CN103450008B - Method for recovering mandelic acid from waste water - Google Patents
Method for recovering mandelic acid from waste water Download PDFInfo
- Publication number
- CN103450008B CN103450008B CN201310391825.6A CN201310391825A CN103450008B CN 103450008 B CN103450008 B CN 103450008B CN 201310391825 A CN201310391825 A CN 201310391825A CN 103450008 B CN103450008 B CN 103450008B
- Authority
- CN
- China
- Prior art keywords
- amygdalic acid
- waste water
- calcium
- acid
- add
- 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.)
- Active
Links
Abstract
The invention discloses a method for recovering mandelic acid from waste water. The method comprises the following steps: adding alkali to the waste water which contains the mandelic acid to regulate the PH value; then adding calcium or magnesium ions to generate calcium/magnesium mandelate; depositing, filtering deposited mandelate, and then reducing the mandelic acid by using strong acid in an appropriate solvent; crystallizing to obtain a pure product. The recovery method disclosed by the invention has the advantages of simplicity, high efficiency, safety in operation and suitability for industrial production.
Description
Technical field
The present invention relates to a kind of recovery organic acid method, be specifically related to the method reclaiming amygdalic acid from waste water.
Background technology
Now in fermentation, during chemical industry synthesis and Application in Chemical Engineering split, a large amount of use amygdalic acid, and there is a large amount of amygdalic acids in its fermentation mother liquor and in the mother liquor split, if this part amygdalic acid mother liquor is directly abandoned as waste water, not only waste resource but also increase pollution, and it reclaims also not easily, the solubleness of amygdalic acid in water is large, by traditional condensing crystal, not only inefficiency, and energy consumption is also larger, content in general mother liquor is not all in percentum to percent 30 etc., so reclaim amygdalic acid by traditional condensing crystal, both uneconomically can not well to deal with problems.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of method reclaiming amygdalic acid from waste water is provided, aim to provide the succinct safety of a kind of succinctly efficient, operation, more meet the method for suitability for industrialized production.
For solving the problems of the technologies described above, the present invention adopts following technical scheme to realize:
A kind of method reclaiming amygdalic acid from waste water, described method is regulate pH value to containing adding alkali in the waste water of amygdalic acid, amygdalic acid is made to become ionic state, add calcium again or magnesium ion makes it generate calcium mandelate/magnesium salts, be precipitated out, the mandelate of precipitation filtered, then restore amygdalic acid with strong acid in suitable solvent, crystallization, obtains sterling.
Concrete steps are as follows:
(1) regulating pH value to containing adding alkali in the waste water of amygdalic acid, making amygdalic acid become ionic state.Described alkali is selected from following: potassium hydroxide, sodium hydroxide, sodium carbonate, salt of wormwood, ammoniacal liquor, preferably sodium hydroxide, ammoniacal liquor; PH value scope is 7 ~ 14.
(2) in the waste water regulating PH, add calcium or magnesium ion makes it generate calcium mandelate/magnesium salts, be precipitated out, the mandelate of precipitation is filtered out.Calcium ions and magnesium ions is from following reagent: calcium sulfate, magnesium sulfate, calcium chloride, magnesium chloride, nitrocalcite, magnesium nitrate, preferably calcium chloride; Calcium ions and magnesium ions consumption is 0.5 ~ 1.5 times of mol ratio of amygdalic acid, and consumption is 0.6 ~ 1.0 mol ratio preferably.
(3) in suitable solvent, restore amygdalic acid with strong acid, crystallization, obtain sterling: solvent is selected from water and ethanol water, acetone water, preferred alcohol water and acetone water; Solvent and filter cake weight ratio 1:2 ~ 10, preferred 1:2 ~ 5.
The equation of above-mentioned concrete reactions steps is as follows:
(1) pH value is regulated to generate ionic state
(2) calcium magnesium salts precipitation is generated
(3) reduction crystallization
Beneficial effect of the present invention: succinct efficient, the operational safety of recovery method of the present invention, is applicable to suitability for industrialized production.
Embodiment
Following type reaction is used for illustrating the present invention, and the simple replacement or improvement etc. done the present invention those skilled in the art all belong within the technical scheme that the present invention protects.
embodiment 1
Step 1: in 500 milliliters of four-hole boiling flasks with thermometer and whipping appts, opens and stirs, and adds the waste water of 250g containing 20% amygdalic acid successively, adds sodium hydroxide and pH value is adjusted to 7 ~ 14.
Step 2: the calcium chloride water adding amygdalic acid amount 0.6 mole in the waste water that pH value regulates, slowly has solid to separate out, and after precipitation completely, is leached by solid and dries to obtain 101.3g amygdalic acid calcium salt.
Step 3: in 1000 milliliters of four-hole boiling flasks with thermometer and whipping appts, add and dry to obtain calcium mandelate 101.3g, add the water of 3 times of weight ratios, open and stir, drip hydrochloric acid wherein, to complete molten clearly, molten clear after, stop dripping hydrochloric acid, add the acetone of 0.1 times of water proportion, after adularescent solid is separated out, stop stirring, separate out completely, filter, dry, obtain solid 39.4, the rate of recovery is 78.8%.
embodiment 2
Step 1: in 1000 milliliters of four-hole boiling flasks with thermometer and whipping appts, opens and stirs, and adds the waste water of 500g containing 20% amygdalic acid successively, adds sodium hydroxide and pH value is adjusted to 7 ~ 14.
