CN105237441B - A kind of apparatus and method for reclaiming Loprazolam - Google Patents
A kind of apparatus and method for reclaiming Loprazolam Download PDFInfo
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- CN105237441B CN105237441B CN201510731810.9A CN201510731810A CN105237441B CN 105237441 B CN105237441 B CN 105237441B CN 201510731810 A CN201510731810 A CN 201510731810A CN 105237441 B CN105237441 B CN 105237441B
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- loprazolam
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Abstract
The invention provides a kind of apparatus and method for reclaiming Loprazolam.The device includes：Raw material surge tank, scraper plate preheater, scraper evaporator, scraper plate splitter and MSA recovery towers；Raw material surge tank, scraper plate preheater, scraper evaporator are sequentially communicated；The top of scraper evaporator connects with scraper plate splitter；The bottom of scraper evaporator connects with MSA recovery towers；The top of MSA recovery towers is connected with recovery tower condenser, and the two bottom sides of MSA recovery towers are connected with MSA coolers, recovery tower reboiler respectively；MSA recovery towers are connected with raw material surge tank.Present invention also offers the method for the recovery Loprazolam realized using said apparatus.The apparatus and method of the recovery Loprazolam provided using the present invention can effectively remove water and impurity in sour water, recycling Loprazolam efficiently, environmentally friendly.
Description
Technical field
The present invention relates to a kind of device and method for reclaiming Loprazolam, belong to petrochemical industry separation technology field.
Background technology
Loprazolam (MSA) is a kind of colourless or micro- brown oil liquid, is solid under low temperature, and high boiling strong acid melts
20 DEG C of point, 167 DEG C of boiling point (13.33kPa), relative density 1.4812 (18 DEG C) can be released substantial amounts of when being dissolved in water, alcohol and ether
Heat, insoluble in alkane, benzene, toluene etc., does not decompose to boiling water, heat alkali liquid, has strong corrosion to act in metallic iron, copper and lead etc.,
Be medicine and agricultural chemicals raw material, also act as dehydrating agent, paint solidification accelerator, fibre finish, solvent, alkanisation, esterification and
Polymerisation catalysts.
Because MSA is widely used, it is large usage quantity, expensive, so being recycled to MSA very necessary.
In existing MSA recovery technologies, there is many deficiencies, such as U.S. Patent application (US4035242 and
US6531629B1 the MSA more than 99%, Chinese patent application (Application No.) can be obtained using multi-step pressure reduction distillation
200510002684.X and Application No. 200710000080.0) pass sequentially through concentration, vacuum distillation, rectifying and obtain high-purity
MSA.These methods are mainly used in the purification of the MSA for once producing, and raw material is relatively easy, and distillation efficiency is relatively low, and route is more long, energy
Consumption is also higher, especially higher to water content (aqueous 50% or so), but it is not suitable for containing other high-boiling-point impurities
The recovery of useless MSA (MSA after MSA such as is used for into Fu's formula alkylated reaction as catalyst is reclaimed).
The content of the invention
In order to solve the above-mentioned technical problem, can be used to purify the first that production is obtained it is an object of the invention to provide a kind of
Alkyl sulfonic acid can be used for the device and method of the Loprazolam for reclaiming discarded again, the dress of the recovery Loprazolam provided using the present invention
Put back into and receive water and impurity that Loprazolam can be removed effectively in Loprazolam (aqueous solution of MSA), recovery profit efficiently, environmentally friendly
Use Loprazolam.
To achieve these goals, the invention provides a kind of device for reclaiming Loprazolam, the recovery Loprazolam
Device includes：Raw material surge tank, scraper plate preheater, scraper evaporator, scraper plate splitter and MSA recovery towers；
Wherein, the raw material surge tank, scraper plate preheater, scraper evaporator are sequentially communicated；
The top of the scraper evaporator connects with the scraper plate splitter；
The bottom of the scraper evaporator connects with the MSA recovery towers；
The top of the MSA recovery towers connects with recovery tower condenser, the two bottom sides of the MSA recovery towers respectively with
MSA coolers, the connection of recovery tower reboiler；
The MSA recovery towers are connected with the raw material surge tank.
