CN103214361B - Method for regenerative cycle and utilization of iodine-containing methanol under low load - Google Patents
Method for regenerative cycle and utilization of iodine-containing methanol under low load Download PDFInfo
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- CN103214361B CN103214361B CN201310156177.6A CN201310156177A CN103214361B CN 103214361 B CN103214361 B CN 103214361B CN 201310156177 A CN201310156177 A CN 201310156177A CN 103214361 B CN103214361 B CN 103214361B
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Abstract
The invention discloses a method for regenerative cycle and utilization of iodine-containing methanol under a low load. The method comprises the steps of: (1) when stopping work or when the inventory of methanol is lower than 40wt%, absorbing iodine-containing methanol in a methanol storage tank and feeding the iodine-containing methanol into a regeneration tower, cooling bottom effluent of the regeneration tower through a barren liquor cooler and feeding the bottom effluent into a methanol barren liquor tank, and respectively feeding a liquid in the methanol barren liquor tank, partially or completely replacing fresh methanol, into a high-pressure absorption tower and a low-pressure absorption tower; and simultaneously, condensing a top extract of the regeneration tower through a regeneration tower condenser and feeding the top extract into an absorption methanol storage tank through a pipeline when iodomethane in the absorption methanol storage tank is lower than 6wt%; and (2) when the inventory of the methanol is lower than 40%, using the fresh methanol to completely replace barren liquor methanol discharged out of the methanol barren liquor tank, and stopping the regeneration tower; and pressing towards the interior of the storage tank, so as to press all spare liquid in the storage tank into the absorption methanol storage tank. The method improves the layering situation of a layering device when starting once again, and the operating flexibility of the regeneration tower is enhanced.
Description
Technical field
The present invention relates to under low load condition after acetic acid production emergency shutdown and before feeding intake, containing iodine Mathanol regenerating circulation utilization method.
Background technology
Produce at methyl alcohol carbonyl synthetic in the technique of acetic acid, under rhodium/iodine catalyst system, methyl iodide is as promotor, and its concentration plays an important role to speed of reaction.In the high pressure exhaust gas of synthesis procedure and the low-pressure tail gas of rectification working process, all contain methyl iodide, adopt and absorb with methyl alcohol in high-pressure absorber and low-pressure absorption tower, after absorption containing iodine methyl alcohol as reaction raw materials, directly return synthesis system recycle.When normal production operation, iodine Mathanol regenerating supervisor need not be contained.
Drive initial stage and start-stop car frequently time, system still has emptying end gas, but synthesis procedure can not digest and assimilate that tower produces in time containing iodine methyl alcohol, cause containing iodine methyl alcohol too much, regenerated containing iodine methyl alcohol by regenerator column.Be illustrated in figure 1 existing methyl iodide and absorb process flow chart, the absorption methyl alcohol absorbed during normal production in methyl alcohol basin 6 directly sends into reactor by absorbing methanol feed pump 7, reactor cannot complete digestion time, send in the middle part of regenerator column 1, heat through regenerator column reboiler 2, vaporize, tower reactor obtains the higher methyl alcohol of purity, enter methyl alcohol lean solution tank 9 after being cooled by lean solution water cooler 8, then deliver to high-pressure absorber 4 respectively by lean solution methyl alcohol take away pump 10 and low-pressure absorption tower 5 (simultaneously directly having fresh methanol to send into) recycles; Regenerator column overhead vapours is after regenerator column condenser 3 condensation, and obtain the mixture of the azeotropic composition close to methyl iodide and methyl alcohol, a part is back to regenerator column top, and the quantizer 14 of lightness-removing column 11 delivered to by the pipeline of a part through being equipped with middle control regulation valve 17.The non-condensable gas of regenerator column condenser and a small amount of methyl iodide, methyl alcohol, enter low-pressure absorption tower 5.Synthesis procedure material heats through the lightness-removing column reboiler 12 of lightness-removing column 11, by the light constituent such as methyl iodide, water in the thick acetic acid in lightness-removing column 11 by condenser of light component removal column 13 condensation, liquid enters quantizer 14, and gas cools laggard low-pressure absorption tower 5 through whole cooler 16.Quantizer 14 lower liquid (being mainly methyl iodide, hereinafter referred to as heavy phase) turns back to reactor by heavy phase pump 15, ensures the equilibrium iodine of system.
