DE242422C - - Google Patents
Info
- Publication number
- DE242422C DE242422C DENDAT242422D DE242422DA DE242422C DE 242422 C DE242422 C DE 242422C DE NDAT242422 D DENDAT242422 D DE NDAT242422D DE 242422D A DE242422D A DE 242422DA DE 242422 C DE242422 C DE 242422C
- Authority
- DE
- Germany
- Prior art keywords
- phosphoric acid
- acid
- glycerol
- glycerine
- phosphate
- 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.)
- Active
Links
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 9
- 235000011187 glycerol Nutrition 0.000 claims description 9
- XYZZKVRWGOWVGO-UHFFFAOYSA-N Glycerol-phosphate Chemical compound OP(O)(O)=O.OCC(O)CO XYZZKVRWGOWVGO-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 235000021317 phosphate Nutrition 0.000 description 3
- 150000003016 phosphoric acids Chemical class 0.000 description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical class [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 150000008043 acidic salts Chemical class 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002319 glycerophosphoglycerols Chemical class 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/091—Esters of phosphoric acids with hydroxyalkyl compounds with further substituents on alkyl
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Materials For Medical Uses (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
PATENTSCHRIFTPATENT LETTERING
- M 242422 -' KLASSE 12 o. GRUPPE- M 242422 - 'CLASS 12 or GROUP
Verfahren zur Darstellung von Glycerinphosphorsäure.Process for the preparation of glycerol phosphoric acid.
Nach den bisher bekannt gewordenen Verfahren zur Darstellung der Glycerinphosphorsäure geht man gewöhnlich von Phosphorsäure aus, die man auf überschüssiges GIy-cerin in der Wärme einwirken läßt.According to the previously known method for the preparation of glycerol phosphoric acid one usually starts from phosphoric acid, which is based on excess glycerin lets act in the warmth.
Es ist nun gefunden worden, daß die Veresterung wesentlich günstiger bewirkt werden kann, wenn man statt der fertigen Phosphorsäure phosphorsaure Salze anwendet und ausIt has now been found that the esterification can be effected much more favorably can, if you apply phosphoric acid salts instead of the finished phosphoric acid and off
ίο diesen mittels saurer Agenzien (freier Säure oder saurer Salze) die Phosphorsäure in Freiheit setzt, ohne zuvor die durch Umlagerung entstehenden unlöslichen Salze abzuscheiden. Dabei ist es gleichgültig, ob man zunächst die phosphorsauren Salze mit dem Glycerin mischt und dann erst das saure Agens zugibt, oder ob man zuerst die zur Verdrängung der Phosphorsäure geeignete Säure bzw. das saure Salz mit dem Phosphat mischt undίο this by means of acidic agents (free acid or acidic salts) which sets phosphoric acid free, without the prior rearrangement to separate the resulting insoluble salts. It does not matter whether you go first mixes the phosphoric acid salts with the glycerine and only then adds the acidic agent, or whether one should first choose the acid or acid suitable for displacing the phosphoric acid. mix the acid salt with the phosphate and
so dann erst das Glycerin hinzufügt, oder ob man schließlich das saure Agens dem Glycerin vorsichtig zugibt und in dieses Gemisch bzw. diese Lösung nun das Phosphat einträgt. Die auf die eine oder andere Weise hergestellte Mischung wird dann unter gewöhnlichem oder vermindertem Druck erhitzt, bis Stillstand in der Esterbildung eingetreten ist.so only then add the glycerine, or whether finally, the acidic agent is carefully added to the glycerine and poured into this mixture or this solution now enters the phosphate. The one made in one way or another Mixture is then heated under ordinary or reduced pressure until a standstill in the ester formation has occurred.
