CN112521354A - Method for continuously recrystallizing furan ammonium salt crude product - Google Patents
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Abstract
The invention relates to the technical field of medical intermediates, in particular to a method for continuously recrystallizing a coarse furylammonium salt product. Dissolving the furan ammonium salt crude product, decolorizing, feeding into a temperature-controlled evaporation kettle, evaporating and crystallizing, and maintaining the liquid level in the temperature-controlled evaporation kettle constant by controlling the feeding speed and the discharging speed; transferring the materials in the kettle through a pneumatic diaphragm pump, cooling, crystallizing, filtering and drying to obtain the furan ammonium salt, thereby realizing the continuous recrystallization of the furan ammonium salt crude product. According to the invention, the liquid level is kept constant in the recrystallization process, so that the heat utilization rate of equipment is effectively improved, the generation of unqualified wall-hung products is greatly reduced, the recrystallization is carried out in a state of keeping balance and stability in the whole process, the distillation efficiency and the product yield are improved, the heat utilization rate is effectively increased, the waste liquid amount is reduced, and the power cost is reduced.
Description
Technical Field
The invention relates to the technical field of medical intermediates, in particular to a method for continuously recrystallizing a coarse furylammonium salt product.
Background
The furan ammonium salt is a key intermediate for synthesizing the second-generation cephalosporin antibiotics cefuroxime. Cefuroxime has the advantages of wide antibacterial range, beta-lactamase resistance, small toxic and side effects on kidney and the like, and has become one of the world-friendly infection medicaments since the cefuroxime is marketed in 1988.
At present, the refining recrystallization method in the chemical industrial production process of furan ammonium salt mainly comprises reduced pressure distillation, the temperature is raised to dissolve a furan ammonium salt crude product in methanol, activated carbon is added for decolorization to prepare a decolorized solution, and then the reduced pressure distillation is carried out to remove the methanol for recrystallization, so as to obtain a product with higher purity and lower trans-impurity. In the production process, the decolored liquid is transferred to a refining kettle for reduced pressure distillation at one time, the liquid level can continuously drop in the distillation process, and a wall-hanging unqualified product is formed on the inner wall of the kettle, so that the obtained product is reduced, the quality is poor, meanwhile, the distillation efficiency is greatly reduced due to the sharp rise of the water content of a mother liquid system in the later stage of rectification, the whole production period is longer, and more unqualified products and waste liquid are generated after a batch of crude products are refined.
Chinese patent CN107011299A discloses a method for recovering furan ammonium salt from furan ammonium salt waste liquid, wherein furan ammonium salt waste residue liquid reacts under the conditions of a solvent and a catalyst to obtain furan ammonium salt; the catalyst is selected from one or more of metal chloride, metal sulfate, metal nitrate, hydrogen phosphate, metal oxide, inorganic acid, organic acid and inorganic base; the metal is selected from one or more of sodium, potassium, calcium, magnesium, aluminum, zinc, iron and cobalt; the reaction temperature is 50-150 ℃. The method has the advantages that the furan ammonium salt waste residue liquid reacts under the conditions of a specific catalyst system, a specific temperature and a solvent, so that the (E) -type furan ammonium salt is directly turned into the (Z) -type furan ammonium salt by a one-step method, and finally, the thermodynamically stable furan ammonium salt product is obtained. The method disclosed by the patent is simple in steps, economic and environment-friendly, effectively improves the recovery yield of the furan ammonium salt, is suitable for industrial production, and reduces the environment-friendly pressure of the furan ammonium salt waste liquid.
Chinese patent CN107573305A discloses a method for preparing furan ammonium salt, comprising the following steps: reacting 2-acetylfuran with sodium nitrite to prepare furanone acid by taking 2-acetylfuran as a raw material under the catalytic action of metal salt; esterifying furanone acid and alcohol under the action of concentrated sulfuric acid to generate furanone acid ester; reacting the ketofuranonate with methoxyamine to obtain 2-methoxyimino-2-furylacetic acid methyl ester; adjusting the pH value of the 2-methoxyimino-2-furylacetic acid methyl ester solution, and extracting with an organic solvent to obtain a 2-methoxyimino-2-furylacetic acid solution; reacting the 2-methoxyimino-2-furan acetic acid solution with an alcohol ammonia solvent to obtain furan ammonium salt. The metal salt is one or more of ferric salt, copper salt and sulfate of zinc salt. This patent increases the yield of the furan ammonium salt by increasing the conversion of acetylfuran on the one hand and by decreasing the content of trans-furan ammonium salt on the other hand.
