CN107793446A - A kind of purification process of SILVER REAGENT tributyl phosphate - Google Patents
A kind of purification process of SILVER REAGENT tributyl phosphate Download PDFInfo
- Publication number
- CN107793446A CN107793446A CN201610785592.1A CN201610785592A CN107793446A CN 107793446 A CN107793446 A CN 107793446A CN 201610785592 A CN201610785592 A CN 201610785592A CN 107793446 A CN107793446 A CN 107793446A
- Authority
- CN
- China
- Prior art keywords
- tributyl phosphate
- nitric acid
- purification process
- sodium hydroxide
- silver reagent
- 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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Classifications
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- 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 System
- 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
Abstract
The invention provides a kind of purification process of SILVER REAGENT tributyl phosphate, comprise the following steps that：(1) 1.2 1.5% nitric acid are added into tributyl phosphate and are stirred, liquid separation removes nitric acid layer；(2) continuously washed with 0.6 0.8% sodium hydroxide solution again, each sodium hydroxide discards, then not aobvious alkaline with pure water to water layer PH；(3) and then oil reservoir is in distilling flask, is evaporated under reduced pressure under the conditions of≤0.08MPa, discards front-end volatiles, produce；Methods described technique is simple, and product purity is high, and operating condition is gentle, is adapted to the needs of scale industrial production.
Description
Technical field
The present invention relates to a kind of method of purification of chemical reagent, especially a kind of purifying side of SILVER REAGENT tributyl phosphate
Method.
Background technology
Tributyl phosphate, cas126-73-8, as GC stationary liquid, extraction cobalt, iridium, manganese, molybdenum, palladium, rhodium, nickel, uranium
And tungsten, colorimetric estimation molybdenum.Can also be used for the solvent of nitrocellulose and ethyl cellulose, plasticizer, rare earth metal separation agent and
Organic synthesis intermediate.
Tributyl phosphate, major impurity is organic pyrophosphate, only son's based phosphates, dibutylphosphoric acid in industrial products
Salt, butanol etc., product quality do not meet reagent standard, need to be purified applied to reagent.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of purification process of SILVER REAGENT tributyl phosphate.
In order to solve the above technical problems, the technical scheme is that：
A kind of purification process of SILVER REAGENT tributyl phosphate, specific preparation process are as follows：
(1) 1.2-1.5% nitric acid is added into tributyl phosphate and is stirred, liquid separation removes nitric acid layer；
(2) continuously washed with 0.6-0.8% sodium hydroxide solution again, each sodium hydroxide discards, then is washed with pure water
Wash to the not aobvious alkalescence of water layer PH；
(3) and then oil reservoir is in distilling flask, is evaporated under reduced pressure under the conditions of≤- 0.08MPa, discards front-end volatiles, produce.
Preferably, the purification process of mentioned reagent level tributyl phosphate, the tributyl phosphate and 1.2-1.5% nitric acid
Volume ratio is 10:1.
The beneficial effects of the invention are as follows：
The purification process of mentioned reagent level tributyl phosphate, technique is simple, and product purity is high, and operating condition is gentle, is adapted to
The needs of scale industrial production.
Embodiment
Technical scheme of the present invention is further described with reference to specific embodiment.
Embodiment 1
A kind of purification process of SILVER REAGENT tributyl phosphate, specific preparation process are as follows：
(1) 3000ml tributyl phosphates are placed in beaker, add 1.2-1.5% nitric acid 300ml, stirring, liquid separation removes
Nitric acid layer；
(2) 0.6-0.8% sodium hydroxide solution is used again, and continuous to wash 3 times, each 300ml, each sodium hydroxide is abandoned
Go, then it is not aobvious alkaline with pure water to water layer PH；
(3) and then oil reservoir is in distilling flask, is evaporated under reduced pressure under the conditions of≤- 0.08MPa, discards front-end volatiles 20-30ml,
Produce, the positive cut of gained is detected according to GB/T15354-2011, up to 99.5%, content and impurity meet point its content
Analyse pure standard.
The above-mentioned detailed description carried out with reference to embodiment to a kind of purification process of SILVER REAGENT tributyl phosphate, is explanation
Property rather than it is limited, can include several embodiments according to limited scope, therefore of the invention overall not departing from
Changing and modifications under design, should belong within protection scope of the present invention.
Claims (2)
- A kind of 1. purification process of SILVER REAGENT tributyl phosphate, it is characterised in that：Specific preparation process is as follows：(1) 1.2-1.5% nitric acid is added into tributyl phosphate and is stirred, liquid separation removes nitric acid layer；(2) continuously being washed with 0.6-0.8% sodium hydroxide solution again, each sodium hydroxide discards, then with pure water extremely The not aobvious alkalescence of water layer PH；(3) and then oil reservoir is in distilling flask, is evaporated under reduced pressure under the conditions of≤- 0.08MPa, discards front-end volatiles, produce.