In the device of the recovery Loprazolam that the present invention is provided, top discharge mouthful and the raw material surge tank of MSA recovery towers
Connection, the MSA for reclaiming column overhead residual to MSA is reclaimed.
In the device of the recovery Loprazolam that the present invention is provided, it is preferable that the scraper evaporator is reclaimed with the MSA
Scraper plate cooler is provided between tower.
In the device of the recovery Loprazolam that the present invention is provided, it is preferable that the scraper plate cooler is arranged on described scraping
The bottom of plate evaporator.
In the device of the recovery Loprazolam that the present invention is provided, it is preferable that the top of the scraper plate splitter and scraper plate
First-stage condenser is connected, and the top of the scraper plate first-stage condenser connects with scraper plate secondary condenser.
In the device of the recovery Loprazolam that the present invention is provided, it is preferable that the scraper evaporator includes firing equipment
And separation equipment.
In the device of the recovery Loprazolam that the present invention is provided, scraper evaporator is provided with firing equipment and separation sets
It is standby, for being heated to material and being separated.
The present invention provide recovery Loprazolam device in, it is preferable that the scraper plate splitter include knockout tower and
Two-stage scraper condenser.
The present invention provide recovery Loprazolam device in, the scraper plate splitter be used for material carry out condensation and
Separate.
In the device of the recovery Loprazolam provided in the present invention, scraper evaporator not only can be evenly distributed to liquid
In tower, flowed from top to bottom into uniform films, realize being sufficiently separated for gas-liquid, and can by control scraper plate and evaporation wall away from
From the liquid film that 2mm-5mm is formed with scraper plate speed, the temperature of evaporation wall is reduced, effectively suppressed while greatly improving evaporation efficiency
Loprazolam is rotten caused by high temperature.Scraper plate splitter can efficiently separate the Loprazolam carried secretly in gas phase, realize outer waste discharge
Remained without Loprazolam in water, realized without waste water draining, high-efficiency environment friendly while improving the Loprazolam rate of recovery.
In the device of the recovery Loprazolam that the present invention is provided, it is preferable that the recovery tower condenser is vertical recovery
Tower condenser.
In the device of the recovery Loprazolam that the present invention is provided, it is preferable that the MSA recovery towers are buffered with the raw material
Recovery tower cooler is provided between tank.
Specific embodiment of the invention, the liquid-phase outlet of described scraper evaporator is provided with MSA coolers, and
Connected with the MSA recovery towers.
In the device of the recovery Loprazolam that the present invention is provided, by controlling the raw material into raw material surge tank, regulation is scraped
Plate evaporator, the temperature of scraper plate splitter and MSA recovery towers, pressure, it is possible to achieve once produced to aqueous 10%-60% and obtained
Loprazolam separating-purifying and high-boiling-point impurity content be 5%-20%, the discarded Loprazolam of aqueous 10%-80%
High efficiente callback.And the rate of recovery of Loprazolam is up to more than 95%, aqueous to be less than 0.1%, outer draining pH is 6.5-7.5,
Substantially discharged without waste acid water, efficient and environment-friendly realizes that MSA purifies and discard the recycling of MSA.
A kind of method of the recovery Loprazolam realized present invention also offers device using above-mentioned recovery Loprazolam,
The method is comprised the following steps：
The aqueous solution of Loprazolam by scraper plate preheater preheating after, into scraper evaporator；
Liquid phase material by scraper evaporator enters in MSA recovery towers；
MSA recovery towers are used cooperatively with recovery tower reboiler, and material enters the heated rear partial gasification of MSA recovery towers, are steamed
The recovered tower condenser of tower top that vapour rises to MSA recovery towers is cooled to liquid phase；
MSA recovery tower tower top liquid phases are by recovery tower cooler cooling for reflux to raw material surge tank circulation and stress；
MSA gas phases in MSA recovery towers are cooled down through MSA coolers and recycled, and complete the recovery to Loprazolam.
The method of the recovery Loprazolam that the present invention is provided, it is preferable that the operation temperature of the scraper evaporator is 100
DEG C -120 DEG C, operating pressure is -0.092MPa.
