IT202000008212A1 - PROCESS FOR THE TREATMENT OF SOAPY PASTES ARISING FROM THE NEUTRALIZATION OF VEGETABLE OR ANIMAL OILS OR FATS AND / OR THEIR MIXTURES FOR THE RECOVERY OF THE SUBSTANCES CONTAINED THEREIN - Google Patents
PROCESS FOR THE TREATMENT OF SOAPY PASTES ARISING FROM THE NEUTRALIZATION OF VEGETABLE OR ANIMAL OILS OR FATS AND / OR THEIR MIXTURES FOR THE RECOVERY OF THE SUBSTANCES CONTAINED THEREIN Download PDFInfo
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- IT202000008212A1 IT202000008212A1 IT102020000008212A IT202000008212A IT202000008212A1 IT 202000008212 A1 IT202000008212 A1 IT 202000008212A1 IT 102020000008212 A IT102020000008212 A IT 102020000008212A IT 202000008212 A IT202000008212 A IT 202000008212A IT 202000008212 A1 IT202000008212 A1 IT 202000008212A1
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- Prior art keywords
- solvent
- process according
- paste
- soapy
- water
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- 238000000034 method Methods 0.000 title claims description 78
- 239000000203 mixture Substances 0.000 title claims description 19
- 238000011282 treatment Methods 0.000 title claims description 15
- 238000011084 recovery Methods 0.000 title claims description 13
- 238000006386 neutralization reaction Methods 0.000 title claims description 12
- 239000003925 fat Substances 0.000 title claims description 10
- 239000000126 substance Substances 0.000 title claims description 8
- 235000013311 vegetables Nutrition 0.000 title claims description 7
- 239000010775 animal oil Substances 0.000 title claims description 6
- 239000008158 vegetable oil Substances 0.000 title claims description 6
- 239000002904 solvent Substances 0.000 claims description 101
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 239000002253 acid Substances 0.000 claims description 39
- 239000000344 soap Substances 0.000 claims description 36
- 239000003921 oil Substances 0.000 claims description 35
- 239000012071 phase Substances 0.000 claims description 33
- 238000001704 evaporation Methods 0.000 claims description 24
- 230000008020 evaporation Effects 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 15
- 239000000787 lecithin Substances 0.000 claims description 14
- 235000010445 lecithin Nutrition 0.000 claims description 14
- 238000003776 cleavage reaction Methods 0.000 claims description 12
- 230000007017 scission Effects 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000002351 wastewater Substances 0.000 claims description 11
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 9
- 238000006297 dehydration reaction Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000010908 decantation Methods 0.000 claims description 7
- 239000000839 emulsion Substances 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000012808 vapor phase Substances 0.000 claims description 6
- 239000008346 aqueous phase Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 230000020477 pH reduction Effects 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 230000003750 conditioning effect Effects 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000012454 non-polar solvent Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 239000003495 polar organic solvent Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims 1
- 239000007792 gaseous phase Substances 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 claims 1
- 235000019198 oils Nutrition 0.000 description 28
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 17
- 229910052938 sodium sulfate Inorganic materials 0.000 description 10
- 235000011152 sodium sulphate Nutrition 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 9
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 7
- 235000019197 fats Nutrition 0.000 description 7
- 229940067606 lecithin Drugs 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 6
- 235000015927 pasta Nutrition 0.000 description 5
- 238000000265 homogenisation Methods 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 235000011149 sulphuric acid Nutrition 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 235000021588 free fatty acids Nutrition 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- 235000014593 oils and fats Nutrition 0.000 description 2
- 230000007928 solubilization Effects 0.000 description 2
- 238000005063 solubilization Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical class [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 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 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical class [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical class [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical class [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 235000019486 Sunflower oil Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011575 calcium Chemical class 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002458 infectious effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011777 magnesium Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 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
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000002600 sunflower oil Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/04—Refining fats or fatty oils by chemical reaction with acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/06—Refining fats or fatty oils by chemical reaction with bases
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Description
Descrizione del brevetto per invenzione dal titolo: ?PROCESSO PER IL TRATTAMENTO DI PASTE SAPONOSE DERIVANTI DALLA NEUTRALIZZAZIONE DI OLI O GRASSI VEGETALI O ANIMALI E/O LORO MISCELE PER IL RECUPERO DELLE SOSTANZE IVI CONTENUTE?; Description of the patent for invention entitled:? PROCESS FOR THE TREATMENT OF SOAPY PASTES ARISING FROM THE NEUTRALIZATION OF VEGETABLE OR ANIMAL OILS OR FATS AND / OR THEIR MIXTURES FOR THE RECOVERY OF THE SUBSTANCES CONTAINED ?;
Sommario dell?invenzione Summary of the invention
[001] Il presente trovato riguarda un processo per il trattamento di paste saponose che prevede una preliminare disidratazione della massa mediante l?impiego di opportuno solvente ed una successiva scissione mediante addizione di acido onde ottenere, una volta separati, dei prodotti commerciali e/o dei residui di lavorazione che non presentano difficolt? di trattamento nelle fasi successive. [001] The present invention relates to a process for the treatment of soapy pastes which provides for a preliminary dehydration of the mass through the use of a suitable solvent and a subsequent cleavage by addition of acid in order to obtain, once separated, commercial products and / or of processing residues that do not present difficulties? of treatment in the later stages.
Campo dell?invenzione Field of invention
[002] La presente invenzione ? relativa ad un metodo per il trattamento dei prodotti oleosi, in particolare di quelli umidi, che contengono pertanto delle percentuali in peso di acqua che deve essere separata. [002] The present invention? relating to a method for treating oily products, in particular wet ones, which therefore contain percentages by weight of water that must be separated.
