CN210229177U - Methyl formate separation system - Google Patents
Methyl formate separation system Download PDFInfo
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- CN210229177U CN210229177U CN201920702191.4U CN201920702191U CN210229177U CN 210229177 U CN210229177 U CN 210229177U CN 201920702191 U CN201920702191 U CN 201920702191U CN 210229177 U CN210229177 U CN 210229177U
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Abstract
The utility model discloses a methyl formate piece-rate system and methyl formate separation refining technology, piece-rate system includes rectifying part and adsorption component, adsorption component is including parallelly connected setting, first adsorber and the second adsorber of being controlled respectively by the valve, and connect the product export respectively, rectifying part includes first rectifying column, for packed column or plate tower, the lower part sets up the feed inlet, upper portion sets up the extractant charge door, the first condenser of top of the tower exit linkage, the upper portion of first condenser is connected respectively in the export of first condenser, first adsorber and second adsorber, first reboiler is connected to the tower cauldron of first rectifying column, the first rectifying column of gas phase exit linkage of first reboiler. The utility model discloses an extractive distillation and the mode that adsorbs and combine together have reduced the equipment investment and the energy consumption problem that the simple dependence brought that improve rectification column plate quantity, save the investment, and the operation elasticity is big, and factor of safety is high, low in production cost.
Description
Technical Field
The utility model belongs to the technical field of methyl formate production and coal system ethylene glycol production are relevant, concretely relates to methyl formate piece-rate system.
Technical Field
Methyl formate is an important organic synthetic raw material, is widely applied to the fields of bactericides, fumigants, spices, solvents, drug synthetic raw materials, pesticides and the like, and can be used for preparing chemical products such as formic acid, methyl acetate, methyl acrylate, dimethyl formamide, dimethyl carbonate and the like. Methyl formate is also an important chemical intermediate, is extremely important in many chemical synthesis reactions of C1, and can also be used as a nontoxic carbonylation reagent. Methyl formate can also be used as a gasoline high octane additive to replace the methyl tert-butyl ether which is limited in use. In the international market, the demand of methyl formate is generally in the rising trend of short supply and demand, and the yield of methyl formate is low and the cost is high in China. At present, a methanol carbonylation method and a methanol dehydrogenation method are main methods for producing methyl formate, the product is methyl formate, a mixture of methanol and methylal, and a clamping section exists in a binary phase diagram of the methanol and the methyl formate, so that certain difficulty is brought to the preparation of more than 96 percent of methyl formate by simple rectification. In addition, a large amount of mixture containing methyl formate, methanol and methylal is generated in the production process of the coal-to-ethylene glycol, and in order to ensure the quality of ethylene glycol products and avoid the accumulation of the by-product impurities in the whole system, the by-product impurities can only be sent out to a torch system for incineration. If the mixture of the byproduct methyl acetal waste liquid of the coal-to-ethylene glycol is used as a raw material to separate and produce methyl formate, the product price of the methyl formate has good market competitiveness. On the other hand, the products such as methylal, methanol and the like obtained in the separation process can be further separated or recycled, and the method has higher utilization value.
SUMMERY OF THE UTILITY MODEL
To the problem, the utility model provides a system and methyl formate separation refining technology of separating refined methyl formate from methyl formate production process and coal system ethylene glycol waste liquid, with low costs, the energy consumption is low, operation elasticity is big, factor of safety is high.
In order to achieve the above object, the utility model adopts the following technical scheme:
a methyl formate separation system comprises a rectification part and an adsorption part,
the adsorption part comprises a first adsorber and a second adsorber which are arranged in parallel, a first valve is arranged at the inlet of the first adsorber, a second valve is arranged at the inlet of the second adsorber, the outlet of the first adsorber and the outlet of the second adsorber are connected with a product outlet,
the rectifying part comprises a first rectifying tower which is a packed tower or a plate tower, a feed inlet is formed in the lower part of the first rectifying tower, an extractant feed inlet is formed in the upper part of the first rectifying tower, a tower top outlet of the first rectifying tower is connected with a first condenser, an outlet of the first condenser is respectively connected with the upper part of the first rectifying tower, a first adsorber and a second adsorber, a tower kettle of the first rectifying tower is connected with a first reboiler, and a gas phase outlet of the first reboiler is connected with the first rectifying tower.
