EP3417047A1 - Procede de fabrication de savon - Google Patents
Procede de fabrication de savonInfo
- Publication number
- EP3417047A1 EP3417047A1 EP17710333.0A EP17710333A EP3417047A1 EP 3417047 A1 EP3417047 A1 EP 3417047A1 EP 17710333 A EP17710333 A EP 17710333A EP 3417047 A1 EP3417047 A1 EP 3417047A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- soap
- weight
- mixture
- acid
- sodium hydroxide
- 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.)
- Pending
Links
- 239000000344 soap Substances 0.000 title claims abstract description 179
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 239000000203 mixture Substances 0.000 claims abstract description 90
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 74
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 57
- 229930195729 fatty acid Natural products 0.000 claims abstract description 57
- 239000000194 fatty acid Substances 0.000 claims abstract description 57
- 150000003839 salts Chemical class 0.000 claims abstract description 50
- 238000005406 washing Methods 0.000 claims abstract description 48
- 235000011187 glycerol Nutrition 0.000 claims abstract description 37
- 239000007864 aqueous solution Substances 0.000 claims abstract description 34
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 30
- -1 fatty acid ester Chemical class 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 19
- 238000009499 grossing Methods 0.000 claims abstract description 16
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 14
- 238000010411 cooking Methods 0.000 claims abstract description 10
- 239000000159 acid neutralizing agent Substances 0.000 claims abstract description 4
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract 2
- 239000008158 vegetable oil Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 185
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 239000003921 oil Substances 0.000 claims description 26
- 235000019198 oils Nutrition 0.000 claims description 26
- 239000000126 substance Substances 0.000 claims description 17
- 238000010907 mechanical stirring Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000010465 pomace olive oil Substances 0.000 claims description 7
- 235000019864 coconut oil Nutrition 0.000 claims description 6
- 239000003240 coconut oil Substances 0.000 claims description 6
- 241000196324 Embryophyta Species 0.000 claims description 5
- 240000007817 Olea europaea Species 0.000 claims description 5
- 235000019482 Palm oil Nutrition 0.000 claims description 5
- 238000010923 batch production Methods 0.000 claims description 5
- 239000004006 olive oil Substances 0.000 claims description 5
- 235000008390 olive oil Nutrition 0.000 claims description 5
- 239000002540 palm oil Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 235000013311 vegetables Nutrition 0.000 claims 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 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 2
- 235000011837 pasties Nutrition 0.000 claims description 2
- 238000010936 aqueous wash Methods 0.000 claims 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 17
- 238000005360 mashing Methods 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 description 100
- 238000005086 pumping Methods 0.000 description 33
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 22
- 238000007127 saponification reaction Methods 0.000 description 19
- 239000012535 impurity Substances 0.000 description 11
- 239000011780 sodium chloride Substances 0.000 description 11
- 239000002585 base Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000012267 brine Substances 0.000 description 6
- KHAVLLBUVKBTBG-UHFFFAOYSA-N dec-9-enoic acid Chemical compound OC(=O)CCCCCCCC=C KHAVLLBUVKBTBG-UHFFFAOYSA-N 0.000 description 6
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 6
- 239000003925 fat Substances 0.000 description 6
- 235000019197 fats Nutrition 0.000 description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 6
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 6
- SECPZKHBENQXJG-FPLPWBNLSA-N palmitoleic acid Chemical compound CCCCCC\C=C/CCCCCCCC(O)=O SECPZKHBENQXJG-FPLPWBNLSA-N 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- ZQPPMHVWECSIRJ-MDZDMXLPSA-N elaidic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(O)=O ZQPPMHVWECSIRJ-MDZDMXLPSA-N 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000007670 refining Methods 0.000 description 5
- 238000010008 shearing Methods 0.000 description 5
- GWHCXVQVJPWHRF-KTKRTIGZSA-N (15Z)-tetracosenoic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCCCC(O)=O GWHCXVQVJPWHRF-KTKRTIGZSA-N 0.000 description 4
- YWWVWXASSLXJHU-AATRIKPKSA-N (9E)-tetradecenoic acid Chemical compound CCCC\C=C\CCCCCCCC(O)=O YWWVWXASSLXJHU-AATRIKPKSA-N 0.000 description 4
- 235000021292 Docosatetraenoic acid Nutrition 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 4
- MBMBGCFOFBJSGT-KUBAVDMBSA-N all-cis-docosa-4,7,10,13,16,19-hexaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCC(O)=O MBMBGCFOFBJSGT-KUBAVDMBSA-N 0.000 description 4
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 4
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 238000010908 decantation Methods 0.000 description 4
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 4
- 235000020673 eicosapentaenoic acid Nutrition 0.000 description 4
- 229960005135 eicosapentaenoic acid Drugs 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- KEMQGTRYUADPNZ-UHFFFAOYSA-N heptadecanoic acid Chemical compound CCCCCCCCCCCCCCCCC(O)=O KEMQGTRYUADPNZ-UHFFFAOYSA-N 0.000 description 4
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 description 4
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- ISYWECDDZWTKFF-UHFFFAOYSA-N nonadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCCC(O)=O ISYWECDDZWTKFF-UHFFFAOYSA-N 0.000 description 4
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 4
- IJTNSXPMYKJZPR-UHFFFAOYSA-N parinaric acid Chemical compound CCC=CC=CC=CC=CCCCCCCCC(O)=O IJTNSXPMYKJZPR-UHFFFAOYSA-N 0.000 description 4
- 238000009938 salting Methods 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 235000003441 saturated fatty acids Nutrition 0.000 description 4
- 150000004671 saturated fatty acids Chemical class 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- ZDPHROOEEOARMN-UHFFFAOYSA-N undecanoic acid Chemical compound CCCCCCCCCCC(O)=O ZDPHROOEEOARMN-UHFFFAOYSA-N 0.000 description 4
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 4
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 4
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 3
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 3
- 239000005639 Lauric acid Substances 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- 235000021314 Palmitic acid Nutrition 0.000 description 3
- 235000021319 Palmitoleic acid Nutrition 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000003570 air Substances 0.000 description 3
