CN110339585A - Maleic anhydride unit solvent dehydration dry treatment process and equipment - Google Patents
Maleic anhydride unit solvent dehydration dry treatment process and equipment Download PDFInfo
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- CN110339585A CN110339585A CN201910694456.5A CN201910694456A CN110339585A CN 110339585 A CN110339585 A CN 110339585A CN 201910694456 A CN201910694456 A CN 201910694456A CN 110339585 A CN110339585 A CN 110339585A
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- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
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Abstract
The invention belongs to cis-butenedioic anhydride solvent recovery technical field, it is specifically related to a kind of maleic anhydride unit solvent dehydration dry treatment process and equipment.Demineralized water is centrifuged after mixing with organic solvent, obtained organic phase is after the preheating of flash tank heat exchanger, 95-100 DEG C is heated in into flash tank heater, subsequently into being flashed in solvent flash tank, make moisture content≤0.02% in solvent, obtained dry solvent enters maleic anhydride absorption tower recycling.Maleic anhydride unit solvent dehydration drying process of the present invention and equipment, for the solvent of centrifugation motor spindle discharge, solvent seasoning is after heating flash evaporation, further reduce the moisture that solvent washing room brings absorption section into, reduce the decomposition loss of cis-butenedioic anhydride, reduce the generation of impurity, guarantees that solvent absorption resolution system being capable of steady long-term operation.
Description
Technical field
The invention belongs to cis-butenedioic anhydride solvent recovery technical fields, are specifically related to a kind of maleic anhydride unit solvent dehydration drying process
Processes and apparatus.
Background technique
N butane oxidation solvent absorption maleic anhydride production technique is the prevailing technology of domestic and international production cis-butenedioic anhydride.The technique is logical
It crosses n butane oxidation reaction and generates the admixture of gas containing cis-butenedioic anhydride, then with solvent absorption cis-butenedioic anhydride, parse cis-butenedioic anhydride in Analytic Tower
Out.Solvent a part after parsing enters solvent recovery unit processing, and another part is directly entered absorption tower and recycles.
Following reaction mainly occurs in reactor:
Main reaction:
n-C4H10+3.5O2→C4H2O3+4H2O
Side reaction:
n-C4H10+4.5O2→4CO+5H2O
n-C4H10+6.5O2→4CO2+5H2O
C4H2O3+O2→4CO+H2O
C4H2O3+3O2→4CO2+H2O
n-C4H10+2.5O2→2C2H4O2+H2O
n-C4H10+3.25O2→C3H4O2+0.5CO+0.5CO2+3H2O
7C4H10+12.5O2→2C14O10+25H2O。
The isolated solvent phase organic solvent of centrifuge can accumulate a certain amount of by-product during recycling,
Solvent pyrolytic, cis-butenedioic anhydride hydrolysis generate fumaric acid, phthalic anhydride, butanol impurity in such as solvent absorption, resolving.These are secondary
The removal of product not in time, will accumulate in a solvent, and further esterification or auto polymerization formation macromolecular are poly- under the high temperature conditions
Object is closed, can not only make the efficiency absorbed decline, but also heat exchange equipment can be blocked, device is caused to stop work.
Currently, being dibutyl phthalate (DBP) using more organic solvent, recycles the country and carried out
A series of researchs, process flow are described with patent CN2018211689115.Solvent and desalted water mixing, stirring are washed
It washs, separates solvent phase and water phase into centrifuge, be further reduced the water in solvent into solvent surge tank or solvent decanter
Content is recycled subsequently into absorption tower.
In actual motion, water content is 2-3wt% from the solvent phase that centrifuge separates, and illustrates centrifuge treating in good point
From state, after solvent surge tank or solvent decanter, water content is down to 1% or so, and solvent water content is still reached to less than work
0.02% or less skill requirement.Exceeded will lead to of lean solvent water content absorbs bad or is formed in system along acid, fumaric acid, drop
The low yield of cis-butenedioic anhydride, the difficulty of subsequent solvent processing and loss also rise with it.
Therefore, it needs to explore a kind of novel maleic anhydride unit solvent dehydration dry treatment process and equipment, to centrifuge point
It is recycled from obtained organic phase solvent, reduces the loss of cis-butenedioic anhydride, enable the steady long-term operation of cis-butenedioic anhydride system.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of maleic anhydride unit solvent dehydration drying process work
Skill further removes the moisture in solvent, reaches technic index requirement, reduces the loss of cis-butenedioic anhydride, makes solvent absorption desorption system
System being capable of steady long-term operation；Invention also provides maleic anhydride unit solvent dehydration equipment for drying.
