CN105461667A - Treatment method and system for recycling tetrahydrofuran in solution discharged in parecoxib normal-phase workshop section - Google Patents
Treatment method and system for recycling tetrahydrofuran in solution discharged in parecoxib normal-phase workshop section Download PDFInfo
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- CN105461667A CN105461667A CN201610011629.5A CN201610011629A CN105461667A CN 105461667 A CN105461667 A CN 105461667A CN 201610011629 A CN201610011629 A CN 201610011629A CN 105461667 A CN105461667 A CN 105461667A
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- tetrahydrofuran
- liquid
- thf
- membrane separation
- separation unit
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/04—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D307/06—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D307/08—Preparation of tetrahydrofuran
Abstract
The invention discloses a treatment method and system for recycling tetrahydrofuran in a solution discharged in a parecoxib normal-phase workshop section. The treatment system comprises a waste liquid storage tank, a lifting pump, a membrane separation device, a condensation recycling device, a tetrahydrofuran collection tank and a vacuum pump device. The waste liquid storage tank is connected with the lifting pump, the lifting pump is connected with a liquid inlet of the membrane separation device through a pipeline, a liquid outlet of the membrane separation device is connected with the waste liquid storage tank, a gas outlet of the membrane separation device is connected with the condensation recycling device, a liquid outlet of the condensation recycling device is connected with the tetrahydrofuran collection tank, a gas outlet of the condensation recycling device is connected with the vacuum pump device, and the vacuum pump device is connected with the membrane separation device. Compared with the traditional art, the treatment way of recycling tetrahydrofuran in the solution discharged in the parecoxib normal-phase workshop section is charged, secondary pollution is avoided, no distillation still residual liquid is produced, the purity of separated-out tetrahydrofuran is high, the tetrahydrofuran is directly reused in a front end production process, the whole process is carried out at the temperature smaller than 70 DEG C, a product in the solution will not be damaged, and the running cost is low.
Description
Technical field
The present invention relates to a kind of sewage treatment process and equipment thereof, be specifically related to treatment process and system thereof that a kind of Parecoxib positive workshop section discharge solution reclaims tetrahydrofuran (THF).
Background technology
Parecoxib is a kind of COX-2 (COX-2) specific inhibitor.Belong to the former times dry goods anodyne in anti-arthritic.
The synthesis of Parecoxib medicine comprises: centrifugal workshop section, positive workshop section, anti-phase workshop section.In positive workshop section, the filtrate after reaction terminates is the production waste liquid containing high density tetrahydrofuran (THF) and ethyl acetate.Waste liquid component comprises: tetrahydrofuran (THF) 88.00% (W/W), ethyl acetate 11.00% (W/W), by product 1.00% (W/W), other material trace.The conventional processing mode of this type of waste liquid is rectification under vacuum recovery tetrahydrofuran (THF), but due to ethyl acetate can volatilize for organic gas with tetrahydrofuran (THF) in still-process simultaneously, inorganic thorough separation.Each distillation all has the tetrahydrofuran (THF) of more than 5.0% to enter air with waste gas form, produces the vinasse of about 1.0% simultaneously, and this raffinate can only be used as hazardous substance refuse to process.Meanwhile, tetrahydrofuran (THF), as a kind of chemical industry organic solvent, in the difficult degradation of occurring in nature pole, has stronger restraining effect to the microorganism in Sewage treatment systems simultaneously, belongs to hardly degraded organic substance.
Therefore, a series of improvement has been carried out in order to solve the problem.
Summary of the invention
The object of the invention is to, the treatment process providing a kind of Parecoxib positive workshop section to discharge solution recovery tetrahydrofuran (THF) and system thereof, to overcome the above-mentioned shortcoming and defect existing for prior art.
