CN103012270B - Method for recovering antipyrine from mother solution after crystallization of antipyrine crude oil - Google Patents
Method for recovering antipyrine from mother solution after crystallization of antipyrine crude oil Download PDFInfo
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Abstract
The invention discloses a method for recovering antipyrine from a mother solution after crystallization of antipyrine crude oil. The method sequentially comprises the steps of concentrating, decoloring, cooling and crystallizing, re-crystallizing, refining, centrifuging and drying, wherein the re-crystallizing procedure is realized by adopting the following steps of: re-dissolving concentrated crystals obtained in the cooling and crystallizing procedure by using alcohol, then adding active carbon in a re-dissolved solution while raising the temperature to 55-65 DEG C, wherein the weight ratio of the active carbon to the concentrated crystals is 1:(180-220), continuously raising the temperature to 75-85 DEG C, insulating heat for 25-40min and then filtering, cooling filtrate and insulating heat for 8-15min after the crystals occur, continuously cooling to 10-15 DEG C and then centrifuging to obtain an antipyrine re-crystallized product; and refining, centrifuging and drying the re-crystallized product to obtain the antipyrine. The method has the advantages of fully and reasonably utilizing the crystallized mother solution, ensuring the quality of analginum, and being simple in operation and high in recovering rate; and the antipyrine is high in purity.
Description
Technical field
The present invention relates to a kind of production method of quinizine, be specifically related to a kind of method that reclaims quinizine from the mother liquor the crystallization of quinizine crude oil.
Background technology
Sulpyrine, chemistry [(1,5-dimethyl-2-phenyl-3-oxo-2,3-dihydro-1 h-pyrazole-4-yl) methylamino-] methanesulfonic sodium salt-hydrate by name, molecular formula is C
13h
16n
3naO
4sH
2o; its conventional preparation method is that pyrazolone is produced quinizine oil through first reaction, hydrolysis, alkaline purification; quinizine oil is produced aminoantipyrene oil through nitrosation reaction, reduction reaction, hydrolysis neutralization reaction; aminoantipyrene oil generates formyl amino antipyrine through acylation reaction; through first, hydrolysis, once neutralization, secondary neutralization, dehydration, generate novalgin oil again; then pass through condensation reaction; refining crystallization generates Sulpyrine wet product, through dry packing, obtains Sulpyrine finished product.Aforesaid method can be reduced to following technical process: pyrazolone-quinizine oil-aminoantipyrene oil-formyl amino antipyrine-novalgin oil-Sulpyrine.
Quinizine finished product repeats crystallization decolouring by quinizine oil and produces, process flow sheet is referring to Fig. 1, the first workshop section that its raw material quinizine oil is generally produced by Sulpyrine provides, as can see from Figure 1, raw material quinizine oil can produce the mother liquor after the crystallization of quinizine crude oil after crystallization is for the first time centrifugal, although contain a large amount of quinizines in this mother liquor, but the reason due to its impurity, be not used further in the follow-up production process of quinizine, but through oversalting, forming the quinizine oil of saltouing comes back in the corresponding workshop section of Sulpyrine technique and is used as the raw material of producing aminoantipyrene oil.But the increase day by day due to the market demand of quinizine, need to strengthen the output of quinizine, and the words of carrying out according to existing technique, when strengthening quinizine turnout, must cause back the corresponding increase of oily amount of saltouing of quinizine in Sulpyrine production workshop section, and saltout a large amount of uses of oil of quinizine can affect the quality of Sulpyrine, so will guarantee that the quality of Sulpyrine is just difficult to strengthen the output of quinizine.If mother liquor is not all saltoutd and gets back in the production workshop section of Sulpyrine, by the mother liquor producing after a large amount of quinizine crude oil crystallizations, and in this mother liquor, also contain a large amount of quinizines, therefore need a kind of quinizine that reclaims from this mother liquor in the situation that not changing original technique and guaranteeing Sulpyrine quality to increase the output of quinizine.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method that reclaims quinizine from the mother liquor the crystallization of quinizine crude oil is provided.The method takes full advantage of the mother liquor after the crystallization of quinizine crude oil, in the situation that do not change the production technique of original Sulpyrine and guarantee that Sulpyrine quality reclaims quinizine to increase the output of quinizine from this mother liquor, thereby meet the demand in market, in addition, the method is simple, the rate of recovery is high, can realize suitability for industrialized production.
