CN102336650B - Stripping process and device for removing organic impurities in brufen sodium salt - Google Patents
Stripping process and device for removing organic impurities in brufen sodium salt Download PDFInfo
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- CN102336650B CN102336650B CN2011102033561A CN201110203356A CN102336650B CN 102336650 B CN102336650 B CN 102336650B CN 2011102033561 A CN2011102033561 A CN 2011102033561A CN 201110203356 A CN201110203356 A CN 201110203356A CN 102336650 B CN102336650 B CN 102336650B
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000012535 impurity Substances 0.000 title claims abstract description 35
- -1 brufen sodium salt Chemical class 0.000 title abstract description 6
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 32
- 239000000706 filtrate Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 claims description 89
- 229960001680 ibuprofen Drugs 0.000 claims description 89
- 159000000000 sodium salts Chemical class 0.000 claims description 84
- 239000000243 solution Substances 0.000 claims description 42
- 239000012267 brine Substances 0.000 claims description 38
- PTTPUWGBPLLBKW-UHFFFAOYSA-M sodium;2-[4-(2-methylpropyl)phenyl]propanoate Chemical compound [Na+].CC(C)CC1=CC=C(C(C)C([O-])=O)C=C1 PTTPUWGBPLLBKW-UHFFFAOYSA-M 0.000 claims description 38
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000003513 alkali Substances 0.000 claims description 21
- 239000002351 wastewater Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 8
- XENVCRGQTABGKY-ZHACJKMWSA-N chlorohydrin Chemical compound CC#CC#CC#CC#C\C=C\C(Cl)CO XENVCRGQTABGKY-ZHACJKMWSA-N 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000013505 freshwater Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 230000000717 retained effect Effects 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000000737 periodic effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims 1
- 239000002918 waste heat Substances 0.000 claims 1
- 238000007599 discharging Methods 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- 239000007864 aqueous solution Substances 0.000 description 14
- 239000012074 organic phase Substances 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 9
- 238000001256 steam distillation Methods 0.000 description 8
- 238000004042 decolorization Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 2
- 238000004807 desolvation Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
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- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
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- 230000003247 decreasing effect Effects 0.000 description 1
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Abstract
The invention relates to a device for removing organic impurities in brufen sodium salt. The device comprises a filter, a pre-heater and a stripping tower; the filter is arranged at the front end of the pre-heater and communicated with the pre-heater through a filtrate pipeline; the stripping tower is arranged at the rear part of the pre-heater and connected with the pre-heater through the filtrate pipeline; a chromatography apparatus is arranged at the top of the stripping tower; and the interior of the chromatography apparatus is divided into an upper layer and a lower layer. A heating device and a cooling device are arranged in the pre-heater, and the heating device is not intercommunicated with the cooling device. The invention relates to a stripping process flow for removing organic impurities in brufen sodium salt, and a continuous stripping treatment process route for stably removing the organic impurities in the brufen sodium salt is formed.
Description
Technical field
The invention belongs to the separation and purification field of pharmaceutical industry, be specifically related to remove stripping process and the device of organic impurity in the Ibuprofen BP/EP sodium salt.
Background technology
Ibuprofen BP/EP is a kind of non-steroidal anti-inflammatory analgesics thing, has the advantages such as the good and side effect of result for the treatment of is little, is developed rapidly in recent years.At present, developed the synthetic method of multiple Ibuprofen BP/EP, but real industrialized only have epoxy carboxylicesters method and IBPE carbonyl process.In these two kinds of industrial manufacture processes, all relate to the treating process of crude product Ibuprofen BP/EP sodium salt, both at home and abroad generally adopt the method for steam distillation to remove the organism in the Ibuprofen BP/EP sodium salt, then remove foreign pigment with gac, usually generate one waste water in this process.An important indicator weighing waste water is chemical oxygen demand (COD) (COD), and (COD) is larger for chemical oxygen demand (COD), illustrates that water body is subject to organic pollution more serious.
The technical scheme of existing steam distillation is: at first the Ibuprofen BP/EP sodium salt is dissolved in a certain proportion of water and forms the Sodium ibuprofen salt brine solution, then the Sodium ibuprofen salt brine solution is transported in the retort of 10 cubic metres, fresh water steam is passed into to this tank to be heated solution, when in tank, solution reaches 100 ℃, draw steam by tank deck, extraction after the vapor condensation of drawing, become high-COD waste water.The Ibuprofen BP/EP sodium salt that every processing is 1 ton, can access 1500 liters of this waste water, and its COD is 1500mg/L～2500mg/L.Above process continues, after 8～10 hours, to stop passing into water vapor, and the Sodium ibuprofen salt brine solution in tank is purified, and enters subsequent processing and is decoloured.
