CN110102074A - The device and technique of two-tower rectification production dimethyl sulfone - Google Patents
The device and technique of two-tower rectification production dimethyl sulfone Download PDFInfo
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- CN110102074A CN110102074A CN201910394709.7A CN201910394709A CN110102074A CN 110102074 A CN110102074 A CN 110102074A CN 201910394709 A CN201910394709 A CN 201910394709A CN 110102074 A CN110102074 A CN 110102074A
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- female
- rectifying column
- sub
- tower
- dimethyl sulfone
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
Abstract
The present invention provides the device of two-tower rectification production dimethyl sulfone, it is connect in the middle part of feed pipe and female rectifying column, female rectifier bottoms are connect with reboiler, reboiler is connect with sub- rectifier bottoms, it is connect at the top of sub- rectifying column with atomization crystallizer, atomization crystallizer is connect with storage tank one, and atomization crystallizer and one bottom of storage tank are connected to product zone all the way after pipeline converges respectively, is connected to sub- rectifier all the way.Its technique includes opening reboiler, female rectifying column and sub- rectifying column are vacuumized, female rectifying column will be entered by feed inlet to fraction seperation object, a large amount of dimethyl sulfones are produced by sub- the top of the distillation column, and sub- rectifying tower tops obtains dimethyl sulfone product after atomization crystallizer is granulated screening.Traditional long-term low temperature crystallization centrifuge separation mode has been broken using the mode of rectifying separation under vacuum conditions in the process program, has greatly improved the purity and credit rating of the product；Selected rectifying device is two-tower rectification, and double tower shares reboiler, saved energy consumption.
Description
Technical field
The present invention relates to the devices and technique of a kind of two-tower rectification production dimethyl sulfone, belong to field of chemical equipment.
Background technique
Dimethyl sulfoxide in process of production, first synthesis intermediate products dimethyl sulfide, in-between product dimethyl
Thioether is further oxided to obtain purpose product dimethyl sulfoxide.Since the particularity of oxidation reaction and security control need,
The excessive variation with the residence time of oxidant has a certain amount of dimethyl sulfoxide to be further oxidized to diformazan after leading to oxidation
Base sulfone.By kettle after rectifying it is residual in dimethyl sulfone from dimethyl sulfoxide finishing column bottom produce, then after crystallized centrifugation recycling contain
There is the thick dimethyl sulfone of certain dimethyl sulfoxide and inorganic salts.
In kettle raffinate thick dimethyl sulfone (dimethyl sulfone content >=95%, water≤2%, inorganic salts≤2%, dimethyl sulfoxide≤
1%) by further crystallization centrifuge separation, the finished product dimethyl sulfone of different meshes is obtained after screening, due to kettle it is residual in contain one
Quantitative inorganic salts have micro inorganic salts and are coated by dimethyl sulfone crystal grain, lead to finished product dimethyl in crystallization process
The purity and being greatly limited property of the scope of application of sulfone.Simultaneously with the dimethyl sulfoxide in oxidizing thick dimethyl sulfone
When (or full utilization finished product sulfoxide oxidation produces dimethyl sulfone technique), due to the presence of strong oxidizer, spot corrosion occurs for equipment
Residue can cause detrimental effects, table of the simultaneous oxidation agent to purpose product dimethyl sulfone to the minor metallic element of dimethyl sulfone
Seeing color will also result in certain influence.The difficult point and bottleneck that factors above is controlled at dimethyl sulfone industry production, and utilize point
The mode of step rectification and purification can effectively solve the problems, such as this.Since dimethyl sulfone, dimethyl sulfoxide and water have well mutually
Dissolubility, using single column essence mode, the operation mode that different location produces different fractions be difficult to realize dimethyl sulfone purity into one
Step is promoted.
Summary of the invention
The present invention is the physicochemical characteristic in conjunction with each substance in dimethyl sulfone, according to the difference of its respective boiling point, in negative pressure ring
In border, using double columns rectification process scheme, from the fraction of overhead extraction dimethyl sulfone, produced to obtain high-purity dimethyl sulfone
Product.
Contain inorganic salts, a certain amount of dimethyl sulfoxide and water in the dimethyl sulfone for needing crystallization and purification, according to association
Spend the difference of the water, inorganic salts, dimethyl sulfoxide and target product dimethyl sulfone boiling point that are affected, under vacuum conditions, benefit
With two-tower rectification mode (primary and secondary tower shares a reboiler), heavy component after extraction concentration at primary and secondary tower bottom reboiler without
Machine salt and a certain amount of dimethyl sulfone are adopted in the mixture of female column overhead extraction light component dimethyl sulfoxide and water in sub- column overhead
Target product dimethyl sulfone out.