- SECPZKHBENQXJG-UHFFFAOYSA-N cis-palmitoleic acid Natural products CCCCCCC=CCCCCCCCC(O)=O SECPZKHBENQXJG-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 230000003020 moisturizing effect Effects 0.000 description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 3
- 230000003472 neutralizing effect Effects 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 229960002446 octanoic acid Drugs 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- XSXIVVZCUAHUJO-AVQMFFATSA-N (11e,14e)-icosa-11,14-dienoic acid Chemical compound CCCCC\C=C\C\C=C\CCCCCCCCCC(O)=O XSXIVVZCUAHUJO-AVQMFFATSA-N 0.000 description 2
- BBWMTEYXFFWPIF-CJBMEHDJSA-N (2e,4e,6e)-icosa-2,4,6-trienoic acid Chemical compound CCCCCCCCCCCCC\C=C\C=C\C=C\C(O)=O BBWMTEYXFFWPIF-CJBMEHDJSA-N 0.000 description 2
- FPRKGXIOSIUDSE-SYACGTDESA-N (2z,4z,6z,8z)-docosa-2,4,6,8-tetraenoic acid Chemical compound CCCCCCCCCCCCC\C=C/C=C\C=C/C=C\C(O)=O FPRKGXIOSIUDSE-SYACGTDESA-N 0.000 description 2
- YUFFSWGQGVEMMI-JLNKQSITSA-N (7Z,10Z,13Z,16Z,19Z)-docosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCCCC(O)=O YUFFSWGQGVEMMI-JLNKQSITSA-N 0.000 description 2
- TWSWSIQAPQLDBP-CGRWFSSPSA-N (7e,10e,13e,16e)-docosa-7,10,13,16-tetraenoic acid Chemical compound CCCCC\C=C\C\C=C\C\C=C\C\C=C\CCCCCC(O)=O TWSWSIQAPQLDBP-CGRWFSSPSA-N 0.000 description 2
- HOBAELRKJCKHQD-UHFFFAOYSA-N (8Z,11Z,14Z)-8,11,14-eicosatrienoic acid Natural products CCCCCC=CCC=CCC=CCCCCCCC(O)=O HOBAELRKJCKHQD-UHFFFAOYSA-N 0.000 description 2
- HVGRZDASOHMCSK-UHFFFAOYSA-N (Z,Z)-13,16-docosadienoic acid Natural products CCCCCC=CCC=CCCCCCCCCCCCC(O)=O HVGRZDASOHMCSK-UHFFFAOYSA-N 0.000 description 2
- FRPZMMHWLSIFAZ-UHFFFAOYSA-N 10-undecenoic acid Chemical compound OC(=O)CCCCCCCCC=C FRPZMMHWLSIFAZ-UHFFFAOYSA-N 0.000 description 2
- PIFPCDRPHCQLSJ-WYIJOVFWSA-N 4,8,12,15,19-Docosapentaenoic acid Chemical compound CC\C=C\CC\C=C\C\C=C\CC\C=C\CC\C=C\CCC(O)=O PIFPCDRPHCQLSJ-WYIJOVFWSA-N 0.000 description 2
- FKLSONDBCYHMOQ-UHFFFAOYSA-N 9E-dodecenoic acid Natural products CCC=CCCCCCCCC(O)=O FKLSONDBCYHMOQ-UHFFFAOYSA-N 0.000 description 2
- YWWVWXASSLXJHU-UHFFFAOYSA-N 9E-tetradecenoic acid Natural products CCCCC=CCCCCCCCC(O)=O YWWVWXASSLXJHU-UHFFFAOYSA-N 0.000 description 2
- 235000021357 Behenic acid Nutrition 0.000 description 2
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- PIFPCDRPHCQLSJ-UHFFFAOYSA-N Clupanodonic acid Natural products CCC=CCCC=CCC=CCCC=CCCC=CCCC(O)=O PIFPCDRPHCQLSJ-UHFFFAOYSA-N 0.000 description 2
- 235000021298 Dihomo-γ-linolenic acid Nutrition 0.000 description 2
- 235000021294 Docosapentaenoic acid Nutrition 0.000 description 2
- 235000021297 Eicosadienoic acid Nutrition 0.000 description 2
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 description 2
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- OPGOLNDOMSBSCW-CLNHMMGSSA-N Fursultiamine hydrochloride Chemical compound Cl.C1CCOC1CSSC(\CCO)=C(/C)N(C=O)CC1=CN=C(C)N=C1N OPGOLNDOMSBSCW-CLNHMMGSSA-N 0.000 description 2
- 235000021353 Lignoceric acid Nutrition 0.000 description 2
- CQXMAMUUWHYSIY-UHFFFAOYSA-N Lignoceric acid Natural products CCCCCCCCCCCCCCCCCCCCCCCC(=O)OCCC1=CC=C(O)C=C1 CQXMAMUUWHYSIY-UHFFFAOYSA-N 0.000 description 2
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- 239000005643 Pelargonic acid Substances 0.000 description 2
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- 150000001735 carboxylic acids Chemical class 0.000 description 2
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- 238000004448 titration Methods 0.000 description 2
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- 235000013731 Passiflora van volxemii Nutrition 0.000 description 1
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 235000019774 Rice Bran oil Nutrition 0.000 description 1
- 239000003568 Sodium, potassium and calcium salts of fatty acids Substances 0.000 description 1
- 235000019486 Sunflower oil Nutrition 0.000 description 1
- 235000019498 Walnut oil Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 238000010669 acid-base reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000008168 almond oil Substances 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000010478 argan oil Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 235000021302 avocado oil Nutrition 0.000 description 1
- 239000008163 avocado oil Substances 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 239000010495 camellia oil Substances 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010636 coriander oil Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000008524 evening primrose extract Nutrition 0.000 description 1
- 239000010475 evening primrose oil Substances 0.000 description 1
- 229940089020 evening primrose oil Drugs 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 239000008169 grapeseed oil Substances 0.000 description 1
- 159000000011 group IA salts Chemical class 0.000 description 1
- 239000010468 hazelnut oil Substances 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- DNHVXYDGZKWYNU-UHFFFAOYSA-N lead;hydrate Chemical compound O.[Pb] DNHVXYDGZKWYNU-UHFFFAOYSA-N 0.000 description 1
- 239000010501 lemon oil Substances 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 235000021388 linseed oil Nutrition 0.000 description 1
- 239000010469 macadamia oil Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000011929 mousse Nutrition 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000001944 prunus armeniaca kernel oil Substances 0.000 description 1
- 235000015136 pumpkin Nutrition 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 239000008165 rice bran oil Substances 0.000 description 1
- 235000019719 rose oil Nutrition 0.000 description 1
- 239000010666 rose oil Substances 0.000 description 1
- 235000005713 safflower oil Nutrition 0.000 description 1
- 239000003813 safflower oil Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
- 235000013875 sodium salts of fatty acid Nutrition 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000002600 sunflower oil Substances 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- 239000008170 walnut oil Substances 0.000 description 1
- 239000010497 wheat germ oil Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- C11D13/00—Making of soap or soap solutions in general; Apparatus therefor
- C11D13/02—Boiling soap; Refining
-
- 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
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/06—Inorganic compounds
- C11D9/08—Water-soluble compounds
- C11D9/10—Salts
-
- 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
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/22—Organic compounds, e.g. vitamins
- C11D9/26—Organic compounds, e.g. vitamins containing oxygen
- C11D9/265—Organic compounds, e.g. vitamins containing oxygen containing glycerol
Definitions
- the subject of the present invention is a new process for the production of solid soap in batch form, in particular a Marseille soap making process, which is more respectful of the environment, by optimizing the consumption of water and energy necessary for its implementation. implementing and limiting releases.