Because methyl alcohol and methyl iodide can form azeotrope, regenerator column tower top liquid phase production enters in the material of quantizer, necessarily have part methyl alcohol and enter quantizer together with methyl iodide, generate ritalin, cause heavy phase density to decline, to such an extent as to not stratified, again go into operation after feeding intake, heavy phase cannot return reactor, and system cannot realize iodine circulation, makes to feed intake unsuccessfully.Especially, when absorption system total methyl iodide content is less, in Produced Liquid, methyl alcohol meeting content is higher.If but the long-term not extraction of tower top liquid phase, for ensureing that in lean solution methyl alcohol, methyl iodide content is lower, regenerator column operation easier can be made very big, steam consumption continues to increase, and after steam heating ability reaches capacity, methyl iodide cannot distillate completely, cause the lean solution methyl alcohol boiled again at the bottom of tower tower containing iodine, after lean solution methyl alcohol sends into high-pressure absorber, low-pressure absorption tower, make to contain methyl iodide in high-pressure absorber, low-pressure absorption tower tower top emptying gas, cause environmental protection accident.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, before arriving total system production cycle again after stopping work under a kind of different operating mode is provided, when system still has an emptying end gas, be beneficial to operation, do not affect quantizer layered effect and heavy phase proportion, reduce regenerator column steam consumption and operation easier simultaneously, avoid a kind of underload of environmental pollution under containing iodine Mathanol regenerating circulation utilization method.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Containing iodine Mathanol regenerating circulation utilization method under a kind of underload of the present invention, it comprises the following steps:
(1) stop work or with the charging capacity of mass ratio range methyl alcohol lower than less than 40% time, the iodine methyl alcohol that contains absorbed in methyl alcohol basin is sent in the middle part of regenerator column by absorbing methyl alcohol take away pump, regenerator column tower bottom flow fluid enters methyl alcohol lean solution tank after the cooling of lean solution water cooler, and the liquid in methyl alcohol lean solution tank partially or completely substitutes fresh methanol through lean solution methyl alcohol take away pump and sends into high-pressure absorber and low-pressure absorption tower respectively; Simultaneously when absorb the methyl iodide weight percentage in methyl alcohol basin lower than 6% time, the overhead extraction thing of regenerator column is sent into by pipeline and is absorbed methyl alcohol basin after regenerator column condenser condenses; When absorbing the methyl iodide weight percentage in methyl alcohol basin and being not less than 6%, the overhead extraction thing of regenerator column is for subsequent use by pipeline feeding basin after condenser condenses, after for some time, when to absorb in methyl alcohol basin methyl iodide weight percentage lower than 6% time, the overhead extraction thing of regenerator column is sent into by pipeline again and is absorbed methyl alcohol basin after condenser condenses;
(2) when the charging capacity of methyl alcohol is not less than 40%, fresh methanol substitutes the lean solution methyl alcohol that methyl alcohol lean solution tank is sent completely, and regenerator column is stopped using; Then to punching press in basin, liquid for subsequent use in basin is all depressed into and absorbs methyl alcohol basin, making the reserve liquid in basin return synthesis system with the iodine methyl alcohol that contains absorbed in methyl alcohol basin by absorbing methyl alcohol take away pump, after hydraulic fluid completes, the gas emptying in basin being entered low-pressure absorption tower;
Described produces in the technique of acetic acid from methyl alcohol carbonyl synthetic containing iodine methyl alcohol.
The invention has the beneficial effects as follows:
The methyl iodide avoiding regenerator column condenser liquid phase to obtain and carbinol mixture enter quantizer, reduce methyl alcohol and acetic acid reaction in quantizer and generate ritalin, improve again point layer status of driving layered device.The turndown ratio reducing regenerator column is larger, can adapt to the demand after the shut-down of various operating mode, reduce its steam consumption.