Maleic anhydride unit solvent dehydration dry treatment process of the present invention, demineralized water carried out after being mixed with organic solvent from
The heart separation, obtained organic phase through flash tank heat exchanger preheating after, into flash tank heater in be heated to 95-100 DEG C, so
Enter in solvent flash tank afterwards and flashed, make moisture content≤0.02% in solvent, obtained dry solvent enters cis-butenedioic anhydride suction
Tower is received to recycle.
Wherein:
Demineralized water and being blended in agitator tank for organic solvent carry out, and then carry out centrifuge and are centrifuged, in which:
The mixed volume ratio of demineralized water and organic solvent is 6:4；Demineralized water is preheating to 70-80 DEG C；The mixing time of agitator tank is
30min, the operation temperature of agitator tank are 65-70 DEG C；The revolving speed of centrifuge is 4800r/min.
Centrifugation motor spindle solvent phase mass flow be 8000kg/h, 60-65 DEG C of temperature.
It is as follows to be centrifuged the outlet solvent phase composition of motor spindle solvent phase: solvent DBP content: 98-98.5wt%；Water content:
1.5-2wt%.
Flash tank heat exchanger outlet temperature is 70-75 DEG C, pressure 0.38-0.42MPa.
Flash tank heater outlet temperature is 95-100 DEG C, pressure 0.35-0.42MPa.
Solvent flash tank operating pressure is absolute pressure 8.5-9.2mmHg.
Solvent flash tank bottom temperature is 85-90 DEG C.
Solvent flash drum overhead gas phase temperature is 93-98 DEG C.
Solvent flash drum overhead gas phase composition: water content 93-97wt%, solvent content 3-7wt%.
The composition of the dry solvent of solvent flash tank bottom discharge are as follows: DBP content: 99-99.4wt%；Water content :≤
0.02wt%, temperature: 76-80 DEG C.
Maleic anhydride unit solvent dehydration equipment for drying of the present invention, including centrifuge are centrifuged motor spindle solvent phase
Discharge port is connected by pipeline with solvent decanter, and solvent decanter is connected by pipeline with flash tank heat exchanger, and flash tank changes
Hot device is connected by pipeline with flash tank heater, flash tank heater pass through pipeline and solvent flash tank middle and upper part solvent into
Mouth is connected, and flash tank heater top connects low-pressure steam air inlet pipe.
Wherein:
It further include demineralized water preheating can, demineralized water preheating pot bottom feed inlet is connected with desalination water pipeline, desalination water pipeline
Be connected by the first pipeline with agitator tank after converging with organic solvent feeding line, agitator tank bottom discharge port by pipeline with
Centrifuge upper feed inlet is connected, and centrifuge upper aqueous phase discharge port is connected by pipeline with waste water tank, waste water tank bottom discharge
Mouth is connected with wastewater discharge pipe road.
Solvent flash drum overhead gaseous phase outlet is connected by pipeline with vacuum system, and solvent flash tank bottom liquid-phase outlet is logical
Overdrying solvent pipe is connected with flash tank heat exchanger, and flash tank heat exchanger is connected by pipeline with maleic anhydride absorption tower.
Solvent flash tank device parameter is as follows: diameterHeight 3000mm (is free of end socket), bed stuffing height:
1000mm, filler are located in the middle part of equipment；Colvent inlet DN300mm, top gas phase export DN350mm, and solvent outlet is done in bottom
DN50mm。
Drying and the removal process for being centrifuged the solvent phase of motor spindle discharge are as follows:
After the solvent being discharged by centrifugation motor spindle mutually enters solvent decanter, solvent delivery to flash tank is changed by solvent pump
Hot device is tentatively exchanged heat with solvent flash tank bottom discharge port by doing the dry solvent that solvent pipe conveying comes, and flash tank changes
The outlet temperature of hot device is 70-75 DEG C, pressure 0.38-0.42MPa；Then flash tank heater is entered back into, is steamed using low pressure
The low-pressure steam heating that the conveying of vapour air inlet pipe comes reaches required temperature, and flash tank heater outlet temperature is 95-100 DEG C, pressure
For 035-0.42MPa.Solvent, which mutually eventually enters into, after heating steams moisture remaining in solvent in solvent flash tank, make in solvent
Moisture content reach 0.02% and hereinafter, exhaust gas is discharged into vacuum system by pipeline by the gas outlet of solvent flash drum overhead.
Solvent after flash distillation, by dry solvent pipe conveying, sends maleic anhydride absorption tower back to after the cooling of flash tank heat exchanger through dry solvent pump
It recycles.
