CN108218916A - A kind of method for preparing dioctyl phosphine oxide - Google Patents
A kind of method for preparing dioctyl phosphine oxide Download PDFInfo
- Publication number
- CN108218916A CN108218916A CN201611151407.XA CN201611151407A CN108218916A CN 108218916 A CN108218916 A CN 108218916A CN 201611151407 A CN201611151407 A CN 201611151407A CN 108218916 A CN108218916 A CN 108218916A
- Authority
- CN
- China
- Prior art keywords
- distilled water
- organic layer
- extraction
- dioctyl
- chloroform
- 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
- 238000000034 method Methods 0.000 title claims abstract description 27
- ZZSSCCQEJRAFTD-UHFFFAOYSA-N 1-octylphosphonoyloctane Chemical compound CCCCCCCCP(=O)CCCCCCCC ZZSSCCQEJRAFTD-UHFFFAOYSA-N 0.000 title claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000012153 distilled water Substances 0.000 claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012044 organic layer Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 230000007062 hydrolysis Effects 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- HUKAPJGYUOHWLS-UHFFFAOYSA-N chloro(dioctyl)phosphane Chemical compound CCCCCCCCP(Cl)CCCCCCCC HUKAPJGYUOHWLS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000003809 water extraction Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- -1 Dioctyl phosphorus chloride Chemical compound 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 abstract description 7
- 239000010865 sewage Substances 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract 1
- 229910052770 Uranium Inorganic materials 0.000 description 10
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 8
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 238000000638 solvent extraction Methods 0.000 description 6
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000003747 Grignard reaction Methods 0.000 description 3
- 239000007818 Grignard reagent Substances 0.000 description 3
- 150000004795 grignard reagents Chemical class 0.000 description 3
- 239000012074 organic phase Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229910052776 Thorium Inorganic materials 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 206010051093 Cardiopulmonary failure Diseases 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BNMJSBUIDQYHIN-UHFFFAOYSA-N butyl dihydrogen phosphate Chemical compound CCCCOP(O)(O)=O BNMJSBUIDQYHIN-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 231100000518 lethal Toxicity 0.000 description 1
- 230000001665 lethal effect Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000956 solid--liquid extraction Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000002351 wastewater Substances 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
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/50—Organo-phosphines
- C07F9/53—Organo-phosphine oxides; Organo-phosphine thioxides
- C07F9/5304—Acyclic saturated phosphine oxides or thioxides
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)
Abstract
The invention discloses a kind of methods for preparing dioctyl phosphine oxide, and dioctyl phosphorus chloride is added in distilled water, 10~30min of stirring hydrolysis at room temperature, pH ＞ 13 are adjusted to 5~15wt%NaOH solution, chloroform extraction takes organic layer, neutrality is washed with distilled water to, organic layer solvent is evaporated off in Rotary Evaporators, with acetic acid, filtering, filter residue is thrown aside, and adds in chloroform and distilled water extraction filtrate, collected organic layer, water washing is distilled to neutrality, and vacuum drying obtains white solid；The preparation method reaction step of the present invention is simple, and environmentally protective, Atom economy is good, and product purity is high, is easily isolated, and has the prospect of industrialization.Products application of the present invention is in water quality detection and sewage treatment industry.
Description
Technical field
The invention belongs to technical field of phosphorous chemical industry, and in particular to a kind of method for preparing trialkyl phosphorus.
Background technology
Extraction refers to compound because of the solubility in two kinds of mutual solubility very littles or fairly insoluble solvent
(distribution coefficient) is different, so as to partially or completely enter one of which solvent.When the number of extraction is enough, compound will be complete
Enter one of which solvent entirely.
Extractant is various in style, generally comprises inorganic and organic extractant.And most of used in industrial production are
Organic extractant has good dissolubility in organic solvent.It is to be treated to increase it with metal to be allowed to be dissolved in organic solvent
Extract the dissolubility of object, and enhance its extraction ability, while its volatility, viscosity and water solubility can also be weakened.Organic extractant
Non-ferrous metal hydrometallurgy industry is largely used to, is mainly used for extracting copper and various noble metals and rare earth.
There are many kinds of the methods of extraction, generally comprises solvent extraction, solid-liquid extraction (leaching), chemical precipitation method, tree
Fat method, aqueous two-phase method, oxidation-reduction method, floatation and electric stripping process.