In view of the above-mentioned problems, the present invention provides the device of two-tower rectification production dimethyl sulfone, in feed pipe and female rectifying column
Portion's connection, female rectifier bottoms are connect with reboiler, and reboiler is connect with sub- rectifier bottoms, are tied at the top of sub- rectifying column with atomization
Brilliant device connection, atomization crystallizer are connect with storage tank one, and atomization crystallizer connects after pipeline converges all the way respectively with one bottom of storage tank
It is connected to product zone, is connected to sub- rectifier all the way.
It is connect at the top of female rectifying column with condenser, condenser bottom is connect with female rectifier.
Condenser is connect with storage tank two, and storage tank two is connect after pipeline converges with storage tank with condenser bottom；Reboiler
Bottom is connect with storage tank.Storage tank one, storage tank two are provided with vacuum tube on storage tank.Female rectifying tower height degree is higher than sub- rectifying
Tower height degree, and the height of sub- rectifying column is higher than female rectifying column and feeds open height.The difference of primary and secondary tower height degree depends on separative efficiency
(unit time separating degree and fractional dose).
The contents of the present invention also provide a kind of technique of two-tower rectification production dimethyl sulfone, include the following steps:
Reboiler is opened, female rectifying column and sub- rectifying column are vacuumized, it, will be to fraction seperation when vacuum degree reaches 85KPa or more
Object enters female rectifying column by feed inlet, carries out rectification under vacuum, is controlled by the reflux of sub- rectifying tower top phegma, usual reflux ratio
It is 1 ~ 2 or so, to realize the purpose for controlling sub- column overhead temperatures, under this vacuum degree, tower top temperature is controlled at 140 DEG C to 145
Between DEG C, produce the dimethyl sulfone of a large amount of qualifications by sub- the top of the distillation column, under same operating condition, temperature is closer to low value, product
Purity is higher, and a large amount of dimethyl sulfones are produced by sub- the top of the distillation column, and sub- rectifying tower tops is granulated screening through atomization crystallizer
After obtain dimethyl sulfone product；The mixture circulating and recovering of female rectifying column extraction dimethyl sulfoxide and water；Female rectifying tower bottom with
Sub- rectifying tower bottom produces inorganic salts.Due to dimethyl sulfone have distil this physical characteristic and its flash-point it is lower, be more suitable for
Distillation operation is realized under vacuum state.
Control is negative-pressure operation in female rectifying column and sub- rectifying column, is negative-pressure operation in female rectifying column and sub- rectifying column,
Vacuum degree is usually in 85KPa or more, this vacuum degree is by operational load in local atmospheric pressure, tower and to the variation of fraction component
In regular fluctuation, temperature control under corresponding vacuum degree at the boiling point of dimethyl sulfone, it is normal in 140 DEG C to 145 DEG C it
Between.Primarily to reducing the boiling point of dimethyl sulfone, while saving energy consumption, tower top temperature controls and practical operation in tower negative pressure
Negative pressure is related, and vacuum degree is higher, and tower top temperature is lower, according to Y (temperature)=K*(100- vacuum degree) variation, vacuum degree unit
KPa.The mentioning after fraction seperation object includes thick dimethyl sulfone or is converted into dimethyl sulfone using dimethyl sulfoxide finished product
Pure isolate.
The quantity of female rectifying column or sub- rectifying column is more than or equal to 2 but is not limited to 2, this technique can also be used and adopt
It is realized with tower mode under multitower multistage rectification or upper tower.The inorganic salt concentration of the sub- rectifying column and female rectifying tower bottom
When reaching 20%, extraction raffinate waited for female the top of the distillation column distillate and together with target fraction seperation object return to sub- rectifying column and
Female rectifying column is recycled.