Moisture in solvent is further removed for the solvent of centrifugation motor spindle discharge, reaches technique and refer to by the above process
Mark requires, and reduces the loss of cis-butenedioic anhydride, enables the steady long-term operation of solvent absorption resolution system.
Compared with the prior art, the present invention has the following beneficial effects:
(1) maleic anhydride unit solvent dehydration drying process of the present invention and equipment, for the molten of centrifugation motor spindle discharge
Agent, solvent seasoning further reduce the moisture that solvent washing room brings absorption section into, reduce after heating flash evaporation
The decomposition of cis-butenedioic anhydride is lost, and the generation of impurity is reduced, and guarantees that solvent absorption resolution system being capable of steady long-term operation.
(2) maleic anhydride unit solvent dehydration drying process of the present invention and equipment, by the solvent phase solvent of centrifuge separation
It recycles, rationally, easy to operate, highly-safe, operating cost is low, reduces the loss of cis-butenedioic anhydride, molten after processing for system design
Agent reaches technic index requirement, has achieved the purpose that solvent zero is lost.
Detailed description of the invention
Fig. 1 is maleic anhydride unit solvent dehydration equipment for drying structural schematic diagram.
Fig. 2 is solvent flash tank structural schematic diagram.
In figure: 1, agitator tank；2, centrifuge；3, solvent decanter；4, flash tank heat exchanger；5, flash tank heater；6, solvent
Flash tank；7, solvent pipe is done；8, demineralized water preheating can；9, desalination water pipeline；10, organic solvent feeding line；11, first
Pipeline；12, waste water tank；13, wastewater discharge pipe road；14, low-pressure steam air inlet pipe；15, wire mesh demister；16, packing layer；17,
Gaseous phase outlet；18, solvent inlet；19, liquid-phase outlet.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
A kind of maleic anhydride unit solvent dehydration dry treatment process, demineralized water are centrifuged after mixing with organic solvent,
Obtained organic phase through flash tank heat exchanger preheating after, into flash tank heater in be heated to 100 DEG C, subsequently into solvent
It is flashed in flash tank, makes moisture content≤0.02% in solvent, obtained dry solvent enters maleic anhydride absorption tower recycling benefit
With.
Wherein:
Demineralized water and being blended in agitator tank for organic solvent carry out, and then carry out centrifuge and are centrifuged, in which:
The mixed volume ratio of demineralized water and organic solvent is 6:4；Demineralized water is preheating to 75 DEG C；The mixing time of agitator tank is 30min,
The operation temperature of agitator tank is 68 DEG C；The revolving speed of centrifuge is 4800r/min.
Centrifugation motor spindle solvent phase mass flow be 8000kg/h, 63 DEG C of temperature.
It is as follows to be centrifuged the outlet solvent phase composition of motor spindle solvent phase: solvent DBP content: 98.5wt%；Water content:
1.5wt%.
Flash tank heat exchanger outlet temperature is 75 DEG C, pressure 0.4MPa.
Flash tank heater outlet temperature is 100 DEG C, pressure 0.39MPa.
Solvent flash tank operating pressure is absolute pressure 9mmHg.
Solvent flash tank bottom temperature is 85 DEG C.
Solvent flash drum overhead gas phase temperature is 95 DEG C.
Solvent flash drum overhead gas phase composition: water content 94.49wt%, solvent content 5.51wt%.
The composition of the dry solvent of solvent flash tank bottom discharge are as follows: DBP content: 99.4wt%；Water content: 0.02wt%,
Temperature: 78 DEG C.
Maleic anhydride unit solvent dehydration equipment for drying described in the present embodiment 1, including centrifuge 2,2 bottom of centrifuge are molten
Agent phase discharge port is connected by pipeline with solvent decanter 3, and solvent decanter 3 is connected by pipeline with flash tank heat exchanger 4,
Flash tank heat exchanger 4 is connected by pipeline with flash tank heater 5, and flash tank heater 5 passes through pipeline and solvent flash tank 6
Middle and upper part solvent inlet 18 is connected, and 5 top of flash tank heater connects low-pressure steam air inlet pipe 14.
Wherein:
It further include demineralized water preheating can 8,8 bottom feed inlet of demineralized water preheating can is connected with desalination water pipeline 9, desalination water pipe
Line 9 is connected by the first pipeline 11 with agitator tank 1 after converging with organic solvent feeding line 10, and 1 bottom discharge port of agitator tank is logical
It crosses pipeline to be connected with 2 upper feed inlet of centrifuge, 2 upper aqueous phase discharge port of centrifuge is connected by pipeline with waste water tank 12, is given up
12 bottom discharge port of water pot is connected with wastewater discharge pipe road 13.