What is be wherein most widely used is the precipitation method and solvent extraction.The precipitation method are mainly used for sewage disposal, method master
If adding specific chemical reagent into sewage, it is made to react with the substance to be handled being dissolved in waste water, generated
The precipitation of salts of water is insoluble in, so as to which success is removed from sewage.But due to the use of a large amount of chemical reagent, which can cause greatly
The secondary pollution of amount is unfavorable for the green environment advocated energetically now close friend and sustainable development, and is of limited application.
Solvent-extracted extraction process is full liquid process, and two kinds of liquid phases of participation process are respectively water phase and organic phase.Water
The density of phase is typically larger than used organic phase density so that after static layering, organic phase is always located in above water phase.Solvent
Extraction can be used for the element of processing tonne in the industry, can be used for laboratory treatment gram and the element of milligram grade separation and
Enrichment.Solvent extraction is because of spies such as its operation is very simple while cheap, rate of extraction fast, high selectivity, separation rate height
Point has become an indispensable basic fundamental, industrially in the Separation ＆ Purification of current every field
It has been obtained for being widely applied, and wherein most has obtained good effect.Solvent extraction is research in recent years
Red heat point.
Organic phosphates extractant is one of several main extractants of solvent extraction extracting metals ion now, so far for
Only it is widely used to numerous areas.Organic phosphates extractant is various in style, various structures, but generally speaking, in being generally divided into
Property phosphorous and two major class of acidic phosphorus type.
At 1945, people have found that tributyl phosphate (TBP) has effects that extract uranium for the first time.From then on, TBP is gradually
It is taken seriously, till now, is used to post-process nuclear fuel in the world, extract the elements such as thorium therein, uranium.
TBP is under high temperature and radiation, and can degrade generation dibutylphosphoric acid ester (DBP) and monobutyl phosphate (MDP), but DBP and MDP to zirconium,
Niobium member is known as higher mating capability, in addition, DBP and MDP can be combined into thorium, zirconium etc. both it is not soluble in water be also insoluble in it is organic molten
The substance of agent, a large amount of precipitation can cover whole system, extraction efficiency caused to drastically reduce.Therefore, the use of TBP extractants
Service life is very short.
Therefore, people begin one's study modified technique flow, and have carried out research extensively and profoundly to phosphorus-contained extractant.People
It was found that when using D2When EHPA makees extractant, two different amine solvents are screened, such as ethylene diamine, 1,2- propane diamine, 1,3- the third two
Amine etc., the extraction yield of uranium can promote 18~36 times.On the other hand, if in neutral ligand, such as dihexyl-N, N- diethyl
Tributyl phosphate and trioctylphosphine oxide are added in base-carbamyl phosphate methyl esters, the extraction efficiency of uranium ion can be greatly improved.When
Tributyl phosphate (TBP), trioctylphosphine oxide (TOPO), D2EHPA is used with when making extractant, and effect of extracting is very good.
The uranium mill in China is all using eluex process to extract uranium ion mostly, which uses organophosphor as extraction
Di-(2-ethylhexyl)phosphoric acid (the D of agent, i.e. 0.2mol/L2EHPA) with the trialkyl phosphorus of 0.1mol/L (TRPO) system,
The uranium product purity obtained by this flow is high not enough, wherein still containing various metals impurity.This crude product need to pass through TBP
Extraction process can obtain purified product after refining, and it is pure to reach core.
Trioctylphosphine oxide is widely used in the extraction of uranium in industry, usually with the D of different proportion2EHPA is combined, extraction effect
Rate is all very high, but has realized that industrialized trialkyl phosphorus also only has trioctylphosphine oxide, therefore, researchs and develops other at present
The industrialized production route of trialkyl phosphorus has great importance to finding new efficient extractant.
