- Example 1 10,000 kg of an aqueous paste containing 65% by weight sodium lauryl sulfate (52% C12 / 21% C 14/10% C 16/17% C 18) with a free alkali content of 0J% by weight. % Sodium hydroxide continuously injected at 2,000 kg per hour at a temperature of 70 ° C into the fluidized bed system (SKET system), the drying air having a temperature of 160 ° C when entering the fluidized bed and 90 ° C at the outlet. The temperature in the fluidized bed was 60 ° C.
- a 1% aqueous solution of the granules showed a pH of 9.2 at 25 ° C.
- 500 g of this sodium lauryl sulfate granulate were stored in a porcelain bowl in a drying cabinet at 80 ° C. for 72 hours. After this time, gray specks appeared in the product, which were isolated and had an acidic pH.
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Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19853893A DE19853893A1 (de) | 1998-11-23 | 1998-11-23 | Verfahren zur Herstellung von Tensidgranulaten |
DE19853893 | 1998-11-23 | ||
PCT/EP1999/008763 WO2000031230A1 (de) | 1998-11-23 | 1999-11-13 | Verfahren zur herstellung von tensidgranulaten |
Publications (2)
Publication Number | Publication Date |
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EP1131400A1 true EP1131400A1 (de) | 2001-09-12 |
EP1131400B1 EP1131400B1 (de) | 2010-12-22 |
Family
ID=7888656
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP99963299A Expired - Lifetime EP1131400B1 (de) | 1998-11-23 | 1999-11-13 | Verfahren zur herstellung von tensidgranulaten |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP1131400B1 (de) |
AT (1) | ATE492626T1 (de) |
DE (2) | DE19853893A1 (de) |
ES (1) | ES2357380T3 (de) |
WO (1) | WO2000031230A1 (de) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
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EP2801606A1 (de) * | 2013-05-07 | 2014-11-12 | The Procter and Gamble Company | Sprühgetrocknete Partikel enthaltend Sulfat |
CN117280017A (zh) | 2021-05-10 | 2023-12-22 | 巴斯夫欧洲公司 | 基于异构十三烷醇混合物的醚硫酸盐 |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4216629A1 (de) * | 1992-05-20 | 1993-11-25 | Henkel Kgaa | Verfahren zur Herstellung aniontensidhaltiger Wasch- und Reinigungsmittel |
DE4304062A1 (de) * | 1993-02-11 | 1994-08-18 | Henkel Kgaa | Verfahren zur Herstellung von Tensidgranulaten |
DE19707649C1 (de) * | 1997-02-26 | 1998-10-22 | Henkel Kgaa | Verfahren zur Herstellung von Waschmittelrohstoffen |
DE19710152C2 (de) * | 1997-03-12 | 1999-04-22 | Henkel Kgaa | Verfahren zur Herstellung von Aniontensidgranulaten |
-
1998
- 1998-11-23 DE DE19853893A patent/DE19853893A1/de not_active Withdrawn
-
1999
- 1999-11-13 AT AT99963299T patent/ATE492626T1/de active
- 1999-11-13 WO PCT/EP1999/008763 patent/WO2000031230A1/de active Application Filing
- 1999-11-13 ES ES99963299T patent/ES2357380T3/es not_active Expired - Lifetime
- 1999-11-13 DE DE59915230T patent/DE59915230D1/de not_active Expired - Lifetime
- 1999-11-13 EP EP99963299A patent/EP1131400B1/de not_active Expired - Lifetime
Non-Patent Citations (1)
Title |
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See references of WO0031230A1 * |
Also Published As
Publication number | Publication date |
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DE19853893A1 (de) | 2000-05-25 |
WO2000031230A1 (de) | 2000-06-02 |
EP1131400B1 (de) | 2010-12-22 |
ATE492626T1 (de) | 2011-01-15 |
ES2357380T3 (es) | 2011-04-25 |
DE59915230D1 (de) | 2011-02-03 |
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