[003] In particolare la presente invenzione ? relativa ad un processo per il trattamento di paste saponose derivanti dalla neutralizzazione di oli o grassi vegetali o animali e/o loro miscele, che contengono acqua derivante dal loro normale processo produttivo. [003] In particular the present invention? relating to a process for the treatment of soapy pastes deriving from the neutralization of vegetable or animal oils or fats and / or their mixtures, which contain water deriving from their normal production process.
Stato dell?arte State of the art
[004] ? noto che sia i prodotti oleosi naturali, sia quelli di origine industriale, vengono trattati per la produzione ed il recupero di oli e grassi alimentari e/o industriali ed altri prodotti ivi contenuti. [004]? It is known that both natural oily products and those of industrial origin are treated for the production and recovery of food and / or industrial oils and fats and other products contained therein.
[005] Nei processi noti le paste saponose, eventualmente preriscaldate, vengono addizionate con un acido, tipicamente acido solforico, in modo che il calore generato porti la miscela ad una temperatura finale superiore a 90?C [005] In known processes, the soapy pastes, possibly preheated, are added with an acid, typically sulfuric acid, so that the heat generated brings the mixture to a final temperature above 90 ° C
[006] Generalmente ? necessario operare in eccesso di acido rispetto alla quantit? stechiometrica al fine ottenere una completa scissione dei saponi; ci? comporta che l?acqua contenuta nella pasta saponosa presenti valori di pH anche inferiori a 2. [006] Generally? it is necessary to operate in excess of acid with respect to the quantity? stoichiometric in order to obtain a complete splitting of the soaps; there? implies that the water contained in the soap paste has pH values even lower than 2.
[007] La miscela cos? ottenuta viene fatta decantare per permettere la separazione della frazione grassa da quella acquosa; questa fase ? spesso la pi? difficoltosa poich? la separazione delle due frazioni ? ostacolata dalla presenza di prodotti che favoriscono la formazione di emulsioni pi? o meno stabili. [007] The mixture so? obtained, it is decanted to allow the separation of the fat fraction from the aqueous one; this phase ? often the pi? difficult since? the separation of the two fractions? hindered by the presence of products that favor the formation of emulsions pi? or less stable.
[008] Tra i prodotti che favoriscono la formazione di emulsioni e che, quindi, ostacolano il processo di separazione, si possono citare ad esempio le lecitine; queste infatti mostrano la tendenza a formare una frazione intermedia costituita da emulsioni, rispetto quella grassa e quella acquosa, sostanzialmente contenente una parte oleosa, le lecitine, una frazione non saponificabile ed una parte acquosa fortemente acida. [008] Among the products which favor the formation of emulsions and which, therefore, hinder the separation process, lecithins can be mentioned for example; these in fact show the tendency to form an intermediate fraction consisting of emulsions, with respect to the fatty and aqueous ones, substantially containing an oily part, the lecithins, an unsaponifiable fraction and a strongly acidic aqueous part.
[009] La fase acquosa separata con questo metodo noto presenta un COD molto elevato (15.000-30.000 mg/l) ed una quantit? di sali disciolti (60.000 ? 100.000 ppm) che ne rendono molto difficile e costoso il trattamento di depurazione. [009] The aqueous phase separated with this known method has a very high COD (15,000-30,000 mg / l) and an amount of? of dissolved salts (60,000? 100,000 ppm) which make the purification treatment very difficult and expensive.
[0010] Inoltre l?acqua ottenuta dalla decantazione dovr? essere sottoposta ad un condizionamento chimico/fisico per permetterne la depurazione biologica. [0010] Furthermore, the water obtained from the decantation will have to? be subjected to a chemical / physical conditioning to allow biological purification.
[0011] Esistono anche altri processi di trattamento delle paste saponose, come ad esempio quello descritto in US 6399802 che prevede la miscelazione della pasta saponosa con un alcool monoidrossilico - tipicamente isopropanolo, normal propanolo, alcool isoamilico o una miscela di alcoli- e acido, cui segue una separazione delle fasi per sedimentazione, per ottenere una fase acquosa contenente sali e tracce di solvente ed una fase oleosa contenente il solvente, il quale pu? essere recuperato da entrambe le fasi mediante evaporazione. [0011] There are also other treatment processes of soap pastes, such as for example the one described in US 6399802 which involves mixing the soap paste with a monohydroxyl alcohol - typically isopropanol, normal propanol, isoamyl alcohol or a mixture of alcohol- and acid, followed by a separation of the phases by sedimentation, to obtain an aqueous phase containing salts and traces of solvent and an oily phase containing the solvent, which can? be recovered from both phases by evaporation.
[0012] Tuttavia il metodo ora descritto necessita per la separazione di un pH inferiore o al limite uguale a 4, il che impone l?utilizzo di un metodo di decantazione naturale (abbastanza lento) oppure di una separazione meccanica con macchinari speciali di elevato costo (per i normali separatori centrifughi viene solitamente indicato un pH maggiore di 4 come limite di esercizio in sicurezza); anche la successiva evaporazione dell?alcool dovr? essere eseguita dopo una neutralizzazione della fase acquosa per evitare l?impiego di evaporatori realizzati in leghe speciali molto costose; in ultimo la neutralizzazione produce sali che, come gi? evidenziato, rendono le acque di difficile trattamento. [0012] However, the method just described requires for the separation of a pH lower than or at the limit equal to 4, which requires the use of a natural decantation method (quite slow) or mechanical separation with special high-cost machinery (for normal centrifugal separators a pH greater than 4 is usually indicated as a safe operating limit); also the subsequent evaporation of the alcohol will have to? be performed after a neutralization of the aqueous phase to avoid the use of evaporators made of very expensive special alloys; finally, the neutralization produces salts which, as already? highlighted, make the water difficult to treat.
Compito del trovato Task of the found
[0013] Scopo del presente trovato ? quello di fornire un processo che permetta di superare gli inconvenienti della tecnica nota, che sia compatibile con le metodiche e le tempistiche industriali e che permetta di ottenere dei prodotti commerciali e/o residui di lavorazione che non presentino difficolt? di trattamento nelle fasi successive. [0013] Purpose of the present invention? that of providing a process which allows to overcome the drawbacks of the known art, which is compatible with industrial methods and timing and which allows to obtain commercial products and / or processing residues which do not present difficulties? of treatment in the later stages.