The present invention provide recovery Loprazolam method, it is preferable that the operation temperature of the MSA recovery towers be 150 DEG C-
180 DEG C, operating pressure is -0.092MPa.
The method of the above-mentioned recovery Loprazolam that the present invention is provided, specifically includes following steps：
The aqueous solution of Loprazolam after scraper plate preheater is preheating to 100 DEG C -120 DEG C, from the side of scraper evaporator
Into in scraper evaporator；
By heating and separation, gas-liquid is sufficiently separated material in scraper evaporator, and gas is separated from top into scraper plate
Post is further purified, and waste water is condensed into liquid phase discharge through scraper plate first-stage condenser and scraper plate secondary condenser；
Liquid phase material in scraper evaporator enters in MSA recovery towers by the cooling of scraper plate cooler；
MSA recovery towers are used cooperatively with recovery tower reboiler, and material enters the heated rear partial gasification of MSA recovery towers, are steamed
Vapour rises to the recovered tower condenser of tower top and is cooled to liquid phase；
Liquid phase in MSA recovery towers is by recovery tower cooler cooling for reflux to raw material surge tank circulation and stress；
MSA recovery towers side take-off MSA gas phases are cooled down through MSA coolers and recycled, as the rectifying time is more and more long,
Residue is accumulated in MSA recovery towers, is produced by recovery tower reboiler, completes the recovery to Loprazolam.
The apparatus and method of the recovery Loprazolam that the present invention is provided are that can be used for the Loprazolam that process for producing is obtained, and
Can be used to reclaim discarded Loprazolam.Can realize once producing dividing for the Loprazolam for obtaining for 10%-60% to aqueous
From the high efficiente callback for purifying and high-boiling-point impurity content is 5%-20%, the discarded Loprazolam of aqueous 10%-80%.Methane
Up to more than 95%, aqueous to be less than 0.1%, the pH of outer draining is 6.5-7.5 to the yield of sulfonic acid, is discharged without waste acid water substantially, both
Efficiently and environmental protection realizes Loprazolam purification and discards the recycling of Loprazolam.
The apparatus and method of the Loprazolam of the recovery that the present invention is provided, can effectively remove water in sour water mixture and
Impurity, recycles Loprazolam, reduces the loss of raw material, reduces cost.
Brief description of the drawings
Fig. 1 is the structural representation of the device of the recovery Loprazolam of embodiment 1.
Main Reference symbol description
The scraper plate of 1 raw material surge tank, 2 scraper plate preheater, 3 scraper evaporator, 4 scraper plate splitter, 5 scraper plate first-stage condenser 6
The recovery tower reboiler of 7 10 recovery tower cooler of scraper plate cooler 8MSA 9 recovery tower condensers of recovery tower of secondary condenser 11
12MSA coolers
Specific embodiment
In order to be more clearly understood to technical characteristic of the invention, purpose and beneficial effect, now to skill of the invention
Art scheme carry out it is described further below, but it is not intended that to it is of the invention can practical range restriction.
Embodiment 1
A kind of device for reclaiming Loprazolam is present embodiments provided, the structure of the device is as shown in figure 1, the recovery methane
The device of sulfonic acid includes：Raw material surge tank 1, scraper plate preheater 2, scraper evaporator 3, scraper plate splitter 4 and MSA recovery towers 8；
Wherein, raw material surge tank 1, scraper plate preheater 2, scraper evaporator 3 are sequentially communicated；
Scraper evaporator 3 includes firing equipment and separation equipment, and the top of scraper evaporator 3 connects with scraper plate splitter 4,
The top of scraper plate splitter 4 connects with scraper plate first-stage condenser 5, top and the scraper plate secondary condenser 6 of scraper plate first-stage condenser 5
Connection；
Scraper evaporator 3 is connected with MSA recovery towers 8, and is set between the liquid-phase outlet and MSA recovery towers 8 of scraper evaporator 3
It is equipped with scraper plate cooler 7；
The top of MSA recovery towers 8 connects with vertical recovery tower condenser 9, the two bottom sides of MSA recovery towers 8 respectively with MSA
Cooler 12 is connected with recovery tower reboiler 11；
MSA recovery towers 8 are connected with raw material surge tank 1, and it is cold to be provided with recovery tower between MSA recovery towers 8 and raw material surge tank 1
But device 10, for the recovery of the tower top MSA of MSA recovery towers 8.
