CN110102074B - Process for producing dimethyl sulfone by double-tower rectification - Google Patents
Process for producing dimethyl sulfone by double-tower rectification Download PDFInfo
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- CN110102074B CN110102074B CN201910394709.7A CN201910394709A CN110102074B CN 110102074 B CN110102074 B CN 110102074B CN 201910394709 A CN201910394709 A CN 201910394709A CN 110102074 B CN110102074 B CN 110102074B
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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
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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
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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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
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
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- 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 invention provides a device for producing dimethyl sulfone by double-tower rectification, wherein a feeding pipe is connected with the middle part of a mother rectifying tower, the bottom part of the mother rectifying tower is connected with a reboiler, the reboiler is connected with the bottom part of a sub-rectifying tower, the top part of the sub-rectifying tower is connected with an atomizing crystallizer, the atomizing crystallizer is connected with a first storage tank, the atomizing crystallizer and the bottom part of the first storage tank are respectively converged by a pipeline, one path of the atomizing crystallizer is connected to a product area, and the other path of the atomizing crystallizer is connected to the upper part of the sub-rectifying tower. The process comprises the steps of starting a reboiler, vacuumizing a mother rectifying tower and a subsidiary rectifying tower, feeding a to-be-distilled separation into the mother rectifying tower from a feeding hole, extracting a large amount of dimethyl sulfone from the top of the subsidiary rectifying tower, and granulating and screening the top fraction of the subsidiary rectifying tower through an atomizing crystallizer to obtain a dimethyl sulfone product. The process scheme breaks through the traditional long-term low-temperature crystallization centrifugal separation mode by adopting a rectification separation mode in a vacuum state, and greatly improves the purity and quality grade of the product; the selected rectifying equipment is double-tower rectifying, and the double towers share a reboiler, so that the energy consumption is saved.
Description
Technical Field
The invention relates to a device and a process for producing dimethyl sulfone by double-tower rectification, belonging to the field of chemical equipment.
Background
During the production process of dimethyl sulfoxide, intermediate dimethyl sulfide is firstly synthesized, and the intermediate dimethyl sulfide is further oxidized to obtain the target product dimethyl sulfoxide. Due to the specificity and safety control requirements of the oxidation reaction, the excess of oxidant and the change in residence time result in a certain amount of further oxidation of dimethyl sulfoxide to dimethyl sulfone after oxidation. And extracting dimethyl sulfone in the residue after rectification from the bottom of a dimethyl sulfoxide finished product tower, and recovering crude dimethyl sulfone containing a certain amount of dimethyl sulfoxide and inorganic salt after crystallization and centrifugation.
Crude dimethyl sulfone (the content of dimethyl sulfone is more than or equal to 95 percent, the content of water is less than or equal to 2 percent, the content of inorganic salt is less than or equal to 2 percent and the content of dimethyl sulfoxide is less than or equal to 1 percent) in the still residual liquid is further crystallized, centrifugally separated and screened to obtain finished products of dimethyl sulfone with different meshes. Meanwhile, when the dimethyl sulfoxide in the crude dimethyl sulfone is oxidized by using an oxidizing agent (or a process for producing the dimethyl sulfone by completely utilizing the oxidation of the finished product sulfoxide), due to the existence of a strong oxidizing agent, the residue of equipment pitting corrosion can cause fatal influence on trace metal elements of the dimethyl sulfone, and meanwhile, the oxidizing agent can cause certain influence on the apparent color of the target product dimethyl sulfone. The factors form the difficulty and bottleneck of production control in the dimethyl sulfone industry, and the problem can be effectively solved by using a fractional distillation purification mode. Because dimethyl sulfone, dimethyl sulfoxide and water have good intersolubility, a single-tower refining mode is adopted, and the further improvement of the purity of the dimethyl sulfone is difficult to realize in an operation mode of extracting different fractions from different positions.
Disclosure of Invention
The invention combines the physicochemical characteristics of all substances in the dimethyl sulfone, adopts a double-tower rectification process scheme to collect dimethyl sulfone fraction from the tower top in a negative pressure environment according to the difference of respective boiling points, thereby obtaining a high-purity dimethyl sulfone product.