Technical solution of the present invention is at 85KPa and the above vacuum state, and the boiling point of water is about at 45 DEG C, dimethyl sulfoxide
Boiling point be 106 DEG C, the boiling point of dimethyl sulfone is 145 DEG C, and the boiling point of inorganic salts is at 200 DEG C or more.Under this vacuum degree, and tower
Bottom temperature maintains under 160 DEG C or more of operating condition that (this temperature is related to inlet amount and female tower feed points temperature, need to maintain to feed
Point temperature is more than the boiling point of dimethyl sulfoxide and water, below dimethyl sulfone boiling point), to rectifying isolate by female tower middle and upper part
Feed points enter, since diformazan machine sulfoxide and water have good intersolubility, dimethyl sulfoxide and water effective from female column overhead
Separation, a possibility that effectively controlling dimethyl sulfoxide and water to tower bottom, the inorganic salts and dimethyl sulfone of primary and secondary tower bottom pass through essence
It evaporates, wherein the tower top movement of a large amount of dimethyl sulfone towards sub- tower (controls sub- column overhead temperatures in dimethyl sulfone by reflux ratio
It is more than boiling point), 99.95% or more, while crystal grain color (finally can be increased to by traditional 99.9% with high-purity dimethyl sulfone product
Damp accordance is stronger, and minor metallic element can be controlled in 10ppm or less) it is produced from sub- column overhead, as primary and secondary tower top is to be separated
The continuous extraction of object, the inorganic salt concentration of primary and secondary tower bottom are constantly promoted, when the residual middle inorganic salt concentration of tower bottom kettle reaches 20% or so
(or when column bottom temperature persistently rises under identical operating condition) reduces the residual concentration of tower bottom kettle, dimension using the residual operation mode of interval row's kettle
Hold whole system balance.
Female column overhead distillate and primary and secondary tower bottom kettle it is residual together enter preamble process pretreatment after and target wait for fraction seperation
Object returns to primary and secondary double tower circulation together.
In the process program under vacuum conditions using rectifying separation mode broken traditional long-term low temperature crystallization from
Heart clastotype greatly improves the purity and credit rating of the product；Selected rectifying device is two-tower rectification, and double tower shares weight
Boil device, in order to energy saving, but it is not limited to double tower, the multitower substep after isolation can also be used realizes this purpose.
Detailed description of the invention
Fig. 1 is the device of two-tower rectification production dimethyl sulfone, wherein 1. female rectifying columns, 2. sub- rectifying columns, and 3. reboilers,
4. being atomized crystallizer, 5. storage tanks, 6. condensers, 7. feed pipes, 8. storage tanks one, 9. storage tanks two, 10. vacuum tubes.
Specific embodiment
Embodiment 1
Two-tower rectification produces the device of dimethyl sulfone, connects in the middle part of feed pipe 7 and female rectifying column 1, female 1 bottom of rectifying column and reboiling
Device 3 connects, and reboiler 3 is connect with sub- 2 bottom of rectifying column, and sub- 2 top of rectifying column is connect with atomization crystallizer 4, is atomized crystallizer 4
It is connect with storage tank 1, atomization crystallizer 4 and one 8 bottom of storage tank are connected to product zone all the way after pipeline converges respectively, connect all the way
It is connected to sub- 2 top of rectifying column.
Female 1 top of rectifying column is connect with condenser 6, and 6 bottom of condenser is connect with 1 top of female rectifying column.
Condenser 6 is connect with storage tank 29, and storage tank 29 is connect after pipeline converges with storage tank 5 with 6 bottom of condenser；Weight
Boiling 3 bottom of device is connect with storage tank 5.
Storage tank 1, storage tank 29 are provided with vacuum tube 10 on storage tank 7.
Female 1 height of rectifying column is higher than sub- 2 height of rectifying column, and the height of sub- rectifying column 2 is higher than female rectifying column 1 feed inlet height
Degree.
Embodiment 2
A kind of operation of the process program using two-tower rectification principle production high purity dimethyl sulfone:
Enter female tower by female tower feed points to fraction seperation object, water, dimethyl sulfoxide are adopted with a small amount of dimethyl sulfone from female column overhead
Out；
It is controlled by reflux ratio, a large amount of higher dimethyl sulfones of purity are produced by sub- column overhead；Primary and secondary tower bottom using it is continuous or
The residual operation mode of the row's of having a rest kettle removes the dimethyl sulfone solution of inorganic salt concentration rising in time；The residual and female column overhead distillate of tower bottom kettle
Double tower is returned to together after pretreatment and to fraction seperation object, realizes the recycling of dimethyl sulfone.Sub- column overhead fraction is through mist
Change after crystallizer is granulated screening and obtains high-purity dimethyl sulfone product.The residual extraction clastotype of tower bottom kettle can also be connected with intermittently operated
Continuous extraction control.