Soluzione proposta Suggested solution
[0014] Secondo il trovato ci? ? stato ottenuto con un processo in cui si sfrutta l?addizione di un solvente non polare addizionato alla pasta saponosa, detto solvente dovendo essere sostanzialmente immiscibile con l?acqua contenuta nella carica stessa il che permette di separare selettivamente l?acqua contenuta nella pasta saponosa mediante evaporazione. [0014] According to the finding there? ? been obtained with a process in which the addition of a non-polar solvent added to the soap paste is exploited, said solvent having to be substantially immiscible with the water contained in the charge itself which allows to selectively separate the water contained in the soap paste by means of evaporation.
[0015] La descrizione dell?invenzione risulter? pi? chiara facendo riferimento alla allegata tavola di disegno in cui ? illustrata una preferita forma di realizzazione del trovato. [0015] The description of the invention will result? pi? clear by referring to the attached drawing table in which? a preferred embodiment of the invention is illustrated.
Elenco figure List of figures
La figura 1 mostra uno schema a blocchi del trovato. Descrizione particolareggiata dell?invenzione [0016] In genere le paste saponose, derivanti dalla neutralizzazione di oli e grassi vegetali ed animali, sono miscele di: Figure 1 shows a block diagram of the invention. Detailed description of the invention [0016] In general, the soapy pastes, deriving from the neutralization of vegetable and animal oils and fats, are mixtures of:
? saponi degli acidi grassi; ? fatty acid soaps;
? gliceridi degli acidi grassi; ? glycerides of fatty acids;
? acqua; ? water;
? eventuale eccesso di agente neutralizzante; ? possible excess of neutralizing agent;
? frazioni insaponificabili ed eventuali fosfolipidi (lecitine, ecc) caratteristici degli oli o dei grassi di origine dei saponi stessi. ? unsaponifiable fractions and any phospholipids (lecithins, etc.) characteristic of the oils or fats of origin of the soaps themselves.
[0017] I saponi sopra citati corrispondono solitamente a sali di sodio, ma in tale categoria rientrano anche sali di potassio, litio, calcio, magnesio, di altri metalli bivalenti e trivalenti e di ammonio salificati con gli acidi grassi liberi presenti nell?olio di origine dei saponi stessi. [0017] The aforementioned soaps usually correspond to sodium salts, but this category also includes salts of potassium, lithium, calcium, magnesium, other divalent and trivalent metals and ammonium salified with the free fatty acids present in the oil of origin of the soaps themselves.
[0018] I costituenti di cui sopra sono presenti in percentuali diverse a seconda sia dell?origine della pasta saponosa (tipi di oli o grassi, vegetali o animali), sia dei trattamenti che questa ha gi? effettuato. [0018] The above constituents are present in different percentages depending both on the origin of the soapy paste (types of oils or fats, vegetable or animal), and on the treatments it already has. carried out.
[0019] Secondo il trovato il processo ? costituito dalle seguenti fasi: [0019] According to the invention, the process? consisting of the following phases:
? Miscelazione ed omogeneizzazione della pasta saponosa con un solvente puro o miscela di solventi; ? Mixing and homogenization of the soapy paste with a pure solvent or mixture of solvents;
? Ottenimento di una pasta saponosa disidrata mediante allontanamento di acqua e di almeno parte del solvente ottenibile tramite evaporazione; ? Obtaining a dehydrated soapy paste by removing water and at least part of the solvent obtainable by evaporation;
? Condensazione della fase vapore ottenuta con conseguente separazione del solvente, praticamente puro, dall?acqua; ? Condensation of the vapor phase obtained with consequent separation of the practically pure solvent from water;
? Acidificazione della pasta saponosa diluita con solvente e conseguente scissione dei saponi; ? Acidification of the soapy paste diluted with solvent and consequent splitting of the soaps;
? Eventuale desolventizzazione dell?olio acido prodotto e recupero del solvente all?inizio del processo; ? Possible desolventization of the acid oil produced and recovery of the solvent at the beginning of the process;
? Eventuale desolventizzazione degli ulteriori prodotti ottenuti. ? Possible desolventization of the further products obtained.
[0020] Nell?ambito della presente descrizione, per solvente sostanzialmente immiscibile idoneo alla attuazione della invenzione si intende un solvente che oltre all?immiscibilit?, per le caratteristiche di peso molecolare e di tensione di vapore, sia idoneo alla estrazione sotto forma di miscela (determinata dalla legge delle pressioni parziali) di fasi vapore dell?acqua e del solvente da un bagno di distillazione che li contenga. [0020] In the context of the present description, by substantially immiscible solvent suitable for carrying out the invention is meant a solvent which in addition to immiscibility, due to its molecular weight and vapor pressure characteristics, is suitable for extraction in the form of a mixture (determined by the law of partial pressures) of vapor phases of water and solvent from a distillation bath that contains them.
[0021] Il trovato prevede preferibilmente l?impiego di un solvente organico non polare, puro o in miscela con altri solventi dello stesso tipo, sostanzialmente immiscibile con l?acqua contenuta nella carica stessa. [0021] The invention preferably provides for the use of a non-polar organic solvent, pure or mixed with other solvents of the same type, substantially immiscible with the water contained in the charge itself.
[0022] Detto solvente permette di diluire la massa di pasta saponosa, favorendo la separazione dell?acqua ivi contenuta, detta acqua essendo separata selettivamente mediante evaporazione. [0022] Said solvent allows to dilute the mass of soapy paste, favoring the separation of the water contained therein, said water being selectively separated by evaporation.