Most of the patents on the furan ammonium salt are concentrated on the preparation method, raw material recovery and cis-trans conversion, and the recovery is carried out through secondary treatment on the problem of more waste residues and waste liquid generated in the reaction, so that the energy consumption is higher. The product refining mode is mainly an intermittent discharging mode, the distillation efficiency of the product in the second half period of distillation is greatly reduced along with the enrichment of water content, the energy consumption is increased, the heat utilization rate is greatly reduced due to the sharp reduction of the liquid level, a large amount of wall-hanging unqualified products are separated out from the kettle wall for reducing the liquid level, the product quality is reduced quickly, the heat utilization rate is low, the time period is long, and the production efficiency is low. If the rectification efficiency and the heat utilization rate can be improved, the consumption of power cost can be greatly reduced, and the yield and the quality of products can be improved by reducing the amount of generated wall hanging and the amount of distilled waste liquid.
Disclosure of Invention
The invention aims to provide a method for continuously recrystallizing a furan ammonium salt crude product, which effectively improves the heat utilization rate of equipment by keeping the liquid level constant in the recrystallization process, greatly reduces the generation of unqualified wall-hung products, maintains a balanced and stable state in the whole process for recrystallization, improves the distillation efficiency and the product yield, effectively increases the heat utilization rate, reduces the waste liquid amount and reduces the power cost.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the method for continuously recrystallizing the coarse furan ammonium salt comprises the following steps: dissolving the furan ammonium salt crude product, decolorizing, feeding into a temperature-controlled evaporation kettle, evaporating and crystallizing, and maintaining the liquid level in the temperature-controlled evaporation kettle constant by controlling the feeding speed and the discharging speed; transferring the materials in the kettle through a pneumatic diaphragm pump, cooling, crystallizing, filtering and drying to obtain the furan ammonium salt, thereby realizing the continuous recrystallization of the furan ammonium salt crude product.
Wherein:
the feeding speed is 20-35 g/min, the discharging speed is 20-35 g/min, and the feeding speed and the discharging speed are the same.
The evaporation crystallization temperature is 22-30 ℃.
The jacket temperature of the temperature-controlled evaporation kettle is 50-60 ℃, and the vacuum degree is 0.070-0.095 MPa.
Dissolving a furan ammonium salt crude product by using a methanol aqueous solution, wherein the dosage ratio of the furan ammonium salt crude product to the methanol aqueous solution is 1: 5.5-6, wherein the furan ammonium salt crude product is calculated by g, and the methanol aqueous solution is calculated by ml; the water content in the methanol aqueous solution is 3-6 wt.%.
The dissolving temperature is 58-63 ℃, and the dissolving time is 10-15 min.
Decoloring by using activated carbon, wherein the decoloring temperature is 58-63 ℃, and the decoloring time is 40-75 min; the using amount of the active carbon is 1-6% of the mass of the coarse product of the furan ammonium salt.
The cooling crystallization temperature is 10-15 ℃, and the cooling crystallization time is 1-1.5 h.
Returning the filtered mother liquor to the temperature-controlled evaporation kettle, leaching the filtered wet product by using methanol, wherein the mass ratio of the filtered wet product to the methanol is 1: 1.1-1.3.
The drying temperature is 35-40 ℃, and the drying time is 40-70 min.
Dissolving a furan ammonium salt crude product by using a methanol aqueous solution, and decoloring by using activated carbon to obtain a decoloring solution; feeding a decolored liquid into a temperature-controlled evaporation kettle for evaporation and crystallization, maintaining the liquid level in the temperature-controlled evaporation kettle constant by controlling the feeding speed and the discharging speed, transferring materials in the kettle into a pressure filter through a pneumatic diaphragm pump, cooling, crystallizing and filtering; returning the filtered mother liquor to the temperature-controlled evaporation kettle, leaching the filtered material with methanol, and drying to obtain the furylammonium salt, thereby realizing continuous recrystallization of the furylammonium salt crude product.