A kind of Parecoxib positive workshop section discharge solution reclaims treatment process and the system thereof of tetrahydrofuran (THF), it is characterized in that, equipment comprises: waste liquor storage tank, lift pump, membrane separation unit, condensate recycling device, tetrahydrofuran (THF) holding tank and vacuum pump apparatus, described waste liquor storage tank is connected with lift pump, described lift pump is connected with the liquid inlet of membrane separation unit by pipeline, the liquid exit of described membrane separation unit is connected with waste liquor storage tank, the pneumatic outlet of described membrane separation unit is connected with condensate recycling device, the liquid exit of described condensate recycling device is connected with tetrahydrofuran (THF) holding tank, the pneumatic outlet of described condensate recycling device is connected with vacuum pump apparatus, described vacuum pump apparatus is connected with membrane separation unit,
Wherein, described waste liquor storage tank comprises: tank body and heating unit, described tank body and heating unit, described tank body is connected with heating unit, collect the waste liquid had containing high density tetrahydrofuran (THF) in tank body, then heated by heating unit, be heated to heat to 70 DEG C;
Described lift pump is recycle pump, and waste liquid, after being heated to 70 DEG C, being sent into membrane separation unit through lift pump and circulated;
Described membrane separation unit comprises: liquid circulation inlet side, liquid circulation portion, liquid circulation outlet side, gas circulation inlet side, gas circulation portion and gas loop exit side, described liquid circulation inlet side is connected with lift pump, waste liquid is made to enter liquid circulation portion, described liquid circulation outlet side is connected with waste liquor storage tank, described liquid circulation portion is communicated with gas circulation portion, waste liquid infiltrates gas circulation portion by liquid circulation portion, described gas circulation inlet side is connected with vacuum pump apparatus, described gas circulation outlet side is connected with condensate recycling device, in this operation, waste liquid opens vacuum pump apparatus while circulation, tetrahydrofuran (THF) in waste liquid is by the liquid impervious of membrane separation unit, together be pulled away with intake-gas, thus reach the object of separation of tetrahydrofuran.
Described condensate recycling device comprises: condensing works and unit cooler, the liquid outlet of described condensing works is connected with tetrahydrofuran (THF) holding tank, the air outlet of described condensing works is connected with unit cooler and vacuum pump apparatus, the inlet mouth of described condensing works is connected with unit cooler and membrane separation unit, in whole condensation removal process, by adding the aqueous glycol solution refrigerant of-5 DEG C, the tetrahydrofuran (THF) in mixed gas is made directly to be condensed into liquid, enter in tetrahydrofuran (THF) holding tank by the liquid outlet of condensing works, recovery is in production process.Remain the gas containing a small amount of tetrahydrofuran (THF) enters membrane separation unit again gas circulation inlet side through vacuum pump apparatus.
Further, described membrane separation unit adopts composite silicone rubber membrane, its separation principle is intermolecular penetration principle, but not work principle of filter, therefore can not cause the blocking of film, and composite silicone rubber membrane has the high elastic coefficient of quality of rubber materials due to it, when concentration polarization or fouling appear in membrane module surface, by means of only rinsing at a high speed the cleaning that can realize film, do not need special chemical.
Further, the swabbing pressure in described gas circulation portion controls at-0.003 ~-0.005MPa.
Further, the flow-ratio control in described liquid circulation portion and gas circulation portion is at 1:200 ~ 1:300.
Further, the solution in described liquid circulation portion crosses Flow Velocity is 4 ~ 6m/s.
Further, in whole technique, the temperature of waste water controls at 60 ~ 65 DEG C.
Beneficial effect of the present invention:
The present invention, compared with conventional art, changes the processing mode of the tetrahydrofuran (THF) recovery of Parecoxib positive workshop section waste liquid; Non-secondary pollution, produces without still kettle raffinate, and after being separated, tetrahydrofuran (THF) purity is high, and direct reuse is to front end production process; Whole process is carried out being less than at the temperature of 70 DEG C, can not damage the product in solution; Running cost is low.
Accompanying drawing explanation
Fig. 1 is structure iron of the present invention.
Reference numeral:
Waste liquor storage tank 100, tank body 110 and heating unit 120.
Lift pump 200, membrane separation unit 300, liquid circulation inlet side 310, liquid circulation portion 320, liquid circulation outlet side 330, gas circulation inlet side 340, gas circulation portion 350 and gas loop exit side 360.
Condensate recycling device 400, condensing works 410, liquid outlet 411, air outlet 412, inlet mouth 413 and unit cooler 420.
Tetrahydrofuran (THF) holding tank 500 and vacuum pump apparatus 600.
Embodiment
Below in conjunction with specific embodiment, progressive explanation is done to the present invention.Should be understood that following examples only for illustration of the present invention but not for limiting scope of the present invention.
Embodiment 1
Fig. 1 is structure iron of the present invention.