Two adsorbers connected in parallel can work alternately.
Further, a liquid phase outlet of the first reboiler is connected with an inlet of a second rectifying tower, a tower kettle of the second rectifying tower is connected with a second reboiler, a gas phase outlet of the second reboiler is connected with the second rectifying tower, and a liquid phase outlet of the second reboiler is connected with the extractant charging port.
Further, the outlet of the top of the second rectifying tower is connected with a second condenser, and the outlet of the second condenser is connected with the upper part of the second rectifying tower.
Further, the second rectifying tower is an atmospheric tower.
Further, the second rectifying tower is a packed tower.
Further, a second reflux tank is arranged at an outlet of the second condenser.
Furthermore, a side gas phase extraction port is arranged in the middle of the first rectifying tower.
Further, the side gas phase extraction outlet is connected with an azeotropic liquid condenser. The azeotropic liquid of methylal and methanol is taken out from the side line.
Further, the first rectifying tower is a pressurized tower or an atmospheric tower.
Further, a first reflux tank is arranged at an outlet of the first condenser.
Further, a first pump is arranged at the outlet of the first condenser.
Furthermore, heat exchange jackets are arranged on the first adsorber and the second adsorber.
Further, the heat exchange jacket is connected with steam. The water vapor is used for supplying heat to the heat exchange jacket.
Furthermore, the bottoms of the first adsorber and the second adsorber are provided with an eluted gas inlet, and the tops of the first adsorber and the second adsorber are provided with an eluted gas outlet.
Further, the elution gas outlet is connected with an elution condenser, and a gas phase outlet of the elution condenser is connected with the elution gas inlet.
Further, the purge gas is compressed nitrogen.
Further, the first adsorber or the second adsorber is a fixed bed adsorber.
Further, the first adsorber or the second adsorber is filled with polyethylene glycol copolymer microspheres, polystyrene microspheres or polyethylene glycol grafted microspheres.
The utility model discloses a rectification and the method that adsorbs the joint, adopt the mode of extractive distillation to carry out the initial gross separation to each component in the mixed solution, recycle in the adsorber adsorbent to methanol and methyl formate adsorption efficiency's difference, advance to refine methyl formate. The rectifying tower can realize primary separation by adopting a lower number of theoretical plates and adopts a pressurizing operation mode. The adsorbent is a reproducible adsorbent, the whole system can realize step-by-step separation, the separation is more thorough, the purity of the finally obtained product is higher, the industrial requirements are met, the investment is less, and the energy consumption is low.
The rectifying tower in the utility model can adopt lower theoretical plate number, thus reducing investment cost and energy consumption; the cooling can be performed by using a low-cost cooling medium such as circulating cooling water, and the cooling cost is greatly reduced. The method of adding the extracting agent effectively improves the amount of methyl formate in the discharged material at the top of the tower, lightens the load of the absorber and simultaneously ensures the purity of the product; the adsorber adopts reproducible adsorbent, can be recycled, and reduces the production cost.
The utility model has the advantages that:
1. the utility model discloses a compare in traditional technology, adopt the mode that extraction rectification and absorption combined together, reduced equipment investment and energy consumption problem that the simple dependence brought by improvement rectification column plate quantity, sparingly invest in.
2. Compared with the traditional process, the process has the advantages that due to the adoption of a side line extraction mode, disturbance can be responded as soon as possible within the design range of the rectifying tower under the condition of disturbance of material flow, and the interference on products is small; therefore, the process has high operation flexibility and high safety factor.