Step 2: the calcium sulfate aqueous solution adding amygdalic acid amount 0.65 mole in the waste water that pH value regulates, slowly has solid to separate out, and after precipitation completely, is leached by solid and dries to obtain 210.6g amygdalic acid calcium salt.
Step 3: in 2000 milliliters of four-hole boiling flasks with thermometer and whipping appts, add and dry to obtain calcium mandelate 210.6g, add the water of 3 times of weight ratios, open and stir, drip hydrochloric acid wherein, to complete molten clearly, molten clear after, stop dripping sulfuric acid, add the acetone of 0.1 times of water proportion, after adularescent solid is separated out, stop stirring, separate out completely, filter, dry, obtain solid 80.2, the rate of recovery is 80.2%.
embodiment 3
Step 1: in 1000 milliliters of four-hole boiling flasks with thermometer and whipping appts, opens and stirs, and adds the waste water of 500g containing 10% amygdalic acid successively, adds sodium hydroxide and pH value is adjusted to 7 ~ 14.
Step 2: the calcium chloride water adding amygdalic acid amount 0.65 mole in the waste water that pH value regulates, slowly has solid to separate out, and after precipitation completely, is leached by solid and dries to obtain 99.8g amygdalic acid calcium salt.
Step 3: in 1000 milliliters of four-hole boiling flasks with thermometer and whipping appts, add and dry to obtain calcium mandelate 99.8g, add the water of 3 times of weight ratios, open and stir, drip hydrochloric acid wherein, to complete molten clearly, molten clear after, stop dripping hydrochloric acid, add the acetone of 0.1 times of water proportion, after adularescent solid is separated out, stop stirring, separate out completely, filter, dry, obtain solid 38.9g, the rate of recovery is 77.8%.
Above-described embodiment is only in order to illustrate technical scheme of the present invention; but not design of the present invention and protection domain are limited; those of ordinary skill of the present invention is modified to technical scheme of the present invention or equivalent replacement; and not departing from aim and the scope of technical scheme, it all should be encompassed in right of the present invention.
Claims (4)
1. one kind is reclaimed the method for amygdalic acid from waste water, amygdalic acid is made to become ionic state to containing adding alkali adjust ph in the waste water of amygdalic acid, add calcium or magnesium ion again to make it generate calcium mandelate/magnesium salts to be precipitated out, filtered by the mandelate of precipitation, in suitable solvent, restore amygdalic acid with strong acid again, crystallization obtains sterling; It is characterized in that, comprise the following steps:
Step 1: open in the four-hole boiling flask with thermometer and whipping appts and stir, add the waste water containing amygdalic acid, add alkali and pH value is adjusted to 7 ~ 14;
Step 2: add calcium or magnesium ion in the waste water that pH value regulates, slowly have solid to separate out, after precipitation completely, leaches solid and dries to obtain amygdalic acid calcium salt;
Step 3: add the calcium mandelate of oven dry and the water of 3 times of weight ratios in the four-hole boiling flask with thermometer and whipping appts, opens and stirs; Drip hydrochloric acid wherein, to complete molten clear; Molten clear after, stop dripping hydrochloric acid, add the acetone of 0.1 times of water proportion, after adularescent solid is separated out, stop stirring, separate out completely, filter, dry, obtain solid amygdalic acid.
2. the method reclaiming amygdalic acid from waste water according to claim 1, is characterized in that, in described step 1, amygdalic acid is D-amygdalic acid or L-amygdalic acid.
3. the method reclaiming amygdalic acid from waste water according to claim 1, is characterized in that, in described step 1, alkali is sodium hydroxide, and pH value scope is 7 ~ 14.
