CN109503352A - A method of recycling acetic acid and separation other elements from acetate solution - Google Patents

A method of recycling acetic acid and separation other elements from acetate solution Download PDF

Info

Publication number
CN109503352A
CN109503352A CN201811475881.7A CN201811475881A CN109503352A CN 109503352 A CN109503352 A CN 109503352A CN 201811475881 A CN201811475881 A CN 201811475881A CN 109503352 A CN109503352 A CN 109503352A
Authority
CN
China
Prior art keywords
acetic acid
organic phase
acid
acetate
solution
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
Application number
CN201811475881.7A
Other languages
Chinese (zh)
Inventor
肖超
李义兵
孟征兵
李玉平
姜艳丽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guilin University of Technology
Original Assignee
Guilin University of Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Guilin University of Technology filed Critical Guilin University of Technology
Priority to CN201811475881.7A priority Critical patent/CN109503352A/en
Publication of CN109503352A publication Critical patent/CN109503352A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment

Abstract

The method that the invention discloses a kind of to recycle acetic acid from acetate solution and separate other elements.First using adjusting acid system that acetate solution pH value is adjusted to 1.0 ~ 2.5, liquid to be extracted is obtained, completes to adjust pH process；Then liquid to be extracted is mixed with organic, obtains negative acetic acid organic phase, completes extraction acetic acid process；Finally negative acetic acid organic phase is mixed with stripping agent, obtains acetic acid solution and empty organic phase, wherein empty organic phase can be back to extraction acetic acid process, completes stripping process.Present invention process is simple, realizes and recycles acetic acid from acetate solution, while acetic acid being separated with other elements in solution.