The temperature control evaporation kettle provided by the invention is provided with two inlet paths and one outlet path, wherein the inlet path I is a destaining solution feeding port, the inlet path II is a pressure filtrate loop, and the outlet path is a pneumatic diaphragm pump and pressure filter separation path. In the continuous recrystallization process, under the condition of pressure, a pneumatic diaphragm pump presses materials into a pressure filter, solid-liquid separation is carried out in the pressure filter by depending on the pressure of the whole closed system, mother liquor returns to a temperature control evaporation kettle through a pressure filtrate loop, the materials are stored to a certain amount, and the pressure filtrate loop is closed to take out products. The continuous distillation and continuous discharging under the condition of whole vacuum are realized, the stability of pressure, vacuum degree, moisture, distillation liquid level, temperature and product quality is maintained in the whole distillation process, the decoloration liquid is added continuously, and the product is separated continuously.
The invention has the following beneficial effects:
(1) in the prior art, a furylammonium salt crude product is heated and dissolved in a methanol water solution, activated carbon is added for decolorization to obtain a decolorized solution, the decolorized solution is added into a refining kettle for distillation at one time, the liquid level is gradually reduced to generate a hanging wall material, the one-time yield of the product is low, and the product quality is reduced by about 10% during refining; the refining kettle jacket has low utilization rate and high power cost; the product quality is influenced by falling of the wall built-up material in the distillation process, and the floating range of the content of the trans-product is large (0.0200-0.1000%). In addition, if the quality of the product is required to be ensured in the crystallization process, the liquid level at the evaporation crystallization end point needs to be controlled to be 2-7L, the fluctuation range of the liquid level at the evaporation crystallization end point is large, so that the trans-form content in the product cannot be stably controlled, batch production is interrupted, the trans-form content difference is large, i.e. trans-form products and impurities in part of batches swell, and the product quality is influenced.
The invention keeps continuous feeding and continuous discharging in the refining distillation process, maintains the stability of the liquid level, obviously reduces the existence of the wall-hanging material, has high jacket utilization rate of the temperature control evaporation kettle, can improve the primary yield of the product by 7 percent, and simultaneously ensures that the quality of the product is not influenced by the wall-hanging material; the product has high purity, and low trans and impurity content and is stable. The invention adopts methanol water solution to dissolve the furylammonium salt crude product, and adds a certain amount of water into pure methanol, thereby effectively reducing the accumulation of trans-form and impurities in the continuous crystallization process and ensuring the stable product quality. The invention does not need excessive operation, optimizes the reaction steps and is easy to realize industrialized production.
(2) The existing process needs to evaporate the mother liquor of a whole evaporation kettle to a low liquid level, discharge more materials as much as possible, and the change of a reaction system when the liquid level is low slows down the evaporation efficiency by 15%. The invention can maintain the stability of the system in the kettle when the inlet and the outlet are balanced, continuously keep higher evaporation efficiency, improve the efficiency of the whole process, make the process more stable and efficient, obviously reduce the power cost by 5 percent and the heat energy cost by 10 percent.
(3) In the prior art, the throwing filtration is carried out after the distillation in the whole kettle is finished every time, the thrown and filtered mother liquor is recycled, and part of un-distilled furan ammonium salt in the recycled mother liquor causes waste and needs to be recycled. The invention can discharge partial mother liquor periodically according to the condition of the mother liquor in the kettle to maintain the stable quality of the mother liquor in the kettle and produce products with the same quality, the amount of the mother liquor replaced by the invention is less than 80 percent of the amount of the mother liquor required by the normal process, thereby reducing waste, improving the yield of the products and reducing the recovery cost.
(4) In the prior art, when each batch of distillation is pressurized, the phenomenon of bumping can occur, and a large amount of inert gas is needed to be used for flushing a kettle to prevent bumping. The invention adopts a continuous and uninterrupted mode to only use the inert gas in the first batch at the beginning of refining, saves more than 95 percent of the inert gas and reduces the cost.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
(1) Dissolving: adding 1.6kg of crude furan ammonium salt into 9L of methanol aqueous solution with the water content of 3 wt.%, and dissolving at the high temperature of 58 ℃ for 10min to obtain a dissolved solution;
(2) and (3) decoloring: adding 90g of activated carbon into the dissolved solution obtained in the step (1) at 63 ℃ for decoloring for 40min, and carrying out hot filtration to obtain a decolored solution;
(3) evaporation and crystallization: adjusting the jacket temperature of the temperature-controlled evaporation kettle to 50 ℃ and the vacuum degree to 0.070MPa, continuously adding the decolorized solution obtained in the step (2) into the temperature-controlled evaporation kettle, recording the liquid level to 16L, adjusting the feeding speed and the discharging speed to be 20g/min, maintaining the liquid level constant, and evaporating and crystallizing at 22 ℃; in the process, the material feeding amount is measured, and the total feeding amount is 8.5 kg;
(4) discharging: transferring the precipitated product into a filter press by a pneumatic diaphragm pump under the condition of ensuring vacuum environment, cooling and crystallizing at 10 ℃ for 1.5h, and filtering to obtain 1360g of wet product; returning the filtered mother liquor to the temperature-controlled evaporation kettle;
(5) leaching and drying: and (4) leaching the wet product obtained in the step (4) by using 1.5kg of pure methanol, and drying at 40 ℃ for 50min to obtain 1328g of furan ammonium salt product, wherein the yield is 83%, and the chromaticity is qualified. The purity of the furan ammonium salt product is 99.86 percent, the content of the trans-furan ammonium salt is 0.0488 percent and the content of impurities is 0.0912 percent through detection.