In order to address the above problem, the present invention is the Sulpyrine workshop section of no longer all saltouing back of the mother liquor after the crystallization of quinizine crude oil, but partial mother liquid condensing crystal is processed to produce quinizine again, and so both increased the output of quinizine, do not affect again the quality of Sulpyrine.The above-mentioned mother liquor condensing crystal again method of process for producing quinizine is the method that reclaims quinizine from the mother liquor the crystallization of quinizine crude oil provided by the invention, it comprises concentrated, decolouring, decrease temperature crystalline, recrystallization, refining, centrifugal and drying process successively, specific as follows:
Described enrichment process is not particularly limited, and can be the enrichment process of this area routine, but be preferably concentrating under reduced pressure, and the concentrated solution volume after concentrated is the 25-35% of mother liquor cumulative volume before concentrated, and exemplary can be 28%, 30%, 33%; More preferably, temperature during described concentrating under reduced pressure be 75-85 ℃, vacuum tightness for-more than 0.04Mpa.The temperature of exemplary concentrating under reduced pressure can be 76 ℃, 80 ℃, 83 ℃, vacuum tightness can for-0.04Mpa ,-0.08Mpa ,-0.10Mpa.
Described bleaching process is not particularly limited, and can be the bleaching process of this area routine, but preferably adopt gac to decolour; More preferably decolour as follows: when described concentrated solution is stirred, be heated, when being heated to 60-70 ℃, add gac to continue to stir and be warming up to 75-85 ℃, insulation 50-70min.When the weight ratio of gac and concentrated solution is 0.02-0.03:1, decolorizing effect is best.
Described decrease temperature crystalline operation is not particularly limited, and can be the decrease temperature crystalline operation of this area routine, but be preferably, the concentrated solution through decolouring is cooled to 10-20 ℃, then the centrifugal condensing crystal that obtains.
Described recrystallization operation is with alcohol, described condensing crystal to be dissolved again, the gac that to add with described condensing crystal weight ratio while being then warming up to 55-65 ℃ be 1:180-220, continue to be warming up to 75-85 ℃, be incubated after 25-40 minute and filter, then filtrate is lowered the temperature and after there is crystallization, is incubated 8-15 minute, continue to be cooled to 10-15 ℃ after the centrifugal quinizine recrystallized product that obtains.Preferably, the weight ratio of described alcohol and described condensing crystal is 1:2-4, and exemplary can be 1:2,1:3,1:4.The purity of described alcohol is more than 75wt%, can adopt recovered alcohol, such as the alcohol (concentration is 93wt%) of the alcohol recycle section in the production process from pyramidon dissolves condensing crystal again.
Described refining step can be the finished product decolorizing and refining operation (referring to Fig. 1) in common quinizine technique, it is specific as follows: the purified water that to use with described recrystallized product weight ratio be 1:2.4-2.45 is dissolved described recrystallized product, and drop into gac in the solution after dissolving to described recrystallized product under the temperature condition of 65 ± 5 ℃, wherein the weight ratio of recrystallized product and gac is 1:0.015-0.03; Then continue to heat up, control temperature is decoloured and is incubated 50-70min under 75-85 ℃ of condition; Again solution press filtration after decolouring is entered in crystallisation vessel, when in crystallisation vessel, temperature is 70 ℃-75 ℃, the little salt water for cooling of opening, close salt solution, then slow cooling is to 10-15 ℃ when being down to 25-29 ℃, the described slow cooling time is controlled at 50-70min, thereby obtains refined products.The weight ratio of described recrystallized product and gac is preferably 1:0.022, can make like this colorimetric of final finished product quinizine more meet the requirements.While refining together with the de-crystallization (referring to Fig. 1 or Fig. 2) of described recrystallized product and one in former quinizine technique, the recrystallized product in this refining step can replace with the mixture of recrystallized product and a de-crystallization.