- the basic principle of the preparation of soaps is based on a saponification reaction in which fatty acids and / or fatty acid esters contained in fatty substances are hydrolysed in a basic medium to form alkaline salts (carboxylates), constituting the soap , and glycerine.
- the base used in the saponification reaction is soda (NaOH)
- the soap obtained is called “hard”
- the base is potassium hydroxide (KOH)
- the soap is called “soft” or "liquid” .
- the properties and the quality of the soap produced also depend on the type of process used for its manufacture, which can be discontinuous (also called “batch” or in tank) according to an "old-fashioned” method where the cooking of the paste was made in a cauldron, or continuous for a more industrial manufacture.
- the mashing and cooking consist in introducing the fatty substances, most often oils or pastes of vegetable origin, rich in fatty acids and / or fatty acid esters, and the aqueous solution of excess sodium hydroxide in a vat or a cauldron large capacity, and mix them by heating at high temperatures of the order of 120 ° C to reach boiling.
- the saponification starts.
- the high temperature makes it possible to initiate the saponification reaction, which is then exothermic and difficult to control. It is therefore often necessary to introduce the soda in several times to prevent a runaway reaction.
- the oils and soda being immiscible, it is generally customary to introduce a soap base from a previous manufacture to facilitate the formation of an emulsion between the oily and aqueous phases.
- the dough is thus cooked up to 12 hours to ensure complete saponification. Indeed, any residual unsaponified oils may rancid, and alter the color and smell of the final soap.
- the terms of pasting and cooking constitute the two stages of the saponification reaction: the pasting designates the start of the saponification reaction, and the baking is aimed at following the reaction, kinetically slower, allowing the complete saponification .
- the salting and washing steps consist essentially in adding salt water to the soap paste obtained during the mashing and baking steps in order to extract the glycerine formed, but also the various impurities present in the raw materials used or in the soap base used, or formed during manufacture due to the operating conditions implemented during the pasting and baking steps.
- the terms “salting out” and “washing” both refer to the same type of operation, the term “salting out” being generally used to designate the first step of washing the obtained soap paste, allowing the extraction of a portion of the dies. impurities and glycerine.
- the salting steps are carried out, washing with a saturated aqueous solution of sodium chloride (360 g of NaCl per liter), at elevated temperature (> 104 ° C.).
- the soap is very slightly soluble in salt water unlike soda and glycerin, it precipitates and can be recovered after decantation.
- an additional smoothing step is necessary to obtain a homogeneous soap paste, having controlled contents of water, salt and sodium to allow its subsequent drying and shaping.
- the smoothing can in particular be carried out by liquidation, that is to say by washing the grained soap with large quantities of pure water to drive the excess salt (NaCl), to boiling, then decantation to remove the water salty.
- the subject of the present invention is therefore a new soap manufacturing process, particularly suitable for the manufacture of Marseille soap, whose consumption of water and energy is reduced compared to traditional Marseille soap making processes, thus limiting the quantities of discharges emitted.
- the Marseille soap thus obtained presents the peculiarity to contain a controlled content of glycerin, resulting from the saponification reaction, without the latter being added to the soap formed.
- the soap must not only be prepared according to the particular process steps described above, but must not be modified by the introduction of additives.
- additive is meant here any ingredient introduced after the saponification, apart from the reagents necessary for the manufacture and the constituents of the washing and smoothing solutions.
- a soap is processable if it comprises, before drying, less than 33% by weight of water, less than 0.7% by weight of salt and less than 0.2 % by weight of free sodium hydroxide (in NaOH form).
- glycerin is a humectant and moisturizing agent for the skin, and gives the soap a creamier mousse. It may therefore be desirable to retain it, at least in part, in the soap during its manufacture, since this could be considered as an additive if it were to be added after soap manufacture, which could impact the product designation. under the term "Marseille soap" according to certain definitions.
- FR 1 337 212, FR 2 008 916 and FR 946 742 describe soap manufacturing processes. However, the purpose of these processes is not to obtain a soap with a controlled glycerin content, but on the contrary is to remove the glycerin soap to recover and value it.
- the present invention therefore proposes a new process for the preparation of soap, and in particular of Marseille soap, comprising the essential steps for the manufacture of Marseille soap implemented in an optimized manner to obtain an efficient and more environmentally friendly process.
- a processable soap that is to say comprising before drying less than 33% by weight of water, less than 0.7% by weight of salt and less than 0.2% by weight of sodium hydroxide free (NaOH)
- said soap comprising a controlled content of glycerine, without it being added as an additive to the soap, to give it moisturizing properties, and therefore better dermatological qualities, and guarantee a creamier foam.
- the object of the invention is, according to a first aspect, a batch soap manufacturing process comprising at least the following steps:
- At least one fatty acid and / or fatty acid ester is mixed with an aqueous solution of sodium hydroxide,
- the soap paste is mixed with an aqueous solution comprising 1 to 42% by weight of a mixture of sodium hydroxide and salt,
- the mixture is heated and left to settle until two phases are formed: the grained soap comprising salt, sodium hydroxide and glycerine, and an aqueous solution comprising salt, sodium hydroxide and glycerine,
- step b. a step of smoothing the grained soap obtained in step b. by neutralization in which:
- the grained soap is mixed with at least one neutralization agent which may be an acid, a fatty acid or a fatty acid ester,
- the invention thus has, according to a second aspect, a smooth soap capable of being manufactured by means of the method described above.
- batch process also called “batch” or in the form of a vessel
- batch process is understood to mean a process in which the soap is manufactured in discrete lots from reagents placed in specified quantities in a tank of specific capacity, as opposed to continuous processes based on a metering pump system which continuously feeds the saponification reactor with raw materials.
- the batch process is preferably carried out in open tanks or reactors, that is to say non-hermetic.
- the various stages are conducted at atmospheric pressure, in the presence of air.