Example 2
(1) Dissolving: adding 1.6kg of furan ammonium salt crude product into 9L of methanol aqueous solution with the water content of 3 wt.%, and dissolving at the high temperature of 60 ℃ for 15min to obtain a dissolved solution;
(2) and (3) decoloring: adding 90g of activated carbon into the dissolved solution obtained in the step (1) at 60 ℃ for decoloring for 60min, and carrying out hot filtration to obtain a decolored solution;
(3) evaporation and crystallization: adjusting the jacket temperature of the temperature-controlled evaporation kettle to 55 ℃ and the vacuum degree to 0.080MPa, continuously adding the decolorized solution obtained in the step (2) into the temperature-controlled evaporation kettle, recording the liquid level to 16L, adjusting the feeding speed and the discharging speed to be 25g/min, maintaining the liquid level constant, and evaporating and crystallizing at 25 ℃; in the process, the material feeding amount is measured, and the total feeding amount is 8.5 kg;
(4) discharging: transferring the precipitated product into a filter press by a pneumatic diaphragm pump under the condition of ensuring vacuum environment, cooling and crystallizing for 1h at 15 ℃, and filtering to obtain 1365g of a wet product; returning the filtered mother liquor to the temperature-controlled evaporation kettle;
(5) leaching and drying: and (4) leaching the wet product obtained in the step (4) by using 1.65kg of pure methanol, and drying at 35 ℃ for 70min to obtain 1331g of a furan ammonium salt product, wherein the yield is 83%, and the chroma quality is qualified. The purity of the furan ammonium salt product is 99.85 percent, the content of the trans-furan ammonium salt is 0.050 percent, and the content of impurities is 0.10 percent through detection.
Example 3
(1) Dissolving: adding 1.6kg of furan ammonium salt crude product into 9L of methanol aqueous solution with the water content of 6 wt.%, and dissolving at the high temperature of 63 ℃ for 15min to obtain a dissolved solution;
(2) and (3) decoloring: adding 90g of activated carbon into the dissolved solution obtained in the step (1) at 58 ℃ for decoloring for 75min, and carrying out hot filtration to obtain a decolored solution;
(3) evaporation and crystallization: adjusting the jacket temperature of the temperature-controlled evaporation kettle to be 60 ℃ and the vacuum degree to be 0.085MPa, continuously adding the decolorized solution obtained in the step (2) into the temperature-controlled evaporation kettle, recording the liquid level to be 16L, adjusting the feeding speed and the discharging speed to be 35g/min, maintaining the liquid level to be constant, and evaporating and crystallizing at 30 ℃; in the process, the material feeding amount is measured, and the total feeding amount is 8.5 kg;
(4) discharging: transferring the precipitated product into a filter press by a pneumatic diaphragm pump under the condition of ensuring vacuum environment, cooling and crystallizing for 1.2h at the temperature of 12 ℃, and filtering to obtain 1363g of wet product; returning the filtered mother liquor to the temperature-controlled evaporation kettle;
(5) leaching and drying: and (4) leaching the wet product obtained in the step (4) by using 1.77kg of pure methanol, and drying at 40 ℃ for 60min to obtain 1330g of a furan ammonium salt product, wherein the yield is 83%, and the chromaticity is qualified. The purity of the furan ammonium salt product is 99.84 percent, the content of the trans-furan ammonium salt is 0.0472 percent and the content of impurities is 0.1128 percent through detection.