Description

A method of recycling acetic acid and separation other elements from acetate solution
Technical field
The invention belongs to field of smelting, and in particular to a kind of to recycle acetic acid from acetate solution and separate other elements Method.
Background technique
Acetic acid is important industrial chemicals, is widely used in the fields such as medicine, organic chemical industry, organic synthesis.With metallurgy The development discovery acetic acid of technology is applied to processing steel clinker, and the cigarette ashes such as leaded, zinc of non-ferrous metal and nickeliferous cobalt raw material have back Outstanding advantages of high income, good selectivity, therefore acetic acid gradually starts to be applied to field of metallurgy.Application of the acetic acid in field of metallurgy Then a kind of solution containing acetate of output, it is therefore desirable to the solution be handled, to recycle acetic acid therein, final realize subtracts The purpose of few acetic acid consumption and discharge.
Existing research recycling acetic acid is mostly recycled from the waste water containing acetic acid that chemical field generates at present, main method packet The method for including distillation and extraction.The above method is suitable for acetic acid in solution to be existed with free acid form, rather than acetate form is deposited ?.And acetic acid mainly exists in the form of acetate in the similar solution in field of metallurgy, form is extremely complex, and leads in metallurgy The research that the recycling acetic acid from acetate solution is engaged in domain is few.Therefore it needs to develop and a kind of recycles second from acetate solution The method of acid.
Summary of the invention
The purpose of the present invention is in view of the deficienciess of the prior art, provide one kind from acetate solution recycle acetic acid and The method for separating other elements.
Specific steps are as follows:
(1) acid is added in the acetate solution that concentration is 0.05 ~ 15 mol/L makes pH value be adjusted to 1.0 ~ 2.5, obtains wait extract Liquid.
(2) extractant and the pure sulfonated kerosene of solvent oil analysis are mixed to get organic phase according to volume ratio 1:20 ~ 9:1.
(3) liquid to be extracted obtained by 5mL step (1) is mixed 10 ~ 30 points in normal temperature condition with organic phase obtained by 30mL step (2) Split-phase is stood after clock obtains negative acetic acid organic phase.
(4) negative acetic acid organic phase obtained by 30mL step (3) is mixed 20 ~ 30 minutes with 30mL stripping agent pure water room temperature, is obtained Stripping process is completed to acetic acid solution and empty organic phase wherein empty organic phase can be back to extraction acetic acid process.
Finally realize a kind of method that acetic acid is recycled from acetate solution.
The acetate solution is one in calcium acetate, magnesium acetate, cobalt acetate, nickel acetate, copper acetate and sodium acetate solution Kind is a variety of.
The acid is analytical pure sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid.
The extractant is to analyze one of pure TBP, sec-octyl alcohol and N235 or a variety of.
Present invention process is simple, realizes and recycles acetic acid from acetate solution, while by other yuan in acetic acid and solution Element separation.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below with reference to implementation, the invention will be further described, and following embodiment is intended to illustrate invention rather than to hair Bright further limits.
Embodiment 1:
It (1) is the calcium acetate (Ca (Ac) that 5.6 concentration are 1.6 mol/L in pH value2) analysis pure hydrochloric acid is added in solution makes pH value 1.0 are adjusted to, liquid to be extracted is obtained.
(2) by extractant analyze pure TBP and the pure sulfonated kerosene of solvent oil analysis to be by volume that 7:3 is mixed to get organic Phase.
(3) liquid to be extracted obtained by 5mL step (1) is mixed 20 minutes with organic phase obtained by 30mL step (2) in normal temperature condition Split-phase is stood afterwards and obtains negative acetic acid organic phase, and acetic acid extraction rate is 80%.
(4) negative acetic acid organic phase obtained by 30mL step (3) is mixed 30 minutes with 30mL stripping agent pure water room temperature, obtains second Acid solution and empty organic phase, wherein acetic acid and calcium concentration are respectively 0.501mol/L, 0.005g/L in acetic acid solution, realize from Acetic acid and separation impurity are recycled in acetate solution.
Embodiment 2:
It (1) is the magnesium acetate (Mg (Ac) that 6.8 concentration are 2.2 mol/L in pH value2) analysis pure hydrochloric acid is added in solution makes pH value 2.3 are adjusted to, liquid to be extracted is obtained.
(2) by extractant analyze pure N235 and the pure sulfonated kerosene of solvent oil analysis to be by volume that 4:6 is mixed to get organic Phase.
(3) liquid to be extracted obtained by 5mL step (1) is mixed 12 minutes with organic phase obtained by 30mL step (2) in normal temperature condition Split-phase is stood afterwards and obtains negative acetic acid organic phase, and acetic acid extraction rate is 65%.
(4) negative acetic acid organic phase obtained by 30mL step (3) is mixed 20 minutes with 30mL stripping agent pure water room temperature, obtains second Acid solution and empty organic phase, wherein acetic acid and magnesium density are respectively 0.430mol/L, 0.0005g/L in acetic acid solution, are realized Acetic acid and separation impurity are recycled from acetate solution.
Although having been combined exemplary embodiment is described in detail method of the invention, those skilled in the art are answered This is understood, without departing from the spirit and scope defined by the claims, can modify to embodiment.

Claims (1)

1. a kind of method for recycling acetic acid from acetate solution and separating other elements, it is characterised in that specific steps are as follows:
(1) acetate solution that concentration is 0.05 ~ 15 mol/L is added acid and its pH value is adjusted to 1.0 ~ 2.5, obtains wait extract Liquid；
(2) extractant and analytically pure sulfonated kerosene are mixed to get organic phase according to volume ratio 1:20 ~ 9:1；
(3) by obtained by 5mL step (1) wait extract liquid with 30mL step (2) gained organic phase after normal temperature condition mixes 10 ~ 30 minutes It stands split-phase and obtains negative acetic acid organic phase；
(4) negative acetic acid organic phase obtained by 30mL step (3) is mixed 20 ~ 30 minutes with 30mL stripping agent pure water room temperature, obtains second Acid solution and empty organic phase, wherein empty organic phase can be back to extraction acetic acid process, completion stripping process；
The acetate solution be one of calcium acetate, magnesium acetate, cobalt acetate, nickel acetate, copper acetate and sodium acetate solution or It is a variety of；
The acid is analytical pure sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid；
The extractant is to analyze one of pure TBP, sec-octyl alcohol and N235 or a variety of.
CN201811475881.7A 2018-12-04 2018-12-04 A method of recycling acetic acid and separation other elements from acetate solution Pending CN109503352A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811475881.7A CN109503352A (en) 2018-12-04 2018-12-04 A method of recycling acetic acid and separation other elements from acetate solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811475881.7A CN109503352A (en) 2018-12-04 2018-12-04 A method of recycling acetic acid and separation other elements from acetate solution