There are two types of the methods of the synthesis trialkyl phosphorus of mainstream in the world：Grignard reagent method and hydrogen phosphide synthetic method are led to
It crosses grignard reaction and prepares trioctylphosphine oxide, the biggest advantage is to only need to can obtain product by single step reaction, and produce
Object purity is very high.It is well known that grignard reaction has disadvantages that：Operation difficulty is high, and the condition for preparing Grignard Reagent is very tight
Lattice, for Grignard Reagent to water and oxygen all extreme sensitivities, yield is generally very low.Grignard reaction condition is too harsh, is not suitable for out very much
Send out into industrial manufacture process.Hydrogen phosphide addition process, product purity is relatively low, there is many impurity and by-product.In addition, used original
Expect phosphatization.Hydrogen is also violent in toxicity, not only irritant but also be system.Toxic agent, if sucking can be to heart, respiratory system.Kidney, intestines
Stomach, nervous system.Damaged with liver, gently then cause shed tears, cough, dizziness, headache, the symptoms such as nausea and vomiting, it is heavy then can
It can cause to tremble, spasm, cardiorespiratory failure and death.Concentration reaches 9.7mg/m3Poisoning will be caused above；550~
830mg/m3Dead, 2798mg/m occurs for 0.5~1.0 hour for contact3It can be lethal rapidly.And the hydrogen phosphide of trace in air can
Spontaneous combustion, the aerial concentration of hydrogen phosphide reach 1.8% (26g/m3) more than can explode.
Neutral organophosphorus extractant is widely used in the extraction process of uranium, they generally have very high selectivity to uranium
With certain chemical radiation stability, but carried out currently on the market industrialized production only three n-octyl phosphorous oxides, and
Production method or toxicity is larger or low yield, it is still desirable to improve, and need to develop a greater variety of trialkyl phosphorus
Production method.
Invention content
In view of this, the purpose of the present invention is to provide a kind of methods for preparing dioctyl phosphine oxide, are reacted in the hope of reducing
Pollution and toxicity, and improve yield and product purity.
To achieve the above object, the present invention provides following technical solution：
Dioctyl phosphorus chloride is added in distilled water, stirring hydrolysis by a kind of method for preparing dioctyl phosphine oxide at room temperature
10~30min is adjusted to pH ＞ 13 with 5~15wt%NaOH solution, and chloroform extraction takes organic layer, is washed with distilled water to
Organic layer solvent is evaporated off in neutrality, Rotary Evaporators, and with acetic acid, filtering, filter residue is thrown aside, and adds in chloroform and distilled water extraction
Filtrate, collected organic layer are taken, distillation water washing to neutrality is dried in vacuo and obtains white solid.
Preferably, dioctyl phosphorus chloride is added in into distilled water, stirring hydrolysis 15min at room temperature.
Preferably, pH ＞ 13 are adjusted to 10wt%NaOH solution.
The preparation method reaction step of the present invention is simple, and environmentally protective, Atom economy is good, and product purity is high, is easy to point
From the prospect with industrialization.
Specific embodiment
The technical solution in the embodiment of the present invention will be described in detail below, it is clear that described embodiment is only
Only it is part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's all other embodiments obtained under the premise of creative work is not made belong to the model that the present invention protects
It encloses.
Embodiment 1
Dioctyl phosphorus chloride is added in into distilled water at room temperature, stirring hydrolysis 10min is adjusted to pH with 5wt%NaOH solution
＞ 13, chloroform extraction take organic layer, are washed with distilled water to neutrality, and Rotary Evaporators are evaporated off organic layer solvent, use acetic acid
Dissolving, filtering, filter residue are thrown aside, addition chloroform and distilled water extraction filtrate, collected organic layer, distillation water washing to neutrality,
Vacuum drying obtains white solid, yield 98%.
Embodiment 2
Dioctyl phosphorus chloride is added in into distilled water at room temperature, stirring hydrolysis 30min is adjusted to pH with 15wt%NaOH solution
＞ 13, chloroform extraction take organic layer, are washed with distilled water to neutrality, and Rotary Evaporators are evaporated off organic layer solvent, use acetic acid
Dissolving, filtering, filter residue are thrown aside, addition chloroform and distilled water extraction filtrate, collected organic layer, distillation water washing to neutrality,
Vacuum drying obtains white solid, yield 98.5%.
Embodiment 3
Dioctyl phosphorus chloride is added in into distilled water at room temperature, stirring hydrolysis 20min is adjusted to pH with 10wt%NaOH solution
＞ 13, chloroform extraction take organic layer, are washed with distilled water to neutrality, and Rotary Evaporators are evaporated off organic layer solvent, use acetic acid
Dissolving, filtering, filter residue are thrown aside, addition chloroform and distilled water extraction filtrate, collected organic layer, distillation water washing to neutrality,
Vacuum drying obtains white solid, yield 99%.