[0023] Vantaggiosamente il solvente ? inoltre atto a solubilizzare i componenti oleosi presenti durante e dopo la scissione nella stessa pasta saponosa. [0023] Advantageously the solvent? furthermore suitable for solubilizing the oily components present during and after the cleavage in the same soapy paste.
[0024] Il solvente corrispondente alle caratteristiche sopra indicate pu? appartenere indifferentemente sia alla famiglia degli alifatici, sia a quella degli aromatici o naftenici. [0024] The solvent corresponding to the characteristics indicated above can? belong indifferently both to the aliphatic family and to that of the aromatics or naphthenics.
[0025] In una forma realizzativa preferita, ma non limitativa, il solvente organico ? costituito da idrocarburi, puri o in miscela, della famiglia degli idrocarburi alifatici, contenenti da 8 a 15 atomi di carbonio, con temperature di ebollizione dei componenti puri comprese tra i 125?C ed i 270?C. In a preferred, but non-limiting embodiment, the organic solvent? consisting of hydrocarbons, pure or in mixture, of the family of aliphatic hydrocarbons, containing from 8 to 15 carbon atoms, with boiling temperatures of the pure components between 125? C and 270? C.
[0026] Vantaggiosamente si ? scelto di operare utilizzando come solvente il decano C10 che presenta le seguenti caratteristiche: [0026] Advantageously yes? chosen to operate using decane C10 as solvent which has the following characteristics:
? un buon rapporto di evaporazione con l?acqua, pari a circa il 50% in volume; ? a good evaporation ratio with water, equal to about 50% by volume;
? delle caratteristiche di compatibilit? e non reattivit? sia con i prodotti trattati sia con i reagenti utilizzati nel processo; ? of the compatibility features? and not reactivity? both with the treated products and with the reagents used in the process;
? non ? esplosivo, infiammabile, accelerante, comburente, tossico, infettivo, radioattivo o corrosivo; ? Not ? explosive, flammable, accelerating, oxidizing, toxic, infectious, radioactive or corrosive;
? facilmente reperibile commercialmente. ? easily available commercially.
[0027] Il processo prevede una prima fase di miscelazione ed omogeneizzazione della pasta saponosa, comprendente un tenore conosciuto di acqua, con detto solvente in eccesso, con un rapporto solvente/acqua compreso nell?intervallo tra 1 e 4 in modo da favorire la solubilizzazione dei componenti organici in questo. [0027] The process involves a first phase of mixing and homogenizing the soap paste, comprising a known water content, with said excess solvent, with a solvent / water ratio included in the range between 1 and 4 in order to favor solubilization of the organic components in this.
[0028] Preferibilmente l?eccesso di solvente ? in rapporto solvente/acqua pari a 2. [0028] Preferably the excess of solvent? in a solvent / water ratio equal to 2.
[0029] In questa prima fase ? possibile, eventualmente, correggere la viscosit? della pasta saponosa aggiungendo una percentuale di acido, che concorre a favorire la solubilizzazione della frazione grassa nel solvente. [0029] In this first phase? possible, possibly, to correct the viscosity? of the soapy paste by adding a percentage of acid, which helps to favor the solubilization of the fat fraction in the solvent.
[0030] Una seconda fase del processo prevede che l?emulsione ottenuta, costituita da pasta saponosa e solvente, sia alimentata ad almeno un evaporatore in cui avviene la disidratazione della pasta saponosa, mediante allontanamento di acqua stessa e di parte del solvente. [0030] A second step of the process provides that the emulsion obtained, consisting of soapy paste and solvent, is fed to at least one evaporator in which the dehydration of the soapy paste takes place, by removing the water itself and part of the solvent.
[0031] Detto processo di evaporazione ed allontanamento dell?acqua pu? avvenire sia a pressione atmosferica, sia a pressione ridotta; la scelta delle condizioni operative migliori non pregiudica il risultato e dipende solamente da criteri di progettazione dell?apparato legati soprattutto ad eventuali considerazioni di recupero energetico. [0031] Said process of evaporation and removal of the water can? take place both at atmospheric pressure and at reduced pressure; the choice of the best operating conditions does not jeopardize the result and depends solely on the design criteria of the apparatus linked above all to any energy recovery considerations.
[0032] In una preferita forma realizzativa, ma non limitativa, si ? scelto di operare a pressione ridotta effettuando l?allontanamento dell?acqua a circa 62?C; regolando opportunamente la pressione del sistema, si ottiene l?evaporazione dell?acqua e di parte del solvente alla pressione assoluta di 230 mbar, ottenendo un vapore che, una volta condensato, produce una fase di acqua ed una di solvente in rapporto 1:1 in volume. [0032] In a preferred but non-limiting embodiment, yes? chosen to operate at reduced pressure by removing the water at about 62 ° C; by appropriately regulating the pressure of the system, evaporation of the water and part of the solvent is obtained at the absolute pressure of 230 mbar, obtaining a vapor which, once condensed, produces a water phase and a solvent phase in a 1: 1 ratio by volume.
[0033] Risultati analoghi sono ottenibili operando a pressioni e relative temperature sia pi? che meno elevate. [0033] Analogous results can be obtained by operating at pressures and relative temperatures as well as at higher temperatures. than less high.
[0034] La fase vapore costituita da acqua e solvente viene condensata, ottenendo cos? la separazione naturale del solvente dall?acqua, ricavando una frazione costituita da solvente sostanzialmente puro che pu? essere ricircolato al processo, ed una frazione costituita da acqua. [0034] The vapor phase consisting of water and solvent is condensed, thus obtaining? the natural separation of the solvent from the water, obtaining a fraction consisting of a substantially pure solvent that can? be recirculated to the process, and a fraction consisting of water.
[0035] La fase di disidratazione precedentemente descritta pu? avvenire in uno o pi? stadi, ognuno dei quali produrr? una fase vapore costituita da acqua e solvente che, dopo condensazione, potranno essere separati in modo da permettere di ricircolare il solvente ad inizio processo. [0035] The previously described dehydration step can take place in one or more? stages, each of which will produce? a vapor phase consisting of water and solvent which, after condensation, can be separated in order to allow the solvent to be recirculated at the beginning of the process.