According to the difference of the boiling points of water, inorganic salt, dimethyl sulfoxide and a target product dimethyl sulfone which are greatly influenced by the degree of correlation, a double-tower rectification mode (a reboiler is shared by primary and secondary towers) is utilized to extract the concentrated heavy component inorganic salt and a certain amount of dimethyl sulfone at the reboiler at the bottom of the primary and secondary towers in a vacuum state, a mixture of light component dimethyl sulfoxide and water is extracted from the top of the primary tower, and the target product dimethyl sulfone is extracted from the top of the secondary tower.
Aiming at the problems, the invention provides a device for producing dimethyl sulfone by double-tower rectification, wherein a feeding pipe is connected with the middle part of a mother rectifying tower, the bottom part of the mother rectifying tower is connected with a reboiler, the reboiler is connected with the bottom part of a subsidiary rectifying tower, the top part of the subsidiary rectifying tower is connected with an atomizing crystallizer, the atomizing crystallizer is connected with a first storage tank, one path of the atomizing crystallizer is connected to a product area after the atomizing crystallizer and the bottom part of the first storage tank are respectively converged by a pipeline, and the other path of the atomizing crystallizer is connected to the upper part of the subsidiary rectifying tower.
The top of the mother rectifying tower is connected with a condenser, and the bottom of the condenser is connected with the upper part of the mother rectifying tower.
The condenser is connected with a second storage tank, and the second storage tank is connected with a storage tank after being converged with the bottom of the condenser through a pipeline; the bottom of the reboiler is connected with the storage tank. Vacuum tubes are arranged on the first storage tank, the second storage tank and the storage tank. The height of the mother rectifying tower is higher than that of the son rectifying tower, and the height of the son rectifying tower is higher than that of a feed inlet of the mother rectifying tower. The difference in the heights of the sub-sub columns depends on the separation efficiency (degree of separation per unit time and amount of separation).
The invention also provides a process for producing dimethyl sulfone by double-tower rectification, which comprises the following steps:
starting a reboiler, vacuumizing a mother rectifying tower and a sub rectifying tower, when the vacuum degree reaches more than 85KPa, feeding a to-be-distilled separated substance into the mother rectifying tower from a feeding hole, performing vacuum rectification, controlling the reflux ratio of reflux liquid at the top of the sub rectifying tower to be about 1-2 generally to achieve the purpose of controlling the temperature at the top of the sub rectifying tower, controlling the temperature at the top of the sub rectifying tower to be 140-145 ℃ under the vacuum degree, so that a large amount of qualified dimethyl sulfone is extracted from the top of the sub rectifying tower, and under the same working condition, the temperature is closer to a low value, the product purity is higher, a large amount of dimethyl sulfone is extracted from the top of the sub rectifying tower, and the top fraction of the sub rectifying tower is granulated and screened by an atomizing crystallizer to obtain a dimethyl sulfone product; the mixture of dimethyl sulfoxide and water extracted from the mother rectifying tower is recycled; and inorganic salt is extracted from the bottoms of the mother rectifying tower and the son rectifying tower. Because dimethyl sulfone has the physical characteristic of sublimation and has a low flash point, the dimethyl sulfone is more suitable for realizing the rectification operation in a vacuum state.
The inside of the mother rectifying tower and the inside of the son rectifying tower are controlled to be operated at negative pressure, the inside of the mother rectifying tower and the inside of the son rectifying tower are operated at negative pressure, the vacuum degree is usually over 85KPa, the vacuum degree is regularly fluctuated under the local atmospheric pressure, the operation load in the towers and the change of the components of the to-be-fractionated matters, and the temperature of the vacuum degree is controlled at the boiling point of dimethyl sulfone under the corresponding vacuum degree and is normally between 140 ℃ and 145 ℃. The negative pressure is mainly used for reducing the boiling point of the dimethyl sulfone and saving energy consumption, the control of the tower top temperature is related to the actual operation negative pressure in the tower, the higher the vacuum degree is, the lower the tower top temperature is, the change is according to Y (temperature) = K (100-vacuum degree), and the unit KPa of the vacuum degree is. The distillate to be separated comprises crude dimethyl sulfone or a purified isolate obtained after dimethyl sulfoxide finished products are converted into dimethyl sulfone.
