CN112479162B - Method for washing and purifying hydrogen peroxide working solution - Google Patents
Method for washing and purifying hydrogen peroxide working solution Download PDFInfo
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- CN112479162B CN112479162B CN202011490112.1A CN202011490112A CN112479162B CN 112479162 B CN112479162 B CN 112479162B CN 202011490112 A CN202011490112 A CN 202011490112A CN 112479162 B CN112479162 B CN 112479162B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/022—Preparation from organic compounds
- C01B15/023—Preparation from organic compounds by the alkyl-anthraquinone process
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Treatment Of Water By Oxidation Or Reduction (AREA)
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Abstract
The invention provides a method for washing and purifying hydrogen peroxide working solution, which is characterized by comprising the following steps: feeding, adding alkali, adding acid, complexing, washing, adding a buffering agent and carrying out vacuum treatment. The washing and purifying of the hydrogen peroxide working solution of the invention has the following advantages: the energy consumption during the purification of the hydrogen peroxide working solution is reduced, and the energy waste is avoided; economic loss is reduced, and cost is saved; the stability of the produced hydrogen peroxide is improved, and the stability is increased from the original 93 percent to 95 percent; the TOC content of the produced hydrogen peroxide is reduced, and the TOC content of the produced hydrogen peroxide is reduced to 90ppm from 180ppm originally; the workload of workers for adjusting wastewater indexes is reduced, the safety is improved, and the distillation high-risk process and the like of the existing process are eliminated.
Description
Technical Field
The invention relates to a working solution purification method, in particular to a hydrogen peroxide working solution washing purification method.
Background
The main raw material for producing the hydrogen peroxide is working solution which is prepared by mixing and dissolving three materials of polar solvent, non-polar solvent and anthraquinone. As the operation time of the device is prolonged, anthraquinone in the device can be degraded to generate various degradation products, impurities in a polar solvent and a non-polar solvent can be gradually accumulated to finally cause the deterioration of the working solution, the content of the degradation products in the deteriorated working solution is up to more than 10%, mainly octahydro anthraquinone, anthrone, hydroxyl anthrone and the like are used, the degradation products can not generate hydrogen peroxide, and the degradation products can enter products along with the extraction, so that the quality of the products is reduced. And the degradation product enables the working solution to have larger viscosity and higher density, increases the circulating resistance of the working solution, causes the rapid increase of side reaction, and causes the serious problems of links such as catalytic hydrogenation, extraction and the like.
In order to avoid this, it is common to replace all or part of the working fluid and dispose of the replaced old working fluid when the working fluid deteriorates. This measure is convenient and effective, but requires a large investment and requires the apparatus to be shut down during replacement, resulting in a large economic loss. In order to slow down the time for replacing the working fluid, the working fluid can be cleaned during operation, so that the health degree of the working fluid is ensured, but the effect is general. At present, most manufacturers distill working solution or recovered solvent, so that energy consumption is high, and certain energy waste is caused.
Disclosure of Invention
The invention provides a method for washing and purifying hydrogen peroxide working solution aiming at the defects.
A washing and purifying method of hydrogen peroxide working solution is characterized by comprising the following steps: settling, adding alkali, adding acid, complexing, washing, adding buffer and vacuum treating.
And (3) settling, namely stirring the working solution to be treated to finish the settling of the working solution, wherein the stirring speed is 35-45rpm, the water content of the working solution before settling is 3.2-3.6g/L, and the water content of the working solution after settling is 2.8-3.0 g/L.
Adding alkali, adding 15% by mass of sodium hydroxide solution into the working solution while stirring, stabilizing the temperature of the working solution at 65-75 ℃ after adding sodium hydroxide, then continuing to stir for 20-40min, stopping stirring, and standing for 20-40min, wherein the volume ratio of sodium hydroxide to the working solution is 1 (2-4).