4. the method reclaiming amygdalic acid from waste water according to claim 1, is characterized in that, in described step 2, calcium ions and magnesium ions is calcium chloride, and the mol ratio of calcium ions and magnesium ions and amygdalic acid is 1:0.6 ~ 1.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310391825.6A CN103450008B (en) | 2013-09-02 | 2013-09-02 | Method for recovering mandelic acid from waste water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310391825.6A CN103450008B (en) | 2013-09-02 | 2013-09-02 | Method for recovering mandelic acid from waste water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103450008A CN103450008A (en) | 2013-12-18 |
| CN103450008B true CN103450008B (en) | 2015-02-25 |
Family
ID=49732904
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310391825.6A Active CN103450008B (en) | 2013-09-02 | 2013-09-02 | Method for recovering mandelic acid from waste water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103450008B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859546B (en) * | 2016-04-19 | 2019-04-26 | 艾美科健（中国）生物医药有限公司 | The method of S-MA is recycled from tomoxetine hydrochloride production waste liquid |
| CN107162897A (en) * | 2017-06-08 | 2017-09-15 | 南京工业大学 | A kind of method that mandelic acid is prepared by styrene oxide |
| CN109627174B (en) * | 2018-12-05 | 2021-11-12 | 上虞京新药业有限公司 | Preparation method of chiral sertraline hydrochloride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059512A (en) * | 1990-09-06 | 1992-03-18 | 黄石市实用化工技术研究所 | From antibiotic waste water, reclaim the method for oxalic acid |
| CN1886359A (en) * | 2003-11-28 | 2006-12-27 | 阿斯利康(瑞典)有限公司 | A process for resolving, optionally substituted, mandelic acids by salt formation with a chiral base cyclic amide |
| CN1944381A (en) * | 2006-10-25 | 2007-04-11 | 福州大学 | Method for preparing mandelic acid by macroporous adsorptive resin |
| CN102575059A (en) * | 2009-10-15 | 2012-07-11 | 美利肯公司 | Thermoplastic polymer composition |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55147237A (en) * | 1979-05-08 | 1980-11-17 | Yamakawa Yakuhin Kogyo Kk | Separation of optically active body and racemic body from partially optically active body of mandelic acid |
-
2013
- 2013-09-02 CN CN201310391825.6A patent/CN103450008B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059512A (en) * | 1990-09-06 | 1992-03-18 | 黄石市实用化工技术研究所 | From antibiotic waste water, reclaim the method for oxalic acid |
| CN1886359A (en) * | 2003-11-28 | 2006-12-27 | 阿斯利康(瑞典)有限公司 | A process for resolving, optionally substituted, mandelic acids by salt formation with a chiral base cyclic amide |
| CN1944381A (en) * | 2006-10-25 | 2007-04-11 | 福州大学 | Method for preparing mandelic acid by macroporous adsorptive resin |
| CN102575059A (en) * | 2009-10-15 | 2012-07-11 | 美利肯公司 | Thermoplastic polymer composition |
Non-Patent Citations (1)
| Title |
|---|
| 陈剑锋等.手性药物扁桃酸的理化特性测定.《福州大学学报(自然科学版)》.2005,第33卷(第3期),395-399页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103450008A (en) | 2013-12-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101691239B (en) | Comprehensive utilization method for bittern | |
| CN103706325B (en) | A kind of preparation method carrying the lithium slag adsorbent of lithium for liquid state | |
| CN103924090B (en) | A kind of method utilized containing vanadium waste residue production high-purity vanadium pentoxide | |
| CN101760651A (en) | Process for extracting vanadium by acid leaching of stone coal | |
| WO2018041272A1 (en) | Method for preparing industrial grade lithium carbonate from crude lithium fluoride, and a lithium carbonate product | |
| CN104477960B (en) | A kind of production method of potassium alum | |
| CN104495925B (en) | The preparation method of sodium metavanadate | |
| CN103450008B (en) | Method for recovering mandelic acid from waste water | |
| CN105776254A (en) | Technology for preparing lithium carbonate by means of recycling of slag obtained in purifying process of lepidolite | |
| CN103539164B (en) | A kind of by the method containing the refining glauber salt of chromium saltcake | |
| CN112978805A (en) | Comprehensive recovery method of titanium, iron and sulfate radicals in titanium white waste acid | |
| CN106748900B (en) | A kind of Waste Sulfuric Acid prepares the environment-protection production method of paratoluenesulfonic acid sodium salt | |
| CN103663505A (en) | Method for treating potassium feldspar according to sub-molten salt method to prepare potassium carbonate | |
| CN108358969A (en) | A method of synthesizing benzyl arsenic acid with arsenic-containing smoke dust is smelted | |
| CN105366713B (en) | A kind of method utilizing stannum waste residue to produce high-purity sodium stannate | |
| CN102628105A (en) | Method for comprehensively recycling and using baric waste slag in refined aluminum production process | |
| CN105060320A (en) | Method for preparing magnesium hydroxide by high magnesium-lithium ratio salt lake brine | |
| CN101898770A (en) | Method for recycling sodium hydroxide | |
| CN103966438B (en) | A kind of method of vanadium and chromium in electrolytic separation containing vanadium and chromium solution | |
| CN107140662B (en) | A kind of new method producing cesium hydroxide | |
| CN109534369A (en) | A kind of film is integrated to prepare lithium chloride device and method thereof | |
| CN102051481A (en) | Method for separating calcium and magnesium in hydrochloric acid soluble salt system | |
| CN103864496B (en) | The technique of potash fertilizer prepared by a kind of potassium felspar sand | |
| CN103950976A (en) | Method for preparing titanium dioxide by utilizing mixed alkali of sodium hydroxide and sodium nitrate | |
| CN104030324B (en) | A kind of salt lake brine extracts the method for Quilonum Retard |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 226500 No.10, Yuejiang Road, Changjiang Town, Rugao City, Nantong City, Jiangsu Province Patentee after: Jiangsu Baozhong Baoda Pharmaceutical Co.,Ltd. Address before: 226500 No.10, Yuejiang Road, Changjiang Town, Rugao City, Nantong City, Jiangsu Province Patentee before: JIANGSU BAOZONG & BAODA PHARMACHEM Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |