Method for cleanly producing citric acid by coupling calcium salt method with precipitation displacement

A technology of clean production and citric acid, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve problems such as difficult to eliminate calcium sulfate, and achieve the effect of overcoming calcium sulfate waste residue

Active Publication Date: 2014-03-26
INST OF PROCESS ENG CHINESE ACAD OF SCI
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Problems solved by technology

[0009] In summary, the crystallization step of calcium citrate in the current calcium salt process has a very significant effect on the removal of impurities (Wu Shihua et al., Research Progress in Extracting Citric Acid from Fermented Broth, Journal of Guangxi Institute of Technology, No. Volume 16, Issue 3: 9~14), the quality of the citric acid product obtained is also better than other methods, but it is difficult to eliminate calcium sulfate

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  • Method for cleanly producing citric acid by coupling calcium salt method with precipitation displacement
  • Method for cleanly producing citric acid by coupling calcium salt method with precipitation displacement
  • Method for cleanly producing citric acid by coupling calcium salt method with precipitation displacement

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preparation example Construction

[0061] The specific method for the preparation of ammonium carbonate, sodium carbonate or potassium carbonate is: the CO containing 2 The gas is passed into the alkali chamber of the bipolar membrane electrodialyzer in step 2), or the regenerated NH obtained in step 2) 3 (ammonia water, liquid ammonia or ammonia gas), sodium hydroxide solution or potassium hydroxide solution and citric acid neutralization step 2 The gas is passed into the absorption container at the same time to obtain ammonium carbonate, sodium carbonate or potassium carbonate solution; the obtained ammonium carbonate, sodium carbonate or potassium carbonate solution can be further evaporated and concentrated to obtain ammonium carbonate, sodium carbonate or potassium carbonate solid.

[0062] The obtained ammonium carbonate, sodium carbonate or potassium carbonate solution or solid can be used in step 1) precipitation replacement reaction.

[0063]In the implementation of step 2), the solution containing am...

Embodiment 1

[0090]Step 1) Precipitation replacement reaction:

[0091] Take 841g of solid calcium citrate from the citric acid workshop of COFCO Biochemical (Anhui) Co., Ltd., add it to 1.0L of water, stir properly to make it a suspension, and add 5.0mol / L ammonium carbonate solution to the In the suspension of calcium citrate, use the offline method to measure the pH of the system during the reaction. When the pH is higher than 10.0, stop feeding the ammonium carbonate solution, keep stirring to make it react completely, and consume 1.02L of the ammonium carbonate solution in total; filter Obtain 2.0 L of ammonium citrate-containing solution of 512 g of calcium carbonate solids and 308.0 g / L of citric acid concentration.

[0092] Step 2) Bipolar Membrane Electrodialysis:

[0093] The bipolar membrane electrodialyzer is a "salt-alkali" two-chamber bipolar membrane electrodialyzer with one stage and one independent operation, and the liquid flow direction in adjacent compartments adopts a...

Embodiment 2

[0097] Step 1) Precipitation replacement reaction:

[0098] Take the calcium monohydrogen citrate solid from the citric acid workshop of COFCO Biochemical (Anhui) Co., Ltd. and add it to 1.02L of 3.9mol / L sodium carbonate solution in batches, stir properly, and use an online pH measuring device to measure the system during the replacement reaction. pH change, when the calcium monohydrogen citrate solid addition was 551g, the pH of the system was lower than 7.0, stop adding the monohydrogen calcium citrate solid, keep stirring to make it fully carry out the precipitation replacement reaction; filter to obtain calcium carbonate solid 241g and 1.01L of a solution containing sodium citrate with a citric acid concentration of 450g / L.

[0099] Step 2) Bipolar Membrane Electrodialysis:

[0100] Bipolar membrane electrodialysis is the same as Step 2 of Example 1). The solution 1.0L containing sodium citrate obtained by step 1) is passed into the salt chamber of the bipolar membrane ...

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Abstract

The invention relates to a method for cleanly producing citric acid by coupling a calcium salt method with precipitation displacement. The method comprises the following steps: using calcium carbonate, magnesium carbonate or zinc carbonate as a neutralizing agent in the citric acid neutralizing step of a conventional calcium salt method, obtaining a calcium citrate and / or calcium monohydrogen citrate, magnesium citrate or zinc citrate solid after neutralization reaction and simultaneously obtaining CO2; then reacting calcium citrate and / or calcium monohydrogen citrate, magnesium citrate or zinc citrate with ammonium carbonate, sodium carbonate or potassium carbonate by utilizing precipitation displacement reaction to obtain a solution containing ammonium citrate, sodium citrate or potassium citrate and a calcium carbonate, magnesium carbonate or zinc carbonate precipitate; finally treating the solution containing ammonium citrate, sodium citrate or potassium citrate by utilizing the bipolar membrane electrodialysis technology to obtain a solution containing citric acid and a regenerated NH3, NaOH or KOH solution. The method has the beneficial effects that calcium sulfate waste residues are not produced; the method can be directly linked with the neutralizing step and achieve material closed recycling.

Description

technical field [0001] The invention relates to the field of organic acid production, in particular to a method for cleanly producing citric acid coupled with a calcium salt method and precipitation replacement. Background technique [0002] Citric acid, also known as citric acid, its chemical name is 2-hydroxypropane-1,2,3-tricarboxylic acid, is the largest acid among organic acids. Due to the superior performance of citric acid and its derivatives in terms of physical and chemical properties, it is widely used in the food industry, pharmaceutical industry and chemical industry, and is widely used in electronics, textiles, petroleum, leather, construction, photography, plastics, casting and ceramics There are also very broad applications in other fields. my country is a major producer of citric acid, with a national production capacity of 1 million tons. [0003] In existing industrial production, the methods for extracting citric acid from citric acid fermentation clear ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/02C07C59/265
CPCC07C51/02C07C51/412C07C59/265
Inventor 丛威杨鹏波刘明杨文龙王倩田原
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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