- the process of the invention is preferably carried out in a stirred reactor, guaranteeing the homogeneity of the medium and under mild temperature conditions, losses of material by evaporation can be considerably limited without the need to operate in reactors. sealed.
- the operating conditions make it possible to preserve the quality of the raw materials and not to denature the product during its manufacture and thus to guarantee the quality of the soap obtained.
- the manufacturing method of the invention implements at least one step a. for pasting and cooking in which: at least one fatty acid and / or fatty acid ester is mixed with an aqueous solution of sodium hydroxide,
- the pasting and baking step implements the saponification reaction itself.
- At least one fatty acid and / or fatty acid ester is mixed with an aqueous solution of sodium hydroxide and optionally with brine (an aqueous solution comprising at least 3.5% by weight of sodium chloride (NaCl) preferably between 10 and 30% NaCl).
- brine an aqueous solution comprising at least 3.5% by weight of sodium chloride (NaCl) preferably between 10 and 30% NaCl.
- fatty acid is meant carboxylic acids comprising a hydrocarbon radical, saturated or unsaturated, linear or branched, comprising 6 to 30 carbon atoms, and preferably 12 to 22 carbon atoms.
- saturated fatty acids examples include caproic acid, enanthic acid, caprylic acid, pelargonic acid, capric acid, undecylic acid, lauric acid, tricecylic acid, myristic acid, pentadecyl acid, palmitic acid, margaric acid, stearic acid, nonadecylic acid, eicosanoic acid, behenic acid, tetracosanoic acid, and their mixtures.
- unsaturated fatty acids By way of example of unsaturated fatty acids, mention may be made of sorbic acid, decylenic acid, caproleic acid, undecylenic acid, lauroleic acid, myristoleic acid, pentadecenoic acid, palmitoleic acid, palmiteaic acid, oleic acid, elaidic acid and acid.
- vaccenic linoleic acid, gamma-linolenic acid, alpha-linolenic acid, steradonic acid, parinaric acid or stearidonic acid, gadoleic acid, dihomo-linoleic acid, dihomo-gamma-linolenic acid, arachidonic acid, timnodonic acid or eicosapentaenoic acid, erucic acid, acid brassic acid, cetoleic acid, adrenic acid, clupanodonic acid, docosahexaenoic acid, nervonic acid or selacholeic acid, eicosadienoic acid, eicosatrienoic acid, docosadienoic acid, docosatetraenoic acid, docosapentaenoic acid.
- the fatty acid and / or the fatty acid ester used in step a. is usually contained in a fatty substance, preferably of vegetable origin.
- the fatty acid and / or the fatty acid ester used in step a. is a fatty substance, preferably still, the fatty substance is an oil or a pasty vegetable or plant origin. According to the criteria of some soap makers, the name "Marseille soap" may indeed require the exclusive implementation of vegetable or vegetable fats.
- oil any lipophilic compound, nonionic, insoluble in water and liquid at room temperature (25 ° C) and at atmospheric pressure (760 mmHg, 101 325 Pa).
- insoluble in water means a compound whose solubility at spontaneous pH in water at 25 ° C. and at atmospheric pressure is less than 1%, and preferably less than 0.5%. in weight.
- the oils preferably have a viscosity of less than 500 cPs at 25 ° C at a shear rate of 1 sec -1 .
- Paste means any lipophilic compound, nonionic, insoluble in water and semi-solid or solid at room temperature (25 ° C) and at atmospheric pressure.
- the pastes preferably have a viscosity greater than 500 cPs at 25 ° C. at a shear rate of 1 to 1.
- the fatty substance comprising the fatty acid and / or the fatty acid ester is extracted from A species belonging to the plant kingdom
- olive oil in particular acid olive pomace oil, coconut
- acid olive pomace oil means an acid oil obtained from olive pomace.
- Such an oil may, for example, be derived from the acid hydrolysis of the neutralization pastes obtained during the refining of olive-pomace oil intended for feeding. Indeed, during the refining of olive-pomace oil, one step is to neutralize the free fatty acids by adding sodium hydroxide. An oil free of free fatty acids is obtained on one side (for food use) and sodium salts of fatty acids and thus neutralization pastes on the other. It is these neutralization pastes that are then re-acidified for get oil: acid olive oil. Any other method of manufacturing acid oil from olive pomace known to those skilled in the art can also be envisaged.
- the fatty substances and in particular the oils and pastes used in the process of the invention are refined, in order to limit the impurities introduced into the soap during step a., Which could impact the smell, color and dermatological qualities of the final soap.
- Refining consists of removing the metals (P, Ca, Mg, Zn, Cu, Fe) naturally present in the oil. Refining also eliminates pigments, impurities that can impart bad odor, color and quality to soap, as well as traces of pesticides. Refining can consist in the neutralization of fatty acids by addition of sodium hydroxide or distillation, washing with water and drying, discoloration on activated charcoal, steam deodorization, filtrations ...
- the aqueous sodium hydroxide solution implemented in step a preferably comprises 20% to 31% by weight of sodium hydroxide, preferably 25% to 30% by weight. It can be introduced into the reactor in a more concentrated form and be diluted by a water supply so that its concentration in the reactor is within the aforementioned ranges.
- the amount of aqueous sodium hydroxide solution is preferably adjusted in step a. so that the sodium hydroxide is in excess of less than 5% relative to the stoichiometry, more preferably less than 2%, even more preferably less than 1%, so as to ensure the saponification of all the fatty acids and / or fatty acid esters used in the process.
- the amount of brine optionally introduced in step a. may especially be between 0.1 and 5% by weight of the mixture of step a.
- the mixture of fatty substance and aqueous sodium hydroxide solution preferably consists of:
- aqueous sodium hydroxide solution 25 to 40% by weight of aqueous sodium hydroxide solution, preferably 29 to 36% by weight,
- brine preferably 1 to 3% by weight.
- the mixture is heated so that its temperature is between 60 and 110 ° C, in particular between 75 and 99 ° C, more particularly between 80 ° C and 90 ° C, for a period of 1 to 6 hours, preferably from 2h to 5h.
- the heating makes it possible to initiate the saponification reaction.
- the saponification reaction is then exothermic, the reaction temperature required in step a. is between 75 and 110 ° C.
- a thermal compensation system is used, for example by means of a reactor double jacket (which can be heated by a hot fluid), insulated, thermostated or not, in order to optimize energy consumption.
- the amount of sodium hydroxide present in the reaction medium of step a. is controlled by assay (titration of the base contained in the soap, therefore the sodium hydroxide, with an acid, here hydrochloric acid, after solubilization of the soap in hot ethanol, according to the standard NFT60-306 - determination of the caustic free alkali content), allowing a monitoring of the progress of the reaction. It is essential to ensure that the majority of fat has been saponified since any unsaponified triglycerides could oxidize and become rancid, thus affecting the color and smell of the final soap.