- 2. the purification process of SILVER REAGENT tributyl phosphate according to claim 1, it is characterised in that：The tributyl phosphate Volume ratio with 1.2-1.5% nitric acid is 10:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610785592.1A CN107793446A (en) | 2016-08-31 | 2016-08-31 | A kind of purification process of SILVER REAGENT tributyl phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610785592.1A CN107793446A (en) | 2016-08-31 | 2016-08-31 | A kind of purification process of SILVER REAGENT tributyl phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107793446A true CN107793446A (en) | 2018-03-13 |
Family
ID=61527657
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610785592.1A Pending CN107793446A (en) | 2016-08-31 | 2016-08-31 | A kind of purification process of SILVER REAGENT tributyl phosphate |
Country Status (1)
| Country | Link |
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| CN (1) | CN107793446A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115105857A (en) * | 2021-03-23 | 2022-09-27 | 郑州天一萃取科技有限公司 | Purifying treatment agent and purifying method for tributyl phosphate waste organic phase |
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|---|---|---|---|---|
| CN85104673A (en) * | 1985-06-14 | 1987-01-21 | 南开大学 | The production process of tributyl phosphate |
| CN1257075A (en) * | 1998-12-14 | 2000-06-21 | 旭化成工业株式会社 | Method for preparing phosphate ester |
| CN1544439A (en) * | 2003-11-14 | 2004-11-10 | 无锡市红星化工厂 | High purity tributyl phosphate production method |
| CN1633441A (en) * | 2001-02-08 | 2005-06-29 | 阿克佐诺贝尔股份有限公司 | Process for purification of phosphate esters |
| CN101381375A (en) * | 2008-09-25 | 2009-03-11 | 无锡市红星化工厂 | Preparation method of Tri-iso-butyl phosphate |
| CN101633670A (en) * | 2008-07-25 | 2010-01-27 | 气体产品与化学公司 | Removal of trace arsenic impurities from triethylphosphate (tepo) |
| CN101985452A (en) * | 2010-11-17 | 2011-03-16 | 中化重庆涪陵化工有限公司 | Regeneration technology of tributyl phosphate |
| CN104211727A (en) * | 2014-08-01 | 2014-12-17 | 洛阳市三诺化工有限公司 | Preparation method of tributyl phosphate |
| CN104230983A (en) * | 2014-09-18 | 2014-12-24 | 徐州市建平化工有限公司 | Production method of tributyl phosphate |
| CN104292257A (en) * | 2014-02-14 | 2015-01-21 | 郑州市德众化学试剂厂 | Preparation method of dialkyl hypophosphorous acid |
| CN104892666A (en) * | 2015-06-26 | 2015-09-09 | 四川中萃化工有限公司 | Method for preparing high-purity tributyl phosphate |
| CN105859770A (en) * | 2016-05-09 | 2016-08-17 | 云南云天化以化磷业研究技术有限公司 | Method of synthesizing alkyl phosphate |
-
2016
- 2016-08-31 CN CN201610785592.1A patent/CN107793446A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85104673A (en) * | 1985-06-14 | 1987-01-21 | 南开大学 | The production process of tributyl phosphate |
| CN1257075A (en) * | 1998-12-14 | 2000-06-21 | 旭化成工业株式会社 | Method for preparing phosphate ester |
| CN1633441A (en) * | 2001-02-08 | 2005-06-29 | 阿克佐诺贝尔股份有限公司 | Process for purification of phosphate esters |
| CN1544439A (en) * | 2003-11-14 | 2004-11-10 | 无锡市红星化工厂 | High purity tributyl phosphate production method |
| CN101633670A (en) * | 2008-07-25 | 2010-01-27 | 气体产品与化学公司 | Removal of trace arsenic impurities from triethylphosphate (tepo) |
| CN101381375A (en) * | 2008-09-25 | 2009-03-11 | 无锡市红星化工厂 | Preparation method of Tri-iso-butyl phosphate |
| CN101985452A (en) * | 2010-11-17 | 2011-03-16 | 中化重庆涪陵化工有限公司 | Regeneration technology of tributyl phosphate |
| CN104292257A (en) * | 2014-02-14 | 2015-01-21 | 郑州市德众化学试剂厂 | Preparation method of dialkyl hypophosphorous acid |
| CN104211727A (en) * | 2014-08-01 | 2014-12-17 | 洛阳市三诺化工有限公司 | Preparation method of tributyl phosphate |
| CN104230983A (en) * | 2014-09-18 | 2014-12-24 | 徐州市建平化工有限公司 | Production method of tributyl phosphate |
| CN104892666A (en) * | 2015-06-26 | 2015-09-09 | 四川中萃化工有限公司 | Method for preparing high-purity tributyl phosphate |
| CN105859770A (en) * | 2016-05-09 | 2016-08-17 | 云南云天化以化磷业研究技术有限公司 | Method of synthesizing alkyl phosphate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115105857A (en) * | 2021-03-23 | 2022-09-27 | 郑州天一萃取科技有限公司 | Purifying treatment agent and purifying method for tributyl phosphate waste organic phase |
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Application publication date: 20180313 |