6 top gas phase of solvent flash tank outlet 17 is connected by pipeline with vacuum system, and 6 bottom liquid phases of solvent flash tank go out
Mouth 19 is connected by dry solvent pipe 7 with flash tank heat exchanger 4, and flash tank heat exchanger 4 passes through pipeline and maleic anhydride absorption tower phase
Even.
6 device parameter of solvent flash tank is as follows: diameterHeight 3000mm (is free of end socket), bed stuffing height:
1000mm, filler are located in the middle part of equipment；Solvent inlet DN300mm, top gas phase export DN350mm, bottom liquid phases outlet
DN50mm。
Embodiment 2
A kind of maleic anhydride unit solvent dehydration dry treatment process, demineralized water are centrifuged after mixing with organic solvent,
Obtained organic phase through flash tank heat exchanger preheating after, into flash tank heater in be heated to 95 DEG C, subsequently into solvent dodge
It is flashed in steaming pot, makes moisture content≤0.02% in solvent, obtained dry solvent enters maleic anhydride absorption tower recycling benefit
With.
Wherein:
Demineralized water and being blended in agitator tank for organic solvent carry out, and then carry out centrifuge and are centrifuged, in which:
The mixed volume ratio of demineralized water and organic solvent is 6:4；Demineralized water is preheating to 70 DEG C；The mixing time of agitator tank is 30min,
The operation temperature of agitator tank is 65 DEG C；The revolving speed of centrifuge is 4800r/min.
Centrifugation motor spindle solvent phase mass flow be 8000kg/h, 62 DEG C of temperature.
It is as follows to be centrifuged the outlet solvent phase composition of motor spindle solvent phase: solvent DBP content: 98wt%；Water content: 2wt%.
Flash tank heat exchanger outlet temperature is 72 DEG C, pressure 0.42MPa.
Flash tank heater outlet temperature is 95 DEG C, pressure 0.40MPa.
Solvent flash tank operating pressure is absolute pressure 9.2mmHg.
Solvent flash tank bottom temperature is 87 DEG C.
Solvent flash drum overhead gas phase temperature is 97 DEG C.
Solvent flash drum overhead gas phase composition: water content 97wt%, solvent content 3wt%.
The composition of the dry solvent of solvent flash tank bottom discharge are as follows: DBP content: 99.3wt%；Water content: 0.018wt%,
Temperature: 80 DEG C.
Maleic anhydride unit solvent dehydration equipment for drying used by the present embodiment 2 is same as Example 1.
Embodiment 3
A kind of maleic anhydride unit solvent dehydration dry treatment process, demineralized water are centrifuged after mixing with organic solvent,
Obtained organic phase through flash tank heat exchanger preheating after, into flash tank heater in be heated to 98 DEG C, subsequently into solvent dodge
It is flashed in steaming pot, makes moisture content≤0.02% in solvent, obtained dry solvent enters maleic anhydride absorption tower recycling benefit
With.
Wherein:
Demineralized water and being blended in agitator tank for organic solvent carry out, and then carry out centrifuge and are centrifuged, in which:
The mixed volume ratio of demineralized water and organic solvent is 6:4；Demineralized water is preheating to 80 DEG C；The mixing time of agitator tank is 30min,
The operation temperature of agitator tank is 70 DEG C；The revolving speed of centrifuge is 4800r/min.
Centrifugation motor spindle solvent phase mass flow be 8000kg/h, 65 DEG C of temperature.
It is as follows to be centrifuged the outlet solvent phase composition of motor spindle solvent phase: solvent DBP content: 98.2wt%；Water content:
1.8wt%.
Flash tank heat exchanger outlet temperature is 73 DEG C, pressure 0.38MPa.
Flash tank heater outlet temperature is 98 DEG C, pressure 0.39MPa.
Solvent flash tank operating pressure is absolute pressure 8.8mmHg.
Solvent flash tank bottom temperature is 88 DEG C.
Solvent flash drum overhead gas phase temperature is 95 DEG C.
Solvent flash drum overhead gas phase composition: water content 93.49wt%, solvent content 6.51wt%.
The composition of the dry solvent of solvent flash tank bottom discharge are as follows: DBP content: 99.2wt%；Water content: 0.02wt%,
Temperature: 78 DEG C.
Maleic anhydride unit solvent dehydration equipment for drying used by the present embodiment 3 is same as Example 1.
Claims (10)
1. a kind of maleic anhydride unit solvent dehydration dry treatment process, it is characterised in that: demineralized water carries out after mixing with organic solvent
Centrifuge separation, obtained organic phase through flash tank heat exchanger preheating after, into flash tank heater in be heated to 95-100 DEG C, so
Enter in solvent flash tank afterwards and flashed, make moisture content≤0.02% in solvent, obtained dry solvent enters cis-butenedioic anhydride suction
Tower is received to recycle.