Utilize the method for steam distillation to remove organic technique in the Ibuprofen BP/EP sodium salt and have at present following problem: be at first that the operational cycle is long, the batch of material distillation time used of processing 800kg is 8 hours, and production efficiency is lower; Next is subject to the impact of foreign matter content fluctuation in charging, and the organism decreasing ratio in the Ibuprofen BP/EP sodium salt is unstable; Again, this technique steam that water COD is high, the water yield is large, cause larger burden to follow-up biochemical treatment.In addition, when the Ibuprofen BP/EP sodium salt dissolves, separate out part alkali mud, easily stop up activated carbon capillary during decolouring, cause activated carbon dosage in the decolorization of the Sodium ibuprofen salt brine solution after steam distillation to increase.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, a kind of stripping process and device that removes organic impurity in the Ibuprofen BP/EP sodium salt proposed, formed the serialization stripping treatment process route of stable except organic impurity in the Ibuprofen BP/EP sodium salt, and the device of realizing above-mentioned technological process is provided.
Technical scheme of the present invention is: a kind of device that removes organic impurity in the Ibuprofen BP/EP sodium salt, comprise strainer, preheater and stripping tower, described strainer is arranged on the front end of preheater, and be connected with preheater by the filtrate pipeline, described stripping tower is arranged on the rear portion of described preheater, by described filtrate pipeline, with described preheater, be connected, tower top at described stripping tower is provided with a chromatography device, be connected with the pipeline of extraction organic liquid on the top of chromatography device, the bottom of chromatography device is connected with stripping tower by the liquid return pipeline.
Described preheater inside is provided with heating unit and cooling unit, and described heating unit is not communicated with mutually with cooling unit.
A kind of stripping process flow process that removes organic impurity in the Ibuprofen BP/EP sodium salt, described flow process be take the Ibuprofen BP/EP sodium salt as main raw material, comprises the following steps:
The first step: the insoluble alkali mud in filtering and removing Sodium ibuprofen salt brine solution
The Ibuprofen BP/EP sodium salt is dissolved in a certain proportion of water and forms the Sodium ibuprofen salt brine solution, be mixed with water-fast material in described Sodium ibuprofen salt brine solution, by strainer, insolubles is retained down, the filter residue periodic cleaning formed, the Sodium ibuprofen salt brine solution after filtration comprises sherwood oil impurity and chloro-hydrin(e) impurity;
Second step: the Sodium ibuprofen salt brine solution is heated
In shell and tube heat exchanger, the Sodium ibuprofen salt brine solution is heated to 60～95 ℃ by normal temperature, the pattern that interchanger is single tube Cheng Dan shell side, filtrate add thermal recovery from the Ibuprofen BP/EP sodium salt cleansing soln of stripping tower as thermal source;
The 3rd step: the stripping tower with the chromatography device removes organic impurity in the Sodium ibuprofen salt brine solution
By the Sodium ibuprofen salt brine solution after the resulting heating of step (2) by pump delivery in stripping tower, pass into fresh water vapor at the bottom of tower, make tower bottom pressure maintain 2kPa～20kPa;
In stripping tower, tower top pressure maintains 0kPa～2kPa, and sherwood oil impurity and chloro-hydrin(e) impurity contained in the Sodium ibuprofen salt brine solution have certain relative volatility, through the multistage vapor-liquid equilibrium in stripping tower, constantly enrichment in gas phase, finally left by tower top with the form of gas; In stripping tower, Sodium ibuprofen salt brine solution and fresh water steam carry out the exchange of heat and quality, and because the Ibuprofen BP/EP sodium salt is non-volatile, so the Ibuprofen BP/EP sodium salt leaves at the bottom of by tower, forms Ibuprofen BP/EP sodium salt cleansing soln;
In stripping tower, after the vapor condensation that tower top rises, in the chromatography device, form upper and lower two-layerly, upper strata organism extraction, recycle in other techniques of Ibuprofen BP/EP as solvent; Lower floor contains organic water and is turned back in stripping tower by tower top, has avoided the generation of the chemical oxygen demand COD waste water of height.