As shown in Figure 1, the equipment that a kind of Parecoxib positive workshop section discharge solution reclaims tetrahydrofuran (THF) comprises: waste liquor storage tank 100, lift pump 200, membrane separation unit 300, condensate recycling device 400, tetrahydrofuran (THF) holding tank 500 and vacuum pump apparatus 600, waste liquor storage tank 100 is connected with lift pump 200, lift pump 200 is connected by the liquid inlet of pipeline with membrane separation unit 300, the liquid exit of membrane separation unit 300 is connected with waste liquor storage tank 100, the pneumatic outlet of membrane separation unit 300 is connected with condensate recycling device 400, the liquid exit of condensate recycling device 400 is connected with tetrahydrofuran (THF) holding tank 500, the pneumatic outlet of condensate recycling device 400 is connected with vacuum pump apparatus 600, vacuum pump apparatus 600 is connected with membrane separation unit 300.
Wherein, waste liquor storage tank 100 comprises: tank body 110 and heating unit 120, tank body 110 and heating unit 120, tank body 110 is connected with heating unit 120, collect the waste liquid had containing high density tetrahydrofuran (THF) in tank body 110, then heated by heating unit 120, be heated to heat to 70 DEG C.
Lift pump 200 is recycle pump, and waste liquid, after being heated to 70 DEG C, being sent into membrane separation unit 300 through lift pump 200 and circulated.
Membrane separation unit 300 comprises: liquid circulation inlet side 310, liquid circulation portion 320, liquid circulation outlet side 330, gas circulation inlet side 340, gas circulation portion 350 and gas loop exit side 360, liquid circulation inlet side 310 is connected with lift pump 200, waste liquid is made to enter liquid circulation portion 320, liquid circulation outlet side 330 is connected with waste liquor storage tank 100, liquid circulation portion 320 is communicated with gas circulation portion 350, waste liquid infiltrates gas circulation portion 350 by liquid circulation portion 320, gas circulation inlet side 340 is connected with vacuum pump apparatus 600, gas circulation outlet side 360 is connected with condensate recycling device 400, in this operation, waste liquid opens vacuum pump apparatus 600 while circulation, tetrahydrofuran (THF) in waste liquid is by the liquid impervious of membrane separation unit 300, together be pulled away with intake-gas, thus reach the object of separation of tetrahydrofuran.
Condensate recycling device 400 comprises: condensing works 410 and unit cooler 420, the liquid outlet 411 of condensing works 410 is connected with tetrahydrofuran (THF) holding tank 500, the air outlet 412 of condensing works 410 is connected with unit cooler 420 and vacuum pump apparatus 600, the inlet mouth 413 of condensing works 410 is connected with unit cooler 420 and membrane separation unit 300, in whole condensation removal process, by adding the aqueous glycol solution refrigerant of-5 DEG C, the tetrahydrofuran (THF) in mixed gas is made directly to be condensed into liquid, enter in tetrahydrofuran (THF) holding tank 500 by the liquid outlet 411 of condensing works 410, recovery is in production process.Remain the gas containing a small amount of tetrahydrofuran (THF) enters membrane separation unit 300 again gas circulation inlet side 340 through vacuum pump apparatus 600.
Membrane separation unit 300 adopts composite silicone rubber membrane, its separation principle is intermolecular penetration principle, but not work principle of filter, therefore the blocking of film can not be caused, and composite silicone rubber membrane has the high elastic coefficient of quality of rubber materials due to it, when concentration polarization or fouling appear in membrane module surface, by means of only rinsing at a high speed the cleaning that can realize film, do not need special chemical.
The swabbing pressure in gas circulation portion 350 controls at-0.003 ~-0.005MPa.
The flow-ratio control in liquid circulation portion 320 and gas circulation portion 350 is at 1:200 ~ 1:300.
It is 4 ~ 6m/s that the solution in liquid circulation portion 320 crosses Flow Velocity.
In whole technique, the temperature of waste water controls at 60 ~ 65 DEG C.
Parecoxib positive workshop section waste liquid: day quantity discharged be about 0.1 ton, waste liquid component comprises: tetrahydrofuran (THF) 88.00% (W/W), ethyl acetate 11.00% (W/W), by product 1.00% (W/W), other material trace.