3. Compared with the traditional process, the utility model discloses a can palingenetic adsorbent, reduced manufacturing cost.
Drawings
Fig. 1 is a schematic structural diagram of a methyl formate separation system of the present invention.
Wherein, C1 is a first rectifying tower, C2 is a second rectifying tower, C3 is a first adsorber, C4 is a second adsorber, a is an extractant charging port, b is a charging port, V1 is a first valve, V2 is a second valve, T1 is a first reflux tank, T2 is a second reflux tank, T3 is a product storage tank, E1 is a first condenser, E2 is an azeotropic liquid condenser, E3 is a first reboiler, E4 is a second condenser, E5 is a second reboiler, E6 is an elution condenser, and P1 is a first pump.
Detailed Description
The following detailed description of the embodiments of the present invention will be made with reference to the accompanying drawings.
A methyl formate separation system comprises a rectification part and an adsorption part,
the adsorption part comprises a first adsorber and a second adsorber which are arranged in parallel, a first valve is arranged at the inlet of the first adsorber, a second valve is arranged at the inlet of the second adsorber, the outlet of the first adsorber and the outlet of the second adsorber are connected with a product outlet,
the rectifying part comprises a first rectifying tower which is a packed tower or a plate tower, a feed inlet is formed in the lower part of the first rectifying tower, an extractant feed inlet is formed in the upper part of the first rectifying tower, a tower top outlet of the first rectifying tower is connected with a first condenser, an outlet of the first condenser is respectively connected with the upper part of the first rectifying tower, a first adsorber and a second adsorber, a tower kettle of the first rectifying tower is connected with a first reboiler, and a gas phase outlet of the first reboiler is connected with the first rectifying tower.
Two adsorbers connected in parallel can work alternately.
And a liquid phase outlet of the first reboiler is connected with an inlet of the second rectifying tower, a tower kettle of the second rectifying tower is connected with the second reboiler, a gas phase outlet of the second reboiler is connected with the second rectifying tower, and a liquid phase outlet of the second reboiler is connected with the extractant charging port.
And the outlet of the top of the second rectifying tower is connected with a second condenser, and the outlet of the second condenser is connected with the upper part of the second rectifying tower.
The second rectifying tower is an atmospheric tower.
The second rectifying tower is a packed tower.
And a second reflux tank is arranged at the outlet of the second condenser.
And a side gas phase extraction outlet is arranged in the middle of the first rectifying tower.
And the side line gas phase extraction outlet is connected with an azeotropic liquid condenser. The azeotropic liquid of methylal and methanol is taken out from the side line.
The first rectifying tower is a pressurized tower or an atmospheric tower.
And a first reflux tank is arranged at the outlet of the first condenser.
And a first pump is also arranged at the outlet of the first condenser.
And heat exchange jackets are arranged on the first adsorber and the second adsorber.
The heat exchange jacket is connected with water vapor. The water vapor is used for supplying heat to the heat exchange jacket.
And the bottoms of the first adsorber and the second adsorber are provided with an eluted gas inlet, and the tops of the first adsorber and the second adsorber are provided with an eluted gas outlet.
The elution gas outlet is connected with an elution condenser, and the gas phase outlet of the elution condenser is connected with the elution gas inlet.
The purge gas is compressed nitrogen.
The first adsorber or the second adsorber is a fixed bed adsorber.
And polyethylene glycol copolymer microspheres, polystyrene microspheres or polyethylene glycol grafted microspheres are filled in the first adsorber or the second adsorber.
The methyl formate separation system of the utility model can be operated by adopting the conventional process in the field as required, and can also be operated by adopting the following method.
