Emergency stop method of acetone one-step synthesis MIBK device and acetone synthesis MIBK method

An emergency shutdown and acetone technology, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve problems such as catalyst activity reduction, raw material waste, and impact on rectification process, so as to prevent reduction and loss, The effect of reducing heat

Pending Publication Date: 2019-08-09
ZHEJIANG OCEANKING DEVELOPMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Since the Pd/resin type will be affected by the temperature and the existing environment, the catalyst activity will be affected when the MIBK unit is shut down in an emergency. Impro

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1.15,000 tons / year MIBK production device; the reactor is a shell-and-tube reactor, the catalyst is filled in the tube side, and the circulating cooling water goes through the shell side; the raw materials are acetone and hydrogen, of which the purity of hydrogen is 99.8% (on a dry basis) volume fraction) above, the oxygen content is lower than 0.03% (volume fraction under dry basis), the acetone purity is greater than 99.5% (mass fraction), and the water content is lower than 0.3% (mass fraction); Cation exchange resin with 1% palladium content. The normal reaction conditions of the reactor are: reaction temperature 85°C, pressure 3.1MPa, acetone feed rate 10t / h, hydrogen feed rate 1900Nm 3 / h, cooling water flow is about 30m 3 / h, the cooling water inlet temperature is 83~85℃. The reaction result is: acetone conversion ≥ 30%, MIBK selectivity ≥ 92%.

[0026] Emergency stop procedures are as follows:

[0027] (1) stop heating the feed acetone;

[0028] (2) Increas...

Embodiment 2

[0037] The apparatus used in the experiment is identical with raw material and embodiment 1.

[0038] The reaction conditions are: temperature 90°C, pressure 3.1MPa, acetone feed rate 8.7t / h, hydrogen feed rate 1600Nm 3 / h, cooling water flow is about 28m 3 / h, cooling water inlet temperature is 88 ~ 90 ℃. The reaction result is: acetone conversion ≥ 30%, MIBK selectivity ≥ 92%. Then use the following parking steps:

[0039] (1) stop heating the feed acetone;

[0040] (2) Increase the cooling water flow rate to 45m 3 / h, and gradually reduce the cooling water temperature at a cooling rate of 9°C / h, and reduce the reactor temperature to 75°C, and at the same time gradually reduce the acetone feed in the reactor at a rate of 1.8t / h, and When the feed rate was reduced to 6.5t / h, stop reducing the acetone feed rate. Acetone continues to be fed into the reactor at a rate of 6.5t / h. Due to the high cooling water temperature and the large amount of acetone feed in the initial ...

Embodiment 3

[0047] Experiment equipment, raw material and reaction condition are identical with embodiment 1.

[0048] Use the following parking steps:

[0049] (1) stop heating the feed acetone;

[0050] (2) Maintain the cooling water flow rate, and gradually reduce the cooling water temperature at a cooling rate of 7°C / h, lower the reactor temperature to 75°C, and at the same time gradually reduce the acetone feed in the reactor at a rate of 1.8t / h , and when the acetone feed rate was reduced to 6.5t / h, stop reducing the acetone feed rate. Acetone continues to be fed into the reactor at a rate of 6.5t / h. At this time, the cooling rate of the reactor is 4-6°C / h, and the cooling time is 1.7-2.5h;

[0051] (3) When the reactor temperature drops to 75°C, the cooling water temperature continues to drop to 28°C at a cooling rate of 25°C / h, and the reactor temperature drops to 30°C. At this time, the cooling rate of the reactor is 12 to 18°C. °C / h, the cooling time is 2.5~3.8h;

[0052] (...

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PUM

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Abstract

The invention relates to an emergency stop method of an acetone one-step synthesis MIBK device and an acetone synthesis MIBK method. The emergency stop method is characterized by including the steps of firstly, stopping heating the raw material acetone; secondly, lowering the temperature of cooling water, controlling the cooling rate of the cooling water to be 1-15 DEG C/h when the temperature ina reactor is higher than 75+/-5 DEG C, and controlling the cooling rate of the cooling water to be 10-30 DEG C/h when the temperature in the reactor is lower than 75+/-5 DEG C until the temperature inthe reactor is lowered to be 15-35 DEG C; thirdly, stopping feeding the material acetone into the reactor; fourthly, guiding process water into the reactor to wet a catalyst, wherein the volume ratioof the guided process water to the catalyst is 0.35-1.2; fifthly, stopping the discharging of the reactor and stopping the feeding of nitrogen so that stopping can be completed. The emergency stop method is high in stopping speed and well protects the catalyst.

Description

technical field [0001] The invention relates to chemical reactions, in particular to a method for emergency shutdown of a methyl isobutyl ketone synthesis device from acetone and a method for synthesizing methyl isobutyl ketone from acetone. Background technique [0002] Methyl isobutyl ketone (MIBK) is an excellent medium-boiling point solvent and an important organic chemical product, mainly used in agriculture, medicine, coatings, surfactants and other fields. At present, there are three-step and one-step processes for synthesizing MIBK from acetone in industry. Among them, the one-step process is through the asynchronous and synergistic effect of multifunctional catalysts, and three reactions of condensation, dehydration, and hydrogenation occur simultaneously to generate MIBK. It has the advantages of simple process flow and low product cost, so it has become the mainstream process for MIBK production today. It is also basically a one-step process for the production pr...

Claims

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Application Information

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IPC IPC(8): C07C45/73C07C49/04B01J33/00
CPCB01J33/00C07C45/73C07C49/04
Inventor 周文斌陆佳冬夏天昊赵洪彬郑金成
Owner ZHEJIANG OCEANKING DEVELOPMENT CO LTD
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