The number of the mother rectifying tower or the son rectifying tower is more than or equal to 2 but not limited to 2, and the process can also be realized by adopting multi-tower multi-stage rectification or a mode of upper tower and lower tower. When the concentration of the inorganic salt at the bottoms of the sub-rectifying tower and the mother rectifying tower reaches 20%, the extracted residual liquid, the distillate at the top of the mother rectifying tower, the target distillate to be distilled and the target separator to be distilled return to the sub-rectifying tower and the mother rectifying tower for circulation.
The technical scheme of the invention is that under the vacuum state of 85KPa or above, the boiling point of water is about 45 ℃, the boiling point of dimethyl sulfoxide is 106 ℃, the boiling point of dimethyl sulfone is 145 ℃, and the boiling point of inorganic salt is above 200 ℃. Under the vacuum degree, the temperature of the tower bottom is maintained at the working condition of above 160 ℃ (the temperature is related to the temperature of the feeding point of the mother tower, the temperature of the feeding point is required to be maintained above the boiling point of dimethyl sulfoxide and water and below the boiling point of dimethyl sulfone), a to-be-rectified isolate enters from the feeding point at the middle upper part of the mother tower, because dimethyl sulfoxide and water have good intersolubility, dimethyl sulfoxide and water are effectively separated from the top of the mother tower, the possibility of dimethyl sulfoxide and water reaching the tower bottom is effectively controlled, inorganic salt and dimethyl sulfone at the bottom of the mother and mother tower are rectified, wherein a large amount of dimethyl sulfone moves towards the top of the son tower (the temperature at the top of the son tower is controlled above the boiling point of dimethyl sulfone through a reflux ratio), and finally a high-purity dimethyl sulfone product (which can be increased from the traditional 99.9% to above 99.95%, the crystal grain color conformity is stronger, and trace metal elements can be controlled below 10 ppm) is extracted from the top of the son tower, along with the continuous extraction of the to-be-separated objects at the top of the primary and secondary towers, the concentration of inorganic salts at the bottom of the primary and secondary towers is continuously increased, and when the concentration of the inorganic salts in the kettle residue at the bottom of the tower reaches about 20 percent (or the temperature of the bottom of the tower continuously increases under the same working condition), the operation mode of intermittently discharging the kettle residue is adopted to reduce the concentration of the kettle residue at the bottom of the tower, so that the balance of the whole system is maintained.
The distillate at the top of the primary tower and the residue at the bottom of the secondary tower enter a pre-treatment procedure and then return to primary and secondary double-tower circulation together with the target to-be-distilled fraction.
The process scheme breaks through the traditional long-term low-temperature crystallization centrifugal separation mode by adopting a rectification separation mode in a vacuum state, and greatly improves the purity and quality grade of the product; the selected rectification equipment is double-tower rectification, the double towers share a reboiler, the purpose is to save energy consumption, but not limited to the double towers, and the purpose can be realized by adopting multiple isolated towers step by step.
Drawings
FIG. 1 is a device for producing dimethyl sulfone by double-tower rectification, wherein 1 is a mother rectification tower, 2 is a son rectification tower, 3 is a reboiler, 4 is an atomization crystallizer, 5 is a storage tank, 6 is a condenser, 7 is a feeding pipe, 8 is a first storage tank, 9 is a second storage tank, and 10 is a vacuum pipe.
Detailed Description
Example 1
Device of two tower rectification production dimethyl sulfone, inlet pipe 7 is connected with 1 middle part of mother rectifying column, and 1 bottom of mother rectifying column is connected with reboiler 3, and reboiler 3 is connected with 2 bottoms of son rectifying column, and 2 tops of son rectifying column are connected with atomizing crystallizer 4, and atomizing crystallizer 4 is connected with storage tank 8 bottom respectively through pipeline converge back all the way and is connected to the product area, is connected to 2 upper portions of son rectifying column all the way.
The top of the mother rectifying tower 1 is connected with a condenser 6, and the bottom of the condenser 6 is connected with the upper part of the mother rectifying tower 1.
The condenser 6 is connected with the second storage tank 9, and the second storage tank 9 is connected with the storage tank 5 after being converged with the bottom of the condenser 6 through a pipeline; the bottom of the reboiler 3 is connected with a storage tank 5.