Comparative example 1
(1) Dissolving: adding 1.6kg of furan ammonium salt crude product into 9L of pure methanol solution, and dissolving at the high temperature of 60 ℃ for 15min to obtain a solution;
(2) and (3) decoloring: adding 90g of activated carbon into the dissolved solution obtained in the step (1) at 58 ℃ for decoloring for 75min, and carrying out hot filtration to obtain a decolored solution;
(3) evaporation and crystallization: adjusting the jacket temperature of the temperature-controlled evaporation kettle to be 60 ℃ and the vacuum degree to be 0.085MPa, continuously adding the decolorized solution obtained in the step (2) into the temperature-controlled evaporation kettle, recording the liquid level to be 16L, adjusting the feeding speed and the discharging speed to be 35g/min, maintaining the liquid level to be constant, and evaporating and crystallizing at 30 ℃;
(4) discharging: transferring the precipitated product into a filter press by a pneumatic diaphragm pump under the condition of ensuring vacuum environment, cooling and crystallizing at 12 ℃ for 1.2h, and filtering to obtain 1248g of wet product; the filtered mother liquor returns to the temperature control evaporation kettle.
(5) Leaching and drying: and (4) leaching the wet product obtained in the step (4) by using 1.77kg of pure methanol, and drying at 40 ℃ for 60min to obtain 1215g of a furan ammonium salt product with the yield of 76%. The purity of the furan ammonium salt product is 99.62%, the content of trans-furan ammonium salt is 0.1196%, and the content of impurities is 0.2604% through detection.
Comparative example 2
(1) Dissolving: adding 1.6kg of furan ammonium salt crude product into 9L of pure methanol solution, and dissolving at a high temperature of 58 ℃ for 10min to obtain a solution;
(2) and (3) decoloring: adding 90g of activated carbon into the dissolved solution obtained in the step (1) at 63 ℃ for decoloring for 40min, and carrying out hot filtration to obtain a decolored solution;
(3) evaporation and crystallization: adjusting the jacket temperature of the temperature-controlled evaporation kettle to 50 ℃ and the vacuum degree to 0.070MPa, continuously adding the decolorized solution obtained in the step (2) into the temperature-controlled evaporation kettle, recording the liquid level to 16L, adjusting the feeding speed and the discharging speed to be 20g/min, maintaining the liquid level constant, and evaporating and crystallizing at 22 ℃;
(4) discharging: transferring the precipitated product into a filter press by a pneumatic diaphragm pump under the condition of ensuring vacuum environment, cooling and crystallizing for 1.5h at 10 ℃, and filtering to obtain 1240g of a wet product; returning the filtered mother liquor to the temperature-controlled evaporation kettle;
(5) leaching and drying: and (4) leaching the wet product obtained in the step (4) by using 1.5kg of pure methanol, and drying at 40 ℃ for 50min to obtain 1210g of a furan ammonium salt product with the yield of 76%. The purity of the furan ammonium salt product is 99.65%, the content of the trans-furan ammonium salt is 0.1329% and the content of impurities is 0.2171% through detection.
Comparative example 3
(1) Dissolving: adding 1.6kg of crude furan ammonium salt into 9L of methanol aqueous solution with the water content of 3 wt.%, and dissolving at the high temperature of 58 ℃ for 10min to obtain a dissolved solution;
(2) and (3) decoloring: adding 90g of activated carbon into the dissolved solution obtained in the step (1) at 63 ℃ for decoloring for 40min, and carrying out hot filtration to obtain a decolored solution;
(3) evaporation and crystallization: adjusting the temperature of a jacket of the temperature-controlled evaporation kettle to 50 ℃ and the vacuum degree to 0.070MPa, adding the decolorized solution obtained in the step (2) into the temperature-controlled evaporation kettle, recording the liquid level to 16L, evaporating and crystallizing at 22 ℃, controlling the liquid level at the end point of evaporation and crystallization to be 2-7L, and finishing distillation;
(4) discharging: discharging under normal pressure after pressure relief, cooling and crystallizing at 10 ℃ for 1.5h, and filtering to obtain 1235g of wet product; hanging a defective product 125 g;
(5) leaching and drying: and (4) leaching the wet product obtained in the step (4) by using 1.5kg of pure methanol, and drying at 40 ℃ for 50min to obtain 1205g of furan ammonium salt product with the yield of 75%. The purity of the furan ammonium salt product is 99.56 percent, the content of the trans-furan ammonium salt is 0.1547 percent and the content of impurities is 0.2895 percent through detection.