The method that the present embodiment additionally provides the recovery Loprazolam realized using the device of above-mentioned recovery Loprazolam, should
Method is comprised the following steps：
The aqueous solution of Loprazolam by raw material surge tank 1 after scraper plate preheater 2 is preheating to 100 DEG C -120 DEG C, from scraping
The side of plate evaporator 3 enters in scraper evaporator 3, and the operation temperature of scraper evaporator 3 is 100 DEG C -120 DEG C, operating pressure
For -0.092MPa；
By heating and separation, gas-liquid is sufficiently separated material in scraper evaporator 3, and gas is separated from top into scraper plate
Post 4, scraper plate first-stage condenser 5 and scraper plate secondary condenser 6, are condensed into liquid phase；
Liquid phase material in scraper evaporator 3 enters in MSA recovery towers 8 by the cooling of scraper plate cooler 7；
MSA recovery towers 8 are used cooperatively with recovery tower reboiler 11, and material enters the heated rear part gas of MSA recovery towers 8
Change, steam rises to the recovered tower condenser 9 of tower top and is cooled to liquid phase, and the operation temperature of MSA recovery towers 8 is 150 DEG C -180 DEG C,
Operating pressure is -0.092MPa；
Liquid phase in MSA recovery towers 8 is by the cooling for reflux of recovery tower cooler 10 to the circulation and stress of raw material surge tank 1；
The side take-off MSA gas phases of MSA recovery towers 8 are cooled down through MSA coolers 12 and recycled, with the rectifying time increasingly
Long, residue accumulation in MSA recovery towers 8 is produced by recovery tower reboiler 11, completes the recovery to Loprazolam.
Separating-purifying is carried out to aqueous 60% Loprazolam for obtaining that once produces using the above method, Loprazolam
Yield is 96%, and the pH of outer draining is 6.5.
The discarded Loprazolam that high-boiling-point impurity content is 20%, aqueous 50%, Loprazolam are reclaimed using the above method
Yield be 95%, outer draining pH be 7.5.
Above example can be seen that the recovery methane sulphur that the device of the recovery Loprazolam provided by the present invention is realized
The method of acid, you can for the Loprazolam that process for producing is obtained, can be used to reclaim discarded Loprazolam again, Loprazolam
The rate of recovery is high, and is discharged without waste acid water substantially, realizes efficient, the environmentally friendly purification and recycling of Loprazolam.
Claims (3)
1. a kind of method for reclaiming Loprazolam, the method comprises the following steps：
The aqueous solution of Loprazolam by scraper plate preheater preheating after, into scraper evaporator；
The liquid phase material processed by scraper evaporator enters in Loprazolam recovery tower；
Loprazolam recovery tower is used cooperatively with recovery tower reboiler, and liquid phase material enters the heated rear portion of Loprazolam recovery tower
Divide gasification, the recovered tower condenser of tower top that gas rises to Loprazolam recovery tower is cooled to liquid phase；
Liquid phase in Loprazolam recovery tower is by recovery tower cooler cooling for reflux to raw material surge tank circulation and stress；
Loprazolam gas phase in Loprazolam recovery tower is cooled down through Loprazolam cooler and recycled, and is completed to Loprazolam
Recovery；
The method of the recovery Loprazolam is completed by the device of following recovery Loprazolam, the device for reclaiming Loprazolam
Including：Raw material surge tank, scraper plate preheater, scraper evaporator, scraper plate splitter and Loprazolam recovery tower；
Wherein, the raw material surge tank, scraper plate preheater, scraper evaporator are sequentially communicated；
The top of the scraper evaporator connects with the scraper plate splitter；
The bottom of the scraper evaporator connects with the Loprazolam recovery tower；
The top of the Loprazolam recovery tower connects with recovery tower condenser, the two bottom sides point of the Loprazolam recovery tower
Do not connected with Loprazolam cooler, recovery tower reboiler；
The Loprazolam recovery tower is connected with the raw material surge tank；
Scraper plate cooler is provided between the scraper evaporator and the Loprazolam recovery tower；The scraper plate cooler is set
In the bottom of the scraper evaporator；
The top of the scraper plate splitter connects with scraper plate first-stage condenser, top and the scraper plate two of the scraper plate first-stage condenser
Level condenser connection；
The scraper evaporator includes firing equipment and separation equipment；
The scraper plate splitter includes knockout tower and two-stage scraper condenser；
The recovery tower condenser is vertical recovery tower condenser；
Recovery tower cooler is provided between the Loprazolam recovery tower and the raw material surge tank.