Equipment in the present embodiment specifically comprises: 0.2m
3volume waste liquor storage tank 1, circulation lift pump 200 two, silicone rubber membrane tripping device 300 are a set of, 2 ㎡ condensate recycling device 400 1, Vacuum suction pump one, and refrigerant selects the enough supplies of plant area's chilled brine.
Treatment process:
Separation waste liquid is pumped into the liquid circulation portion 320 of silicone rubber membrane tripping device 300 by lift pump 200, open condensate recycling device 400 and vacuum pump apparatus 600 simultaneously.
Adjustment gas circulation portion 350 swabbing pressure controls the operating pressure at-0.004MPa;
Control the import refrigerant temperature of solidifying retrieving arrangement 400 at-5 DEG C, and keep steady temperature;
Rearrange liquids circulation portions 320 and gas circulation portion 350 flow, make liquid circulation portion 320 and gas circulation portion 350 flow-ratio control at 1:300.In membrane separation unit 300, the solution overcurrent speed control in liquid circulation portion 320 is in 6m/s scope.
Tetrahydrofuran (THF) in waste liquid is under the effect of osmotic pressure, shifted to gas circulation portion 350 from liquid circulation portion 320 by membranous wall, and taken away by recirculated air, and larger molecular organics is all trapped within liquid circulation portion 320, thus realizes being separated of tetrahydrofuran (THF) and waste liquid.
Above-mentioned Parecoxib positive workshop section liquid waste treatment system is used to coordinate Parecoxib positive workshop section of aforesaid method process drugmaker waste liquid.Find within cycle of operation of 60 days altogether, after being separated, tetrahydrofuran (THF) is substantially gone up and can be realized reclaiming completely, and non-volatile waste, produces without vinasse.Many recovery every day tetrahydrofuran (THF) about 0.08 ton.In whole treatment cycle, membrane module is without considerable change.
Be illustrated the specific embodiment of the present invention above, but the present invention is not as limit, only otherwise depart from aim of the present invention, the present invention can also have various change.
Claims (6)
1. treatment process and the system thereof that solution reclaims tetrahydrofuran (THF) is discharged by a Parecoxib positive workshop section, it is characterized in that, equipment comprises: waste liquor storage tank (100), lift pump (200), membrane separation unit (300), condensate recycling device (400), tetrahydrofuran (THF) holding tank (500) and vacuum pump apparatus (600), described waste liquor storage tank (100) is connected with lift pump (200), described lift pump (200) is connected by the liquid inlet of pipeline with membrane separation unit (300), the liquid exit of described membrane separation unit (300) is connected with waste liquor storage tank (100), the pneumatic outlet of described membrane separation unit (300) is connected with condensate recycling device (400), the liquid exit of described condensate recycling device (400) is connected with tetrahydrofuran (THF) holding tank (500), the pneumatic outlet of described condensate recycling device (400) is connected with vacuum pump apparatus (600), described vacuum pump apparatus (600) is connected with membrane separation unit (300),
Wherein, described waste liquor storage tank (100) comprising: tank body (110) and heating unit (120), described tank body (110) and heating unit (120), described tank body (110) is connected with heating unit (120), the waste liquid had containing high density tetrahydrofuran (THF) is collected in tank body (110), then heated by heating unit (120), be heated to heat to 70 DEG C;
Described lift pump (200) is recycle pump, and waste liquid, after being heated to 70 DEG C, being sent into membrane separation unit (300) through lift pump (200) and circulated;
Described membrane separation unit (300) comprising: liquid circulation inlet side (310), liquid circulation portion (320), liquid circulation outlet side (330), gas circulation inlet side (340), gas circulation portion (350) and gas loop exit side (360), described liquid circulation inlet side (310) is connected with lift pump (200), waste liquid is made to enter liquid circulation portion (320), described liquid circulation outlet side (330) is connected with waste liquor storage tank (100), described liquid circulation portion (320) is communicated with gas circulation portion (350), (waste liquid infiltrates gas circulation portion (350) by liquid circulation portion (320), described gas circulation inlet side (340) is connected with vacuum pump apparatus (600), described gas circulation outlet side (360) is connected with condensate recycling device (400), in this operation, waste liquid opens vacuum pump apparatus (600) while circulation, tetrahydrofuran (THF) in waste liquid is by the liquid impervious of membrane separation unit (300), together be pulled away with intake-gas, thus reach the object of separation of tetrahydrofuran.
