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 PDFInfo
- 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
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- CN
- China
- Prior art keywords
- acetic acid
- organic phase
- acetate
- acid
- solution
- Prior art date
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 238000000034 method Methods 0.000 title claims abstract description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 title claims abstract description 20
- 238000000926 separation method Methods 0.000 title description 5
- 238000004064 recycling Methods 0.000 title description 4
- 239000012074 organic phase Substances 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003350 kerosene Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 3
- 239000001639 calcium acetate Substances 0.000 claims description 3
- 229960005147 calcium acetate Drugs 0.000 claims description 3
- 235000011092 calcium acetate Nutrition 0.000 claims description 3
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 3
- 239000011654 magnesium acetate Substances 0.000 claims description 3
- 229940069446 magnesium acetate Drugs 0.000 claims description 3
- 235000011285 magnesium acetate Nutrition 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- 238000005191 phase separation Methods 0.000 claims 1
- 238000010979 pH adjustment Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000011575 calcium Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 235000019504 cigarettes Nutrition 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
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- -1 leaded Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
本发明公开了一种从乙酸盐溶液中回收乙酸和分离其他元素的方法。首先采用调酸法将乙酸盐溶液pH值调至1.0~2.5，得到待萃液，完成调pH过程；然后待萃液与有机相混合，得到负乙酸有机相，完成萃取乙酸过程；最后负乙酸有机相与反萃剂混合，得到乙酸溶液和空有机相，其中空有机相可以返回至萃乙酸过程，完成反萃过程。本发明工艺简单，实现了从乙酸盐溶液中回收乙酸，同时将乙酸与溶液中其他元素分离。
The invention discloses a method for recovering acetic acid and separating other elements from acetate solution. First, the pH value of the acetate solution is adjusted to 1.0~2.5 by the acid adjustment method to obtain the liquid to be extracted, and the pH adjustment process is completed; then the liquid to be extracted is mixed with the organic phase to obtain a negative acetic acid organic phase, and the extraction process of acetic acid is completed; finally, the negative acetic acid organic phase is obtained. The acetic acid organic phase is mixed with the stripping agent to obtain an acetic acid solution and an empty organic phase, wherein the empty organic phase can be returned to the acetic acid extraction process to complete the stripping process. The invention has a simple process, realizes the recovery of acetic acid from the acetate solution, and simultaneously separates the acetic acid from other elements in the solution.
Description
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)
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)
| 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 |
-
2018
- 2018-12-04 CN CN201811475881.7A patent/CN109503352A/en active Pending
Patent Citations (3)
| 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)
| 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》 * |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| WD01 | Invention patent application deemed withdrawn after publication | ||
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Application publication date: 20190322 |