The principle that the present invention realizes is:
Impurity in the Ibuprofen BP/EP sodium salt mainly comprises alkali mud, sherwood oil, chloro-hydrin(e), pigment etc., the present invention is at first water-soluble by the Ibuprofen BP/EP sodium salt, utilize alkali mud different from the physical properties of Sodium ibuprofen salt brine solution, adopt filter operation that alkali mud is filtered out, reach the purpose that reduces activated carbon dosage in follow-up decolorization.For organic impuritys such as the sherwood oil in the Sodium ibuprofen salt brine solution and chloro-hydrin(e)s, traditional processing mode is that water vapor is passed in the Sodium ibuprofen salt brine solution, principle based on Dalton's law (of partial pressures), utilize water vapor that organism is taken out of, according to Raoult's law, the organic content in gas phase is directly proportional to the organic content in the Ibuprofen BP/EP sodium salt simultaneously.From the angle of stream-liquid phase balance, only there is the one-level stream-liquid phase balance in wet distillation process.Organism in the Sodium ibuprofen salt brine solution will be extracted under several ppm, need continuous extraction overhead product, cause the operational cycle of still-process long, the overhead product of the continuous extraction of tower top becomes a large amount of high-COD waste waters simultaneously.The present invention adopts the stripping tower desolvation that can realize multistage stream-liquid phase balance, the Sodium ibuprofen salt brine solution enter into after stripping tower with tower in the steam that rises carry out continuous passage of heat and mass, completed the stream-liquid phase balance of 10～30 grades with water vapor before the Sodium ibuprofen salt brine solution leaves stripping tower, make from the organic content in the aqueous solution of tower Ibuprofen BP/EP sodium salt under 3ppm.After multistage balancing each other, the constantly enrichment in gas phase of organism in stripping tower reaches certain concentration when leaving stripping tower, and mass percent is between 5%～50%, by being divided into organic phase after the overhead condenser condensation and water is two-layer.In order to reduce the growing amount of high-COD waste water, the present invention turns back to the water of tower top chromatography device in the middle of stripping the exchange that re-starts heat and quality, the solvent that the organic phase of tower top can be used as relevant operation in Ibuprofen BP/EP production is used, and has realized the Clean Production Scheme of this workshop section.In order to effectively reduce the consumption of steam in stripping process, the present invention adopts the integrated method of heat to be optimized technological process, adopts the charging of draining preheating stripping tower at the bottom of the stripping tower tower, has reduced the running cost of technique.
The present invention has following beneficial effect:
1) the present invention has improved the removal effect of organic impurity in the Ibuprofen BP/EP sodium salt.While adopting steam distillation to remove in the Ibuprofen BP/EP sodium salt organic impurity, residual in the Ibuprofen BP/EP sodium salt of the organic impuritys such as sherwood oil is 8～20ppm, and residual after processing of the present invention is 0～3ppm.
2) the present invention has improved the stability that removes of organic impurity in the Ibuprofen BP/EP sodium salt.While adopting steam distillation to remove in the Ibuprofen BP/EP sodium salt organic impurity, owing to being batch production, the residual fluctuation of the organic impuritys such as the sherwood oil between each batch in the Ibuprofen BP/EP sodium salt is larger, and the present invention adopts continuous production technology, and treatment effect is stable.
3) the present invention has improved the processing efficiency of Ibuprofen BP/EP sodium salt.While adopting steam distillation to remove in the Ibuprofen BP/EP sodium salt organic impurity, every batch of material is about the aqueous solution of 6 tons of Ibuprofen BP/EP sodium salts, need to process 8 hours, and the present invention adopts continuous production technology, in the situation that floor space is identical, the aqueous solution of processing 6 tons of Ibuprofen BP/EP sodium salts only needs 1 hour.
4) the present invention has reduced the consumption of fresh water steam, has reduced production cost.Filtrate after the pre-heat filtering of high temperature Ibuprofen BP/EP sodium-salt aqueous solution after the present invention adopts stripping at the bottom of tower to purify, improved temperature when filtrate enters stripping tower, the integrated mode of this heat makes stripping tower when processing Sodium ibuprofen salt brine solution per ton, and the live steam consumption is only 20kg～180kg.