Described refined products obtains quinizine wet product through getting rid of material after being centrifugal, then the dry finished product quinizine that obtains.
Mother liquor after the crystallization of described quinizine crude oil refers in quinizine production technique remaining solution after the crystallization of quinizine Crude Oil Lower-Temp.
Beneficial effect of the present invention: existing technique is that this mother liquor is saltoutd and formed that quinizine is saltoutd oil and the corresponding workshop section of all getting back to Sulpyrine, and the present invention is in the situation that do not change the production technique of original Sulpyrine and guarantee that Sulpyrine quality reclaims quinizine to increase the output of quinizine from remaining mother liquor, overcome the defect that will destroy the quality of Sulpyrine when strengthening quinizine output in prior art or cause the idle waste of the mother liquor after the crystallization of quinizine crude oil, method of the present invention has not only fully rationally been utilized the mother liquor after the crystallization of quinizine crude oil, guaranteed the quality of Sulpyrine and quinizine output is increased.In addition, this recovery method is simple, and the rate of recovery is high, can reach 25%-30%, and quinizine product purity is more than 99.2%, can realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that existing quinizine is produced.
Fig. 2 is the process flow sheet that the quinizine after improving is produced, and has wherein comprised technical process of reclaiming quinizine from the mother liquor the crystallization of quinizine crude oil of the present invention.
Embodiment
Below by specific embodiment, the present invention will be further described, but the present invention is not limited to this.
Embodiment 1
That the method that reclaims quinizine from the mother liquor the crystallization of quinizine crude oil provided by the invention comprises is successively concentrated, decolouring, decrease temperature crystalline, recrystallization, refining, centrifugal and drying process, specific as follows:
Mother liquor after the crystallization of quinizine crude oil is extracted in concentration tank, and temperature is controlled under the condition that 80 ℃, vacuum are-0.04Mpa carries out concentrating under reduced pressure, when be concentrated to original nut liquid volume 30% time, stop concentrating, again concentrated solution is extracted into bleacher, open stirs, open steam heating, when temperature reaches 65 ℃, add the gac that the weight ratio with concentrated solution is 0.02:1, continue to be warming up to 80 ℃ of insulations 1 hour, then the concentrated solution press filtration after decolouring is entered to crystallizer, open salt solution and lower the temperature, centrifugal when temperature is down to 15 ℃, obtain condensing crystal, then condensing crystal is put into the enamel pot of 3000 liters, alcohol with 93% dissolves, the weight ratio of alcohol and condensing crystal is 1:3, the gac that to add with condensing crystal weight ratio while being warming up to 60 ℃ be 1:200, continues to be warming up to 78 ℃ of insulations suction filtration after 30 minutes, retains filtrate, proceeded in decrease temperature crystalline tank and lowered the temperature, after there is crystallization, keep 10 minutes, continue to be cooled to 15 ℃ and get rid of material, obtain quinizine recrystallized product, the recrystallized product obtaining is refining with take off crystallization by one of common quinizine explained hereafter together with, the purified water that to be about to recrystallized product weight ratio be 1:2.4 joins bleacher, heat up and in this bleacher, add recrystallized product simultaneously, when rising to 70 ℃, the crystallization CL until refining and temperature drop into the gac that the weight ratio with recrystallized product is 1:0.022, continue to heat up, control temperature is decoloured and is incubated 1 hour under 80 ℃ of conditions, again solution press filtration after decolouring is entered to crystallizer, after decolouring, 3/4 of the volume of solution while having entered crystallizer, open the whipping appts of crystallizer, after decolouring, solution enters crystallizer when complete, in crystallization control tank, temperature is 70 ℃, the then little salt water for cooling of opening, when being down to 27 ℃, close salt solution, slow cooling to 12 ℃ again, the slow cooling time is controlled at 1 hour and obtains refined products, last refined products is centrifugal, the dry finished product quinizine that obtains.Its rate of recovery is 28%, and product purity is 99.3%, and colorimetric is 1.5.