2. maleic anhydride unit solvent dehydration dry treatment process according to claim 1, it is characterised in that: demineralized water with it is organic
Being blended in agitator tank for solvent carries out, and then carries out centrifuge and is centrifuged, in which: demineralized water and organic solvent it is mixed
Conjunction volume ratio is 6:4；Demineralized water is preheating to 70-80 DEG C；The mixing time of agitator tank is 30min, and the operation temperature of agitator tank is
65-70℃；The revolving speed of centrifuge is 4800r/min.
3. maleic anhydride unit solvent dehydration dry treatment process according to claim 1, it is characterised in that: centrifugation motor spindle is molten
Agent phase mass flow be 8000kg/h, 60-65 DEG C of temperature；It is as follows to be centrifuged the outlet solvent phase composition of motor spindle solvent phase: solvent DBP
Content: 98-98.5wt%；Water content: 1.5-2wt%.
4. maleic anhydride unit solvent dehydration dry treatment process according to claim 1, it is characterised in that: flash tank heat exchanger
Outlet temperature is 70-75 DEG C, pressure 0.38-0.42MPa；Flash tank heater outlet temperature is 95-100 DEG C, and pressure is
0.35-0.42MPa。
5. maleic anhydride unit solvent dehydration dry treatment process according to claim 1, it is characterised in that: solvent flash tank behaviour
Making pressure is absolute pressure 8.5-9.2mmHg；Solvent flash tank bottom temperature is 85-90 DEG C；Solvent flash drum overhead gas phase temperature
Degree is 93-98 DEG C.
6. maleic anhydride unit solvent dehydration dry treatment process according to claim 1, it is characterised in that: solvent flashes tank deck
Portion's gas phase composition: water content 93-97wt%, solvent content 3-7wt%；The composition of the dry solvent of solvent flash tank bottom discharge
Are as follows: DBP content: 99-99.4wt%；Water content :≤0.02wt%, temperature: 76-80 DEG C.
7. a kind of maleic anhydride unit solvent dehydration equipment for drying described in claim 1, it is characterised in that: including centrifuge
(2), centrifuge (2) bottom solvent phase discharge port is connected by pipeline with solvent decanter (3), and solvent decanter (3) passes through pipe
Road is connected with flash tank heat exchanger (4), and flash tank heat exchanger (4) is connected by pipeline with flash tank heater (5), and flash tank adds
Hot device (5) is connected by pipeline with solvent flash tank (6) middle and upper part solvent inlet (18), the connection of flash tank heater (5) top
Low-pressure steam air inlet pipe (14).
8. maleic anhydride unit solvent dehydration equipment for drying according to claim 7, it is characterised in that: further include demineralized water
Preheating can (8), demineralized water preheating can (8) bottom feed inlet are connected with desalination water pipeline (9), desalination water pipeline (9) with it is organic molten
Agent feeding line (10) is connected by the first pipeline (11) with agitator tank (1) after converging, and agitator tank (1) bottom discharge port passes through pipe
Road is connected with centrifuge (2) upper feed inlet, and centrifuge (2) upper aqueous phase discharge port is connected by pipeline with waste water tank (12),
Waste water tank (12) bottom discharge port is connected with wastewater discharge pipe road (13).
9. maleic anhydride unit solvent dehydration equipment for drying according to claim 7, it is characterised in that: solvent flash tank
(6) top gas phase outlet (17) is connected by pipeline with vacuum system, and solvent flash tank (6) bottom liquid phases export (19) by doing
Solvent pipe (7) is connected with flash tank heat exchanger (4), and flash tank heat exchanger (4) is connected by pipeline with maleic anhydride absorption tower.
10. maleic anhydride unit solvent dehydration equipment for drying according to claim 7, it is characterised in that: solvent flash tank
(6) device parameter is as follows: diameterHeight 3000mm, bed stuffing height: 1000mm, filler are located in the middle part of equipment；It is molten
Agent entrance DN300mm, top gas phase export DN350mm, and solvent outlet DN50mm is done in bottom.
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| CN201910694456.5A CN110339585B (en) | 2019-07-30 | 2019-07-30 | Maleic anhydride device solvent dehydration drying treatment process and equipment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113548712A (en) * | 2021-08-28 | 2021-10-26 | 洛阳炼化九源石化有限公司 | Desolventizing, regenerating and alkali washing system for maleic anhydride by n-butane method |
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| Publication number | Publication date |
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| CN110339585B (en) | 2022-04-12 |
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