5) the present invention has reduced the growing amount of high-COD waste water, has reduced cost for wastewater treatment.The chromatography device of stripping tower tower top of the present invention setting makes organism and waste water carry out layering, and water returns to stripping tower, and outwards the high-COD waste water of discharge is reduced.
6) the present invention has reduced the activated carbon dosage in follow-up decolorization.While adopting steam distillation to remove in the Ibuprofen BP/EP sodium salt organic impurity, the alkali mud that the Ibuprofen BP/EP sodium salt contains can stop up activated carbon capillary, causes activated carbon dosage larger.The present invention, before the Sodium ibuprofen salt brine solution enters stripping tower, uses strainer that alkali mud is held back, and can reduce activated carbon dosage in follow-up decolorization.The Ibuprofen BP/EP sodium salt is after above-mentioned technical process is processed, and the activated carbon dosage in follow-up decolorization is compared with original technique and reduced 5%～30%.
The accompanying drawing explanation
Further illustrate the present invention below in conjunction with the drawings and specific embodiments.
Accompanying drawing is structural representation of the present invention.
In figure, 1. admission port; 2. solution storage unit; 3. strainer; 4. filtrate pipeline; 5. taphole; 6. Sodium ibuprofen salt brine solution unit; 7. preheater; 8. go out material unit at the bottom of the stripping tower tower; 9. stripping tower; 10. the tower top organic phase goes out material unit; 11. alkali mud unit.
Embodiment
Below in conjunction with accompanying drawing, further illustrate, and unrestricted scope involved in the present invention.
Shown in accompanying drawing, at first the present invention is dissolved in the Ibuprofen BP/EP sodium salt in a certain proportion of water, makes the aqueous solution of Ibuprofen BP/EP sodium salt, by admission port 1, enters solution storage unit 2.In strainer 3, mixing insolubles is separated with the Sodium ibuprofen salt brine solution, the insolubles be retained down becomes alkali mud and enters alkali mud unit 11, liquid by filtration unit becomes filtrate and enters in the heating unit of preheater 7 through filtrate pipeline 4, enter stripping tower 9 be heated to certain temperature by normal temperature in the heating unit of preheater 7 after, this heat transfer process goes out material unit 8 at the bottom of utilizing the stripping tower tower, the Sodium ibuprofen salt brine solution that becomes desolvation after the refrigerating unit of preheater 7 is cooling enters Sodium ibuprofen salt brine solution unit 6, then from taphole 5, flow out.Carry out layering after the tower top rising steam of stripping tower 9 is cooling, the tower top organic phase on upper strata enters the tower top organic phase and goes out material unit 10, and the water of lower floor returns to stripping tower 9 and enters stripping flow process again.
Below embodiment of the present invention:
Embodiment 1: the Ibuprofen BP/EP sodium salts of 1000 kilograms are dissolved in the water of 9000 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 10 tons, filter out 30 kilograms, alkali mud.In interchanger, filtrate is heated to 80 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 40 ℃ by 101 ℃.The effective theory plate number of stripping tower is 20, and the stripping tower feed entrance point is the 3rd theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 50 liters.The treatment capacity of stripping tower is 10 tons/hour, and steam consumption is 900 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing is 1ppm.
Embodiment 2: the Ibuprofen BP/EP sodium salts of 1000 kilograms are dissolved in the water of 9000 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 10 tons, filter out 25 kilograms, alkali mud.In interchanger, filtrate is heated to 75 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 45 ℃ by 101 ℃.The effective theory plate number of stripping tower is 15, and the stripping tower feed entrance point is the 2nd theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 70 liters.The treatment capacity of stripping tower is 10 tons/hour, and steam consumption is 1000 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing does not detect, and is less than 1ppm.
Embodiment 3: the Ibuprofen BP/EP sodium salts of 2000 kilograms are dissolved in the water of 16000 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 18 tons, filter out 65 kilograms, alkali mud.In interchanger, filtrate is heated to 80 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 40 ℃ by 101 ℃.The effective theory plate number of stripping tower is 25, and the stripping tower feed entrance point is the 5th theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 120 liters.The treatment capacity of stripping tower is 10 tons/hour, and steam consumption is 850 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing does not detect, and is less than 1ppm.