Example 1
The continuous operation of the system is adopted, the processing raw material comprises 57 percent of methyl formate, 7 percent of methylal, 34 percent of methanol and 2 percent of DMC mixture, the processing amount is 1000kg/h, and the method comprises the following steps:
feeding raw materials into a feed inlet of a first rectifying tower, wherein the first rectifying tower has 42 layers of tower plates in total, the feed inlet is 30 layers, pressurizing operation is carried out, the operation pressure is 0.1MPa, the temperature of a tower kettle is controlled to be 80-110 ℃, the temperature of a tower top is 35-55 ℃, the reflux ratio of the first rectifying tower is adjusted to be 2.5, the pressure drop of the whole tower is 5KPa, an extracting agent (the extracting agent is a mixture of ethanol and ethylene glycol) is added from an extracting agent feed inlet of the 3 rd layer of tower plate at the upper part of the first rectifying tower, the adding amount is 500kg/h, methyl formate (the content is more than 98 percent by weight) is distilled from the tower top for 580kg/h, the methyl formate is fed into a first adsorber and a second adsorber, and the first adsorber and the second adsorber alternately, in the process, a small amount of methanol in the methyl formate is removed, 560kg/h of methyl formate with the purity of 99 percent wt flows out from the outlet of the adsorber, and the recovery rate of the formic acid is more than 98 percent.
75kg/h of azeotrope (90 percent by weight of methylal) of methylal and methanol is extracted from the side line of the 18 th layer of the tower plate at the upper part of the first rectifying tower and collected after being condensed by an azeotropic liquid condenser, and the recovery rate of the methylal is 97 percent.
845kg/h of liquid phase discharge material of the first rectifying tower kettle is sent into a feed inlet of a second rectifying tower, 345kg/h of mixture of methanol and dimethyl carbonate (94 percent by weight of methanol) is distilled in a tower top of the second rectifying tower, and 500kg/h of liquid phase discharge material of the second rectifying tower kettle returns to an extracting agent feed inlet at the upper part of the first rectifying tower.
After the first adsorber works for 1 month, regeneration treatment is carried out. And at the moment, the distillate material at the top of the first rectifying tower is introduced into a second adsorber by switching the operation of opening a second valve and closing the first valve, saturated water vapor is introduced into a jacket of the first adsorber, the first adsorber is heated to 110 ℃, then nitrogen is introduced from the lower part of the first adsorber for purging, tail gas enters an elution condenser, condensate is introduced into a methanol product tank, and the tail gas is introduced into a compressed nitrogen gas inlet pipeline.
Example 2
The batch operation of the system described above was used to process a batch of 57% methyl formate, 7% methylal, 34% methanol, 2% DMC mixture in a batch size of 1000kg, comprising the following steps:
and disconnecting the second rectifying tower from the system, and adding the raw materials into the tower kettle of the first rectifying tower at one time. Pressurizing, wherein the operating pressure of the first rectifying tower is 0.5MPa, the tower kettle temperature of the first rectifying tower is controlled to be 100-130 ℃, the tower top temperature is controlled to be 55-65 ℃, and 200kg of extracting agent is slowly added from the top. Along with the operation, the reflux ratio of the first rectifying tower is controlled to be adjusted from 2.5 to 5, the pressure drop of the whole tower is 30kPa, 580kg of methyl formate (with the content of more than 98 percent by weight) is distilled from the tower top of the first rectifying tower and sent to the first adsorber and the second adsorber, the first adsorber and the second adsorber are alternately operated, in the process, a small amount of methanol in the methyl formate is removed, 560kg of methyl formate with the purity of 99 percent by weight is output from the adsorber, and the recovery rate of the formic acid is more than 98 percent.
75kg of azeotrope (92 percent by weight of methylal) of methylal and methanol is extracted from the upper side line of the first rectifying tower and collected after being condensed by an azeotropic liquid condenser, and the recovery rate of the methylal is 99 percent.
