CN101759554B - Method for treating and utilizing potassium hydrogen tartrate mother liquor - Google Patents
Method for treating and utilizing potassium hydrogen tartrate mother liquor Download PDFInfo
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- CN101759554B CN101759554B CN 200910155906 CN200910155906A CN101759554B CN 101759554 B CN101759554 B CN 101759554B CN 200910155906 CN200910155906 CN 200910155906 CN 200910155906 A CN200910155906 A CN 200910155906A CN 101759554 B CN101759554 B CN 101759554B
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- hydrogen tartrate
- hydrogen peroxide
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Abstract
The invention discloses a method for treating and utilizing potassium hydrogen tartrate mother liquor. The potassium hydrogen tartrate mother liquor takes maleic anhydride as raw material which is oxidized by hydrogen peroxide, alkali is added and the pH value is adjusted at 3.5-3.7, and the mother liquor containing the residual potassium maleic acid as shown in formula I after centrifugally preparing DL-potassium hydrogen tartrate is prepared. The method comprises the following steps: the potassium hydrogen tartrate mother liquor and the hydrogen peroxide are in oxidation reaction under the action of catalyst sodium tungstate, and the DL-potassium hydrogen tartrate as shown in formula II is prepared. The method has the benefits that through recycling the process wastewater, the COD content of the process wastewater is greatly reduced, the waste material is changed into useful material, the DL-potassium hydrogen tartrate is prepared by using the useful components in the process wastewater, and the resource utilization ratio is improved.
Description
(1) technical field:
The present invention relates to a kind of method of handling and utilizing potassium hydrogen tartrate mother liquor.
(2) background technology
The tartarus chemical name: 2,3 dihydroxybutanedioic acid hydrogen potassium is tartaric salt, and outward appearance is colourless or opaque slightly crystal or white crystalline powder, and 1g is dissolved in 25 ℃ of water of 165mL, is dissolved in 16mL boiling water, is dissolved in 8820mL ethanol.Its saturated solution is acid to reindeer moss.Tartarus is divided into " L-tartarus " and " DL-tartarus ".Industrial winestone potassium hydrogen phthalate is the DL-tartarus.
The main application of industrial winestone potassium hydrogen phthalate is to produce Seignette salt, tartrate series products such as antimonypotassium tartrate, this product is main raw material by MALEIC ANHYDRIDE, after the oxidation of hydrogen peroxide, produce tartaric acid solution, the repeated hydrogenation potassium oxide neutralizes between the pH value 3.5～3.7, and the characteristics centrifuge dehydration at normal temperatures that utilizes tartarus to be insoluble in water then makes tartarus.Centrifugal back mother liquor enters sewage works and handles the back discharging, contains large amount of organic in this processing wastewater, and COD is up to 100,000 mg/litre, and it is very big to deal with difficulty, and causes the ample resources waste.Present technique is exactly that mother liquor is carried out deep research, carries out second stage employ, turns waste into wealth.
(3) summary of the invention
This technology is that the waste water of its production technique is researched and developed utilization, through check analysis, the maleic acid of utilizable main component MALEIC ANHYDRIDE hydrolysis in this mother liquor, this material not by hydrogen peroxide oxidation, and generates maleic acid potassium in the potassium hydroxide and when producing tartarus when producing tartrate.According to test, maleic acid potassium can continue to be continued oxidation by hydrogen peroxide under given conditions, directly generates the DL-tartarus.
The technical solution used in the present invention is:
A kind of method of handling and utilizing potassium hydrogen tartrate mother liquor, described potassium hydrogen tartrate mother liquor is for being raw material with the MALEIC ANHYDRIDE, through hydrogen peroxide oxidation, add the adjusting PH with base value and be 3.5～3.7, the remaining mother liquor that contains suc as formula the maleic acid potassium shown in the I behind the centrifugal DL-of the producing tartarus, described method is: potassium hydrogen tartrate mother liquor and hydrogen peroxide, under the effect of catalyzer sodium wolframate, carry out oxidizing reaction, make suc as formula the DL-tartarus shown in the II;
Comparatively concrete, described method may further comprise the steps: it is 1.25～1.28 (available mother-in-law is U.S., and instrumentation is fixed) that potassium hydrogen tartrate mother liquor is evaporated to relative density under the normal temperature (with respect to the density of water), obtain concentrated solution, add the catalyzer sodium wolframate in the concentrated solution, temperature control is at 70～76 ℃ (preferred 70～72 ℃), slowly add hydrogen peroxide solution, insulation reaction 24 hours, reaction finishes afterreaction liquid and is warming up to 95～100 ℃, be incubated 2 hours, cool to room temperature then, centrifugal, get throw out and reclaim mother liquor, taking precipitate is the DL-tartarus; H in the described hydrogen peroxide solution
2O
2Quality be 11% of concentrated solution quality.
The repetitive operation according to the method described above of described recovery mother liquor is recycled.
Comparatively preferred, the quality percentage composition of described hydrogen peroxide solution is 27.5%, and the quality consumption of described hydrogen peroxide solution is 40% of concentrated solution quality.
The quality consumption of catalyzer sodium wolframate of the present invention is 0.1% of concentrated solution quality.
Beneficial effect of the present invention is: by the recycling to processing wastewater, and the COD content of a large amount of minimizing processing wastewaters, and turn waste into wealth, utilize the useful component in the processing wastewater to produce the DL-tartarus, improved resource utilization.