Embodiment 4: the Ibuprofen BP/EP sodium salts of 2000 kilograms are dissolved in the water of 20000 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 22 tons, filter out 70 kilograms, alkali mud.In interchanger, filtrate is heated to 75 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 45 ℃ by 101 ℃.The effective theory plate number of stripping tower is 10, and the stripping tower feed entrance point is the 2nd theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 80 liters.The treatment capacity of stripping tower is 10 tons/hour, and steam consumption is 1050 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing is 1ppm.
Embodiment 5: the Ibuprofen BP/EP sodium salts of 500 kilograms are dissolved in the water of 4500 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 5 tons, filter out 16 kilograms, alkali mud.In interchanger, filtrate is heated to 80 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 40 ℃ by 101 ℃.The effective theory plate number of stripping tower is 18, and the stripping tower feed entrance point is the 3rd theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 30 liters.The treatment capacity of stripping tower is 5 tons/hour, and steam consumption is 450 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing does not detect, and is less than 1ppm.
Embodiment 6: the Ibuprofen BP/EP sodium salts of 500 kilograms are dissolved in the water of 4000 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 4.5 tons, filter out 18 kilograms, alkali mud.In interchanger, filtrate is heated to 80 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 40 ℃ by 101 ℃.The effective theory plate number of stripping tower is 12, and the stripping tower feed entrance point is the 2nd theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 22 liters.The treatment capacity of stripping tower is 5 tons/hour, and steam consumption is 420 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing is 2ppm.
Embodiment 7: the Ibuprofen BP/EP sodium salts of 4000 kilograms are dissolved in the water of 36000 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 40 tons, filter out 130 kilograms, alkali mud.In interchanger, filtrate is heated to 80 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 40 ℃ by 101 ℃.The effective theory plate number of stripping tower is 30, and the stripping tower feed entrance point is the 6th theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 220 liters.The treatment capacity of stripping tower is 15 tons/hour, and steam consumption is 1300 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing does not detect, and is less than 1ppm.
Embodiment 8: the Ibuprofen BP/EP sodium salts of 4000 kilograms are dissolved in the water of 32000 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 36 tons, filter out 110 kilograms, alkali mud.In interchanger, filtrate is heated to 75 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 45 ℃ by 101 ℃.The effective theory plate number of stripping tower is 15, and the stripping tower feed entrance point is the 3rd theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 190 liters.The treatment capacity of stripping tower is 20 tons/hour, and steam consumption is 1900 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing is 1ppm.
Embodiment 9: the Ibuprofen BP/EP sodium salts of 8000 kilograms are dissolved in the water of 72000 kilograms, make the aqueous solution of the Ibuprofen BP/EP sodium salt of 80 tons, filter out 260 kilograms, alkali mud.In interchanger, filtrate is heated to 80 ℃ by 20 ℃, at the bottom of the stripping tower tower, discharging is cooled to 40 ℃ by 101 ℃.The effective theory plate number of stripping tower is 25, and the stripping tower feed entrance point is the 5th theoretical stage, and the water in tower top chromatography device is returned in stripping tower by tower top, and the volume of the organic phase discharging in tower top chromatography device is 420 liters.The treatment capacity of stripping tower is 20 tons/hour, and steam consumption is 1700 kg/hrs.Organic residue in Ibuprofen BP/EP sodium salt after processing does not detect, and is less than 1ppm.
Claims (7)
1. a device that removes organic impurity in the Ibuprofen BP/EP sodium salt, it is characterized in that: comprise strainer, preheater and stripping tower, described strainer is arranged on the front end of preheater, and be connected with preheater by the filtrate pipeline, described stripping tower is arranged on the rear portion of described preheater, by described filtrate pipeline, with described preheater, be connected, tower top at described stripping tower is provided with a chromatography device, be connected with the pipeline of extraction organic liquid on the top of chromatography device, the bottom of chromatography device is connected with stripping tower by the liquid return pipeline;
Described preheater inside is provided with heating unit and cooling unit, and described heating unit is not communicated with mutually with cooling unit.