The first storage tank 8, the second storage tank 9 and the storage tank 7 are all provided with vacuum tubes 10.
The height of the mother rectifying tower 1 is higher than that of the son rectifying tower 2, and the height of the son rectifying tower 2 is higher than that of a feed inlet of the mother rectifying tower 1.
Example 2
The operation of the technological scheme of producing high purity dimethyl sulfone based on double column rectification principle includes:
after the distillate is separated, the distillate enters a mother tower from a mother tower feeding point, and water, dimethyl sulfoxide and a small amount of dimethyl sulfone are extracted from the top of the mother tower;
through controlling the reflux ratio, a large amount of dimethyl sulfone with higher purity is extracted from the top of the sub-tower; the primary and secondary tower bottoms adopt a continuous or intermittent kettle residue discharging operation mode to timely remove the dimethyl sulfone solution with the rising inorganic salt concentration; the bottoms of the tower bottom and the distillate at the top of the mother tower are pretreated and then return to the double towers together with the separator to be distilled, so that the dimethyl sulfone is recycled. And granulating and screening the top fraction of the sub-tower by an atomizing crystallizer to obtain a high-purity dimethyl sulfone product. The bottom kettle residue extraction separation mode can be operated intermittently or controlled continuously.
Example 3
An example of the operation of a process scheme for the production of high purity dimethyl sulfone using the principle of double column rectification:
when the vacuum degree in the tower reaches more than 85KPa, introducing the distillate (the content of dimethyl sulfone is more than or equal to 95%, the content of water is less than or equal to 2%, the content of inorganic salt is less than or equal to 2%, and the content of dimethyl sulfoxide is less than or equal to 1%) to be distilled into the mother tower from the feeding point of the mother rectifying tower, controlling the temperature of the bottom of the mother tower at about 160 ℃, directly ascending from the stripping section of the mother rectifying tower due to the fact that the low-boiling point substances of water and dimethyl sulfoxide can not reach the bottom of the mother rectifying tower, and extracting from the top of the mother rectifying tower with a small amount of dimethyl sulfone; dimethyl sulfone and salts with higher boiling points enter the sub-rectifying tower through the reboiler, the temperature at the top of the tower is maintained at 145 ℃ by controlling the reflux ratio, usually 1.5, and a large amount of dimethyl sulfone with higher purity is extracted from the top of the sub-rectifying tower; the dimethyl sulfone solution with the rising inorganic salt concentration is timely removed from the bottoms of the primary and secondary towers in an intermittent kettle residue discharging operation mode; the bottoms of the tower bottom and the distillate at the tower top of the mother rectifying tower are pretreated and then return to the double towers together with the separator to be distilled, so that the recycling of the dimethyl sulfone is realized. And (3) rapidly granulating and solidifying the top fraction of the sub-rectifying tower by an atomizing crystallizer under the action of cold nitrogen, and screening to obtain a high-purity dimethyl sulfone product.
The product purity of the technical scheme is high, the main content can reach 99.9%, and the one-time separation recovery rate of the product can reach more than 85%.
And the crystal granularity of the crystallizer can be controlled according to the requirements of customers, and the requirements of the granularity between 20 meshes and 80 meshes of the crystallization grade exceeding 70 percent, the fineness grade and the superfine grade are met.
Example 4
An example of the operation of a process scheme for the production of high purity dimethyl sulfone using the principle of double column rectification:
when the vacuum degree in the tower reaches more than 90KPa, introducing the distillate (the content of dimethyl sulfone is more than or equal to 95%, the content of water is less than or equal to 2%, the content of inorganic salt is less than or equal to 2%, and the content of dimethyl sulfoxide is less than or equal to 1%) to be distilled into the mother tower from the feeding point of the mother rectifying tower, controlling the temperature of the bottom of the mother tower at about 158 ℃, directly ascending from the stripping section of the mother rectifying tower due to the fact that the low-boiling point substances of water and dimethyl sulfoxide can not reach the bottom of the mother rectifying tower, and extracting from the top of the mother rectifying tower with a small amount of dimethyl sulfone; dimethyl sulfone and salts with higher boiling points enter the sub-rectifying tower through the reboiler, the temperature at the top of the tower is maintained at 140 ℃ by controlling the reflux ratio to be 2 at all times, and the dimethyl sulfone with higher purity is extracted from the top of the sub-rectifying tower; the dimethyl sulfone solution with the rising inorganic salt concentration is timely removed from the bottoms of the primary and secondary towers in an intermittent kettle residue discharging operation mode; the bottoms of the tower bottom and the distillate at the tower top of the mother rectifying tower are pretreated and then return to the double towers together with the separator to be distilled, so that the recycling of the dimethyl sulfone is realized. And (3) rapidly granulating and solidifying the top fraction of the sub-rectifying tower by an atomizing crystallizer under the action of cold nitrogen, and screening to obtain a high-purity dimethyl sulfone product.