(4) embodiment
Come the present invention is described further with specific embodiment below, but protection scope of the present invention is not limited thereto.
Embodiment 1
Get 3 tons of the processing wastewaters produced in the DL-tartarus, being evaporated to relative density through thin-film evaporator is 1.26 (mother-in-law is U.S., and instrumentation is fixed, down together), obtain 1 ton of concentrated solution, in concentrated solution, add catalyzer (sodium wolframate) 1kg, temperature control is at 70-72 degree centigrade, slowly add concentration 27.5% hydrogen peroxide 400kg, be incubated 24 hours, reaction finishes afterreaction liquid and is warming up to 95-100 ℃, be incubated 2 hours, cool to room temperature then, centrifugal, obtain throw out and reclaim mother liquor, taking precipitate obtains tartarus product 300kg, purity 95% (with 0.5mol/L sodium hydroxide solution titration determination).
Utilize the recovery mother liquor in kind to reclaim the recyclable product 260kg of per 3 tons of second stage employ mother liquors, product purity 85%.
Embodiment 2
Get 3 tons of the processing wastewaters produced in the DL-tartarus, being evaporated to relative density through thin-film evaporator is 1.26, obtain 1.1 tons of concentrated solutions, in concentrated solution, add catalyzer (sodium wolframate) 1.1kg, temperature control is at 70-72 degree centigrade, slowly add concentration 27.5% hydrogen peroxide 440kg, be incubated 24 hours, reaction finishes afterreaction liquid and is warming up to 95-100 ℃, be incubated 2 hours, cool to room temperature then, centrifugal, taking precipitate obtains tartarus product 285kg, purity 95% (with 0.5mol/L sodium hydroxide solution titration determination).
Claims (3)
1. method of handling and utilizing potassium hydrogen tartrate mother liquor, described potassium hydrogen tartrate mother liquor is for being raw material with the MALEIC ANHYDRIDE, through hydrogen peroxide oxidation, adding the adjusting PH with base value is 3.5～3.7, the remaining mother liquor that contains suc as formula the maleic acid potassium shown in the I behind the centrifugal DL-of the producing tartarus, it is characterized in that described method is: it is 1.25～1.28 to obtain concentrated solution that potassium hydrogen tartrate mother liquor is evaporated under the normal temperature relative density, add the catalyzer sodium wolframate in the concentrated solution, temperature control is at 70～76 ℃, slowly add hydrogen peroxide solution, insulation reaction 24 hours, reaction finishes afterreaction liquid and is warming up to 95～100 ℃, is incubated 2 hours, cools to room temperature then, centrifugal, taking precipitate is the DL-tartarus shown in the formula II; H in the described hydrogen peroxide solution
2O
2Quality be 11% of concentrated solution quality;
2. the method for claim 1, the quality percentage composition that it is characterized in that described hydrogen peroxide solution is 27.5%, the quality consumption of described hydrogen peroxide solution is 40% of concentrated solution quality.
3. the method for claim 1, the quality consumption that it is characterized in that described catalyzer sodium wolframate is 0.1% of concentrated solution quality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200910155906 CN101759554B (en) | 2009-12-31 | 2009-12-31 | Method for treating and utilizing potassium hydrogen tartrate mother liquor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200910155906 CN101759554B (en) | 2009-12-31 | 2009-12-31 | Method for treating and utilizing potassium hydrogen tartrate mother liquor |
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| CN101759554A CN101759554A (en) | 2010-06-30 |
| CN101759554B true CN101759554B (en) | 2013-08-14 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012114B (en) * | 2012-12-04 | 2014-12-24 | 浙江工商大学 | Method of synchronously preparing DL-tartaric acid and DL-potassium hydrogen tartrate |
| CN108314162A (en) * | 2018-04-17 | 2018-07-24 | 天津理工大学 | The method for removing potassium of the aqueous solution containing sylvite under a kind of acidic environment |
| CN113087612A (en) * | 2021-04-14 | 2021-07-09 | 杭州瑞晶生物科技有限公司 | Production method of potassium sodium tartrate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4150241A (en) * | 1975-02-26 | 1979-04-17 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler | Process for the production of pure racemic acid and mesotartaric acid and separation of maleic acid from synthetic tartaric acid |
| CA1058634A (en) * | 1975-02-26 | 1979-07-17 | Gerd Schreyer | Process for producing pure racemic acid and mesotartaric acid |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4839436A (en) * | 1971-09-29 | 1973-06-09 | ||
| JPS4839435A (en) * | 1971-09-29 | 1973-06-09 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4150241A (en) * | 1975-02-26 | 1979-04-17 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler | Process for the production of pure racemic acid and mesotartaric acid and separation of maleic acid from synthetic tartaric acid |
| CA1058634A (en) * | 1975-02-26 | 1979-07-17 | Gerd Schreyer | Process for producing pure racemic acid and mesotartaric acid |
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Effective date of registration: 20170606 Address after: Hangzhou City, Zhejiang Province, China 311300 Fumin Road Industrial Zone of Ling'an Economic Development Zone Yi Yi Park No. 1 Patentee after: Hangzhou Rexchip Biotechnology Co. Ltd. Address before: 311300, Hangzhou, Zhejiang, Ling'an Linglong Industrial Zone Hangzhou Ling'an Jinlong Chemical Co., Ltd. Patentee before: Hangzhou Lin'an Jinlong Chemical Co.Ltd |
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