Publications (1)

Publication Number Publication Date
CN109503352A true CN109503352A (en) 2019-03-22

Family

ID=65751533

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811475881.7A Pending CN109503352A (en) 2018-12-04 2018-12-04 A method of recycling acetic acid and separation other elements from acetate solution

Country Status (1)

Country Link
CN (1) CN109503352A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1084503A (en) * 1993-06-26 1994-03-30 华东化工学院 The method of purifying hydroxy-acetic acid from the aqueous solution that contains organic acid and salt thereof
CN1377335A (en) * 1999-10-04 2002-10-30 卡吉尔道有限责任公司 Process for producing a purified lactic acid solution
CN1938257A (en) * 2004-01-29 2007-03-28 齐凯姆公司 Recovery of organic acids

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1084503A (en) * 1993-06-26 1994-03-30 华东化工学院 The method of purifying hydroxy-acetic acid from the aqueous solution that contains organic acid and salt thereof
CN1377335A (en) * 1999-10-04 2002-10-30 卡吉尔道有限责任公司 Process for producing a purified lactic acid solution
CN1938257A (en) * 2004-01-29 2007-03-28 齐凯姆公司 Recovery of organic acids

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张春燕等: "采用萃取-反萃取技术回收废水中的醋酸", 《石油化工环境保护》 *

Similar Documents

Publication Publication Date Title
Yang et al. Recovery of indium and yttrium from Flat Panel Display waste using solvent extraction
Innocenzi et al. Application of solvent extraction operation to recover rare earths from fluorescent lamps
Liu et al. Recovery and separation of gallium (III) and germanium (IV) from zinc refinery residues: Part II: Solvent extraction
CN101532094B (en) Technology for full-process extracting and separating nickel and cobalt from acid material system with high content of calcium and magnesium impurities
Yin et al. Effect of complexing agent lactic acid on the extraction and separation of Pr (III)/Ce (III) with di-(2-ethylhexyl) phosphoric acid
Li et al. Separation and recovery of scandium and titanium from spent sulfuric acid solution from the titanium dioxide production process
CN105543476B (en) The method of extract and separate yttrium for the mixed extractant of separating yttrium and from rare earth feed liquid
Nishihama et al. Advanced liquid–liquid extraction systems for the separation of rare earth ions by combination of conversion of the metal species with chemical reaction
CN103305708B (en) Method for separating scandium from thorium in organic phase by means of back extraction
CN110184464B (en) Extraction separation method of thorium
Zhang et al. Selective removal of iron from acid leachate of red mud by aliquat 336
CN103740938A (en) Method for recovering cobalt in cobalt carbonate production wastewater by saponification-free solvent extraction method
CN109897976B (en) La-Nd light rare earth pre-separation three-outlet extraction separation process
CN111020196B (en) Method for separating thorium and enriching rare earth from radioactive waste residue leachate based on POAA
CN107475540B (en) A kind of technique of titanium white devil liquor recovery vanadium and titanium
CN105925803B (en) A kind of solvent extraction prepares the process of 4N grades of europiums
Habibpour et al. Comparative study on Ce (III) and La (III) solvent extraction and separation from a nitric acid medium by D2EHPA and Cyanex272
JP2014037608A (en) Gallium extracting method
CN102251253B (en) Method for extracting and separating nickel, iron and copper from electrolyte
CN109503352A (en) A method of recycling acetic acid and separation other elements from acetate solution
CN102465203B (en) Method for directly preparing cerium fluoride by extraction and separation
CN101100707A (en) Saponification method of acidic extract for separating rare earth
CN109680169B (en) P204 polyaniline-doped solid phase extractant and method for extracting light rare earth by using same
JP2013057115A (en) METHOD FOR SEPARATING Sc3+ FROM AQUEOUS SOLUTION CONTAINING Sc3+ AND METAL ION OTHER THAN Sc3+
JP2765740B2 (en) Separation and recovery of rare earth elements from raw materials containing rare earth elements and iron

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20190322

WD01 Invention patent application deemed withdrawn after publication