The product purity of the technical scheme is high, the main content can reach 99.90 percent, and the one-time separation recovery rate of the product can reach more than 80 percent.
And the crystal granularity of the crystallizer can be controlled according to the requirements of customers, and the requirements of the granularity between 20 meshes and 80 meshes of the crystallization grade exceeding 70 percent, the fineness grade and the superfine grade are met.
Claims (6)
1. The process for producing dimethyl sulfone by double-tower rectification is characterized by comprising the following steps:
starting a reboiler, when the vacuum degree reaches more than 85KPa, feeding a to-be-distilled isolate into a mother rectifying tower from a feed inlet, wherein the to-be-distilled isolate comprises crude dimethyl sulfone or a purified isolate obtained after dimethyl sulfoxide finished products are converted into dimethyl sulfone, performing vacuum rectification, controlling the reflux ratio of reflux liquid at the top of a sub-rectifying tower to be 1-2, controlling the temperature at the top of the sub-rectifying tower to be 140-145 ℃ under the vacuum condition, extracting the dimethyl sulfone from the top of the sub-rectifying tower, and granulating and screening the top of the sub-rectifying tower by an atomizing crystallizer to obtain a dimethyl sulfone product; the mixture of dimethyl sulfoxide and water extracted from the mother rectifying tower is recycled; inorganic salt is extracted from the bottoms of the mother rectifying tower and the son rectifying tower, negative pressure is adopted in the mother rectifying tower and the son rectifying tower, the vacuum degree is more than 85KPa, the temperature in the mother rectifying tower and the son rectifying tower is controlled to be 140 plus 145 ℃, and the process adopts the following devices: inlet pipe (7) are connected with female rectifying column (1) middle part, female rectifying column (1) bottom is connected with reboiler (3), reboiler (3) are connected with son rectifying column (2) bottom, son rectifying column (2) top is connected with atomizing crystallizer (4), atomizing crystallizer (4) are connected with storage tank (8), atomizing crystallizer (4) and storage tank (8) bottom are joined the back through the pipeline respectively and are connected to the product area all the way, be connected to son rectifying column (2) upper portion all the way, storage tank (8), storage tank two (9), all be provided with vacuum tube (10) on storage tank (5).
2. The process for producing dimethyl sulfone by double column rectification as claimed in claim 1, wherein the number of the mother rectification column or the son rectification column is 2 or more, and the process can adopt multi-column multi-stage rectification.
3. The process for producing dimethyl sulfone by double-tower rectification as claimed in claim 1, wherein when the concentration of inorganic salts at the bottoms of the subsidiary rectification tower and the mother rectification tower reaches 20%, the extracted residual liquid, the overhead product of the mother rectification tower and the target to-be-distilled fraction isolate are returned to the subsidiary rectification tower and the mother rectification tower for circulation.
4. The process for producing dimethyl sulfone by double column rectification according to claim 1, wherein the top of the mother rectification column (1) is connected with a condenser (6), and the bottom of the condenser (6) is connected with the upper part of the mother rectification column (1).
5. The process for producing dimethyl sulfone by double-tower rectification according to claim 4, characterized in that the condenser (6) is connected with the second storage tank (9), and the bottoms of the second storage tank (9) and the condenser (6) are connected with the storage tank (5) after being converged by a pipeline; the bottom of the reboiler (3) is connected with a storage tank (5).
6. The process for producing dimethyl sulfone by double column rectification according to claim 1, wherein the height of the mother rectification column (1) is higher than that of the son rectification column (2), and the height of the son rectification column (2) is higher than the feed inlet height of the mother rectification column (1).
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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 |
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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 |
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