- step a. Is conducted in a reactor equipped with a mechanical stirring system, preferably allowing shearing and pumping simultaneously, ensures an intimate mixture of the fatty acid and / or the fatty acid ester with the aqueous solution of sodium hydroxide, which avoids the setting zones and the risk of runaway reaction and ensures homogeneity and quality of the dough.
- a soap base from a previous manufacture to allow the emulsion, which is ensured mechanically, which limits the introduction of impurities into the soap.
- the soda can be introduced in a substantially stoichiometric amount (less than 5% excess of sodium hydroxide).
- a soap paste comprising a mixture of sodium carboxylates, that is to say salts of fatty acids constituting soap, soda and water and glycerin.
- the method according to the invention implements at least one step b. washing (can also be called salting / washing since it allows the release of glycerin and impurities) of the soap paste obtained in step a. wherein: the soap paste is mixed with an aqueous solution comprising 1 to 42% by weight of a mixture of sodium hydroxide and salt,
- the mixture is heated and left to settle until two phases are formed: the grained soap comprising salt, sodium hydroxide and glycerine, and an aqueous solution comprising salt, sodium hydroxide and glycerine,
- the grained soap obtained in step b. includes salt and soda, and glycerin.
- the washing step is critical in the process of the invention. The inventors have indeed optimized this step to allow to keep a controlled amount of glycerin, preferably between 1 and 8% by weight of the smooth soap obtained after a single washing step, preferably between 2 and 5% by weight.
- the soap paste resulting from step a. is mixed with an aqueous solution comprising:
- salt 1 to 7% by weight of salt, preferably 2 to 5% by weight of salt, more preferably 2 to 4% by weight of salt, and
- sodium hydroxide From 0.01% to 40% by weight of sodium hydroxide, preferably from 0.9% to 20% by weight of sodium hydroxide, more preferably from 2% to 8% by weight of sodium hydroxide.
- the salt and sodium content may be adjusted by those skilled in the art depending on the nature of the oils used for the manufacture of the soap and the desired glycerin content in the final soap.
- the traditional methods of soap manufacture recommend using as much water as fatty substances for washing the soap paste to allow a good separation of the soap and the aqueous solution comprising salt, sodium hydroxide and sodium hydroxide. glycerin. Due to the particular electrolyte composition of the washing solution implemented in step b. of the process of the invention, it is possible to effectively wash the soap paste from step a. without the need to use too much water.
- the weight ratio of the aqueous washing solution implemented in step b. on the fatty acids and / or fatty acid esters introduced in step a. is less than 1, in particular between 0.2 and 0.99, and more particularly between 0.3 and 0.6.
- the aqueous washing solution implemented in step b. is added to the soap paste resulting from step a., in the same reactor equipped with a mechanical stirring system as that used for step a.
- a mechanical stirring system preferably allowing simultaneous shearing and pumping, ensures an intimate mixing of the soap with the washing solution, thereby reducing the duration of the washing step and the temperatures used and to limit the amount of washing water required.
- energy consumption and rejects are reduced and the quality of the soap is preserved by a limited heating time and mild temperatures.
- the mixture can be heated to a temperature between 70 and 99 ° C, in particular between 80 and 99 ° C and be maintained in these temperature ranges. for 30 minutes to 2 days, or for 45 minutes to 24 hours, or for 1 to 18 hours, depending on the nature of the fatty acids and / or fatty acid esters used in step a.
- the mixture is left to settle, for example between 30 minutes and 2 days.
- the decantation is carried out in two stages: the mixture is left to settle for 30 minutes at 6h, more preferably 1h to 4h, and a first withdrawal makes it possible to recover the aqueous solution having decanted,
- the soap mixture is again allowed to settle for 6h to 2 days, preferably for 8 to 23h, more preferably 12 to 18h and a second withdrawal separates the grained soap from the aqueous solution comprising salt, soda and glycerine.
- the decantation is carried out in a single step: the mixture is thus allowed to settle for a period ranging from 30 minutes to two days, and then the aqueous solution having decanted is withdrawn.
- the yield in aqueous washing solution expressed as a mass of aqueous solution withdrawn on mass of aqueous washing solution (including water + electrolytes) introduced in step b. washing is used to characterize the effectiveness of settling.
- the yield of aqueous washing solution in step b. is preferably greater than 60%, in particular between 75 and 100%, in particular between 75 and 99.5%, and more particularly between 85 and 95%.
- the method according to the invention implements at most two steps b. washing, preferably at most one step b. washing.
- the soap manufacturing process according to the invention comprises at least one step of smoothing the grained soap obtained in step b. by neutralization in which: the grained soap is mixed with at least one neutralizing agent which may be an acid, a fatty acid or a fatty acid ester,
- the introduction of salt water during the various washing steps makes it possible to separate the soap from the aqueous washing solutions containing in particular impurities, sodium hydroxide and glycerin, but the washed soap has a salt content ( NaCl) too high to allow its shaping. It is therefore necessary to reduce the level of salt in the soap.
- the soap is generally smoothed by liquidation, that is to say by adding pure water. This step leads to the formation of an intermediate phase of soap solubilized in water called black fat. This partial solubilization of the soap affects the yields of the reaction, affecting the productivity of the process and creates discharges to be reprocessed.
- the smooth soap should preferably comprise less than 33% by weight of water, less than 0.7% by weight of salt and less than 0.2% by weight of free sodium hydroxide (in NaOH form).
- the method according to the invention thus implements a step of smoothing by neutralization, in particular to reduce the sodium content of the soap.
- the grained soap is thus mixed with at least one neutralizing agent which may be an acid, a fatty acid or a fatty acid ester.
- the use of an acid or a fatty acid allows the rapid neutralization of soda by acid-base reaction.
- the use of a fatty acid ester allows a slower neutralization of sodium hydroxide by saponification.
- the neutralizing agent is a fatty acid or a fatty acid ester.
- fatty acid is meant carboxylic acids comprising a hydrocarbon radical, saturated or unsaturated, linear or branched, comprising 6 to 30 carbon atoms, and preferably 12 to 22 carbon atoms.
- saturated fatty acids that may be mentioned are caproic acid, enanthic acid, caprylic acid, pelargonic acid, capric acid, undecylic acid, lauric acid, tricecylic acid, myristic acid, pentadecyl acid, palmitic acid, margaric acid, stearic acid, nonadecylic acid, eicosanoic acid, behenic acid, tetracosanoic acid, and their mixtures.
