SU166691A1 - METHOD OF ISOLATION OF HIGH-MOLECULAR MONOALYCYL PHOSPHORIC ACIDS - Google Patents
METHOD OF ISOLATION OF HIGH-MOLECULAR MONOALYCYL PHOSPHORIC ACIDSInfo
- Publication number
- SU166691A1 SU166691A1 SU839394A SU839394A SU166691A1 SU 166691 A1 SU166691 A1 SU 166691A1 SU 839394 A SU839394 A SU 839394A SU 839394 A SU839394 A SU 839394A SU 166691 A1 SU166691 A1 SU 166691A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- phosphoric acids
- monoalycyl
- isolation
- molecular
- water
- Prior art date
Links
- 150000003016 phosphoric acids Chemical class 0.000 title description 3
- 238000002955 isolation Methods 0.000 title 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 235000011007 phosphoric acid Nutrition 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- -1 alkyl phosphoric acids Chemical class 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005591 charge neutralization Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000001264 neutralization Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N Octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K [O-]P([O-])([O-])=O Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- JTXUVYOABGUBMX-UHFFFAOYSA-N didodecyl hydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(=O)OCCCCCCCCCCCC JTXUVYOABGUBMX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 159000000011 group IA salts Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003472 neutralizing Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Description
Известен способ выделени высокомолекул рных моноалкилфосфорных кислот из смеси технических продуктов нейтрализацией смеси щелочью с последующей отмывкой образовавшейс щелочной соли моноалкилфосфорной кислоты водой и подкислением.There is a known method for isolating high molecular weight monoalkyl phosphoric acids from a mixture of technical products by neutralizing the mixture with an alkali, followed by washing the alkaline monoalkyl phosphoric acid salt formed with water and acidifying.
С целью упрощени способа и получени продукта с более высокой степенью чистоты предлагаетс обработку водой производить при мол рном соотнощении 1:1.In order to simplify the process and to obtain a product with a higher degree of purity, it is proposed to treat with water at a molar ratio of 1: 1.
Пример. Технический продукт, содержащий 15-189/0 МОНО-, 12-15Vo диалкилфосфорных кислот и небольшие количества триалкилфосфатов и непрореагировавщих спиртов , предварительно концентрируют путем обработки технического продукта водным раствором соды при рН 9,5-10. При этом одновременно происходит частична очистка от триалкилфосфата и непрореагировавшего спирта. Водный раствор затем подкисл ют серной кислотой до рН 1 н алкилфосфорпые кислоты экстрагируют бензолом с получением раствора с концентрацией 20-40э/о по алкилфосфориым кислотам. Затем в бензольный раствор добавл ют твердый едкий кали в количестве, необходимом дл полной нейтрализации , и смесь перемешивают до полного растворени щелочи. В полученный таким образом раствор ири перемешивании добавл ют в течение 1 час воду из расчета 1 моль воды на 1 моль мополаурилфосфорной кислоты (МЛФК). При этом происходит выделение из раствора кристаллогидрата калиевой соли МЛФК. При добавлении больших количеств образуетс плохо фильтрующийс осадок . Диалкилфосфорна кислота практически в этих услови х не осаждаетс . Осадок калиевой солн МЛФК отфильтровывают, промывают бензолом, а затем нейтрализуют серной кислотой и экстрагируют бензолом. После отгонки растворител МЛФК содержит не более 1-2о/о дилаурилфосфорной кислоты. При повторении онерации осаждени удаетс получить МЛФК, содержащую не более 0,1о/о днлаурилфосфориой кислоты.Example. Technical product containing 15-189 / 0 MONO-, 12-15Vo dialkylphosphoric acids and small amounts of trialkylphosphates and unreacted alcohols are pre-concentrated by treating the technical product with an aqueous solution of soda at pH 9.5-10. At the same time, partial purification of trialkyl phosphate and unreacted alcohol occurs. The aqueous solution is then acidified with sulfuric acid to pH 1 with alkyl phosphoric acids extracted with benzene to obtain a solution with a concentration of 20-40 e / o for alkyl phosphoric acids. Then, solid potassium hydroxide is added to the benzene solution in an amount necessary for complete neutralization, and the mixture is stirred until the alkali is completely dissolved. Water is added to the solution of stirring thus obtained for 1 hour at the rate of 1 mol of water per 1 mol of mopolyuryl phosphoric acid (MLFC). When this occurs, the selection of the solution of the hydrochloride of the potassium salt MLFC. When large quantities are added, a poorly filtered precipitate is formed. Dialkylphosphoric acid does not practically precipitate under these conditions. The precipitate of potassium solar MLFC is filtered off, washed with benzene, and then neutralized with sulfuric acid and extracted with benzene. After distilling off the solvent, MLPC contains no more than 1–2 / o dilauryl phosphoric acid. By repeating the deposition of the precipitation, it is possible to obtain MLPC containing not more than 0.1 ° / d of dnlauryl phosphoric acid.
МЛФК представл ет собой прозрачиую, светло-коричневую, слегка оналесцирующую жидкость, уд. вес. 1,043.MLFC is a clear, light brown, slightly onalescent liquid, beats. weight. 1.043.
Определение содержани моно- и диалкилфосфориой кислоты провод т потенциометрическим титрованием в н. октане.The content of mono- and dialkylphosphoric acid is determined by potentiometric titration in n. octane.
Предмет изобретени Subject invention
Способ выделени высокомолекул рных моноалкнлфосфорных кнслот из смеси технических продуктов в среде органического растворител нейтрализацией смеси щелочью с последующей обработкой полученных щелочных солей моноалкилфосфорной кислоты водой н подкислением, о т л и ч а ю щ и и с тем, что, с целью упрощени способа и увелнче 111 степеии чистоты продукта, обработку водой ведут при мол рном соотношенни 1 ; 1.The method of separation of high molecular weight monoalkanol phosphorus slots from a mixture of technical products in an organic solvent medium by neutralization of the mixture with an alkali and subsequent treatment of the obtained alkaline salts of monoalkylphosphoric acid with water and acidification, so that, in order to simplify the process and increase 111 degrees of purity of the product, treatment with water is carried out at a molar ratio of 1; one.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU166691A1 true SU166691A1 (en) |
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