Described colorimetric is according to testing with the method for standard color solution contrast.
Embodiment 2
That the method that reclaims quinizine from the mother liquor the crystallization of quinizine crude oil provided by the invention comprises is successively concentrated, decolouring, decrease temperature crystalline, recrystallization, refining, centrifugal and drying process, specific as follows:
Mother liquor after the crystallization of quinizine crude oil is extracted in concentration tank, and temperature is controlled under the condition that 83 ℃, vacuum are-0.06Mpa carries out concentrating under reduced pressure, when be concentrated to original nut liquid volume 33% time, stop concentrating, again concentrated solution is extracted into bleacher, open stirs, open steam heating, when temperature reaches 60 ℃, add the gac with concentrated solution ratio 0.025:1, continue to be warming up to 85 ℃ of insulation 70min, then the concentrated solution press filtration after decolouring is entered to crystallizer, open salt solution and lower the temperature, centrifugal when temperature is down to 12 ℃, obtain condensing crystal, then condensing crystal is put into the enamel pot of 3000 liters, alcohol with 93% dissolves, the weight ratio of alcohol and condensing crystal is 1:4, the gac that to add with condensing crystal weight ratio while being warming up to 65 ℃ be 1:220, continues to be warming up to 82 ℃ of insulations suction filtration after 40 minutes, retains filtrate, proceeded in decrease temperature crystalline tank and lowered the temperature, after there is crystallization, keep 8 minutes, continue to be cooled to 10 ℃ and get rid of material, obtain quinizine recrystallized product, the recrystallized product obtaining is refining with take off crystallization by one of common quinizine explained hereafter together with, the purified water that to be about to recrystallized product weight ratio be 1:2.45 joins bleacher, heat up and in this bleacher, add recrystallized product simultaneously, when rising to 65 ℃, the crystallization CL until refining and temperature drop into the gac that the weight ratio with recrystallized product is 1:0.015, continue to heat up, control temperature is decoloured and is incubated 1 hour under 80 ℃ of conditions, again solution press filtration after decolouring is entered to crystallizer, after decolouring, 3/4 of the volume of solution while having entered crystallizer, open the whipping appts of crystallizer, after decolouring, solution enters crystallizer when complete, in crystallization control tank, temperature is 75 ℃, the then little salt water for cooling of opening, when being down to 29 ℃, close salt solution, slow cooling to 10 ℃ again, the slow cooling time is controlled at 1 hour and obtains refined products, last refined products is centrifugal, the dry finished product quinizine that obtains.Its rate of recovery is 25%, and product purity is 99.6%, and colorimetric is 2.
Described colorimetric estimation method is with embodiment 1.
Embodiment 3
That the method that reclaims quinizine from the mother liquor the crystallization of quinizine crude oil provided by the invention comprises is successively concentrated, decolouring, decrease temperature crystalline, recrystallization, refining, centrifugal and drying process, specific as follows:
Mother liquor after the crystallization of quinizine crude oil is extracted in concentration tank, and temperature is controlled under the condition that 75 ℃, vacuum are-0.08Mpa carries out concentrating under reduced pressure, when be concentrated to original nut liquid volume 25% time, stop concentrating, again concentrated solution is extracted into bleacher, open stirs, open steam heating, when temperature reaches 70 ℃, add the gac with concentrated solution ratio 0.03:1, continue to be warming up to 78 ℃ of insulation 70min, then the concentrated solution press filtration after decolouring is entered to crystallizer, open salt solution and lower the temperature, centrifugal when temperature is down to 18 ℃, obtain condensing crystal, then condensing crystal is put into the enamel pot of 3000 liters, alcohol with 93% dissolves, the weight ratio of alcohol and condensing crystal is 1:2, the gac that to add with condensing crystal weight ratio while being warming up to 55 ℃ be 1:180, continues to be warming up to 75 ℃ of insulations suction filtration after 25 minutes, retains filtrate, proceeded in decrease temperature crystalline tank and lowered the temperature, after there is crystallization, keep 15 minutes, continue to be cooled to 12 ℃ and get rid of material, obtain quinizine recrystallized product, the recrystallized product obtaining is refining with take off crystallization by one of common quinizine explained hereafter together with, the purified water that to be about to recrystallized product weight ratio be 1:2.4 joins bleacher, heat up and in this bleacher, add recrystallized product simultaneously, when rising to 60 ℃, the crystallization CL until refining and temperature drop into the gac that the weight ratio with recrystallized product is 1:0.03, continue to heat up, control temperature is decoloured and is incubated 1 hour under 75 ℃ of conditions, again solution press filtration after decolouring is entered to crystallizer, after decolouring, 3/4 of the volume of solution while having entered crystallizer, open the whipping appts of crystallizer, after decolouring, solution enters crystallizer when complete, in crystallization control tank, temperature is 70 ℃, the then little salt water for cooling of opening, when being down to 27 ℃, close salt solution, slow cooling to 15 ℃ again, the slow cooling time is controlled at 1 hour and obtains refined products, last refined products is centrifugal, the dry finished product quinizine that obtains.Its rate of recovery is 30%, and product purity is 99.8%, and colorimetric is 2.5.
