Granularity-controllable sodium citrate refining process and implementing device

A sodium citrate, particle size technology, applied in the refining process of sodium citrate and the field of realization equipment, can solve the mismatch between the production speed of crystal nuclei and the growth speed of crystal nuclei, and the easy occurrence of crystals of different sizes and heavy crystals Unable to control and other problems, to achieve the effect of high recrystallization yield, simplified production operation and low cost

Inactive Publication Date: 2017-09-22
湖南新绿方药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But also because of the rapid crystallization, the number of crystal nuclei is difficult to control, and the production speed of crystal nuclei does not match the growth speed of crystal nuclei, so the size of heavy crystals cannot be controlled, resulting in the occurrence of granular crystals of different sizes during the production process, and affecting the yield of finished products with quality
At the same time, if the crystal nucleus growth rate is greater than the crystal nucleus generation rate, resulting in larger crystal particles and a thinner concentrated solution, the mother liquor will contain a large amount of solute, which will easily cause a low yield, about 30% to 40%.
If the crystal nucleus growth rate is lower than the crystal nucleus generation rate, a large number of crystal nuclei will be generated at this time, and the formed crystal particles will be fine, which will bring great difficulties to the drying process in the subsequent process, which may cause the product to be unable to be completely dried, resulting in some finished product indicators failing to meet the standard
[0005] Pharmaceutical grade sodium citrate is an excipient drug, so the production environment and process must meet the requirements of GMP. According to GMP requirements, during the refining process of sodium citrate, it cannot be in contact with external untreated air; while in the existing chemical production, all The seed crystal input is carried out through the feeding port, which limits the use of the seed crystal crystallization method in the refining process of pharmaceutical grade sodium citrate
[0006] Therefore, there is an urgent need to provide a sodium citrate refining process with mild refining conditions, simple operation, high yield, good refining effect and particle control, especially a rapid seeding crystallization process that has the above advantages and meets GMP requirements. The technique of preparing sodium citrate by method is lacking

Method used

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  • Granularity-controllable sodium citrate refining process and implementing device
  • Granularity-controllable sodium citrate refining process and implementing device
  • Granularity-controllable sodium citrate refining process and implementing device

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Embodiment 1

[0046] The refining process of the sodium citrate of the present embodiment adopts the seed crystal crystallization mode, comprises the following steps:

[0047] S1. Dissolving: Dissolve 10kg of crude food-grade anhydrous sodium citrate in 12L of water, and raise the temperature of the feed solution to 90°C;

[0048] S2. Decolorization: add activated carbon with a mass percentage of 0.3% to the solution obtained in S1, stir at a constant temperature of 90°C for 0.5h, and filter to obtain a fine filtrate;

[0049] S3. Concentration and crystallization: depressurize the fine filtrate obtained in S2 to -0.08MPa, stir at a speed of 33r / min, concentrate to a viscous liquid with a specific gravity of 1.34g / ml, and add 5g of seed crystals using a seed crystal register , continue to concentrate for 0.5h, cool the feed liquid at a cooling rate of 10°C / h, cool to 55°C, stir at a speed of 13r / min, and crystallize for 5h to obtain wet granules of sodium citrate;

[0050] S4. Separation a...

Embodiment 2

[0051] The steps of embodiment 2 are the same as those of embodiment 1, except that the specific gravity of the viscous liquid in step S3 is 1.25 g / ml.

Embodiment 3

[0052] The steps of embodiment 3 are the same as those of embodiment 1, except that the specific gravity of the viscous liquid in step S3 is 1.36 g / ml.

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Abstract

The invention discloses a granularity-controllable sodium citrate refining process and an implementing device. The process comprises the following steps: preparing an anhydrous sodium citrate crude product solution, performing decoloring treatment so as to obtain fine filtrate, concentrating the fine filtrate so as to obtain a vicious liquid, performing cooling crystallization so as to obtain wet sodium citrate granules, performing centrifugal treatment on the wet sodium citrate granules, and performing vibration fluidizing drying, thereby obtaining pure sodium citrate crystal granules. By adopting the process, preparation steps and purification processes are optimized, particularly key process parameters of concentration and crystallization are optimized, the purity of the prepared sodium citrate is greater than 99.9% and is as high as 99.99%, the yield of the sodium citrate is greater than 69%, and the sodium citrate is controllable in particle size range, simple in production process, low in cost, simple and feasible to operate, environmentally friendly and safe.

Description

technical field [0001] The present invention relates to a refining process of sodium citrate, more specifically, to a refining process of sodium citrate with controllable particle size and a device for realizing it. Background technique [0002] Sodium citrate is widely used as anticoagulant, chelating agent, antioxidant synergist, expectorant and diuretic in the pharmaceutical industry; in the detergent industry, it can replace sodium tripolyphosphate as a non-toxic detergent Additives; also used in brewing, injection, photography medicine and electroplating and other fields. At present, there is still a gap between food grade anhydrous sodium citrate on the market and medicinal standards, mainly in the high impurities such as calcium salts, oxalates, arsenic salts, insufficient purity, and large particle size fluctuations that are difficult to control and affect citrate. Further use of sodium citrate. [0003] The existing sodium citrate refining technology is mainly to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C51/43C07C51/47C07C59/265
Inventor 唐波彭立辉
Owner 湖南新绿方药业有限公司
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