For those skilled in the art, it is clear that the present invention is not limited to the details of above-mentioned exemplary embodiment, and not
In the case of the spirit or essential attributes of the present invention, the present invention can be realized in other specific forms.Therefore, no matter from
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended right
It is required that rather than above description limit, it is intended that all changes that will be fallen within the meaning and scope of the equivalent requirements of the claims
Change is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in each embodiment can also be properly combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (3)
- A kind of 1. method for preparing dioctyl phosphine oxide, which is characterized in that include the following steps：Dioctyl phosphorus chloride is added in into distilled water, stirring 10~30min of hydrolysis, with 5~15wt%NaOH solution tune at room temperature To pH ＞ 13, chloroform extraction takes organic layer, is washed with distilled water to neutrality, and organic layer solvent is evaporated off in Rotary Evaporators, uses Acetic acid, filtering, filter residue are thrown aside, and add in chloroform and distilled water extraction filtrate, collected organic layer, distillation water washing is into Property, vacuum drying obtains white solid.
- 2. according to the method described in claim 1, it is characterized in that：Dioctyl phosphorus chloride is added in into distilled water at room temperature, is stirred Mix hydrolysis 15min.
- 3. according to the method described in claim 1, it is characterized in that：PH ＞ 13 are adjusted to 10wt%NaOH solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611151407.XA CN108218916A (en) | 2016-12-13 | 2016-12-13 | A kind of method for preparing dioctyl phosphine oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611151407.XA CN108218916A (en) | 2016-12-13 | 2016-12-13 | A kind of method for preparing dioctyl phosphine oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108218916A true CN108218916A (en) | 2018-06-29 |
Family
ID=62638975
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611151407.XA Pending CN108218916A (en) | 2016-12-13 | 2016-12-13 | A kind of method for preparing dioctyl phosphine oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108218916A (en) |
-
2016
- 2016-12-13 CN CN201611151407.XA patent/CN108218916A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106521190B (en) | The phosphine of neutrality containing amino extractant is used for the purposes and method of extracting and separating zirconium and/or hafnium | |
| CN104232896A (en) | Method for separating lithium from salt lake brine | |
| CN108004420A (en) | The technique that lithium is extracted from the bittern of alkalescence containing lithium based on centrifugal extractor | |
| CN109355502A (en) | A method of extracting lithium ion from acid system | |
| CN105018753B (en) | A kind of method of composite extractant and the composite extractant extract and separate recovery indium | |
| CN104263970A (en) | Lithium ion extracting agent | |
| CN109852794A (en) | A method of being used to prepare LITHIUM BATTERY nickel sulfate | |
| CN108218916A (en) | A kind of method for preparing dioctyl phosphine oxide | |
| CN104945436A (en) | Minodronic acid preparing method | |
| CN105944768B (en) | A kind of method that rhodium catalyst is recycled in the waste water phase from rhodium-containing | |
| CN108610374A (en) | A method of preparing didecyl phosphine oxide | |
| CN100400687C (en) | Method of extracting radioactive uranium in phosphate | |
| US3641226A (en) | Method for purification of di-(2-ethyl-hexyl) phosphoric acid | |
| CN115403018B (en) | Method for preparing ferric phosphate by high-impurity phosphoric acid and preparation method of positive electrode material | |
| CN108610377A (en) | A method of preparing trioctylphosphine oxide | |
| CN108610375A (en) | A method of preparing three decyl phosphorous oxides | |
| CN108218915A (en) | A kind of method for preparing octyl group-didecyl phosphorous oxide | |
| CN107674974B (en) | The purposes and method of the phosphine extractant extraction and recovery copper of neutrality containing amino | |
| CN108610376A (en) | A method of preparing hexyl-dioctyl phosphorous oxide | |
| CN108610371A (en) | A method of hydrolysis addition prepares trioctylphosphine oxide | |
| CN108610372A (en) | A method of preparing dioctyl-decyl phosphorous oxide | |
| CN108610373A (en) | A method of preparing hexyl-didecyl phosphorous oxide | |
| CN102992288B (en) | Method for preparing high pure phosphoric acid from calcium hydrogen phosphate | |
| CN104232897A (en) | Lithium ion extraction system | |
| CN108610370A (en) | A method of preparing dioctyl phosphorus chloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180629 |