2. a stripping process flow process that removes organic impurity in the Ibuprofen BP/EP sodium salt, it is characterized in that: described flow process be take the Ibuprofen BP/EP sodium salt as main raw material, comprises the following steps:
The first step; Insoluble alkali mud in filtering and removing Sodium ibuprofen salt brine solution
The Ibuprofen BP/EP sodium salt is dissolved in a certain proportion of water and forms the Sodium ibuprofen salt brine solution, be mixed with water-fast material in described Sodium ibuprofen salt brine solution, by strainer, insolubles is retained down, the filter residue periodic cleaning formed, the Sodium ibuprofen salt brine solution after filtration comprises sherwood oil impurity and chloro-hydrin(e) impurity;
Second step: the Sodium ibuprofen salt brine solution is heated
In shell and tube heat exchanger, the Sodium ibuprofen salt brine solution is heated to 60～95 ℃ by normal temperature, the pattern that interchanger is single tube Cheng Dan shell side, filtrate add thermal recovery from the Ibuprofen BP/EP sodium salt cleansing soln of stripping tower as thermal source;
The 3rd step: the stripping tower with the chromatography device removes organic impurity in the Sodium ibuprofen salt brine solution
By the Sodium ibuprofen salt brine solution after the resulting heating of step (2) by pump delivery in stripping tower, pass into fresh water vapor at the bottom of tower, make tower bottom pressure maintain 2kPa～20kPa;
In stripping tower, tower top pressure maintains 0kPa～2kPa, and sherwood oil impurity and chloro-hydrin(e) impurity contained in the Sodium ibuprofen salt brine solution have certain relative volatility, through the multistage vapor-liquid equilibrium in stripping tower, constantly enrichment in gas phase, finally left by tower top with the form of gas; In stripping tower, Sodium ibuprofen salt brine solution and fresh water steam carry out the exchange of heat and quality, and because the Ibuprofen BP/EP sodium salt is non-volatile, so the Ibuprofen BP/EP sodium salt leaves at the bottom of by tower, forms Ibuprofen BP/EP sodium salt cleansing soln;
In stripping tower, after the vapor condensation that tower top rises, in the chromatography device, form upper and lower two-layerly, upper strata organism extraction, recycle in other operations of Ibuprofen BP/EP production as solvent; Lower floor contains organic water and is turned back in stripping tower by tower top, has avoided the generation of the chemical oxygen demand COD waste water of height.
3. the stripping process flow process that removes organic impurity in the Ibuprofen BP/EP sodium salt according to claim 2, it is characterized in that: the alkali mud contained in handled Ibuprofen BP/EP sodium salt is water-fast solid, its content in the Ibuprofen BP/EP sodium salt is 1%～10%.
4. the stripping process flow process that removes organic impurity in the Ibuprofen BP/EP sodium salt according to claim 2, it is characterized in that: the organism contained in handled Ibuprofen BP/EP sodium salt is sherwood oil, chloro-hydrin(e) impurity, and its content in the Ibuprofen BP/EP sodium salt is 0.2%～8%.
5. the stripping process flow process that removes organic impurity in the Ibuprofen BP/EP sodium salt according to claim 2, it is characterized in that: before entering stripping tower, the Sodium ibuprofen salt brine solution adopts the waste heat of device to be heated to 60～95 ℃ by normal temperature, without the external heat general facilities.
6. the stripping process flow process that removes organic impurity in the Ibuprofen BP/EP sodium salt according to claim 2, it is characterized in that: process Sodium ibuprofen salt brine solution per ton, the needed live steam of stripping tower is 20kg～180kg.
7. the stripping process flow process that removes organic impurity in the Ibuprofen BP/EP sodium salt according to claim 2 is characterized in that: after this technical process is processed, the organic substance residues in the Ibuprofen BP/EP sodium salt is less than 3ppm.
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| CN104844420B (en) * | 2015-01-21 | 2016-09-07 | 青岛科技大学 | The continuous treatment technique of neopentyl glycol condensation water cleaning mother liquor and device |
| CN104926609B (en) * | 2015-04-13 | 2016-08-03 | 青岛科技大学 | The method of neopentyl glycol mother solution and technological process thereof in a kind for the treatment of cloth ibuprofen synthesis procedure |
| CN105016973B (en) * | 2015-06-03 | 2016-11-23 | 青岛科技大学 | A kind of recovery process containing ethanol in ibuprofen ethyl ester-ethanol mother liquor |
| CN109675342A (en) * | 2018-12-21 | 2019-04-26 | 青岛科技大学 | A kind of continuous production process improves the device and decolouring technology of active carbon decoloring ability |
| CN111807949B (en) * | 2020-07-23 | 2022-02-11 | 青岛科技大学 | Method for recovering ibuprofen sodium salt from ibuprofen sodium salt mother liquor |
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