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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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  • Abstract
  • Description
  • Claims
  • Application Information

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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 problem in the prior art that it is difficult to remove sulfate in circulating mother liquor when using sodium citrate method to prepare liquid sulfur dioxide

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

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Embodiment 1

[0034] Detect the content of citrate and vitriol in the sodium citrate circulation mother liquor to be regenerated, the citric acid content is 205g / L (all citrate ions are also converted into citric acid, hereinafter the same) in the sodium citrate circulation mother liquor, sulfate ( Sodium sulfate) content 116g / L, add the calcium hydroxide aqueous solution of concentration 10wt% according to sulfate radical and lemon root total molar ratio 1:0.9 in citric acid mother liquor (citrate radical and sulfate radical total molar number is the ratio of calcium hydroxide molar number 1:0.9), add 0.1% of the total mass of sodium citrate mother liquor antioxidant reagent catechol, stir and mix evenly; feed 100vol% sulfur dioxide gas (i.e. pure sulfur dioxide) into the mixed slurry solution to When the pH of the solution is less than 3.5, stop feeding sulfur dioxide, react for another 30-60 minutes, and then neutralize with 30wt% caustic soda solution to pH 5; filter and separate to obta...

Embodiment 2

[0036] Get 1000L citric acid circulation mother liquor and add in the reactor, the citric acid 210g / L in the sodium citrate circulation mother liquor, sulfate content 126g / L, add the calcium hydroxide of 1800kg concentration 10wt% in the reactor, 0.13kg antioxidant reagent o-Phenylenediamine, stir and mix evenly; feed pure sulfur dioxide gas until the pH of the solution is less than 3.5 (time-consuming about 45min), stop feeding sulfur dioxide, and then react for 30-60min; And to pH is 7; Filtration separation obtains solid mixture 675.5kg (wherein calcium sulfate 173.5kg, calcium citrate 502kg) and mother liquor precursor, the sulfuric acid acid hydrolysis calcium citrate of solid mixture with concentration 60wt% obtains citric acid solution, concentrates , cooling, crystallization and filtration to obtain citric acid crystals, and the sulfuric acid filtrate can be reused to acidify the solid mixture of calcium citrate and calcium sulfate; the sulfate content in the mother liq...

Embodiment 3

[0038] Get 1000L citric acid circulation mother liquor and add in 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 calcium hydroxide with a concentration of 20% in the reactor, 0.12kg of antioxidant reagent hydrazine hydrate, stir and mix evenly; feed 8vol% sulfur dioxide gas and until the pH of the solution is less than 3.5 (time-consuming 240min), stop feeding sulfur dioxide, and then React for 45 minutes; Use 30wt% caustic soda to neutralize the pH of the reaction system to 5-6; Filter and separate to obtain solid mixture 673.2kg (wherein calcium sulfate 170.3kg, calcium citrate 502.9kg) and mother liquor precursor, solid mixture with concentration 70wt % sulfuric acid acid hydrolysis of calcium citrate to obtain citric acid solution, concentration, cooling, crystallization and filtration to obtain citric acid crystals, the sulfuric acid filtrate can be reused for acid hydrolysis ...

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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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