Described colorimetric estimation method is with embodiment 1.
The purposes that should be appreciated that these embodiment only limits the scope of the invention for the present invention being described but not being intended to.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various changes, modification and/or modification to the present invention, within these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (5)
1. from the mother liquor the crystallization of quinizine crude oil, reclaim a method for quinizine, it is characterized in that, comprise successively enrichment process, bleaching process, decrease temperature crystalline operation, recrystallization operation, refining step, rotary process and drying process, wherein:
Described enrichment process is concentrating under reduced pressure, and the concentrated solution volume after concentrated is the 25-35% of mother liquor cumulative volume before concentrated,
Described bleaching process is that described concentrated solution is stirred and heated, and adds gac while being heated to 60-70 ℃, continues to stir and be warming up to 75-85 ℃, insulation 50-70min,
Described decrease temperature crystalline operation is that the concentrated solution through decolouring is cooled to 10-20 ℃, then the centrifugal condensing crystal that obtains, described recrystallization operation is again to dissolve with the condensing crystal that alcohol obtains described decrease temperature crystalline operation, while being then warming up to 55-65 ℃ to gac that to add with described condensing crystal weight ratio in the described solution again dissolving be 1:180-220, continue to be again warming up to 75-85 ℃, be incubated after 25-40 minute and filter, filtrate is lowered the temperature and after there is crystallization, is incubated 8-15 minute, the centrifugal quinizine recrystallized product that obtains after continuing to be cooled to 10-15 ℃,
The purity of described alcohol is more than 75wt%,
Described refining step is as follows: the purified water that to use with described quinizine recrystallized product weight ratio be 1:2.4-2.45 is dissolved described quinizine recrystallized product, and drop into gac in the solution after dissolving to described quinizine recrystallized product under the temperature condition of 65 ± 5 ℃, wherein the weight ratio of quinizine recrystallized product and gac is 1:0.015-0.03; Then continue to heat up, control temperature is decoloured and is incubated 50-70min under 75-85 ℃ of condition; Solution press filtration after decolouring is entered in crystallisation vessel, when in crystallisation vessel, temperature is 70 ℃-75 ℃, the little salt water for cooling of opening closes salt solution when being down to 25-29 ℃ again, then slow cooling is to 10-15 ℃, and the described slow cooling time is controlled at 50-70min, obtains refined products,
Described refined products obtains quinizine wet product after described rotary process, then is dried and obtains finished product quinizine through described drying process,
Mother liquor after the crystallization of described quinizine crude oil refers in quinizine production technique remaining solution after the crystallization of quinizine Crude Oil Lower-Temp.
2. method according to claim 1, is characterized in that, in described recrystallization operation, the weight ratio of described alcohol and described condensing crystal is 1:2-4.
3. method according to claim 1, is characterized in that, in described enrichment process, the temperature of described concentrating under reduced pressure be 75-85 ℃, vacuum tightness for-more than 0.04MPa.