Claims (10)
1. A method for continuously recrystallizing a coarse furylammonium salt is characterized in that: dissolving the furan ammonium salt crude product, decolorizing, feeding into a temperature-controlled evaporation kettle, evaporating and crystallizing, and maintaining the liquid level in the temperature-controlled evaporation kettle constant by controlling the feeding speed and the discharging speed; transferring the materials in the kettle through a pneumatic diaphragm pump, cooling, crystallizing, filtering and drying to obtain the furan ammonium salt, thereby realizing the continuous recrystallization of the furan ammonium salt crude product.
2. The method for continuously recrystallizing the crude furaminium salt according to claim 1, wherein: the feeding speed is 20-35 g/min, the discharging speed is 20-35 g/min, and the feeding speed and the discharging speed are the same.
3. The method for continuously recrystallizing the crude furaminium salt according to claim 1, wherein: the evaporation crystallization temperature is 22-30 ℃.
4. The method for continuously recrystallizing the crude furaminium salt according to claim 1, wherein: the jacket temperature of the temperature-controlled evaporation kettle is 50-60 ℃, and the vacuum degree is 0.070-0.095 MPa.
5. The method for continuously recrystallizing the crude furaminium salt according to claim 1, wherein: dissolving a furan ammonium salt crude product by using a methanol aqueous solution, wherein the dosage ratio of the furan ammonium salt crude product to the methanol aqueous solution is 1: 5.5-6, wherein the furan ammonium salt crude product is calculated by g, and the methanol aqueous solution is calculated by ml; the water content in the methanol aqueous solution is 3-6 wt.%.
6. The method for continuously recrystallizing the crude furaminium salt according to claim 5, wherein: the dissolving temperature is 58-63 ℃, and the dissolving time is 10-15 min.
7. The method for continuously recrystallizing the crude furaminium salt according to claim 1, wherein: decoloring by using activated carbon, wherein the decoloring temperature is 58-63 ℃, and the decoloring time is 40-75 min; the using amount of the active carbon is 1-6% of the mass of the coarse product of the furan ammonium salt.
8. The method for continuously recrystallizing the crude furaminium salt according to claim 1, wherein: the cooling crystallization temperature is 10-15 ℃, and the cooling crystallization time is 1-1.5 h.
9. The method for continuously recrystallizing the crude furaminium salt according to claim 1, wherein: returning the filtered mother liquor to the temperature-controlled evaporation kettle, leaching the filtered wet product by using methanol, wherein the mass ratio of the wet product to the methanol is 1: 1.1-1.3.
10. The method for continuously recrystallizing the crude furaminium salt according to claim 1, wherein: the drying temperature is 35-40 ℃, and the drying time is 40-70 min.
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| CN115501638A (en) * | 2022-10-19 | 2022-12-23 | 安徽金轩科技有限公司 | Crystallization device and method in production of furan ammonium salt |
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| CN101357911A (en) * | 2008-09-19 | 2009-02-04 | 江苏爱利思达清泉化学有限公司 | Method for synthesizing (z)-2-(alpha-methoxyimino)furan-ammonium acetate |
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| CN107892678A (en) * | 2017-12-06 | 2018-04-10 | 成都化润药业有限公司 | The SMIA preparation technology of recyclable furans ketone acid |
| CN107903226A (en) * | 2017-11-29 | 2018-04-13 | 中国科学院长春应用化学研究所 | A kind of preparation method of cis furan ammonium salt |
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| CN101357911A (en) * | 2008-09-19 | 2009-02-04 | 江苏爱利思达清泉化学有限公司 | Method for synthesizing (z)-2-(alpha-methoxyimino)furan-ammonium acetate |
| CN102863407A (en) * | 2012-10-10 | 2013-01-09 | 山东金城医药化工股份有限公司 | Preparation method of 2-methoxyiminofurylacetic acid amonium salt |
| CN107903226A (en) * | 2017-11-29 | 2018-04-13 | 中国科学院长春应用化学研究所 | A kind of preparation method of cis furan ammonium salt |
| CN107892678A (en) * | 2017-12-06 | 2018-04-10 | 成都化润药业有限公司 | The SMIA preparation technology of recyclable furans ketone acid |
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| CN115501638A (en) * | 2022-10-19 | 2022-12-23 | 安徽金轩科技有限公司 | Crystallization device and method in production of furan ammonium salt |
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