Accompanying drawing explanation
Fig. 1 is that the absorption system of prior art reclaims methyl iodide and contains iodine Mathanol regenerating schema;
Fig. 2 is the schematic flow sheet containing iodine Mathanol regenerating circulation utilization method under a kind of underload of the present invention.
Wherein:
1-regenerator column 2-regenerator column reboiler 3-regenerator column condenser 4-high-pressure absorber 5-low-pressure absorption tower 6-absorbs methyl alcohol basin 7-and absorbs control regulation valve 18-basin 19-first ball valve 20-second ball valve in the whole cooler 17-of methyl alcohol take away pump 8-lean solution water cooler 9-methyl alcohol lean solution tank 10-lean solution methyl alcohol take away pump 11-lightness-removing column 12-lightness-removing column reboiler 13-lightness-removing column primary cooler 14-quantizer 15-heavy phase pump 16-
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
The inventive method is the improvement on the existing method basis shown in Fig. 1.
As shown in Figure 2, containing iodine Mathanol regenerating circulation utilization method under a kind of underload of the present invention, it comprises the following steps: (1) stop work or with the charging capacity of mass ratio range methyl alcohol lower than less than 40% time, the iodine methyl alcohol that contains absorbed in methyl alcohol basin 6 is sent in the middle part of regenerator column 1 by absorbing methyl alcohol take away pump 7, regenerator column tower bottom flow fluid enters methyl alcohol lean solution tank 9 after lean solution water cooler 8 cools, and the liquid in methyl alcohol lean solution tank 9 partially or completely substitutes fresh methanol through lean solution methyl alcohol take away pump and sends into high-pressure absorber 4 and low-pressure absorption tower 5 respectively; Simultaneously when absorb the methyl iodide weight percentage in methyl alcohol basin 6 lower than 6% time, the overhead extraction thing of regenerator column is sent into by pipeline and is absorbed methyl alcohol basin 6 and namely open the second ball valve 20 after regenerator column condenser 3 condensation, closes the first ball valve 19.Even if containing a large amount of methyl alcohol in overhead extraction thing, the methyl alcohol of extraction and methyl iodide just circulate in absorption system, can not bring negative impact, significantly increase the turndown ratio of regenerator column.When absorbing the methyl iodide weight percentage in methyl alcohol basin 6 and being not less than 6%, the overhead extraction thing of regenerator column sends into by pipeline after regenerator column condenser 3 condensation that namely basin 18 is for subsequent use opens the first ball valve 19, close the second ball valve 20, after for some time, when to absorb in methyl alcohol basin methyl iodide weight percentage lower than 6% time, the overhead extraction thing of regenerator column is sent into by pipeline again and is absorbed methyl alcohol basin 6 after condenser condenses; Regenerator column steam consumption can be significantly reduced by present method.(2) when the charging capacity of methyl alcohol is not less than 40%, fresh methanol substitutes the lean solution methyl alcohol that methyl alcohol lean solution tank is sent completely, and regenerator column 1 is stopped using; Then to punching press in basin 18, the liquid for subsequent use in basin 18 being all depressed into and absorbing methyl alcohol basin 6, making the reserve liquid in basin 18 return synthesis system with the iodine methyl alcohol that contains absorbed in methyl alcohol basin by absorbing methyl alcohol take away pump 7.(open the first ball valve 19, open the second ball valve 20, control valve 17 in closedown), enters low-pressure absorption tower (close the first ball valve 19, close the second ball valve 20, control valve 17 in closedown) by the gas emptying in basin 18 after hydraulic fluid completes.For shut-down or underrun are prepared again.Described produces in the technique of acetic acid from methyl alcohol carbonyl synthetic containing iodine methyl alcohol.
The gas that punching course in described step (2) adopts can be nitrogen or carbon monoxide gas etc.
The temperature of preferred regenerator column tower top is 66-80 DEG C.Other technic indexs and original device are consistent.