[0036] La pasta saponosa disidratata pu? essere ulteriormente diluita o con lo stesso solvente utilizzato nell?evaporazione dell?acqua o con altro solvente. [0036] The dehydrated soap paste can? be further diluted or with the same solvent used in the evaporation of the water or with another solvent.
[0037] Una terza fase del processo prevede che la miscela liquida costituita dalla pasta saponosa disidratata e diluita dal solvente venga acidificata mediante l?aggiunta di acido onde favorire il processo di scissione dei saponi, detto processo essendo volto a trasformare i saponi degli acidi grassi presenti in acidi grassi liberi e sali. [0037] A third step of the process provides that the liquid mixture consisting of the dehydrated soap paste diluted by the solvent is acidified by adding acid in order to favor the process of splitting the soaps, said process being aimed at transforming the soaps into fatty acids present in free fatty acids and salts.
[0038] Secondo il trovato il dosaggio dell?acido ? quasi stechiometrico; vantaggiosamente ci? comporta che la miscela risultante presenti un pH maggiore di 4, a differenza degli attuali processi noti. [0038] According to the invention, the dosage of the acid? almost stoichiometric; advantageously there? implies that the resulting mixture has a pH greater than 4, unlike the current known processes.
[0039] Ci? permette di utilizzare le normali apparecchiature non essendo necessario l?utilizzo di materiali ad elevata resistenza. [0039] There? it allows you to use normal equipment as it is not necessary to use highly resistant materials.
[0040] Secondo il trovato l?acido utilizzato nel processo pu? essere nitrico, fosforico, cloridrico, solforico, acetico, citrico o una combinazione di questi. [0040] According to the invention, the acid used in the process can? be nitric, phosphoric, hydrochloric, sulfuric, acetic, citric or a combination of these.
[0041] In una preferita forma realizzativa, ma non limitativa, l?acido utilizzato ? acido solforico. [0041] In a preferred but non-limiting embodiment, the acid used? sulfuric acid.
[0042] Data la bassa acidit? minerale della miscela, con un valore di pH maggiore di 4, ? possibile realizzare l?operazione di scissione nello stesso evaporatore, iniettando un?aliquota di acido in questa fase completando eventualmente la reazione di acidificazione della pasta saponosa, in un reattore successivo determinando comunque la scissione totale dei saponi. [0042] Given the low acidity? mineral of the mixture, with a pH value greater than 4,? It is possible to carry out the splitting operation in the same evaporator, by injecting an aliquot of acid in this phase, eventually completing the acidification reaction of the soapy paste, in a subsequent reactor, in any case determining the total splitting of the soaps.
[0043] Dalla scissione si ottengono: [0043] From the split it is possible to obtain:
? una fase costituita da sali cristallizzati e/o in soluzione acquosa la cui composizione dipende dalla natura dei saponi trattati e dell?acido utilizzato (ad esempio si ottiene Na2SO4 nel caso di trattamento di saponi sodici con acido solforico); ? una fase costituita da olio acido e solvente; ? a phase consisting of crystallized salts and / or in aqueous solution whose composition depends on the nature of the treated soaps and the acid used (for example, Na2SO4 is obtained in the case of treatment of sodium soaps with sulfuric acid); ? a phase consisting of acid oil and solvent;
? una eventuale fase intermedia costituita da solvente, lecitina e frazioni insaponificabili derivanti dalla possibile presenza di questi elementi nella pasta saponosa in ingresso al processo. ? a possible intermediate phase consisting of solvent, lecithin and unsaponifiable fractions deriving from the possible presence of these elements in the soapy paste entering the process.
[0044] La fase costituita da olio acido e solvente viene sottoposta ad un processo di separazione del solvente, favorendo il recupero ed il riciclo dello stesso solvente all?inizio del processo. [0044] The phase consisting of acid oil and solvent is subjected to a process of separation of the solvent, favoring the recovery and recycling of the same solvent at the beginning of the process.
[0045] In una preferita forma realizzativa, ma non limitativa, il processo di recupero del solvente avviene mediante evaporazione dello stesso. [0045] In a preferred but non-limiting embodiment, the solvent recovery process takes place by evaporation of the same.
[0046] Tutte le ulteriori frazioni ottenute mediante decantazione, naturale o meccanica, possono essere sottoposte ad un processo di separazione del solvente, dove presente, mediante trattamenti noti in letteratura, al fine di recuperare solvente praticamente puro, da inviare all?inizio del processo, con i seguenti vantaggi rispetto alle tecniche note. [0046] All the further fractions obtained by natural or mechanical decantation can be subjected to a solvent separation process, where present, by means of treatments known in the literature, in order to recover practically pure solvent, to be sent at the beginning of the process , with the following advantages over known techniques.
[0047] Un primo vantaggio consiste nella semplicit? di eliminazione dell?acqua dalle paste saponose a temperature relativamente basse e comunque inferiori a quelle dei processi tradizionali permettendo al tempo stesso di mantenere fluida la miscela, costituita da solvente e pasta saponosa deidratata, destinata ai trattamenti successivi. Ottenendo cos?, durante la fase di evaporazione, una corrente di vapore che, dopo condensazione, si scinde per decantazione in una frazione di solvente praticamente puro, riciclabile al processo, ed una frazione costituita da acqua che presenta valori bassi di COD, non affetta da sali ed acidit? minerale. [0047] A first advantage consists in the simplicity? elimination of water from the soapy pastes at relatively low temperatures and in any case lower than those of traditional processes while allowing the mixture, consisting of solvent and dehydrated soapy paste, to be kept fluid, destined for subsequent treatments. Thus obtaining, during the evaporation phase, a stream of vapor which, after condensation, splits by decantation into a practically pure solvent fraction, recyclable to the process, and a fraction consisting of water with low COD values, not affected from salts and acidity? mineral.