Described condensate recycling device (400) comprising: condensing works (410) and unit cooler (420), the liquid outlet (411) of described condensing works (410) is connected with tetrahydrofuran (THF) holding tank (500), the air outlet (412) of described condensing works (410) is connected with unit cooler (420) and vacuum pump apparatus (600), the inlet mouth (413) of described condensing works (410) is connected with unit cooler (420) and membrane separation unit (300), in whole condensation removal process, by adding the aqueous glycol solution refrigerant of-5 DEG C, the tetrahydrofuran (THF) in mixed gas is made directly to be condensed into liquid, enter in tetrahydrofuran (THF) holding tank (500) by the liquid outlet (411) of condensing works (410), recovery is in production process.Remain the gas containing a small amount of tetrahydrofuran (THF) enters membrane separation unit (300) again gas circulation inlet side (340) through vacuum pump apparatus (600).
2. a kind of Parecoxib positive workshop section according to claim 1 discharge solution reclaims the treatment system of tetrahydrofuran (THF), it is characterized in that: described membrane separation unit (300) adopts composite silicone rubber membrane, its separation principle is intermolecular penetration principle, but not work principle of filter, therefore the blocking of film can not be caused, and composite silicone rubber membrane has the high elastic coefficient of quality of rubber materials due to it, when there is concentration polarization or fouling in membrane module surface, by means of only rinsing at a high speed the cleaning that can realize film, do not need special chemical.
3. a kind of Parecoxib positive workshop section according to claim 1 discharge solution reclaims the treatment process of tetrahydrofuran (THF), it is characterized in that: the swabbing pressure of described gas circulation portion (350) controls at-0.003 ~-0.005MPa.
4. a kind of Parecoxib positive workshop section according to claim 1 discharge solution reclaims the treatment process of tetrahydrofuran (THF), it is characterized in that: the flow-ratio control in described liquid circulation portion (320) and gas circulation portion (350) is at 1:200 ~ 1:300.
5. a kind of Parecoxib positive workshop section according to claim 1 discharge solution reclaims the treatment process of tetrahydrofuran (THF), it is characterized in that: it is 4 ~ 6m/s that the solution of described liquid circulation portion (320) crosses Flow Velocity.
6. a kind of Parecoxib positive workshop section according to claim 1 discharge solution reclaims the treatment process of tetrahydrofuran (THF), and it is characterized in that: in whole technique, the temperature of waste water controls at 60 ~ 65 DEG C.
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| CN201610011629.5A CN105461667A (en) | 2016-01-08 | 2016-01-08 | Treatment method and system for recycling tetrahydrofuran in solution discharged in parecoxib normal-phase workshop section |
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| CN201610011629.5A CN105461667A (en) | 2016-01-08 | 2016-01-08 | Treatment method and system for recycling tetrahydrofuran in solution discharged in parecoxib normal-phase workshop section |
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| CN102206197A (en) * | 2011-03-31 | 2011-10-05 | 天津大学 | Intermediate storage tank-carrying batch distillation and pervaporation coupling method for separating tetrahydrofuran from water and device thereof |
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| CN103408514A (en) * | 2013-08-20 | 2013-11-27 | 江苏九天高科技股份有限公司 | Technique and device for recovering tetrahydrofuran by pervaporation method |
| CN203829926U (en) * | 2014-04-12 | 2014-09-17 | 宁波信远膜工业股份有限公司 | On-line type organic solvent dehydration device |
-
2016
- 2016-01-08 CN CN201610011629.5A patent/CN105461667A/en active Pending
Patent Citations (6)
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| US5559254A (en) * | 1992-11-21 | 1996-09-24 | Basf Aktiengesellschaft | Separation of a mixture of methanol and tetrahydrofuran into its constituents |
| CN101249311A (en) * | 2008-03-20 | 2008-08-27 | 烟台只楚天大化工填料厂 | Coupled barrier separation rectification technique |
| CN102206197A (en) * | 2011-03-31 | 2011-10-05 | 天津大学 | Intermediate storage tank-carrying batch distillation and pervaporation coupling method for separating tetrahydrofuran from water and device thereof |
| CN103193923A (en) * | 2012-01-10 | 2013-07-10 | 苏州国家环保高新技术产业园发展有限公司 | Preparation method and application of pervaporation separation material based on polyacrylate resin |
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