As implementing the structure of plant modification that the inventive method carries out can be: will to be connected with regenerator column condenser 3 exit end and the outlet that the pipeline of middle control regulation valve 17 is housed is connected with absorption methyl alcohol basin 6, at the outlet side being positioned at described pipeline, the second ball valve 20 is installed, the one end that the arm of the first ball valve 19 is housed is connected with the pipeline between middle control regulation valve 17 and the second ball valve 20, the other end of described arm is connected with basin 18, the emptying outlet of described basin 18 by connection line be connected to low-pressure absorption tower and the gas-liquid equilibrium line absorbed between methyl alcohol basin is connected.Basin 18 is provided with pressurising and emptying flow process, and pressurising uses nitrogen or carbon monoxide, enters low-pressure absorption tower during gas emptying in basin 18.
Embodiment 1
Upstream process goes wrong and stops in emergency, and system loading is down to 0 by 100% very short time, and now in absorption methyl alcohol, methyl iodide content is up to 20 ~ 25%wt, and have a large amount of unreacted to transform methyl iodide in simultaneous reactions still, high/low pressure tail gas amount is all reduced to lower value.Control method is:
Absorbing in methyl alcohol basin sends in the middle part of regenerator column 1 containing iodine methyl alcohol by absorbing methyl alcohol take away pump 7, regenerator column underflow fluid is cooled to 25 ~ 30 DEG C through lean solution water cooler by 88 DEG C, then send into high-pressure absorber 4 and low-pressure absorption tower 5 by lean solution methanol pump 10, substitute fresh methanol; The extraction of regenerator column condenser 3 liquid phase is to basin 18, and regenerator column 1 upper temp controls at 66 ~ 68 DEG C, regenerator column reboiler 2 steam consumption 3T/h, regenerator column condenser 3 liquid phase methyl iodide weight percent content 70%; After extraction to basin for some time, the methyl iodide content absorbed in methyl alcohol basin reduces gradually, and after its content is down to below 6%wt, the extraction of regenerator column condenser 3 liquid phase changed into and deliver to absorption methyl alcohol basin 6, regenerator column reboiler 2 steam is down to 1T/h simultaneously;
After system is without emptying end gas, absorption system stops, and regenerator column is stopped using; Before system preparation goes into operation, first absorption system runs, and drives regenerator column, absorbs methyl alcohol basin 6 methyl iodide content lower than 6%, the lean solution methanol absorption of high and low pressure absorption tower in methyl alcohol lean solution tank, repeats itself.After synthesis system starts displacement, in a large amount of reactor, methyl iodide enters absorption system with emptying end gas, regenerator column tower top methyl iodide content constantly increases, when regenerator column tower upper temp drops to after below 70 DEG C, need to strengthen steam heating amount, regenerator column reboiler steam amount reaches 3T/h, to ensure tower reactor lean solution methanol quality, when absorption methyl alcohol basin methyl iodide content reaches more than 6%, control method is:
Regenerator column condenser 3 liquid phase production is delivered to basin 18 through condensation, absorb methyl alcohol basin methyl iodide content and be down to weight percentage lower than after 6%, delivered to through condensation by regenerator column condenser 3 liquid phase production and absorb methyl alcohol basin, now regenerator column upper temp controls at 75 ~ 80 DEG C.According to the methyl iodide content absorbed in methyl alcohol basin, repeat aforesaid operations.
After synthesis system feeds intake, absorb methanol feed pump 7 and absorption methyl alcohol is sent to synthesis system, fresh methanol progressively substitutes lean solution methyl alcohol and absorbs, and when system loading reaches 40%, control method is:
Fresh methanol substitutes the lean solution methyl alcohol that methyl alcohol lean solution tank is sent completely, regenerator column 1 is stopped using, absorb methyl alcohol take away pump 7 and the absorption methyl alcohol absorbed in methyl alcohol basin 6 is all sent to synthesis system, then the liquid in basin 18 is depressed into completely and absorbs methyl alcohol basin 6, making the reserve liquid in basin return synthesis system with the iodine methyl alcohol that contains absorbed in methyl alcohol basin by absorbing methyl alcohol take away pump, after hydraulic fluid completes, the gas emptying in basin 18 being entered low-pressure absorption tower.