[0048] Un secondo vantaggio ? quello di evitare la formazione di emulsioni stabili durante la decantazione, permettendo quindi che il processo avvenga in tempi rapidi. [0048] A second advantage? that of avoiding the formation of stable emulsions during decanting, thus allowing the process to take place quickly.
[0049] Un terzo vantaggio consiste nell?eliminazione del preventivo condizionamento chimico/fisico delle acque di scarico da avviare alla depurazione, necessario nei processi tradizionali, che porta alla produzione di grandi quantit? di fanghi da smaltire a causa dei sali originati sia dalla scissione che dalla neutralizzazione dell?eccesso di acido. [0049] A third advantage consists in the elimination of the preventive chemical / physical conditioning of the waste water to be sent for purification, necessary in traditional processes, which leads to the production of large quantities. of sludge to be disposed of due to the salts originating from both the splitting and the neutralization of the excess acid.
[0050] Un quarto vantaggio consiste nella facilit? di trattamento delle acque di scarico in impianti biologici convenzionali di depurazione, a differenza di quanto accade con le acque di scarico derivanti dai processi noti che contengono grandi quantit? di sali solubili che rimarrebbero comunque nel refluo rendendole non idonee ad essere trattate nei normali impianti di depurazione. [0050] A fourth advantage consists in the ease of use. of waste water treatment in conventional biological purification plants, unlike what happens with waste water deriving from known processes that contain large quantities? of soluble salts that would still remain in the wastewater making them unsuitable for treatment in normal purification plants.
[0051] Un quinto vantaggio consiste nel poter scegliere di operare la scissione mediante acido a temperature inferiori a quelle indispensabili negli impianti operanti con metodi tradizionali. [0051] A fifth advantage consists in being able to choose to perform the cleavage by acid at temperatures lower than those indispensable in plants operating with traditional methods.
[0052] Un sesto vantaggio ? dovuto alla presenza del solvente durante la scissione, operazione che risulta favorita dalla presenza di una frazione residua dello stesso, che vantaggiosamente accelera la decantazione data la notevole differenza di peso specifico tra le fasi. [0052] A sixth advantage? due to the presence of the solvent during the cleavage, an operation which is favored by the presence of a residual fraction of the same, which advantageously accelerates the decantation given the considerable difference in specific weight between the phases.
[0053] Sorprendentemente si ? constato un settimo vantaggio che consiste nella possibilit? di poter operare utilizzando un dosaggio dell?acido quasi stechiometrico, comunque con pH maggiore di 4, a differenza dei processi tradizionali che operano in condizioni di largo eccesso di acido. [0053] Surprisingly yes? I notice a seventh advantage which consists in the possibility? to be able to operate using an almost stoichiometric acid dosage, in any case with a pH greater than 4, unlike traditional processes that operate in conditions of large acid excess.
[0054] Un ulteriore vantaggio consiste nella possibilit? di recuperare come prodotti commerciali le sostanze che costituirebbero gli inquinanti delle acque di scarico dei metodi tradizionali, valutandole caso per caso in dipendenza dalla natura dell?olio o del grasso in ingresso al processo. [0054] A further advantage consists in the possibility? to recover as commercial products the substances that would constitute the pollutants of the waste water of traditional methods, evaluating them case by case depending on the nature of the oil or fat entering the process.
Esempi e prove sperimentali Examples and experimental tests
Esempio 1 Example 1
Scissione paste saponose derivate da neutralizzazione di olio di Soia: Cleavage of soapy pastes derived from neutralization of soybean oil:
? Umidit? pasta 63% ? Humidity pasta 63%
? Acidit? organica olio acido prodotto: 74% (espressa in acido oleico) ? Acidity organic acid oil product: 74% (expressed as oleic acid)
? Campione utilizzato 544 g ? Sample used 544 g
? Solvente utilizzato 580 ml ? Solvent used 580 ml
Fasi prova sperimentale di laboratorio Laboratory experimental test phases
? Omogeneizzazione a temperatura ambiente ? Homogenization at room temperature
? Disidratazione in evaporatore BUCHI Rotovapor ? BUCHI Rotovapor evaporator dehydration
? Temperatura vapori 62?C ? Vapor temperature 62? C
? Pressione 230 mbar ? Pressure 230 mbar
? Acqua recuperata dopo condensazione 260 ml ? Water recovered after condensation 260 ml
? Scissione a ?60?C con addizione di 27,40 g H2SO4 al 96% (pari al 5,04% sulle paste lavorate) ? Cleavage at? 60? C with the addition of 27.40 g H2SO4 at 96% (equal to 5.04% on processed pastes)
? Miscelazione sino a test dei saponi negativo (circa 30 minuti) ? Mixing until the soap test is negative (about 30 minutes)
? Centrifugazione a 3.000 rpm per 5 minuti ottenendo tre fasi ben distinte ? Centrifugation at 3,000 rpm for 5 minutes obtaining three distinct phases
? Olio acido in fase solvente ? Acid oil in the solvent phase
? Lecitine ed Insaponificabili con solvente ? Lecithins and unsaponifiables with solvent