In operation, when the temperature of the top of the first rectifying tower is higher than 65 ℃, the top discharging and the side discharging are stopped. Regulating the whole tower to normal pressure, stopping adding the extracting agent, maintaining the temperature of the tower kettle at 100 ℃, regulating the reflux ratio to 2.5, distilling out about 340kg of a mixture of methanol and dimethyl carbonate from the tower top, and stopping extracting when the temperature of the tower top is higher than 65 ℃. Stopping heating, finishing the operation, and transferring the tower bottom liquid to an extractant tank. The feed was then added to the kettle and the next batch separation was started.
Claims (10)
1. A methyl formate separation system is characterized by comprising a rectification part and an adsorption part,
the adsorption part comprises a first adsorber and a second adsorber which are arranged in parallel, a first valve is arranged at the inlet of the first adsorber, a second valve is arranged at the inlet of the second adsorber, the outlet of the first adsorber and the outlet of the second adsorber are connected with a product outlet,
the rectifying part comprises a first rectifying tower which is a packed tower or a plate tower, a feed inlet is formed in the lower part of the first rectifying tower, an extractant feed inlet is formed in the upper part of the first rectifying tower, a tower top outlet of the first rectifying tower is connected with a first condenser, an outlet of the first condenser is respectively connected with the upper part of the first rectifying tower, a first adsorber and a second adsorber, a tower kettle of the first rectifying tower is connected with a first reboiler, and a gas phase outlet of the first reboiler is connected with the first rectifying tower.
2. The methyl formate separation system of claim 1, wherein the liquid phase outlet of the first reboiler is connected to the inlet of a second rectification column, the bottom of the second rectification column is connected to a second reboiler, the gas phase outlet of the second reboiler is connected to the second rectification column, and the liquid phase outlet of the second reboiler is connected to the extractant charging port.
3. The methyl formate separation system of claim 2, wherein the top outlet of the second rectification column is connected with a second condenser, and the outlet of the second condenser is connected with the upper part of the second rectification column.
4. The methyl formate separation system of claim 1, wherein a side gas phase extraction outlet is arranged in the middle of the first rectifying tower and is connected with an azeotropic liquid condenser.
5. The methyl formate separation system of claim 1 wherein said first adsorber and said second adsorber are provided with heat exchange jackets.
6. A methyl formate separation system as claimed in claim 1 wherein the bottoms of said first and second adsorbers are provided with an eluent gas inlet and the tops of said first and second adsorbers are provided with an eluent gas outlet.
7. A methyl formate separation system as claimed in claim 6 wherein said wash out gas outlet is connected to an elution condenser, the gas phase outlet of said elution condenser being connected to said wash out gas inlet.
8. A methyl formate separation system as claimed in claim 1 wherein said first adsorber or said second adsorber is a fixed bed adsorber.
9. The methyl formate separation system of claim 1, wherein the first or second adsorber is packed with polyethylene glycol copolymer microspheres, polystyrene microspheres, or polyethylene glycol grafted microspheres.
10. The methyl formate separation system of claim 1 wherein said first rectification column is a pressurized column or an atmospheric column.
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| CN201920702191.4U CN210229177U (en) | 2019-05-16 | 2019-05-16 | Methyl formate separation system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124345A (en) * | 2019-05-16 | 2019-08-16 | 江苏凯美普瑞工程技术有限公司 | A kind of methyl formate separation system and methyl formate separation and purification technique |
| CN115490580A (en) * | 2022-10-20 | 2022-12-20 | 西南化工研究设计院有限公司 | Process for preparing methylal and byproduct methyl formate by one-step oxidation of methanol |
-
2019
- 2019-05-16 CN CN201920702191.4U patent/CN210229177U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124345A (en) * | 2019-05-16 | 2019-08-16 | 江苏凯美普瑞工程技术有限公司 | A kind of methyl formate separation system and methyl formate separation and purification technique |
| CN115490580A (en) * | 2022-10-20 | 2022-12-20 | 西南化工研究设计院有限公司 | Process for preparing methylal and byproduct methyl formate by one-step oxidation of methanol |
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