2. method according to claim 1, wherein, the operation temperature of the scraper evaporator is 100 DEG C -120 DEG C, operation
Pressure is -0.092MPa；The operation temperature of the Loprazolam recovery tower be 150 DEG C -180 DEG C, operating pressure for -
0.092MPa。
3. method according to claim 1, wherein, the method specifically includes following steps：
The aqueous solution of Loprazolam enters after scraper plate preheater is preheating to 100 DEG C -120 DEG C from the side of scraper evaporator
In scraper evaporator；
By heating and separation, gas-liquid is sufficiently separated material in scraper evaporator, and gas enters from top into scraper plate splitter
One step is purified, and waste water is condensed into liquid phase discharge through scraper plate first-stage condenser and scraper plate secondary condenser；
Liquid phase material in scraper evaporator enters in Loprazolam recovery tower by the cooling of scraper plate cooler；
Loprazolam recovery tower is used cooperatively with recovery tower reboiler, and material enters the heated rear part gas of Loprazolam recovery tower
Change, steam rises to the recovered tower condenser of tower top and is cooled to liquid phase；
Liquid phase in Loprazolam recovery tower is by recovery tower cooler cooling for reflux to raw material surge tank circulation and stress；
Loprazolam recovery tower side take-off Loprazolam gas phase is cooled down through Loprazolam cooler and recycled, during with rectifying
Between it is more and more long, residue is accumulated in Loprazolam recovery tower, is produced by recovery tower reboiler, completion Loprazolam is returned
Receive.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510731810.9A CN105237441B (en) | 2015-11-02 | 2015-11-02 | A kind of apparatus and method for reclaiming Loprazolam |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510731810.9A CN105237441B (en) | 2015-11-02 | 2015-11-02 | A kind of apparatus and method for reclaiming Loprazolam |
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| CN105237441B true CN105237441B (en) | 2017-06-13 |
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ID=55035314
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| CN201510731810.9A Active CN105237441B (en) | 2015-11-02 | 2015-11-02 | A kind of apparatus and method for reclaiming Loprazolam |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MY191907A (en) * | 2017-05-11 | 2022-07-18 | Arkema Inc | Processes and systems for recovering methanesulfonic acid in purified form |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4035242A (en) * | 1975-09-29 | 1977-07-12 | Ppg Industries, Inc. | Distillative purification of alkane sulfonic acids |
| US4450047A (en) * | 1983-01-28 | 1984-05-22 | Penwalt Corporation | Process for recovering anhydrous alkanesulfonic acids by reduced pressure, falling film evaporation |
| US5589691A (en) * | 1994-06-06 | 1996-12-31 | Merck & Co., Inc. | Process for recovery and recycle of methanesulfonic acid and phosphorous acid |
| CN100348579C (en) * | 2005-01-26 | 2007-11-14 | 河北亚诺化工有限公司 | Methylsulfonic acid preparing process |
| CN101219975B (en) * | 2007-01-10 | 2010-07-21 | 河北亚诺化工有限公司 | Process for producing methanesulfonic acid |
| CN101698653B (en) * | 2009-10-30 | 2013-09-04 | 衢州中科精细化学有限公司 | Process for preparing high-purity methylsulfonic acid |
| CN103073458B (en) * | 2013-01-10 | 2014-11-19 | 广州智特奇生物科技股份有限公司 | Method for recovering trifluoromethanesulfonic acid in wastewater |
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