? Soluzione di solfato di sodio (pH = 5,1) ? Sodium sulphate solution (pH = 5.1)
? Filtrazione dell?olio acido in fase solvente ? Filtration of acid oil in the solvent phase
? Evaporazione del solvente dall?olio acido ? Evaporation of the solvent from the acid oil
? Evaporazione del solvente da lecitina ed insaponificabile ? Evaporation of the solvent from lecithin and unsaponifiables
? Cristallizzazione della soluzione di solfato di sodio Prodotti ottenuti (considerate le perdite tra i vari passaggi di laboratorio) ? Crystallization of the sodium sulphate solution Products obtained (considering the losses between the various laboratory steps)
? Olio acido 182 g ? Sour oil 182 g
? Lecitine ed insaponificabile 13 g ? Lecithin and unsaponifiables 13 g
? Solfato di sodio 28,2 g Analisi prodotti da metodo tradizionale ? Sodium sulphate 28.2 g Analyzes produced by traditional method
Olio acido Sour oil
? Umidit? 1,2% ? Humidity 1.2%
? Impurezze 0,9% ? Impurities 0.9%
? Insaponificabile 4,4% ? Unsaponifiable 4.4%
Acque di scarico (valori tipici industriali) Waste water (typical industrial values)
? COD 15.000?30.000 mg/l ? COD 15,000 - 30,000 mg / l
? Solfati 60.000?100.000 ppm Analisi prodotti da metodo innovativo ? Sulphates 60.000? 100.000 ppm Analysis produced by innovative method
Olio acido Sour oil
? Umidit? 0,1% ? Humidity 0.1%
? Impurezze 0,1% ? Impurities 0.1%
? Insaponificabile 4,09% ? Unsaponifiable 4.09%
Acque di scarico Waste water
? pH ? 7 ? pH? 7
? COD 560 mg/l ? COD 560 mg / l
? solfati totali -Esempio 2 ? total sulphates - Example 2
Scissione paste saponose derivate da neutralizzazione di olio di Girasole: Cleavage of soapy pastes derived from neutralization of sunflower oil:
? Umidit? pasta 52% ? Humidity pasta 52%
? Acidit? organica olio acido prodotto 48% (espressa in acido oleico) ? Acidity organic acid oil produced 48% (expressed as oleic acid)
? Campione utilizzato 402 g ? Sample used 402 g
? Solvente utilizzato 420 ml ? Solvent used 420 ml
Fasi prova sperimentale di laboratorio Laboratory experimental test phases
? Omogeneizzazione a temperatura ambiente ? Homogenization at room temperature
? Disidratazione in evaporatore BUCHI Rotovapor ? BUCHI Rotovapor evaporator dehydration
? Temperatura vapori 62?C ? Vapor temperature 62? C
? Pressione 230 mbar ? Pressure 230 mbar
? Acqua recuperata dopo condensazione 160 mL ? Water recovered after condensation 160 mL
? Scissione a ?60?C con addizione di 17,70 g H2SO4 al 96% (pari al 4,04% sulle paste lavorate) ? Cleavage at? 60? C with the addition of 17.70 g H2SO4 at 96% (equal to 4.04% on processed pasta)
? Miscelazione sino a test dei saponi negativo (circa 30 minuti) ? Mixing until the soap test is negative (about 30 minutes)
? Centrifugazione a 3.000 rpm per 5 minuti ottenendo tre fasi ben distinte ? Centrifugation at 3,000 rpm for 5 minutes obtaining three distinct phases
? Olio acido in fase solvente ? Acid oil in the solvent phase
? Lecitine ed Insaponificabili con solvente ? Lecithins and unsaponifiables with solvent
? Soluzione di solfato di sodio (pH = 4,9) ? Sodium sulphate solution (pH = 4.9)
? Filtrazione dell?olio acido in fase solvente ? Filtration of acid oil in the solvent phase
? Evaporazione del solvente dall?olio acido ? Evaporation of the solvent from the acid oil
? Evaporazione del solvente da lecitina ed insaponificabile ? Evaporation of the solvent from lecithin and unsaponifiables
? Cristallizzazione della soluzione di solfato di sodio Prodotti ottenuti (considerare le perdite tra i vari passaggi di laboratorio) ? Crystallization of the sodium sulphate solution Products obtained (consider the losses between the various laboratory steps)
? Olio acido 166 g ? Acid oil 166 g
? Lecitine ed insaponificabile 12 g ? Lecithin and unsaponifiables 12 g
? Solfato di sodio 16 g ? Sodium sulfate 16 g
Analisi prodotti da metodo tradizionale Analysis of products by traditional method
Olio acido Sour oil
? Umidit? 1,6% ? Humidity 1.6%
? Impurezze 1,1% ? Impurities 1.1%
? Insaponificabile 4,88% ? Unsaponifiable 4.88%
Acque di scarico (valori tipici industriali) Waste water (typical industrial values)
? COD 15.000?30.000 mg/l ? solfati 60.000?100.000 ppm Analisi prodotti da metodo innovativo ? COD 15,000 - 30,000 mg / l? sulphates 60,000? 100,000 ppm Analysis of products by innovative method
Olio acido Sour oil
? Umidit? 0,2% ? Humidity 0.2%
? Impurezze 0,1% ? Impurities 0.1%
? Insaponificabile 5,4% ? Unsaponifiable 5.4%
Acque di scarico Waste water
? pH ? 7 ? pH? 7
? COD 400 mg/l ? COD 400 mg / l
? solfati totali -Esempio 3 ? total sulphates - Example 3
Scissione paste saponose derivate da neutralizzazione di olio di Oliva: Cleavage of soapy pastes derived from neutralization of olive oil:
? Umidit? pasta 63% ? Humidity pasta 63%
? Acidit? organica olio acido prodotto 49% (espressa in acido oleico) ? Acidity organic acid oil produced 49% (expressed as oleic acid)
? Campione utilizzato 598 g ? Sample used 598 g
? Solvente utilizzato 620 ml ? Solvent used 620 ml
Fasi prova sperimentale di laboratorio Laboratory experimental test phases
? Omogeneizzazione a temperatura ambiente ? Homogenization at room temperature
? Disidratazione in evaporatore BUCHI Rotovapor ? BUCHI Rotovapor evaporator dehydration
? Temperatura vapori 62?C ? Vapor temperature 62? C
? Pressione 230 mbar ? Pressure 230 mbar
? Acqua recuperata dopo condensazione 320 mL ? Water recovered after condensation 320 mL
