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Recovery method of mother liquor in preparation process of glucosamine sulfate and sodium chloride double salt

A technology of glucosamine sulfate and glucosamine hydrochloride, which is applied in the field of medicine and chemical industry, can solve problems such as unqualified glucosamine, product impurities exceeding standards, and difficult quality standards, and achieve stable quality and properties, low recovery costs, and good crystal forms.

Active Publication Date: 2017-05-31
GUANGDONG XIANQIANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The main problems in the above mother liquor recovery method are: mother liquor A and mother liquor B are separately recycled and processed, the process is complicated, the recovery rate is low, and the recycling cost is high
In addition, the impurities in the recycled product of mother liquor A or the product after application may exceed the standard; in the recycled product of mother liquor B, the content of glucosamine is usually unqualified, and the impurities are easy to exceed the standard. Even if recrystallization is carried out, the content sometimes does not meet the standard
[0009] In summary, the current method for recycling mother liquor in the preparation process of glucosamine sulfate and sodium chloride double salt mainly has problems such as complicated process, low recovery rate, difficult quality standard, and high recovery cost.

Method used

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  • Recovery method of mother liquor in preparation process of glucosamine sulfate and sodium chloride double salt
  • Recovery method of mother liquor in preparation process of glucosamine sulfate and sodium chloride double salt
  • Recovery method of mother liquor in preparation process of glucosamine sulfate and sodium chloride double salt

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Experimental program
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Effect test

Embodiment 1

[0042] Embodiment 1: The influence of extractant on the removal of impurities

[0043] Mix the mother liquor at 55°C and distill part of the water under reduced pressure to a total volume of about 1L, with a solid content of 16.8%. Divide it into 10 equal parts, number them sequentially, and add ethyl acetate, butyl acetate, dichloromethane, and chloroform respectively. 150 mL each of 9 extractants, such as , methyl tert-butyl ether, diethyl ether, isopropyl ether, toluene, and xylene, were extracted in 3 times, and the 10th group was the blank group. After the above 10 groups were extracted respectively, the aqueous phase was taken to detect related substances.

[0044] Table 1 extraction agent to the removal situation of impurity

[0045]

[0046] Note: For impurities A, B, C, and E, refer to BP 2013 Quality Standard for Glucosamine Sulfate Sodium Chloride Double Salt.

[0047] As can be seen from the results shown in Table 1, the present invention uses extraction agent...

Embodiment 2

[0048] Embodiment 2: the impact of organic precipitant feeding mode on product

[0049] The mixed mother liquor was distilled under reduced pressure at 55°C to a total volume of about 900mL, with a solid content of 18.6%. Added 1.5L of dichloromethane, extracted three times, added 10g of activated carbon to the water phase, raised the temperature to 50°C for 0.5h, filtered, and weighed the filtrate. Detect the content of its glucosamine, sulfate ion and chloride ion, and calculate the respective amounts in the decolorizing solution to be 108.8g, 13.4g and 10.9g respectively. The extraction and decolorization solution was transferred to a reaction kettle, 24 g of anhydrous sodium sulfate was quantitatively added, and the temperature was raised to 50° C. for 1 h. After the reaction is complete, divide the feed solution into 9 parts, number them sequentially, control the temperature at 50° C., add 3 L of an organic precipitant (acetone, 95% ethanol or methanol) in the feeding met...

Embodiment 3

[0054] Embodiment 3: organic precipitating agent dripping temperature influences on product

[0055] The mixed mother liquor was distilled under reduced pressure at 60°C to a total volume of about 800mL, with a solid content of 21.4%. Add 1.5L of ethyl acetate, extract three times, add 15g of activated carbon to the water phase, heat up to 55°C for 1h, filter, weigh the filtrate, and detect The contents of glucosamine, sulfate ion and chloride ion are calculated to be 107.2g, 12.8g and 10.7g respectively. The extraction and decolorization solution was transferred to a reaction kettle, 24 g of anhydrous sodium sulfate was quantitatively added, and the temperature was raised to 55° C. for 1 h. After the reaction is completed, divide the feed liquid into 4 parts, number them in turn, control the temperature at room temperature, 40°C, 50°C, and 60°C, add 3L of 95% ethanol dropwise, drop it in 2.5h, drop to room temperature for 1h, and continue to drop to Crystallize overnight at ...

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Abstract

The invention discloses a recovery method of mother liquor in the preparation process of glucosamine sulfate and sodium chloride double salt. The recovery method comprises the following steps: (1) recovering organic precipitants in refined mother liquor of a glucosamine hydrochloride crude product and crystallized mother liquor after salt-forming reaction of the glucosamine sulfate and sodium chloride double salt, mixing, controlling the solid content, reducing the pressure and evaporating to remove part of water; (2) adding an extracting agent to extract impurities and adding activated carbon into a water phase to decolor; (3) weighing a decoloring solution, sampling and detecting the contents of glucosamine, sulfate ions and chloride ions, and calculating the respective contents; (4) adding quantitative anhydrous sodium sulfate into the decoloring solution and performing temperature rise reaction; (5) controlling the temperature and the dripping speed, adding an organic precipitant, reducing the temperature and crystallizing, filtering and drying to obtain a glucosamine sulfate and sodium chloride double salt recovery product. The recovery method disclosed by the invention is simple in process, easy to operate, high in recovery rate and low in recovery cost; a product with relatively good crystal shape, uniform granularity, good color and luster and stable properties can be prepared; therefore, the recovery method is very suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, in particular to a method for recovering mother liquor in the preparation of glucosamine sulfate sodium chloride double salt. Background technique [0002] In 1956, Swedish researchers first discovered that glucosamine might play a role in the etiology of osteoarthritis. Since then, glucosamine has been widely used as the drug of choice for the treatment of osteoarthritis. [0003] Glucosamine compounds mainly exist in the form of hydrochloride, sulfate and their double salts, and N-acetylglucosamine. The treatment of osteoarthritis is better with glucosamine containing sulfate, but glucosamine sulfate without metal chloride is very easy to absorb moisture and oxidize, and there are still certain technical bottlenecks in the development of drugs. However, glucosamine sulfate and The double salt compounded by metal chloride, although the content of metal chloride is relatively high,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/06C07H1/06
Inventor 刘斌谭珍友程志伟邓军罗统有
Owner GUANGDONG XIANQIANG PHARMA
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