- the saturated fatty acids are selected from caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, and mixtures thereof.
- unsaturated fatty acids By way of example of unsaturated fatty acids, mention may be made of sorbic acid, decylenic acid, caproleic acid, undecylenic acid, lauroleic acid, myristoleic acid, pentadecenoic acid, palmitoleic acid, palmiteaic acid, oleic acid, elaidic acid and acid.
- vaccenic linoleic acid, gamma-linolenic acid, alpha-linolenic acid, steradonic acid, parinaric acid or stearidonic acid, gadoleic acid, dihomo-linoleic acid, dihomo-gamma-linolenic acid, arachidonic acid, timnodonic acid or eicosapentaenoic acid, erucic acid, acid brassic acid, cetoleic acid, adrenic acid, clupanodonic acid, docosahexaenoic acid, nervonic acid or selacholeic acid, eicosadienoic acid, eicosatrienoic acid, docosadienoic acid, docosatetraenoic acid, docosapentaenoic acid.
- unsaturated fatty acids are selected from palmitoleic acid, oleic acid, linoleic acid, and mixtures thereof.
- the fatty acid esters are preferably those previously described for use in step a. pasting / cooking, in particular fatty substances, and in particular the oils described above.
- step c. smoothing is carried out with a mixture of saturated and unsaturated fatty acids, preferably derived from vegetable fats such as for example olive oil, coconut oil or palm oil.
- fatty substances used in step c. smoothing are derived from the same plant species as those used for saponification during step a.
- step c the mixture is heated to a temperature between 70 and 99 ° C, preferably between 80 and 99 ° C for 10min to 5h, preferably for 30min to 2h.
- brine an aqueous solution comprising at least 0.1% by weight of sodium chloride (NaCl), preferably between 10 and 30% of NaCl
- the smoothing implemented in step c. is carried out in the same reactor equipped with a mechanical stirring system as that used for steps a or b. As for the steps a.
- the presence of a mechanical stirring system preferably allowing shearing and pumping simultaneously, ensures an intimate mixture of the grained soap with the fatty acid, allowing effective neutralization of the soda contained in the grained soap , which reduces the duration of the smoothing step and the temperatures used.
- the homogeneity ensured, the reduced durations and temperatures make it possible to ensure the good quality of the soap.
- Steps a., B. and / or c. of the process according to the invention can be implemented in a reactor equipped with a mechanical stirring system.
- the mechanical stirring system preferably simultaneously shear and pump the mixtures of steps a, b. and / or c.
- steps a., B. and / or c. of the process according to the invention can be implemented in the same reactor.
- the reactor comprises in particular a tank having an interior space for producing a mixture of at least one fatty substance and a base (soda) in the interior space of the tank, and heating the mixture.
- the tank has a cylindrical side wall along a central axis of circular cross section
- the reactor further comprises a stirring system displaceable in the interior space of the tank so as to circulate the mixture in the interior space of the tank, and to shear at least locally the mixture, the stirring system comprises at least a first stirring member adapted to shear the mixture and to move the mixture transversely relative to the central axis towards the side wall, and at least a second stirring member, at least the second stirring member being a mobile having a hub and a plurality of equi-parted blades each extending from the hub to a free end, the hub of the mobile being pivotally mounted relative to the vessel in a direction of rotation about a coaxial pivot axis to the central axis.
- a stirring system displaceable in the interior space of the tank so as to circulate the mixture in the interior space of the tank, and to shear at least locally the mixture
- the stirring system comprises at least a first stirring member adapted to shear the mixture and to move the mixture transversely relative to the central axis towards the side wall, and at least a second stirring member,
- the second stirring member is an axially pumped mobile adapted to move the mixture in a pumping direction along the central axis of the tank, the first stirring member being disposed downstream of the second stirring member relative to the pumping direction, each of the blades of the second stirring member having a first edge near the first stirring member and a second edge opposite the first edge along the pivot axis and remote from the first stirring member; first and second edges being arranged such way that the second edge is in front of the first edge relative to the direction of rotation, the second stirring member having:
- the reactor also comprises a heating system adapted to heat the mixture in the interior space of the tank.
- the stirring system is moved into the mixture so as to circulate the mixture in the interior of the vessel and to shear at least locally the mixture.
- the mixture is moved in the direction of pumping along the central axis of the vessel by the second stirring member to the first stirring member, and sheared and displaced transversely with respect to the central axis towards the wall side by the first stirring member.
- the invention implements a second stirring member whose blades are inclined towards the first stirring member and whose pumping number is high while the power number is low.
- the second stirring member has the function of pumping the liquid to the first stirring member and this, minimizing the energy consumed. Indeed, the energy dissipation function is assumed by the first stirring member.
- the stirring system according to the invention which implements a shear also makes it possible to reduce a droplet size of fat and base bodies forming an emulsion and thus to increase a surface area. of exchange between the fatty body and the base. In particular, it is no longer necessary to use an additional reagent to facilitate the formation of the emulsion.
- the soap manufacturing process is simplified and its duration of implementation reduced. In addition, the properties of the soap can be preserved.
- Po2 can be such that - ⁇ 0.3.
- Each of the blades of the second stirring member may have a median plane between the lower and upper edges, the median plane being inclined at an angle less than 60 ° with respect to a horizontal plane perpendicular to the pivot axis.
- the heating system may comprise the side wall of the jacketed tank, and a hot fluid supply source supplying hot fluid a space between the two casings of the side wall of the tank.
- the tank may comprise a bottom from which the side wall extends, the first stirring member being arranged near the bottom of the tank, the second stirring member being arranged at a distance from the bottom of the tank.
- the mixture can be moved to the bottom of the tank by the second stirring member and moved to the side wall near the bottom of the tank by the first stirring member.
- the first stirring member may be a mobile having a hub and a plurality of equidistributed blades each extending from the hub to a free end, the hub of the mobile being pivotally mounted relative to the vessel along a pivot axis coaxial with the central axis, the first stirring member being a mobile radial pumping.
- the radial pumping mobile allows local creation of speed gradients rather than pumping the mixture.
- the mobile radial pump of the first stirring member may have:
- each of the blades of the first stirring member may be shaped to have a substantially constant spacing with a portion of the bottom of the vessel over a substantial portion of a length of said blade.
- the mobile of one and / or the other of the first and second stirring members may have a diameter of between 40% and 80%, preferably between 50% and 70%, of the diameter of the cross-section. of the tank.
- the stirring system may comprise at least one deflection member, such as a counter-blade or, in Anglo-Saxon terms, a baffle, arranged near the side wall facing the second stirring member to deflect a part of the mixture located near the side wall to the second stirring member.
