Calcium Succinate Crystallization for Succinic Acid Purification

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Solution Overview

Problem

Current methods for producing succinic acid through fermentation face challenges in efficiently separating and purifying succinic acid salts, particularly due to issues with calcium succinate deposition and by-product formation, limiting the use of calcium compounds as neutralizing agents and requiring complex purification processes.

Innovation Solution

A method involving the crystallization of calcium succinate trihydrate, its transition to calcium succinate monohydrate, separation, salt substitution with ammonium compounds, and removal of calcium carbonate to produce high-purity ammonium succinate solutions, which can then be used to derive succinic acid, utilizing calcium compounds like calcium hydroxide and ammonium carbonate for efficient salt substitution.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If calcium compound is used as neutralizing agent in fermentation, then succinic acid can be produced with simple purification process, but calcium succinate deposits as crystals making separation difficult

Engineering Contradiction:
Improvepurification process simplicityVSAvoidcrystal separation difficulty
Core Design Contradiction:
Ease of manufactureVSEase of operation

Solution Approach 1:

The patent changes the physical state parameter of calcium succinate from crystalline to amorphous by controlling fermentation conditions (pH, temperature, calcium compound addition rate) to prevent crystal formation, enabling simple filtration instead of complex crystal separation

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent adds calcium compound gradually during fermentation process to maintain supersaturation state without allowing crystal nucleation, preventing crystal formation before separation is needed

Inventive Principle:
Principle #10Preliminary action

2Productivity

If sulfuric acid is used to separate succinic acid from calcium succinate, then succinic acid can be obtained, but large quantity of calcium sulfate by-product is generated

Engineering Contradiction:
Improvesuccinic acid production efficiencyVSAvoidcalcium sulfate by-product
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

The patent changes the chemical form of calcium succinate from crystalline to amorphous, which allows direct acidolysis with sulfuric acid to proceed efficiently while calcium sulfate remains soluble at controlled temperatures, reducing by-product deposition

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent utilizes temperature control to manage phase transitions of calcium sulfate, keeping it in solution during reaction then precipitating it separately for easy removal, thereby improving succinic acid recovery while managing by-product

Inventive Principle:
Principle #36Phase transitions

3Object-generated harmful factors

If electrodialysis is used to separate succinic acid from succinate salts, then no by-product salts are generated, but this method is limited to monovalent bases and cannot be applied to calcium salt

Engineering Contradiction:
Improveby-product salt generationVSAvoidapplicability to different succinate salts
Core Design Contradiction:
Object-generated harmful factorsVSAdaptability or versatility

Solution Approach 1:

The patent changes calcium succinate from crystalline to amorphous form, which then allows electrodialysis to be applied effectively since the amorphous form dissolves completely without scale formation on membranes, enabling separation without by-product salt generation

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses amorphous calcium succinate as an intermediary form that is soluble enough for electrodialysis but can be easily converted back to crystalline form after separation, bridging the gap between calcium salt and electrodialysis compatibility

Inventive Principle:
Principle #24Intermediary (Mediator)

4Object-generated harmful factors

If ammonia is used as neutralizing agent to produce ammonium succinate, then succinic acid can be obtained without by-product salts, but productivity and yield in fermentation are reduced

Engineering Contradiction:
Improveby-product saltVSAvoidfermentation yield
Core Design Contradiction:
Object-generated harmful factorsVSProductivity

Solution Approach 1:

The patent performs preliminary neutralization with calcium compound during fermentation to maintain optimal pH for high productivity, then converts calcium succinate to ammonium succinate in a separate post-fermentation step, combining the benefits of both approaches

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent divides the neutralization process into two separate stages: calcium-based neutralization during fermentation (for high yield) and ammonium-based conversion after fermentation (for no by-product), optimizing both productivity and purity

Inventive Principle:
Principle #1Segmentation

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method enables the efficient production of high-purity ammonium succinate solutions and succinic acid with minimal by-product generation, allowing for the reuse of calcium carbonate as a neutralizing agent and reducing energy consumption in the purification process.

Implementation Method 1

transition crystallization step wherein calcium succinate trihydrate is converted to calcium succinate monohydrate by transition crystallization

Methodology Applied
Scientific EffectTransition crystallization: Phase Change

Implementation Method 2

salt substitution step wherein the calcium succinate monohydrate separated is made into ammonium succinate solution

Methodology Applied
Scientific EffectSalt substitution: Chemical Bonding

Data Source

PatentEP2157185B1Process for production of succinic acid, and process for production of ammonium succinate solution
Publication Date: 2014.05.14 AJINOMOTO CO INC
  • EP2157185B1 patent drawingFigure 1A~2B

AI summary

The object is to produce an ammonium succinate solution which can be used for the production of fermentation-derived succinic acid, and whose all by-products can be re-used in the production of succinic acid, with a high degree of efficiency and without employing any complicated step. Disclosed is a process for producing a solution of fermentation-derived ammonium succinate, which comprises the following steps (1) to (5): (1) a crystallization/fermentation step for producing calcium succinate trihydrate by using a microorganism; (2) a transfer step for transfering/crystallizing calcium succinate trihydrate to calcium succinate monohydrate; (3) a crystal separation step for separating calcium succinate monohydrate; (4) a salt-substitution step for converting calcium succinate monohydrate separated in the proceeding step to an ammonium succinate solution; and (5) a solid/liquid separation step for removing a calcium carbonate precipitate from the ammonium succinate solution.