Preparing method of crystal L-calcium lactate

A calcium lactate, crystallization technology, applied in the direction of organic chemistry, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems such as being unsuitable for separation and purification of fermentation broth, unfavorable for large-scale production and use, low crystallinity, and the like, Achieve good industrial application prospects, save post-processing costs, and achieve the effect of large crystal size

Active Publication Date: 2015-04-22
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In CN102205184A, a kind of production process for crystallization of calcium lactate with rotating hub wheels is reported, and the fermented liquid is exposed to the air to easily breed bacteria; in CN1680256A, it is reported that supercritical fluid carbon dioxide extraction produces refined calcium lactate, and this process requires a pressure of 25-30 MPa. The production cost is high, which is unfavorable for industrialized large-scale production and use; CN1978043A reports the process of spray drying and producing granular calcium lactate. This method is easy to cause dust pollution, has problems such as low crystallinity, and is not suitable for directly separating and purifying the fermented liquid. There will be a lot of soluble impurities in the fermentation broth in the product

Method used

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  • Preparing method of crystal L-calcium lactate
  • Preparing method of crystal L-calcium lactate
  • Preparing method of crystal L-calcium lactate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add activated carbon to the L-calcium lactate fermentation broth with a concentration of 14.7g / mL, and continuously stir for decolorization and deodorization; after filtration, the filtrate is transferred to a crystallizer, and the pH is adjusted to 6.0. Acetone was added at 40° C. at a rate of 10% / hr of the volume of the fermentation broth. Stop adding acetone when its volume consumption is 2 times of the total volume; then filter and separate after cooling down to 20°C at a cooling rate of 5°C / hr, wash with a mixture of acetone and water (volume ratio) of 1:1, and obtain the The crystalline product was dried at 30°C for 4 hours at an absolute pressure of 0.009 MPa. The final crystal main particle size is 19.33 μm, and the crystallization process single-pass yield is 86.0% (molar yield). The drying loss of the product is 24.6%, which is the pentahydrate of L-calcium lactate.

Embodiment 2

[0026] Add activated carbon to the L-calcium lactate fermentation broth with a concentration of 15.5g / ml, and continuously stir for decolorization and deodorization; after filtration, the filtrate is transferred to a crystallizer, and the pH is adjusted to 8.0. Methanol was added at 45°C at a rate of 60% / hr of the volume of the fermentation broth. When the volume consumption is 8 times of the total volume, stop adding methanol; then cool down to 5°C at a cooling rate of 10°C / hr, then filter and separate, wash with a mixture of methanol and water (volume ratio) of 1:2, and the obtained The crystalline product was dried at 45°C for 4 hours at an absolute pressure of 0.1 MPa. The final crystal main particle size is 21.30 μm, and the crystallization process single-pass yield is 82.3% (molar yield). The drying loss of the product is 25.2%, which is the pentahydrate of L-calcium lactate.

Embodiment 3

[0028] Add activated carbon to the 40.5g / ml L-calcium lactate fermented liquid, stir continuously for decolorization and deodorization; after filtering, move the filtrate into a crystallizer, and adjust the pH to 7.3. Add ethanol at 60° C. at a rate of 90% / hr of the volume of the fermentation broth. When the volume consumption is 3.5 times of the total volume, stop adding ethanol; then cool down to 7°C at a cooling rate of 8°C / hr, filter and separate, wash with ethanol, and store the obtained crystal product at 35°C with an absolute pressure of 0.008MPa Dry for 4 hours. The main particle size of the final crystal is 19.60 μm, and the single-pass yield of the crystallization process is 87.4% (molar yield). The product has a weight loss on drying of 19.4%, which is the trihydrate of L-calcium lactate.

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Abstract

The invention provides a preparing method of crystal L-calcium lactate. Activated carbon is added to the crystal L-calcium lactate with the concentration ranging from 14.7 g / mL to 40.5 g / mL, and continuous stirring, decoloring and deodorizing are carried out; after filtration, the filtered liquid is moved into a crystallizer, and pH is adjusted to 6-8; poor solvent is added at the constant temperature ranging from 40 DEG C to 60 DEG C, dilution crystallization is carried out, and at the terminal point of dilution, the volume of the added poor solvent is two to eight times of the volume of fermentation liquid; cooling crystallization is carried out, wherein filtering and separating are carried out after the temperature is lowered to 5-20 DEG C, cleaning solvent is used for carrying out cleaning, and L-calcium lactate crystals are obtained after drying is carried out. According to the preparing method, the production cycle is short, and operation is easy; the crystal L-calcium lactate is pure white, crystals are complete, the granularity of the crystals is large, the crystals are distributed evenly, the main granularity is larger than 19.33 microns, and product postprocessing is facilitated; the once-through yield in the crystallizing process reaches 82.0 percent or above, and the method is suitable for large-scale industrial production and has good industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of crystallization, and in particular relates to a method for preparing crystallization of L-calcium lactate crystals. The method of the invention can obtain needle-shaped L-calcium lactate crystals with uniform particle size distribution. Background technique [0002] Calcium-L-lactate (calcium-L-lactate) is the calcium salt of L-lactic acid, the chemical name is 2-hydroxypropionate calcium, and the molecular formula is C 6 h 10 o 6 .Ca, the molecular weight is 218.22, and its chemical structure is shown in the following formula: [0003] [0004] L-Calcium Lactate is a white powder or granular substance, easily soluble in water, and widely used in medicine, food, beverage, feed and other fields. Calcium L-lactate is a good medicament and calcium fortifier for calcium supplementation. It can reduce the permeability of capillaries, maintain the normal excitability of nerves and muscles, assist in the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/08C07C51/43
CPCC07B2200/13C07C51/43C07C51/47C07C59/08
Inventor 王永莉栾清华郝红勋鲍颖王静康
Owner TIANJIN UNIV
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