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Recovering process of solvent tertiary butanol in production process of ammoximation

A production process and technology of tert-butanol, applied in the preparation/separation of ammonia, preparation of organic compounds, organic chemistry, etc., can solve the problems of increasing the cost of vacuum compression, adverse effects on product performance at the bottom of the column, and low temperature of the gas at the top of the column.

Inactive Publication Date: 2013-07-24
HUNAN BAILI ENGINEERING SCIENCE AND TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the above problems and reduce energy consumption, a combination of high and low pressure towers is used to separate tert-butanol by multi-effect distillation; the operating pressure of the high-pressure tower and low-pressure tower in the separation process determines the performance of the multi-effect separation. If the tower pressure is too high, the temperature of the high-pressure tower will increase, which will adversely affect the performance of the product at the bottom of the tower. Increases vacuum compression costs, or causes other operational problems, making multi-effect distillation impossible

Method used

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  • Recovering process of solvent tertiary butanol in production process of ammoximation
  • Recovering process of solvent tertiary butanol in production process of ammoximation

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Two-effect parallel rectification process of tert-butanol rectification tower, such as figure 1 As shown, the reaction liquid from the reactor enters the flash tank 1 for adiabatic flash evaporation. The operating pressure of the flash tank is normal pressure. Material preheater 3, the temperature of the material after preheating is 84 ℃, under the control of the flow rate, it is respectively sent to the middle part of the first-effect rectification tower 4 and the middle part of the second-effect rectification tower 6, and the first-effect rectification tower 4 The operating pressure is 0.3MPa (absolute pressure), the temperature at the top of the tower is 107°C, and the temperature at the bottom of the tower is 137°C. The reboiler 5 of the tower is heated by low-pressure steam, and part of the reaction liquid is vaporized in the reboiler. Separation occurs, and the materials in the tower kettle that meet the separation requirements are sent to the feed preheater 3 to ...

Embodiment 2

[0033] Two-effect countercurrent series rectification process of tert-butanol rectification tower, such as figure 2 As shown, the reaction liquid from the reactor enters the flash tank 1 for adiabatic flash evaporation. The operating pressure of the flash tank is normal pressure. Material preheater 3, the temperature of the material after preheating is 82°C, and enters the middle part of the second-effect rectification tower 6, the operating pressure in the tower is 0.045MPa (absolute pressure), the temperature at the top of the tower is 57°C, and the temperature at the bottom of the tower is 67 ℃, the reboiler 7 of the tower kettle is heated by first-effect steam, the reaction liquid is vaporized in the reboiler, rectified and separated in the tower, and after preliminary separation, the gas enters the cooling system from the top of the tower, and the reaction liquid after preliminary separation is Under the control of the flow rate, the discharge pump 9 of the second-effect...

Embodiment 3

[0038] Two-effect co-current series rectification process of tert-butanol rectification tower, such as image 3 As shown, the reaction liquid from the reactor enters the flash tank 1 for adiabatic flash evaporation, the operating pressure of the flash tank is normal pressure, the gas phase after flash evaporation enters the cooling system, and the liquid phase enters a In the middle part of the efficient rectification tower 4, the operating pressure in the tower is 0.25MPa (absolute pressure), the temperature at the top of the tower is 85°C, and the temperature at the bottom of the tower is 110°C. Internal gasification, rectification and separation in the tower, the gas phase at the top of the first-effect rectification tower 4 is discharged to the condensation side of the reboiler 7 of the second-effect rectification tower 6, and most of the gas phase is on the condensation side of the reboiler 7 Condensation, the liquid phase enters the reflux system, and the gas phase enter...

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Abstract

The invention discloses a recovering process of a solvent tertiary butanol in a production process of ammoximation. The process comprises the following steps of: combining a rectifying system by a plurality of rectifying towers and configuring corresponding re-boiler, cooling system, reverse-flow system and compressing system; recovering ammonia and tertiary butanol in a reaction liquid of a reactor by a double-effect or multi-effect rectifying tower; using the overhead gas phase of the previous rectifying tower as a heat source of the re-boiler of the next rectifying tower by setting different operating pressures of the rectifying towers so as to utilize the previous gas phase condensing heat energy, wherein the operating pressure of one rectifying tower is 0.08-0.6MPa (absolute pressure) while the operating pressure of the last rectifying tower is 0.001-0.1MPa (absolute pressure), the overhead temperature of one rectifying tower is 60-140 DEG C, while the overhead temperature of the previous rectifying tower is 10-40 DEG C higher than that of the next rectifying tower; condensing the overhead gas phases by the cooling system, controlling the discharge temperature at 10-80 DEG C, the condensate enters into the reverse-flow system, and is pressurized by a pump, and part of the condensate is fed to the rectifying tower to reverse-flow, while the other condensate is fed outside the rectifying system; and feeding noncondensable gases in the cooling system to the compressing system to be compressed and feeding outside the rectifying system. According to the tertiary butanol recovering process flow, steam consumed is just 45-65% of that consumed by a single rectifying tower.

Description

technical field [0001] The invention relates to a process for recovering tert-butanol, in particular to a process for recovering solvent tert-butanol in ammoximation production by means of multi-effect rectification. Background technique [0002] In order to make the ammoximation reaction proceed in a uniform solution, tert-butanol is introduced into the reaction solution as a solvent, so that the reactants, catalysts and reaction products are evenly distributed in the reactor. After the oximation reaction solution is filtered, the catalyst is separated from oxime, water, and tert-butanol. Since tert-butanol acts as a solvent in the reaction system, it does not participate in the reaction itself. In order to improve the utilization rate of tert-butanol, it is recovered and recycle. [0003] Since the boiling point and relative volatility of tert-butanol and oxime and water are quite different, a distillation column can be used to separate tert-butanol. The current conventi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/12C07C29/80C01C1/02
Inventor 蒋东海罗建国方军邵寒梅
Owner HUNAN BAILI ENGINEERING SCIENCE AND TECHNOLOGY CO LTD
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