Embodiment 3
A kind of operational instances of the process program using two-tower rectification principle production high purity dimethyl sulfone:
It, will be (dimethyl sulfone content >=95%, water≤2%, inorganic to fraction seperation object when vacuum degree reaches 85KPa or more in tower
Salt≤2%, dimethyl sulfoxide≤1%) by female rectifying column feed points enter female tower, control column bottom temperature at 160 DEG C or so, due to
Low-boiling substance water, dimethyl sulfoxide cannot reach female rectifying tower bottom, directly be risen by female rectifying column stripping section, entrainment of
A small amount of dimethyl sulfone is produced from female the top of the distillation column；The higher dimethyl sulfone of boiling point and salt enter sub- rectifying by reboiler
Tower, by controlling reflux ratio, Chang Wei 1.5 maintains tower top temperature at 145 DEG C, and a large amount of higher dimethyl sulfones of purity are by Zi Tata
Top extraction；Primary and secondary tower bottom removes the dimethyl sulfone solution of inorganic salt concentration rising using interval row's residual operation mode of kettle in time；Tower
Kettle residual and female the top of the distillation column distillate in bottom returns to double tower after pretreatment and to fraction seperation object together, realizes dimethyl sulfone
It recycles again.Sub- rectifying tower tops is granulated rapidly under the action of cold nitrogen through atomization crystallizer to be solidified, after screening
Obtain high-purity dimethyl sulfone product.
This process program product purity is high, and main content can reach 99.9%, the product first separation rate of recovery can reach 85% with
On.
And the grain size number of crystallizer can be controlled according to customer demand, meeting 20 mesh of crystallization stage to granularity between 80 mesh is more than
70%, fine-grade, the requirement of superfine grade.
Embodiment 4
A kind of operational instances of the process program using two-tower rectification principle production high purity dimethyl sulfone:
It, will be (dimethyl sulfone content >=95%, water≤2%, inorganic to fraction seperation object when vacuum degree reaches 90KPa or more in tower
Salt≤2%, dimethyl sulfoxide≤1%) by female rectifying column feed points enter female tower, control column bottom temperature at 158 DEG C or so, due to
Low-boiling substance water, dimethyl sulfoxide cannot reach female rectifying tower bottom, directly be risen by female rectifying column stripping section, entrainment of
A small amount of dimethyl sulfone is produced from female the top of the distillation column；The higher dimethyl sulfone of boiling point and salt enter sub- rectifying by reboiler
Tower, by controlling reflux ratio, Chang Wei 2 maintains tower top temperature at 140 DEG C, and the higher dimethyl sulfone of purity is produced by sub- column overhead；
Primary and secondary tower bottom removes the dimethyl sulfone solution of inorganic salt concentration rising using interval row's residual operation mode of kettle in time；Tower bottom kettle it is residual and
Female the top of the distillation column distillate returns to double tower after pretreatment and to fraction seperation object together, realizes the circulation again of dimethyl sulfone
It utilizes.Sub- rectifying tower tops is granulated rapidly under the action of cold nitrogen through atomization crystallizer to be solidified, and is obtained after screening high-purity
Dimethyl sulfone product.
This process program product purity is high, and main content can reach 99.90%, the product first separation rate of recovery can reach 80% with
On.
And the grain size number of crystallizer can be controlled according to customer demand, meeting 20 mesh of crystallization stage to granularity between 80 mesh is more than
70%, fine-grade, the requirement of superfine grade.
Claims (10)
1. the device of two-tower rectification production dimethyl sulfone, which is characterized in that it is connect in the middle part of feed pipe (7) and female rectifying column (1), it is female
Rectifying column (1) bottom is connect with reboiler (3), and reboiler (3) is connect with sub- rectifying column (2) bottom, at the top of sub- rectifying column (2) with
It is atomized crystallizer (4) connection, atomization crystallizer (4) is connect with storage tank one (8), atomization crystallizer (4) and storage tank one (8) bottom point
It is not connected to product zone all the way after pipeline converges, is connected to sub- rectifying column (2) top all the way.
2. the device of two-tower rectification production dimethyl sulfone according to claim 1, which is characterized in that female rectifying column (1) top
Portion is connect with condenser (6), and condenser (6) bottom is connect with female rectifying column (1) top.
3. the device of two-tower rectification production dimethyl sulfone according to claim 1, which is characterized in that condenser (6) and storage
Tank two (9) connection, storage tank two (9) are connect after pipeline converges with storage tank (5) with condenser (6) bottom；Reboiler (3) bottom
It is connect with storage tank (5).