Von dem in der Patentschrift 208700 beschriebenen Verfahren, bei dem man saure Phosphate (saures Mononatriumphosphat oder Monoammoniumphosphat) auf Glycerin einwirken läßt, um Diglycerinphosphat zu erhalten, das bei weiterer Behandlung mit Natronlauge gespalten und zu dem Monoester des Dinatriumsalzes verseift wird, unterscheidet sich das vorliegende Verfahren, das die Darstellung von freier Glycerinphosphorsäure zum Gegenstand hat, wesentlich dadurch, daß es hierbei auf die Wirkung von Phosphorsäure in statu nascendi ankommt. Die aus dem phosphorsauren Salz durch das saure Agens in Freiheit gesetzte Phosphorsäure wird im Entstehungszustand mit dem Glycerin verestert.Of the process described in the patent specification 208700, in which one acid Phosphates (acid monosodium phosphate or monoammonium phosphate) act on glycerine leaves to obtain diglycerol phosphate, which upon further treatment with sodium hydroxide solution is split and saponified to the monoester of the disodium salt differs the present process, which relates to the preparation of free glycerol phosphoric acid has, essentially in that it is here on the effect of phosphoric acid in statu nascendi arrives. Those from the phosphoric acid salt by the acidic agent in freedom The phosphoric acid that is added is esterified with the glycerine as it is formed.
Zur Reinigung führt man die Glycerinphosphorsäure zweckmäßig in das Barytsalz über, aus dem dann die reine Säure wieder freigemacht wird, z.B. durch Schwefelsäure. Andere glycerinphosphorsäure Salze kann man direkt durch Wechselzersetzung aus dem Barytsalz gewinnen.For cleaning, the glycerol phosphoric acid is expediently converted into the barite salt, from which the pure acid is then released again, e.g. by sulfuric acid. Other Glycerine phosphoric acid salts can be obtained directly from the barite salt by alternating decomposition to win.
Das neue Verfahren hat wesentliche Vorteile. Abgesehen davon, daß >v man ein sehr billiges Ausgangsmaterial anwenden kann, tritt hierbei eine energischere Esterbildung ein, ferner üben die in dem Phosphorsäureglyceringemisch befindlichen fremden Salze, in dem sie gewissermaßen als Verdünnungsmittel auftreten, eine mäßigende Wirkung auf Nebenreaktionen aus, denen das Glycerin sonst unterliegt. The new process has significant advantages. Apart from the fact that> v can be applied a very cheap starting material in this case occurs, a more vigorous Esterbildung a further, practice the present in the phosphoric acid glycerol mixture foreign salts, in which they are to some extent act as a diluent a moderating effect on side reactions, which otherwise glycerol subject.
100 kg neutraler phosphorsaurer Kalk oder 167 kg sekundäres Calciumphosphat werden mit 95 kg Schwefelsäure von 66° Be. und 75 bzw. 68 kg Glycerin von spez. Gew. 1,25 zu einer breiigen Masse verarbeitet, Man bringt dieses Gemisch in ein Rührwerk und erhitzt es bei 20 bis 40 mrn Druck langsam bei steigender Temperatur, bis herausgenommene Proben eine100 kg of neutral phosphoric acid lime or 167 kg of secondary calcium phosphate are added 95 kg sulfuric acid of 66 ° Be. and 75 or 68 kg of glycerol of spec. Wt. 1.25 to one pasty mass processed, one brings this mixture into a stirrer and heated it at 20 to 40 mrn pressure slowly with increasing temperature, until taken samples a
MICROFILMED BYMICROFILMED BY
• FIAT• FIAT
Abnahme der Phosphorsäure nicht mehr erkennen lassen. Nachdem die Temperatur auf etwa 5"o° gefallen ist, wird die nach vollständigem Erkalten steinharte Masse mit Wasser von derselben Temperatur aufgenommen, der Gips abgepreßt und die wäßrige Glycerinphosphorsäure in bekannter Weise auf die verschiedenen Salze verarbeitet.Do not show a decrease in phosphoric acid. After the temperature up has fallen about 5 "o °, the rock-hard mass after complete cooling becomes rock-hard with water taken from the same temperature, pressed the plaster and the aqueous glycerol phosphoric acid processed in a known manner on the various salts.
Claims (1)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE242422C true DE242422C (en) |
Family
ID=501627
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT242422D Active DE242422C (en) |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE242422C (en) |
-
0
- DE DENDAT242422D patent/DE242422C/de active Active
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