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.)
- Pending
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- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 15
- 238000000746 purification Methods 0.000 title claims abstract description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 10
- 239000004332 silver Substances 0.000 title claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000003039 volatile agent Substances 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000004014 plasticizer 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
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-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
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 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)
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CN201610785592.1A CN107793446A (en) | 2016-08-31 | 2016-08-31 | A kind of purification process of SILVER REAGENT tributyl phosphate |
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CN201610785592.1A CN107793446A (en) | 2016-08-31 | 2016-08-31 | A kind of purification process of SILVER REAGENT tributyl phosphate |
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CN107793446A true CN107793446A (en) | 2018-03-13 |
Family
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Family Applications (1)
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CN201610785592.1A Pending CN107793446A (en) | 2016-08-31 | 2016-08-31 | A kind of purification process of SILVER REAGENT tributyl phosphate |
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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 |
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 |
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 |