And adding acid, namely adding prepared sulfuric acid with the mass fraction of 10% into the working solution, continuing stirring for 20-40min after the addition of the sulfuric acid is finished, stopping stirring, and standing for 20-40min, wherein the volume ratio of the sulfuric acid to the working solution is 1 (5-6).
Performing complexation, continuously adding the prepared disodium ethylene diamine tetraacetate with the mass fraction of 10% into the working solution, and after the addition is finished, continuously stirring for 20-40min and stopping stirring; standing for 20-40min, wherein the volume ratio of the sodium hydroxide to the working solution is 1 (11-13).
The washing step comprises the steps of introducing desalted water into a working solution, stirring for 20-40min, and standing for 20-40min, wherein the volume ratio of the desalted water to the working solution is 1 (1-2); and continuously repeating the step of adding desalted water for 3-5 times.
Adding a buffering agent, namely adding the buffering agent into the working solution, continuously stirring for 20-40min, and standing for 20-40min, wherein the volume ratio of the buffering agent to the working solution is 1 (20-30).
The buffer and the solvent are deionized water, and the solute is phosphoric acid and sodium pyrophosphate, wherein the mass of the phosphoric acid in each cubic meter of the buffer is 78-82kg, and the mass of the sodium pyrophosphate in each cubic meter of the buffer is 28-32 kg.
Performing vacuum treatment, namely raising the temperature of the working solution to 30-40 ℃; then, negative pressure (-95) - (-85) kpa is built up, and the working solution is vacuumized for 10-15 min.
Compared with the prior art, the invention has the following beneficial effects:
1. by adopting the washing and purifying method of the hydrogen peroxide working solution, the energy consumption during the purification of the hydrogen peroxide working solution can be reduced, and the energy waste is avoided;
2. by adopting the method for washing and purifying the hydrogen peroxide working solution, continuous production can be realized, and the device is prevented from being stopped during the replacement of the working solution, so that the economic loss is reduced, and the cost is saved;
3. by adopting the method for washing and purifying the hydrogen peroxide working solution, the stability of the produced hydrogen peroxide is improved, and the stability is increased to 95 percent from the original 93 percent;
4. by adopting the washing and purifying method of the hydrogen peroxide working solution, the TOC content of the produced hydrogen peroxide is reduced, and the TOC content of the produced hydrogen peroxide is reduced to 90ppm from the original 180 ppm;
by adopting the washing and purifying method of the hydrogen peroxide working solution, the waste water generated in the washing and purifying process can be automatically neutralized, the workload of workers for adjusting the indexes of the waste water is reduced, the safety is improved, and the distillation high-risk process of the existing process is eliminated;
by adopting the washing and purifying method of the hydrogen peroxide working solution, the concentration of purified effective anthraquinone can reach 120.0g/L, the concentration of octacyananthraquinone can reach 0.2g/L, the concentration of anthrone can reach 1.5g/L, the concentration of hydroxyl anthrone can reach 0.6g/L, the total amount of impurity solids can reach 2.8g/L, the water content can reach 1.1g/L, and the acidity can reach 0.001 g/L.
Drawings
FIG. 1 is a flow diagram of a wash liquor;
in the figure, 101-working solution buffer tank; 102-washing tank feeding pump; 103-washing kettle; 104-a washing pump; 105-a wastewater neutralization tank; 106-hydrocyclone; 107-vacuum pump.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
The technical scheme adopted by the invention is as follows: feeding the working solution from the working solution buffer tank 101 to the washing kettle 103 through a washing kettle feeding pump 102 to settle the working solution, simultaneously starting stirring on the washing kettle 103, wherein the stirring speed is 40rpm, the feeding volume is 12m3, the feeding speed is less than or equal to 5m3/h, and the liquid level of the working solution buffer tank 101 is controlled to be more than or equal to 30% during feeding; the water content of the feed liquid entering the working liquid buffer tank 101 is 3.5g/L, and the water content of the settled working liquid buffer tank 101 is 2.9 g/L.