After transformation, the layered effect of driving layered device obviously improves again, and heavy phase proportion reaches 1.932-1.910, and heavy phase pump can run well, and is turned back in time in reactor by methyl iodide, ensure that the equilibrium iodine of system, and acetic acid production energy continous-stable carries out.Regenerator column tower top and the upper temp index upper limit need not be very strict control, turndown ratio increase, steam consumption reduce.
Embodiment 2
Stop as planned parking, progressively cut off methyl alcohol pan feeding after load down to 20%, system maintains emptying end gas, and fresh methanol absorbs in tail gas to enter after methyl iodide and absorbs methyl alcohol basin 6, now absorbs methyl iodide content 3 ~ 5.9%wt in methyl alcohol basin.
(1) be pumped in the middle part of regenerator column 1 by absorbing methanol feed, regenerator column underflow fluid is cooled to 25 ~ 30 DEG C through lean solution water cooler by 88 DEG C and sends into methyl alcohol lean solution tank 9, then send into high-pressure absorber 4 and low-pressure absorption tower 5 by lean solution methanol pump 10, substitute fresh methanol; (2) extraction of regenerator column condenser 3 liquid phase is delivered to and is absorbed methyl alcohol basin 6, regenerator column upper temp 68 ~ 75 DEG C, regenerator column reboiler steam consumption 1T/h;
After system is without emptying end gas, absorption system stops, and regenerator column is stopped using; Before system preparation goes into operation, first absorption system runs, and drives regenerator column, absorbs methyl alcohol basin 6 methyl iodide content lower than 6%, the lean solution methanol absorption of high and low pressure absorption tower in methyl alcohol lean solution tank, repeats itself.After synthesis system starts displacement, in reactor, a small amount of methyl iodide enters absorption system with emptying end gas, regenerator column tower top methyl iodide content constantly increases, when regenerator column tower upper temp drops to after below 70 DEG C, need to strengthen steam heating amount, regenerator column reboiler steam amount reaches 3T/h, to ensure tower reactor lean solution methanol quality, when absorption methyl alcohol basin methyl iodide content reaches 6%, control method is:
After regenerator column condenser 3 liquid phase cools, extraction changes and delivers to basin 18, after for some time, absorbing methyl alcohol basin 6 methyl iodide content is after below 6%wt, again regenerator column condenser 3 liquid phase extraction flow process is changed to and absorbs methyl alcohol basin, regenerator column reboiler 2 steam can be down to 1T/h, regenerator column upper temp 75 ~ 80 DEG C simultaneously.According to the methyl iodide content absorbed in methyl alcohol basin, repeat aforesaid operations.
After synthesis system feeds intake, absorb methanol feed pump 7 and absorption methyl alcohol is sent to synthesis system, fresh methanol progressively substitutes lean solution methyl alcohol and absorbs, and when system loading reaches 40%, control method is:
Fresh methanol substitutes the lean solution methyl alcohol that methyl alcohol lean solution tank 9 is sent completely, regenerator column 1 is stopped using, absorb methyl alcohol take away pump 7 and the absorption methyl alcohol absorbed in methyl alcohol basin 6 is all sent to synthesis system, then the liquid in basin 18 is depressed into completely and absorbs methyl alcohol basin 6, making the reserve liquid in basin return synthesis system with the iodine methyl alcohol that contains absorbed in methyl alcohol basin by absorbing methyl alcohol take away pump, after hydraulic fluid completes, the gas emptying in basin 18 being entered low-pressure absorption tower.
After transformation, the layered effect of driving layered device obviously improves again, and heavy phase proportion reaches 1.932-1.910, and heavy phase pump can run well, and is turned back in time in reactor by methyl iodide, ensure that the equilibrium iodine of system, and acetic acid production energy continous-stable carries out.Regenerator column tower top and the upper temp index upper limit need not be very strict control, turndown ratio increase, steam consumption reduce.