- a deflection member such as a counter-blade or, in Anglo-Saxon terms, a baffle, arranged near the side wall facing the second stirring member to deflect a part of the mixture located near the side wall to the second stirring member.
- a deflection member such as a counter-blade or, in Anglo-Saxon terms, a baffle
- the figure represents a reactor 1 for use in a soap making process.
- the soap manufacturing process provides for a mixture of reagents during different steps to obtain soap.
- the reactor 1 comprises a tank 2, preferably insulated and optionally thermostated, having a bottom 3 from which extends a side wall 4 to delimit an interior space 5.
- the bottom 3 is elliptical and the wall 4 cylindrical side of circular cross section along a central axis A.
- the inner space 5 has a diameter T and a filling level H.
- the tank 2 can be dimensioned so that a ratio H / T is between 1, 5 and 5.
- the tank 2 has an upper opening 6.
- the upper opening 6 can be closed by a cover 8.
- the cover 8 can be mounted on an edge of the upper opening 6 in a non-hermetic manner to be able to make tank mixtures 2 called "open", that is to say whose inner space 5 is at atmospheric pressure.
- the tank 2 could have any other suitable shape with preferably a non-flat bottom 3 and in particular a conical bottom.
- the tank 2 may be equipped with a heating system not shown.
- the tank 2 may have a bottom 3 and a side wall 4 jacketed connected to a fluid supply source at an appropriate temperature supplying a space between the two envelopes of the side wall of the tank.
- the reactor 1 further comprises a stirring system 10 adapted to circulate the mixture in the interior space 5 of the tank 2, and to shear at least locally the mixture.
- the stirring system 10 comprises a shaft 1 1 extending along the central axis A in the interior space 5 of the tank 2 and through the cover 8.
- the shaft 1 1 presents a first end 1 connected to a rotary drive device, such as a geared motor 12, and a second end 1 1b disposed in the vicinity of the bottom 3 of the tank 2.
- the shaft 1 1 can thus be rotated its own axis along a pivot axis P coaxial with the central axis A by the drive device 12.
- the drive device 12 may in particular be adapted to drive the shaft 1 1 in its own rotation at a rotation speed of up to at 80 rpm or more.
- the stirring system 10 also comprises a first stirring member 15 mounted on the shaft 1 1 in the vicinity of the second end 1 1b.
- the first stirring member 15 is then pivotally mounted along the pivot axis P with respect to the vessel 2.
- the first stirring member 15, arranged near the bottom 3 of the vessel 2, is adapted to shear the mixture , that is to say locally create speed gradients, and to move the mixture transversely relative to the central axis A to the side wall 4.
- the first stirring member 15 may be a mobile radial pumping, such as a mobile with straight blades.
- the mobile of the first stirring member 15 comprises a hub 16 integral with the shaft January 1, and several blades 17, including four in the embodiment shown, evenly distributed and each extending from the hub 16 to at one free end 18.
- Each of the blades 17 is straight, that is to say that it extends in a plane containing the pivot axis P.
- the mobile of the first stirring member 15 may have a diameter D between 40% and 80%, preferably between 50% and 70%, of the diameter T of the internal space 5 of the tank 2.
- the shape of the mobile of the first stirring member 15 can also be adapted to the shape of the bottom 3 of the tank 2.
- each of the blades 17 may have a lower edge 19 facing the bottom 3 of the tank 2 shaped to have a spacing substantially constant cl with a portion of the bottom 3 of the tank 2 on an essential part, that is to say 50% or more, of a length of the blade 17 measured between the hub 16 and the free end 18.
- the distance between the lower edge 19 of each of the blades 17 and the bottom 3 of the tank 2 may be between 5% and 20% of the diameter T of the internal space 5 of the tank 2.
- the mobile of the first stirring member 15 has:
- the first power number P01 of the mobile radial pumping of the first stirring member 15 is high, for example between 1, 5 and 6, so as to promote shearing.
- the first pumping number Q01 of the radial pumping mobile of the first stirring member 15 may be low, for example between 0.2 and 1.
- the power dissipated per cubic meter of mixture is between 1000 W / m3 and 8000 W / m3, preferably between 2000 W / m3 and 6000 W / m3.
- the mobile of the first stirring member 15 could be a Rushton turbine or other mobile radial flow.
- the stirring system 10 also comprises a second stirring member 25 mounted on the shaft 1 1 on the side of the first end 11a, below the filling level H.
- the second stirring member 25 is then arranged coaxially with the above the first stirring member 15.
- the second stirring member 15 is thus pivotally mounted along the pivot axis P relative to the vessel 2.
- the second stirring member 25, arranged at a distance from the bottom 3 of the tank 2, is adapted to move the mixture in a pumping direction S, shown by an arrow in the figure.
- the second stirring member 20 may be a descending axial pumping mobile, such as a propeller with inclined blades.
- the mobile of the second stirring member 25 comprises a hub 26 integral with the shaft January 1, and several blades 27, including four in the embodiment shown, evenly distributed and each extending from the hub 26 to at one free end 28.
- Each of the blades 27 is inclined, that is to say it deviates from a plane containing the pivot axis P.
- the blade 27 has a median plane relative to the first 29 and second 30 opposite edges along the axis of pivoting P.
- the first edge 29 is located near the first stirring member 15 and the second edge 30 is located at a distance from the first stirring member 15.
- the first edge 29 is a lower edge and the second edge is an upper edge.
- the median plane is at an angle with a horizontal plane perpendicular to the pivot axis P. This angle is less than 60 °, for example 45 ° in the figure, with an inclination such that the upper edge 30 is in front of the lower edge 29 with respect to a direction of rotation R of the shaft 1 1, represented by an arrow, and therefore of the mobile of the second stirring member 25.
- the mobile of the second stirring member 25 has a diameter D identical to that mobile of the first stirring member 15.
- the mobile of the second stirring member 25 may have any other diameter between 40% and 80%, preferably between 50%> and 70%> , of the diameter T of the internal space 5 of the tank 2.
- the mobile of the second stirring member 25 has:
- the second pumping number of the axially pumped mobile of the second stirring member is high, that is to say between 0.5 and 2, so as to promote the implementation of circulation.
- the second power number of the axially pumped mobile of the second stirring member is meanwhile low, that is to say between 0.3 and 1.5.
- a ratio of the second pumping number Qo2 to the second power number Po2 is preferably as
- the invention is not limited to the agitation system 10 described above and could in particular include any other type of stirring member, in appropriate number, in particular between two and five, preferably between two and three, and in any case appropriate arrangement.