4. the device of two-tower rectification production dimethyl sulfone according to claim 1 or 3, which is characterized in that storage tank one (8),
Vacuum tube (10) are provided on storage tank two (9), storage tank (7).
5. the device of two-tower rectification production dimethyl sulfone according to claim 1, which is characterized in that female rectifying column (1) is high
Degree is higher than sub- rectifying column (2) height, and the height of sub- rectifying column (2) is higher than female rectifying column (1) and feeds open height.
6. the work of the device production dimethyl sulfone using the described in any item two-tower rectification production dimethyl sulfones of claim 1-5
Skill, which comprises the steps of:
Reboiler is opened, when vacuum degree reaches 85KPa or more, female rectifying column will be entered by feed inlet to fraction seperation object, is carried out
Rectification under vacuum, the reflux ratio for controlling sub- rectifying column top return liquid is 1 ~ 2, makes under vacuum conditions, to realize and control sub- column overhead
Temperature is 140 DEG C -145 DEG C, produces dimethyl sulfone by sub- the top of the distillation column, and sub- rectifying tower tops is made through being atomized crystallizer
Dimethyl sulfone product is obtained after grain screening；The mixture circulating and recovering of female rectifying column extraction dimethyl sulfoxide and water；Female rectifying column
Tower bottom and sub- rectifying tower bottom produce inorganic salts.
7. the technique of two-tower rectification production dimethyl sulfone according to claim 6, which is characterized in that female rectifying column and son essence
Evaporating Ta Tanei is negative pressure, and vacuum degree is in 85KPa or more, and female rectifying column and the control of sub- temperature inside rectifying tower are 140-145 DEG C.
8. the technique of two-tower rectification production dimethyl sulfone according to claim 6, which is characterized in that described to fraction point
The purification & isolation object for including thick dimethyl sulfone from object or being converted into using dimethyl sulfoxide finished product after dimethyl sulfone.
9. the technique of two-tower rectification production dimethyl sulfone according to claim 6, which is characterized in that female rectifying column or son essence
The quantity for evaporating tower is more than or equal to 2, and multitower multistage rectification can be used in this technique.
10. the technique of two-tower rectification production dimethyl sulfone according to claim 6, which is characterized in that sub- rectifying column and mother
When the inorganic salt concentration at rectifying tower bottom reaches 20%, extraction raffinate waits evaporating with female the top of the distillation column distillate and together with target
Point isolate returns to sub- rectifying column and female rectifying column is recycled.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910394709.7A CN110102074B (en) | 2019-05-13 | 2019-05-13 | Process for producing dimethyl sulfone by double-tower rectification |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910394709.7A CN110102074B (en) | 2019-05-13 | 2019-05-13 | Process for producing dimethyl sulfone by double-tower rectification |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2213649A1 (en) * | 2007-11-27 | 2010-08-04 | Mitsui Chemicals, Inc. | Method of dehydrating tolylenediamine and dehydrator |
| CN101857585A (en) * | 2010-05-21 | 2010-10-13 | 常州大学 | Continuous high vacuum rectification and purification method for lactide |
| CN203144312U (en) * | 2013-03-01 | 2013-08-21 | 天津天中福大科技发展有限公司 | Device for recovering and refining dimethyl sulfoxide |
-
2019
- 2019-05-13 CN CN201910394709.7A patent/CN110102074B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2213649A1 (en) * | 2007-11-27 | 2010-08-04 | Mitsui Chemicals, Inc. | Method of dehydrating tolylenediamine and dehydrator |
| CN101857585A (en) * | 2010-05-21 | 2010-10-13 | 常州大学 | Continuous high vacuum rectification and purification method for lactide |
| CN203144312U (en) * | 2013-03-01 | 2013-08-21 | 天津天中福大科技发展有限公司 | Device for recovering and refining dimethyl sulfoxide |
Non-Patent Citations (1)
| Title |
|---|
| 章思规等: "《精细有机化工制备手册》", 31 May 1996, 科学技术文献出版社 * |
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Effective date of registration: 20221102 Address after: 843099 Zhejiang Industrial Park (West Park), Aksu economic and Technological Development Zone, Aksu Prefecture, Xinjiang Uygur Autonomous Region Patentee after: Xinjiang Xingfa Chemical Co.,Ltd. Address before: 443711 Hunan Road, Gufu Town, Xingshan County, Yichang City, Hubei Province Patentee before: HUBEI XINGFA CHEMICALS GROUP Co.,Ltd. |