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A kind of recovery method of sulfosalicylic acid in doxycycline production waste liquid
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A technology of sulfosalicylic acid and sodium sulfosalicylate, which is applied to the preparation of sulfonate salts, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of high cost of ion exchange equipment and resin, and recovery of sulfowater. Problems such as high cost of salicylic acid and low ion exchange effluent concentration have achieved significant economic and social benefits, are conducive to environmental protection, and reduce emissions
Active Publication Date: 2017-10-31
开封豫港制药有限公司 +2
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This technology has also only completed the small test work in the laboratory, and the cost of ion exchange equipment and resin is high.
The most important thing is that a large amount of water must be removed by distillation to obtain sulfosalicylic acid. As we all know, the water heat capacity is large, the intermolecular association is strong, the evaporation is difficult, and the heat consumption is large. In addition, the outflow concentration of ion exchange is relatively high. Small, the cost of recycling sulfosalicylic acid is higher, and there is no industrial value
[0006] For the sulfosalicylic acid in the mother liquor, domestic manufacturers of doxycycline hydrochloride generally use burning methods or enter the waste water treatment system, and the pressure on environmental protection is huge
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Embodiment 1
[0016] (1) Preparation of sulfosalicylic acid sodium salt
[0017] Add 2L of doxycycline production waste liquid containing sulfosalicylic acid into a 5L reaction bottle, then add sodium hydroxide, stir to make it react, and then use a small amount of sodium hydroxide solid to adjust the pH=7 to make the solution no longer Precipitate solid, filter to remove insoluble tetracycline organic compound, add 40g gac to filtrate, heat and reflux for 30 minutes, then filter, filtrate is concentrated and reclaims ethanol, concentrated solution is cooled and crystallized, filtered, and dried to obtain 248g sulfosalicylic acid sodium salt.
[0018] (2) Recovery of sulfosalicylic acid
[0019] Add 400g of sodium sulfosalicylate and 2L of hydrochloric acid and ethanol solution with a concentration of 10% by mass in a 5L reaction flask, stir to make it react, and reflux for 1 hour. After the reaction is completed, remove sodium chloride by filtration, and concentrate and recover the filtrat...
Embodiment 2
[0021] (1) Preparation of sulfosalicylic acid sodium salt
[0022] Add 2L doxycycline production waste liquid containing sulfosalicylic acid into a 5L reaction bottle, then add sodium carbonate, stir to make it react, and then use a small amount of sodium carbonate solid to adjust the pH to 9, so that the solution no longer precipitates solids , filtered to remove insoluble tetracycline organic compounds, the filtrate was added with 40g gac, heated to reflux for 30 minutes, then filtered, the filtrate was concentrated and reclaimed ethanol, the concentrated solution was crystallized by cooling, filtered, and dried to obtain 248g sulfosalicylic acid sodium salt.
[0023] (2) Recovery of sulfosalicylic acid
[0024] Add 400g of sodium sulfosalicylate and 1L of sulfuric acid and isopropanol solution with a concentration of 20% by mass in a 5L reaction flask, stir to make it react, and reflux for 1 hour. After the reaction finishes, remove sodium chloride by filtration, and the fi...
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Abstract
The invention discloses a method for recycling sulfosalicylic acid from doxycycline production waste liquid and belongs to the field of medicinal chemistry separation and purification. The method includes the following steps that alkali is added to doxycycline production waste liquid, the alkali reacts with sulfosalicylic acid in the doxycycline production waste liquid, sulfosalicylic acid sodium salt is formed, then ethyl alcohol is recycled, crystallization is conducted, and sodium sulfosalicylate is obtained; the recycled sulfosalicylic acid sodium salt is added to an alcohol solution and an acid solution, after a reaction is ended, filtering is conducted, sodium chloride is removed, filter liquor is concentrated, solvent is recycled, crystallization is conducted, sulfosalicylic acid is obtained, the recycling rate reaches 80% or more, and a product is acceptable in quality. Compared with a traditional recycling process, the sulfosalicylic acid is recycled from the doxycycline production waste liquid, emission of pollutants is reduced, environmental protection is facilitated, the sulfosalicylic acid can be recycled, the production cost is lowered, and the economic and social benefits of doxycycline are raised.
Description
technical field [0001] The invention relates to a method for recovering sulfosalicylic acid in doxycycline production waste liquid, belonging to the field of separation and purification of medicinal chemistry. Background technique [0002] Doxycycline, also known as doxycycline or deoxyterraeum, is a long-acting broad-spectrum semi-synthetic tetracycline antibiotic. Mycoplasma, Mycoplasma trachomatis, amoeba, etc., especially the common bacteria in the respiratory tract of patients with chronic bronchitis are more sensitive to doxycycline hydrochloride. In recent years, researchers have found that doxycycline hydrochloride is more sensitive to anthrax bacteria, Vibrio cholerae, etc., and small doses of doxycycline hydrochloride can inhibit vascular coronary sclerosis, thus further stimulating the market demand for doxycycline hydrochloride. [0003] At present, the production process of doxycycline hydrochloride uses oxytetracycline as raw material, undergoes processes such...
Claims
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