? Scissione a ?60?C con addizione di 19,85 g H2SO4 al 96% (pari al 3,32% sulle paste lavorate) ? Cleavage at? 60? C with the addition of 19.85 g H2SO4 at 96% (equal to 3.32% on processed pasta)
? Miscelazione sino a test dei saponi negativo (circa 30 minuti) ? Mixing until the soap test is negative (about 30 minutes)
? Centrifugazione a 3.000 rpm per 5 minuti ottenendo tre fasi ben distinte ? Centrifugation at 3,000 rpm for 5 minutes obtaining three distinct phases
? Olio acido in fase solvente ? Acid oil in the solvent phase
? Lecitine ed Insaponificabili con solvente ? Lecithins and unsaponifiables with solvent
? Soluzione di solfato di sodio (pH = 5,3) ? Sodium sulphate solution (pH = 5.3)
? Filtrazione dell?olio acido in fase solvente ? Filtration of acid oil in the solvent phase
? Evaporazione del solvente dall?olio acido ? Evaporation of the solvent from the acid oil
? Evaporazione del solvente da lecitina ed insaponificabile ? Evaporation of the solvent from lecithin and unsaponifiables
? Cristallizzazione della soluzione di solfato di sodio Prodotti ottenuti (considerare le perdite tra i vari passaggi di laboratorio) ? Crystallization of the sodium sulphate solution Products obtained (consider the losses between the various laboratory steps)
? Olio acido 186 g ? Sour oil 186 g
? Lecitine ed insaponificabile 15 g ? Lecithin and unsaponifiables 15 g
? Solfato di sodio 21 g ? Sodium sulfate 21 g
Analisi prodotti da metodo tradizionale Analysis of products by traditional method
Olio acido Sour oil
? Umidit? 0,8% ? Humidity 0.8%
? Impurezze 0,6% ? Impurities 0,6%
? Insaponificabile 5,92% ? Unsaponifiable 5.92%
Acque di scarico (valori tipici industriali) Waste water (typical industrial values)
? COD 15.000?30.000 mg/l ? Solfati 60.000?100.000 ppm Analisi prodotti da metodo innovativo ? COD 15,000 - 30,000 mg / l? Sulphates 60,000? 100,000 ppm Analysis of products by innovative method
Olio acido Sour oil
? Umidit? 0,1% ? Humidity 0.1%
? Impurezze 0,1% ? Impurities 0.1%
? Insaponificabile 5,45% ? Unsaponifiable 5.45%
Acque di scarico Waste water
? pH ? 7 ? pH? 7
? COD 380 mg/l ? solfati totali ? COD 380 mg / l? total sulphates
Claims (26)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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IT102020000008212A IT202000008212A1 (en) | 2020-04-17 | 2020-04-17 | PROCESS FOR THE TREATMENT OF SOAPY PASTES ARISING FROM THE NEUTRALIZATION OF VEGETABLE OR ANIMAL OILS OR FATS AND / OR THEIR MIXTURES FOR THE RECOVERY OF THE SUBSTANCES CONTAINED THEREIN |
PCT/IB2021/053158 WO2021209968A1 (en) | 2020-04-17 | 2021-04-16 | Process for treating soapy pastes deriving from the neutralization and/or saponification of vegetable or animal oils or fats and/or mixtures thereof for the recovery of the substances contained therein |
Applications Claiming Priority (1)
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Citations (6)
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US2190593A (en) * | 1939-03-03 | 1940-02-13 | Refining Inc | Process of refining animal and vegetable oils |
GB538156A (en) * | 1939-05-23 | 1941-07-22 | Refining Inc | Improvements in or relating to processes of and apparatus for refining vegetable andanimal oils containing free fatty acids |
US2415313A (en) * | 1943-09-20 | 1947-02-04 | Benjamin Clayton | Recovery of valuable fractions from glyceride oils |
GB747256A (en) * | 1951-12-13 | 1956-03-28 | Extraction Continue De Smet | Process for the refining of oils and fatty materials and apparatus for carrying out the process |
US6399802B2 (en) | 2000-03-24 | 2002-06-04 | Kru Feed Energy Company | Method for soapstock acidulation |
KR101727292B1 (en) * | 2013-11-01 | 2017-04-14 | 고려대학교 산학협력단 | Producing Method of Biodiesel Using Acid Oil Derived From Soapstock and Enzymes |
-
2020
- 2020-04-17 IT IT102020000008212A patent/IT202000008212A1/en unknown
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2021
- 2021-04-16 WO PCT/IB2021/053158 patent/WO2021209968A1/en active Application Filing
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US2190593A (en) * | 1939-03-03 | 1940-02-13 | Refining Inc | Process of refining animal and vegetable oils |
GB538156A (en) * | 1939-05-23 | 1941-07-22 | Refining Inc | Improvements in or relating to processes of and apparatus for refining vegetable andanimal oils containing free fatty acids |
US2415313A (en) * | 1943-09-20 | 1947-02-04 | Benjamin Clayton | Recovery of valuable fractions from glyceride oils |
GB747256A (en) * | 1951-12-13 | 1956-03-28 | Extraction Continue De Smet | Process for the refining of oils and fatty materials and apparatus for carrying out the process |
US6399802B2 (en) | 2000-03-24 | 2002-06-04 | Kru Feed Energy Company | Method for soapstock acidulation |
KR101727292B1 (en) * | 2013-11-01 | 2017-04-14 | 고려대학교 산학협력단 | Producing Method of Biodiesel Using Acid Oil Derived From Soapstock and Enzymes |
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Title |
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HENDRIX W B: "Current practices in continuous cottonseed miscella refining", JOURNAL OF THE AMERICAN OIL CHEMISTS' SOCIETY (JAOCS), SPRINGER, DE, vol. 61, no. 8, 1 January 1984 (1984-01-01), pages 1369 - 1372, XP002454298, ISSN: 0003-021X, DOI: 10.1007/BF02542245 * |
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