- the stirring system 10 could comprise two second stirring members, for example identical, mounted coaxially on the shaft above the first stirring member.
- the stirring system 10 may also comprise one or more deflection members 35, for example between two and four, preferably between two and three, arranged to deflect a portion of the mixture located near the side wall 4 of the tank 2 to the second or the second stirring member 25.
- the deflection members 35 can be removably mounted in the inner space 5 of the tank 2.
- the stirring system 10 comprises two counter-blades 36 or, in Anglo-Saxon terms, baffles, arranged near the side wall 4 of the tank 2 facing the free ends of the mobiles of the second stirring members 25.
- the counter-blades 36 can be removable and pivotable about a longitudinal axis L to allow to change an orientation.
- the counter-blades 36 may have a width lb of between 3% and 8% of the diameter T of the internal space 5 of the vessel 2. Furthermore, the counter-blades 36 may be arranged so as to leave a free space with the side wall 4 of the tank 2 between 2% and 8% of the diameter T of the internal space 5 of the tank 2.
- the radial pumping mobile of the first stirring member 15 is disposed downstream of the axially pumping mobile of the second stirring member 25 with respect to the pumping direction S.
- the mixture can thus be moved in the direction of pumping S along the central axis A to the bottom 3 of the tank 2 by the axially pumped mobile of the second stirring member 25 to the radial pumping mobile of the first stirring member 15 and sheared and displaced transversely with respect to the central axis A to the side wall 4 by the mobile radial pumping of the first stirring member 15.
- the mixture can thus return to the mobile device with axial pumping of the second stirring member 25 being deflected towards this mobile by the counter-blades 36.
- step a. mashing and baking can be carried out at temperatures of between 75 and 99 ° C for a period approximately half as long as the traditional processes
- step b. washing can be conducted at temperatures between 70 and 99 ° C, and the number of washes and the amount of wash water can be reduced.
- step c. the process of the invention may be followed by a step of drying the smooth soap to obtain a soap comprising at most 22% by weight of water, in particular at most 16% by weight of water.
- Drying can preferably be accomplished by passing the smooth soap into a vacuum atomizer in which the soap is sprayed. Any other system using natural or forced convection, heated or not, ambient air or a carrier gas can also be used as a means of drying. So the soap can for example also be poured on the ground and dried in the open air
- the soap can be shaped, for example, by passing through series extruders in which it is compressed. Then the soap comes out of the extruders through a die that allows obtaining the desired shape for the finished product. he can alternatively be shaped by cutting, for example when the soap has been dried on the ground in particular.
- the soap can also be shaped by molding.
- the invention also relates to a smooth soap that can be manufactured by means of a batch soap making process comprising at least the following steps: a. a pasting and cooking step in which:
- At least one fatty acid and / or fatty acid ester is mixed with an aqueous solution of sodium hydroxide,
- step b at least one step of washing the soap paste obtained in step a. in which :
- the soap paste is mixed with an aqueous solution comprising 1 to 42% by weight of a mixture of sodium hydroxide and salt,
- the mixture is heated and left to settle until two phases are formed: the grained soap comprising salt, sodium hydroxide and glycerine, and an aqueous solution comprising salt, sodium hydroxide and glycerine,
- step b. a step of smoothing the grained soap obtained in step b. by neutralization in which:
- the grained soap is mixed with at least one neutralization agent that may be an acid, a fatty acid or a fatty acid ester,
- the smooth soap thus obtained preferably comprises: at most 33% by weight of water, preferably 25% to 33% by weight, more preferably 24% to 32% by weight of water,
- salt at most 0.7%) by weight of salt, preferably 0.1% to 0.6%, more preferably 0.35 to 0.5%, more particularly 0.2% to 0.5% by weight of salt, and
- sodium hydroxide at most 0.2% by weight of sodium hydroxide, preferably 0.05% to 0.2%, more preferably 0.05% to 0.1% by weight of free sodium hydroxide (in NaOH form).
- a smooth soap was prepared according to the following method:
- 360g of olive-pomace oil, 120g of coconut oil and 120g of palm oil were introduced into a jacketed reactor equipped with a mechanical stirring system allowing the mixture to be simultaneously sheared and pumped.
- the detergent was then withdrawn including water, sodium hydroxide and salt and glycerine. It was allowed to settle again for 1 hour at 87 ° C. and then the lye containing water, sodium hydroxide and salt and glycerine was again withdrawn. 139g of leached solids were thus recovered.
- the yield is therefore 70.55%.
- the soap was then smoothed. To do this, 24.7 g of coconut oil was introduced into the jacketed reactor equipped with a stirring system containing the grained soap previously obtained.
- the mixture is stirred at 650 rpm at a temperature of 95.degree.
- the smooth soap is then poured and dried in the open air
- the soap obtained is perfectly homogeneous and can benefit from the name Marseille soap. It forms a particularly creamy foam, and moisturizing glycerin protects the skin.
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1651382A FR3047995B1 (fr) | 2016-02-19 | 2016-02-19 | Procede de fabrication de savon |
PCT/FR2017/050376 WO2017140999A1 (fr) | 2016-02-19 | 2017-02-20 | Procede de fabrication de savon |
Publications (1)
Publication Number | Publication Date |
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EP3417047A1 true EP3417047A1 (fr) | 2018-12-26 |
Family
ID=56069075
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP17710333.0A Pending EP3417047A1 (fr) | 2016-02-19 | 2017-02-20 | Procede de fabrication de savon |
Country Status (3)
Country | Link |
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EP (1) | EP3417047A1 (fr) |
FR (1) | FR3047995B1 (fr) |
WO (1) | WO2017140999A1 (fr) |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BE463094A (fr) * | 1943-07-31 | |||
NL275152A (fr) * | 1961-03-23 | |||
FR2008916A1 (fr) * | 1968-05-20 | 1970-01-30 | Colgate Palmolive Co | |
GB8807754D0 (en) * | 1988-03-31 | 1988-05-05 | Unilever Plc | Transparent soap bars |
-
2016
- 2016-02-19 FR FR1651382A patent/FR3047995B1/fr active Active
-
2017
- 2017-02-20 WO PCT/FR2017/050376 patent/WO2017140999A1/fr active Application Filing
- 2017-02-20 EP EP17710333.0A patent/EP3417047A1/fr active Pending
Also Published As
Publication number | Publication date |
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FR3047995A1 (fr) | 2017-08-25 |
FR3047995B1 (fr) | 2020-01-03 |
WO2017140999A1 (fr) | 2017-08-24 |
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