Continuously stirring at the rotating speed of 40rpm, adding a sodium hydroxide solution with the mass fraction of 15% of 4m3 into the washing kettle 103, after the sodium hydroxide is added, opening a steam valve, introducing 0.3Mpa steam at the speed of 100kg/h, stabilizing the temperature of the working solution in the washing kettle 103 at 70 ℃, then continuously stirring for 30min, stopping stirring, standing for 30min, settling red washing water at the bottom of the washing kettle 103, pumping the washing water into a hydrocyclone through a washing pump 104, and introducing the washing water flowing out from the bottom of the hydrocyclone 106 into a wastewater neutralization tank 105.
Continuously stirring at the rotating speed of 40rpm, adding 10% of prepared sulfuric acid into the washing kettle 103, wherein the adding amount is 2m3, and continuously stirring for 30min after the sulfuric acid is added; standing for 30min, and settling light red washing water at the bottom of the washing kettle 103; the dilute washing water is pumped into the hydrocyclone 106 by the washing pump 104, and the dilute washing water flowing out of the bottom of the hydrocyclone 106 is introduced into the waste water neutralization tank 105.
Introducing the prepared disodium ethylene diamine tetraacetate with the mass fraction of 10% into a washing kettle 103, adding the disodium ethylene diamine tetraacetate with the mass fraction of 1m3, continuing stirring at the rotating speed of 40rpm for 30min after the disodium ethylene diamine tetraacetate is added, and stopping stirring; standing for 30min, and settling light red washing water at the bottom of the washing kettle 103; light red washing water is pumped into a hydrocyclone 106 through a washing pump 104, and the washing water flowing out of the bottom of the hydrocyclone 106 is introduced into a waste water neutralization tank 105.
Introducing desalted water into a washing kettle 103, wherein the adding amount is 6m3, continuously stirring at the rotating speed of 40rpm for 30min after the adding is finished, and stopping stirring; standing for 30min, and settling washing water at the bottom of the washing kettle 103; the washing water is pumped into the hydrocyclone 106 by the washing pump 104, and the washing water flowing out of the bottom of the hydrocyclone 106 is introduced into the waste water neutralization tank 105.
The step of adding desalted water is repeated for 3 times, and the adding amount of the 3 times is 3m3,2m3 and 2m3 respectively; after each addition is finished, stirring is continuously carried out for 30min at the rotating speed of 40rpm, and then the stirring is stopped; standing for 30min, and then settling washing water at the bottom of the washing kettle 103; the washing water is pumped into the hydrocyclone 106 by the washing pump 104, and the washing water flowing out of the bottom of the hydrocyclone 106 is introduced into the waste water neutralization tank 105.
Adding a buffer agent into the washing kettle 103, wherein the adding amount is 0.5m3, continuously stirring at the rotating speed of 40rpm for 30min, standing for 30min, and settling washing water at the bottom of the washing kettle 103; the washing water is pumped into the hydrocyclone 106 by the washing pump 104, and the waste water flowing out from the bottom of the hydrocyclone 106 is neutralized by the tank 105.
The buffer, the solvent are deionized water, and the solutes are phosphoric acid and sodium pyrophosphate, wherein the mass ratio of the phosphoric acid to the sodium pyrophosphate is 13: 5, the total mass of phosphoric acid and sodium pyrophosphate per cubic meter of buffer is about 110 kg.
Continuously introducing steam into the washing kettle 103 at the speed of 100kg/h, and raising the temperature of working liquid in the washing kettle 103 to 35 ℃; then starting a vacuum pump to establish negative pressure of-90 kpa; opening a valve between the washing kettle 103 and the vacuum pump 107, and vacuumizing for 10 min; stopping the vacuum pump 107, controlling the flow of the washed working solution to be sent into the hydrocyclone 106 through the washing pump 104, and simultaneously controlling the flow of the outlet of the hydrocyclone 106 to keep the flow difference between the inlet and the outlet at 0.1m 3/h; the wastewater flowing out of the outlet of the hydrocyclone 106 is used as purified hydrogen peroxide working solution, the wastewater flowing out of the bottom of the hydrocyclone 106 is introduced into a wastewater neutralization tank 105, and the wastewater introduced into the wastewater neutralization tank 105 just meets the requirement of delivering the wastewater to a sewage treatment station.
Example 2
Experiments were carried out using the method for cleaning and purifying hydrogen peroxide working fluid described in example 1, the indexes of the working fluid during feeding and the indexes of the purified working fluid were compared as follows:
finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A washing and purifying method of hydrogen peroxide working solution is characterized by comprising the following steps: settling, adding alkali, adding acid, complexing, washing, adding a buffering agent and carrying out vacuum treatment;
adding alkali, adding 15 mass percent of sodium hydroxide solution into the working solution while stirring, stabilizing the temperature of the working solution at 65-75 ℃ after adding sodium hydroxide, then continuing stirring for 20-40min, stopping stirring, and standing for 20-40min, wherein the volume ratio of sodium hydroxide to the working solution is 1 (2-4);
adding acid, namely adding 10% of prepared sulfuric acid into the working solution, continuing stirring for 20-40min after the addition of the sulfuric acid is finished, stopping stirring, and standing for 20-40min, wherein the volume ratio of the sulfuric acid to the working solution is 1 (5-6);
performing complexation, continuously adding 10% disodium ethylene diamine tetraacetate into the working solution, and continuously stirring for 20-40min after the addition is finished, and stopping stirring; standing for 20-40min, wherein the volume ratio of the sodium hydroxide to the working solution is 1 (11-13);
the washing step comprises the steps of introducing desalted water into the working solution, stirring for 20-40min, and standing for 20-40min, wherein the volume ratio of the desalted water to the working solution is 1 (1-2); continuously and repeatedly adding desalted water for 3-5 times;
adding a buffering agent, namely adding the buffering agent into the working solution, continuously stirring for 20-40min, and standing for 20-40min, wherein the volume ratio of the buffering agent to the working solution is 1 (20-30);
the buffer comprises deionized water as a solvent and phosphoric acid and sodium pyrophosphate as solutes, wherein the mass of the phosphoric acid in each cubic meter of the buffer is 78-82kg, and the mass of the sodium pyrophosphate in each cubic meter of the buffer is 28-32 kg;
performing vacuum treatment, namely raising the temperature of the working solution to 30-40 ℃; then, negative pressure (-95) - (-85) kpa is built up, and the working solution is vacuumized for 10-15 min.
2. The method for washing and purifying hydrogen peroxide working fluid according to claim 1, wherein the sedimentation is performed by stirring the working fluid to be treated at a rotation speed of 35-45rpm, the water content of the working fluid before sedimentation is 3.2-3.6g/L, and the water content of the working fluid after sedimentation is 2.8-3.0 g/L.
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| CN112479162B true CN112479162B (en) | 2022-09-06 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2857351A1 (en) * | 2013-10-02 | 2015-04-08 | Solvay SA | Process for manufacturing a purified aqueous hydrogen peroxide solution |
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| FR2788052B1 (en) * | 1998-12-31 | 2001-04-06 | Krebs Speichim | PREPARATION OF HYDROGEN PEROXIDE BY AN IMPROVED ANTHRAQUINONE CYCLIC PROCESS |
| CN101531427A (en) * | 2009-04-23 | 2009-09-16 | 东营华泰纸业化工有限公司 | Method for regenerating working solution used in production of hydrogen peroxide |
| CN104973578A (en) * | 2014-04-09 | 2015-10-14 | 湖北三宁化工股份有限公司 | Device for separating and recovering working fluid from oxydol sewage oily water |
| CN105752939B (en) * | 2016-01-28 | 2018-11-16 | 上海宸鹏化工科技有限公司 | Anthraquinone legal system H2O2With the regeneration treating method and its regenerative system of working solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2857351A1 (en) * | 2013-10-02 | 2015-04-08 | Solvay SA | Process for manufacturing a purified aqueous hydrogen peroxide solution |
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