4. method according to claim 1, is characterized in that, in described bleaching process, the weight ratio of described gac and described concentrated solution is 0.02-0.03:1.
5. method according to claim 1, is characterized in that, in described refining step, the weight ratio of described quinizine recrystallized product and gac is 1:0.022.
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| CN106279030B (en) * | 2016-08-08 | 2018-08-17 | 河北冀衡（集团）药业有限公司 | Using the method for the MAA crystallization production COS analgins that the molten method of wine obtains |
| CN106279031B (en) * | 2016-08-08 | 2018-07-31 | 河北冀衡（集团）药业有限公司 | Using the method for the MAA crystallization production COS analgins that water soluble method obtains |
| CN107185266A (en) * | 2017-06-07 | 2017-09-22 | 合山锌业科技有限公司 | Secondary crystallization system |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SK60493A3 (en) * | 1993-06-11 | 1995-04-12 | Rektorat Univerzity P J Safari | Acetate zinc with phenazone and method of its preparation |
| RU2270751C1 (en) * | 2004-10-12 | 2006-02-27 | ОАО "Тольяттиазот" | Method of production of antipyrine |
| CN101891683A (en) * | 2010-07-22 | 2010-11-24 | 河北冀衡（集团）药业有限公司 | Aminopyrine production method |
| CN102351794A (en) * | 2011-07-28 | 2012-02-15 | 山东新华制药股份有限公司 | Refined recovery process of isopropylantipyrine recycling product |
| CN102584706A (en) * | 2011-12-23 | 2012-07-18 | 山东新华制药股份有限公司 | Recovery process of analginum finished product centrifugal mother liquid |
| CN202555012U (en) * | 2012-05-22 | 2012-11-28 | 河北冀衡（集团）药业有限公司 | Analginum intermediate recovery device |
-
2012
- 2012-12-31 CN CN201210594517.9A patent/CN103012270B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SK60493A3 (en) * | 1993-06-11 | 1995-04-12 | Rektorat Univerzity P J Safari | Acetate zinc with phenazone and method of its preparation |
| RU2270751C1 (en) * | 2004-10-12 | 2006-02-27 | ОАО "Тольяттиазот" | Method of production of antipyrine |
| CN101891683A (en) * | 2010-07-22 | 2010-11-24 | 河北冀衡（集团）药业有限公司 | Aminopyrine production method |
| CN102351794A (en) * | 2011-07-28 | 2012-02-15 | 山东新华制药股份有限公司 | Refined recovery process of isopropylantipyrine recycling product |
| CN102584706A (en) * | 2011-12-23 | 2012-07-18 | 山东新华制药股份有限公司 | Recovery process of analginum finished product centrifugal mother liquid |
| CN202555012U (en) * | 2012-05-22 | 2012-11-28 | 河北冀衡（集团）药业有限公司 | Analginum intermediate recovery device |
Non-Patent Citations (6)
| Title |
|---|
| 上海第五制药厂.氨基比林生产工艺改进.《医药工业》.1974,(第07期),全文. |
| 上海第五制药厂.用氢化法还原4-亚硝基安替比林制备4-氨基安替比林及氨基比林.《医药工业》.1974,(第05期),全文. |
| 氨基安替比林生产工艺条件的优选;西北第二合成药厂两胺车间;《陕西化工》;19751231(第2期);全文 * |
| 氨基比林生产工艺改进;上海第五制药厂;《医药工业》;19741231(第07期);全文 * |
| 用氢化法还原4-亚硝基安替比林制备4-氨基安替比林及氨基比林;上海第五制药厂;《医药工业》;19741231(第05期);全文 * |
| 西北第二合成药厂两胺车间.氨基安替比林生产工艺条件的优选.《陕西化工》.1975,(第2期),全文. |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 053000 No.1, Weiwu street, high tech Zone, Hengshui City, Hebei Province Patentee after: Hebei Jiheng Pharmaceutical Co.,Ltd. Address before: 053000 No.368 Jianshe North Street, Hengshui City, Hebei Province Patentee before: HEBEI JIHENG (Group) PHARMACEUTICAL Co.,Ltd. |