CN1054069A - The improvement of method for synthesis of phosphoric acid diester - Google Patents
The improvement of method for synthesis of phosphoric acid diester Download PDFInfo
- Publication number
- CN1054069A CN1054069A CN 90100823 CN90100823A CN1054069A CN 1054069 A CN1054069 A CN 1054069A CN 90100823 CN90100823 CN 90100823 CN 90100823 A CN90100823 A CN 90100823A CN 1054069 A CN1054069 A CN 1054069A
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- CN
- China
- Prior art keywords
- alkaline hydrolysis
- phosphoric acid
- phosphodiester
- flakes
- pickling
- 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.)
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Abstract
The present invention is the improvement on former method for synthesis of phosphoric acid diester, with pure and mild Vanadium Pentoxide in FLAKES is after raw material carries out esterification, through alkaline hydrolysis, distillation, pickling, wash product (I), content is more than 97%, the organic composite chemical fertilizer of by-product, the no three wastes are advanced technologies routes that are suitable for suitability for industrialized production.
Description
The technical field of the invention is the synthetic of phosphodiester class, relates in particular to the synthetic of pure phosphodiester, and the structural formula of phosphodiester is
Wherein R can be C
4～C
10Straight or branched alkane.
Former synthetic method is to be raw material with pure and mild Vanadium Pentoxide in FLAKES, through esterification, and alkaline hydrolysis, pickling, distillation and get (I).This method is when esterification, and Vanadium Pentoxide in FLAKES is 1: 3～1: 3.05 with the mole ratio of alcohol, the yield instability of phosphodiester.The alkaline hydrolysis temperature is at 140 ℃～160 ℃, the rate of decomposition of monoesters about 95%.Material behind the alkaline hydrolysis is through pickling, during the distillation of washing back, vacuum required very high, otherwise the high slightly dibasic acid esters of temperature promptly can decompose, and the content of the low slightly phosphodiester of temperature is just on the low side, and this brings big difficulty when suitability for industrialized production.
The objective of the invention is, improve original processing condition, the yield of raising and stable phosphodiester is recycled phosphorous water liquid behind the alkaline hydrolysis and pickle solution, eliminates the three wastes.
Technical measures of the present invention are: 1, with the mole ratio of Vanadium Pentoxide in FLAKES in the esterification and alcohol for changing 1: 3.15 into, temperature of reaction is 90 ℃～100 ℃ scope internal programs control intensifications, the stable yield that makes phosphodiester is about 95%.2, the alkaline hydrolysis temperature is brought up to about 170 ℃, reacted 6～8 hours, make the monoesters rate of decomposition 98%.3, behind the alkaline hydrolysis an alkali metal salt of phosphodiester with alcohol mixture distill pickling more earlier, wash product (I), a distillation condition GPRS gets final product in that alcohol is steamed fully like this, and an alkali metal salt of phosphodiester can not decompose, and color does not deepen, and the content that obtains product is more than 97%.4, the water liquid behind the alkaline hydrolysis is transferred PH with phosphoric acid, all makes phosphorus potash fertilizer.After pickle solution recycled certain number of times, the crystallization of separating out with filtering in the warp was potash fertilizer, has eliminated the three wastes, and the economic benefit of this technology is improved.
Reaction equation is:
Alkali be situated between used alkali can be NaOH or KOH, in and the acid of pickling be sulfuric acid.
Embodiment:
In three mouthfuls of reaction flasks, add 598 gram isooctyl alcohol, under agitation add Vanadium Pentoxide in FLAKES 189.4 grams, be warming up to 80 ℃, reacted 10 hours, add behind 10% the water 90 ℃ of reactions 3 hours then the alkali lye of hydro-oxidation sodium or potassium hydroxide 160～170 ℃ of reactions 6 hours.After the reactant layering, isooctyl alcohol is reclaimed in the oil reservoir underpressure distillation, and an alkali metal salt of the pure phosphoric acid di-isooctyl that obtains again through 20% sulfuric acid washing and washing, obtains pure product (I), and content reaches more than 97%.Water layer behind the alkaline hydrolysis with phosphoric acid acid adjustment degree, gets KH
2PO
4, sulfuric acid lotion can be applied mechanically repeatedly to separating out crystallization, transfers to neutrality with KOH again, gets K
2SO
4
Experiment showed, simple synthetic method of the present invention, easy handling, the three wastes can be become useful chemical fertilizer, production cost is than the production cost of existing technology, 6000 yuan/ton of minimum reductions, product purity can reach more than 97%, is the advanced technologies of a suitable suitability for industrialized production.
Claims (1)
1, a kind of synthetic method of phosphodiester, by alcohol with the Vanadium Pentoxide in FLAKES esterification after alkaline hydrolysis, pickling, washing, distillation obtains (I), it is characterized in that, the esterification Vanadium Pentoxide in FLAKES is 1: 3.15 with the mole ratio of alcohol, temperature of reaction heats up 90 ℃～100 ℃ scope internal program controls, and the alkaline hydrolysis temperature is controlled at about 170 ℃, 6～8 hours time, phosphodiester becomes an alkali metal salt behind the alkaline hydrolysis, distillation earlier, pickling again, washing obtains product (I), and alkali solution liquid is transferred PH with phosphoric acid, all make phosphorus potash fertilizer, pickle solution recycles certain number of times post neutralization, and the crystallization that filtering is separated out is potash fertilizer and eliminates the three wastes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90100823 CN1054069A (en) | 1990-02-18 | 1990-02-18 | The improvement of method for synthesis of phosphoric acid diester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90100823 CN1054069A (en) | 1990-02-18 | 1990-02-18 | The improvement of method for synthesis of phosphoric acid diester |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1054069A true CN1054069A (en) | 1991-08-28 |
Family
ID=4876823
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90100823 Pending CN1054069A (en) | 1990-02-18 | 1990-02-18 | The improvement of method for synthesis of phosphoric acid diester |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1054069A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114907902A (en) * | 2021-02-08 | 2022-08-16 | 联泓(江苏)新材料研究院有限公司 | Polyoxyethylene ether phosphate ester composition with high content of diester phosphate, and preparation method and application thereof |
-
1990
- 1990-02-18 CN CN 90100823 patent/CN1054069A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114907902A (en) * | 2021-02-08 | 2022-08-16 | 联泓(江苏)新材料研究院有限公司 | Polyoxyethylene ether phosphate ester composition with high content of diester phosphate, and preparation method and application thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |