A kind of mother liquor regeneration method of sodium citrate method for liquid sulfur dioxide

A liquid sulfur dioxide, sodium citrate technology, applied in the direction of sulfur dioxide/sulfurous acid, calcium/strontium/barium sulfate, etc., can solve the problem of difficult removal of sulfate, and achieve the effect of effective recycling and resource saving

Active Publication Date: 2019-10-15
武汉青江化工黄冈有限公司
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Problems solved by technology

[0012] The invention provides a mother liquor regeneration method for preparing liquid sulfur dioxide by sodium citrate method, aiming at overcoming the pr

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  • A kind of mother liquor regeneration method of sodium citrate method for liquid sulfur dioxide

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[0033] Example 1

[0034] Detect the content of citrate and sulfate in the sodium citrate cycle mother liquor to be regenerated. The content of citric acid in the sodium citrate cycle mother liquor is 205g / L (all citrate ions are also converted into citric acid, the same below), sulfate ( The content of sodium sulfate) is 116g / L. According to the total molar ratio of sulfate and citrate in the mother liquor of citric acid, a calcium hydroxide aqueous solution with a concentration of 10wt% is added (the total moles of citrate and sulfate is the ratio of the moles of calcium hydroxide) 1:0.9), add 0.1% of the total mass of sodium citrate mother liquor, the antioxidant reagent catechol, stir and mix evenly; pass 100vol% sulfur dioxide gas (that is, pure sulfur dioxide) into the mixed slurry solution to If the pH of the solution is less than 3.5, stop introducing sulfur dioxide, and react for 30-60 minutes, then neutralize to pH 5 with 30wt% caustic soda solution; filter and separate...

Example Embodiment

[0035] Example 2

[0036] Take 1000L citric acid circulation mother liquor and add it to the reactor. The citric acid in the sodium citrate circulation mother liquor is 210g / L and the sulfate content is 126g / L. Add 1800kg calcium hydroxide with a concentration of 10wt% and 0.13kg antioxidant reagent to the reactor. O-phenylenediamine, stir and mix uniformly; pass in pure sulfur dioxide gas until the pH of the solution is less than 3.5 (takes about 45 minutes), stop the introduction of sulfur dioxide, and react for 30-60 minutes; use 5wt% sodium bicarbonate to neutralize the reaction system And to pH 7; filtered and separated to obtain 675.5kg of solid mixture (including 173.5kg of calcium sulfate and 502kg of calcium citrate) and mother liquor precursor. The solid mixture was acid hydrolyzed with 60wt% sulfuric acid to obtain citric acid solution and concentrated , Cooling, crystallization and filtration to obtain citric acid crystals. The filtrate containing sulfuric acid can be...

Example Embodiment

[0037] Example 3

[0038] Take 1000L of citric acid circulation mother liquor and add it to the reactor. The citric acid content in the sodium citrate circulation mother liquor is 210g / L and the sulfate content is 126g / L. Add 1800kg of 20% calcium hydroxide and 0.12kg of antioxidant hydrazine hydrate to the reaction kettle, stir and mix evenly; pass in 8vol% sulfur dioxide gas and until the pH of the solution is less than 3.5 (time-consuming 240min), stop the introduction of sulfur dioxide, and then React for 45 minutes; neutralize the pH of the reaction system with 30wt% caustic soda to 5-6; filter and separate 673.2kg of solid mixture (including 170.3kg of calcium sulfate and 502.9kg of calcium citrate) and mother liquor precursor. The concentration of solid mixture is 70wt. % Sulfuric acid hydrolyzes calcium citrate to obtain a citric acid solution, which is concentrated, cooled, crystallized and filtered to obtain citric acid crystals. The filtrate containing sulfuric acid ca...

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Abstract

The invention relates to a method for regenerating a mother solution of liquid sulfur dioxide prepared by using a sodium citrate method. The method comprises the following steps: adding an appropriateamount of sulfate ion precipitator and antioxidant reagent into a sodium citrate mother solution to be regenerated, and carrying out uniform mixing; then, introducing sulfur dioxide gases to the mother solution until the pH value is 2.5-3.5, carrying out stirring and a sufficient reaction, then, adding alkali into the mother solution to neutralize the mother solution until the pH value is 5-8, and carrying out solid-liquid separation to obtain a solid mixture and a mother solution precursor; placing the solid mixture into a sulfur acid solution to dissolve calcium citrate; then, carrying outsolid-liquid separation to remove solid matters and obtain a solution containing citric acid; carrying out concentration, cooling, crystallization and solid-liquid separation on the solution containing citric acid to obtain a citric acid solid and a solution containing sulfur acid; and adding the citric acid solid into the mother solution precursor until the content of citric acid in the mother solution precursor reaches a preset concentration to obtain a regenerated mother solution. The method has the advantages that the content of sulfates in the mother solution is reduced to the maximum extent, and each matter is effectively recycled.

Description

technical field [0001] The invention relates to the field of recycling mother liquor regeneration treatment in the preparation of liquid sulfur dioxide, in particular to a mother liquor regeneration method for preparing liquid sulfur dioxide by sodium citrate method. Background technique [0002] Industrial production of liquid sulfur dioxide production can be roughly divided into two steps. Preparing high-concentration SO 2 gas; then the produced high concentration SO 2 The gas is dried and liquefied to produce liquid sulfur dioxide. The absorbent will SO 2 from containing SO 2 separated from the gas, and then obtained high concentration SO by desorption 2 gas. According to different absorbents, absorption methods can be divided into ammonia-acid method, sodium citrate method, CANSOLV renewable amine method, LABSORB regenerative method and water absorption method. At present, domestic production processes include ammonia-acid method, sodium citrate method and pure ox...

Claims

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Application Information

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IPC IPC(8): C01B17/48C01F11/46
Inventor 欧阳兆辉陈扬周建锋朱传胜
Owner 武汉青江化工黄冈有限公司
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