Claims (3)
1. contain an iodine Mathanol regenerating circulation utilization method under underload, it is characterized in that it comprises the following steps:
(1) stop work or with the charging capacity of mass ratio range methyl alcohol lower than less than 40% time, the iodine methyl alcohol that contains absorbed in methyl alcohol basin is sent in the middle part of regenerator column by absorbing methyl alcohol take away pump, regenerator column tower bottom flow fluid enters methyl alcohol lean solution tank after the cooling of lean solution water cooler, and the liquid in methyl alcohol lean solution tank partially or completely substitutes fresh methanol through lean solution methyl alcohol take away pump and sends into high-pressure absorber and low-pressure absorption tower respectively; Simultaneously when absorb the methyl iodide weight percentage in methyl alcohol basin lower than 6% time, the overhead extraction thing of regenerator column is sent into by pipeline and is absorbed methyl alcohol basin after regenerator column condenser condenses; When absorbing the methyl iodide weight percentage in methyl alcohol basin and being not less than 6%, the overhead extraction thing of regenerator column is for subsequent use by pipeline feeding basin after condenser condenses, after for some time, when to absorb in methyl alcohol basin methyl iodide weight percentage lower than 6% time, the overhead extraction thing of regenerator column is sent into by pipeline again and is absorbed methyl alcohol basin after condenser condenses;
(2) when the charging capacity of methyl alcohol is not less than 40%, fresh methanol substitutes the lean solution methyl alcohol that methyl alcohol lean solution tank is sent completely, and regenerator column is stopped using; Then to punching press in basin, liquid for subsequent use in basin is all depressed into and absorbs methyl alcohol basin, making the reserve liquid in basin return synthesis system with the iodine methyl alcohol that contains absorbed in methyl alcohol basin by absorbing methyl alcohol take away pump, after hydraulic fluid completes, the gas emptying in basin being entered low-pressure absorption tower;
Described produces in the technique of acetic acid from methyl alcohol carbonyl synthetic containing iodine methyl alcohol.
2. contain iodine Mathanol regenerating circulation utilization method under underload according to claim 1, it is characterized in that: the gas that the punching course in described step (2) adopts can be nitrogen or carbon monoxide gas.
3. contain iodine Mathanol regenerating circulation utilization method under underload according to claim 1 and 2, it is characterized in that: the temperature of described regenerator column tower top is 66-80 DEG C.
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| CN201310156177.6A CN103214361B (en) | 2013-04-28 | 2013-04-28 | Method for regenerative cycle and utilization of iodine-containing methanol under low load |
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| CN201310156177.6A CN103214361B (en) | 2013-04-28 | 2013-04-28 | Method for regenerative cycle and utilization of iodine-containing methanol under low load |
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| CN103214361B true CN103214361B (en) | 2015-07-15 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302792A (en) * | 1999-12-29 | 2001-07-11 | 赫多特普索化工设备公司 | Method of reducing iodide in industrial product stream |
| CN1803254A (en) * | 2005-12-02 | 2006-07-19 | 西南化工研究设计院 | Method for recovering useful ingredient from methane end gas containing iodine |
| CN102964236A (en) * | 2012-11-23 | 2013-03-13 | 天津渤海化工有限责任公司天津碱厂 | Method for underload recovery of methyl iodide from low-pressure tail gas in acetic acid production |
-
2013
- 2013-04-28 CN CN201310156177.6A patent/CN103214361B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302792A (en) * | 1999-12-29 | 2001-07-11 | 赫多特普索化工设备公司 | Method of reducing iodide in industrial product stream |
| CN1803254A (en) * | 2005-12-02 | 2006-07-19 | 西南化工研究设计院 | Method for recovering useful ingredient from methane end gas containing iodine |
| CN102964236A (en) * | 2012-11-23 | 2013-03-13 | 天津渤海化工有限责任公司天津碱厂 | Method for underload recovery of methyl iodide from low-pressure tail gas in acetic acid production |
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Address after: 300450 No. ten, No. 3369, Lingang Industrial Zone, Tanggu District, Bohai, Tianjin Patentee after: Bo Huayongli chemical inc, Tianjin Address before: 300450 No. ten, No. 3369, Lingang Industrial Zone, Tanggu District, Bohai, Tianjin Patentee before: Tianjin Alkali Plant, Bohai Chemical Co., Ltd, Tianjin |