Circulating steam distillation apparatus and process for extracting methylcyclopentadienyl manganese tricarbonyl by aid of apparatus

A methylcyclopentadiene manganese tricarbonyl, steam distillation technology, applied in steam distillation, organic chemistry, chemical instruments and methods, etc. The effect of fully mixing, increasing the return water temperature and saving heat energy

Active Publication Date: 2012-11-21
山东东昌精细化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new design for an apparatus called this inventor's cycle steam distiller (CWS) improves upon existing methods like conventional steam distills because it does away with any unnecessary steps or materials that are added during processing instead relying on evaporation techniques. It also includes various technical features including improved efficiency, reduced power consumption, automatic control over process variables, efficient recovery of residual liquid after cleanings, effective removal of harmful substances without causing damage to equipment, environmentally friendly disposal options, etc., resulting in significant benefits compared to current technologies.

Problems solved by technology

Technologies described in this patents involve separating materials based on specific properties such as size, shape, density, surface tension, hydrophility, polarity, melting points, and boiling range. However, current methods require multiple steps involving different techniques like steaming, cooling downstream, and refluxing before further processing. Additionally, traditional processes consume significant quantities of power while also producing unwanted side effects including pollution issues associated with disposers used for washing away nonvolatiles present within the product stream.

Method used

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  • Circulating steam distillation apparatus and process for extracting methylcyclopentadienyl manganese tricarbonyl by aid of apparatus
  • Circulating steam distillation apparatus and process for extracting methylcyclopentadienyl manganese tricarbonyl by aid of apparatus
  • Circulating steam distillation apparatus and process for extracting methylcyclopentadienyl manganese tricarbonyl by aid of apparatus

Examples

Experimental program
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Effect test

example 1

[0058] Example 1 Feeding: 2000kg of viscous waste residue of methylcyclopentadiene manganese tricarbonyl, crude salt (industrial sodium chloride) 150kg (3 bags), soda ash 40kg (1 bag), defoamer 6kg, tap water about 3000kg.

[0059] Heating with heat transfer oil, the set temperature of heat transfer oil is 160℃; in normal distillation, the pressure in the kettle is 0.08MPa, the water temperature in the kettle is 110℃, and the total steam distillation time is 20 hours. Obtained product 140kg, product density 1.227 g / cm 3 (20°C).

[0060] Since the product density is less than 1.3 g / cm 3 , When distilling, pay attention to closing the product outlet valve in time, control the oil-water interface, and prevent water from flowing out of the product outlet.

[0061] Chromatographic test: the product contains methylcyclopentadiene manganese tricarbonyl (referred to as MMT) 73.33%, other components CMT 0.73%, D-MMT 0.79%, DMCPD 0.25%, and the heavy component is about 18.8%. Then fi...

example 2

[0064] Example 2 Feeding: 2000kg of viscous waste residue of methylcyclopentadiene manganese tricarbonyl, crude salt (industrial sodium chloride) 250kg (5 bags), soda ash 40kg (1 bag), defoamer 3kg, tap water about 3000kg.

[0065] Heating with heat-conducting oil, the set temperature of heat-conducting oil is 160°C; in normal distillation, the pressure in the kettle is 0.09-0.1MPa, the water temperature in the kettle is 120-125°C, and the total steam distillation time is 20 hours. Obtained product 135kg, product density 1.239g / cm 3 (20°C).

[0066] Chromatographic test: the product contains MMT 75.02%, other components CMT 0.9%, D-MMT 0.73%, DMCPD 0.95%, MCPD 2.48%, heavy components about 18%, water 1053ppm. Then finally get MMT 101.3kg.

[0067] Take distilled water in the kettle to measure its density of 1.069 (20°C).

example 3

[0068] Example 3 Feeding: 1800kg of methylcyclopentadiene manganese tricarbonyl manganese reaction mixture (1400 liters, density 1.28), because the distilled water of Example 2 was left in the kettle, only about 1500kg of water was added, and the total water volume in the kettle reached about 3600 kg, add 3kg of defoamer, omit coarse salt and soda ash.

[0069] Heating with heat-conducting oil, the actual temperature of heat-conducting oil is 156-160℃; in normal distillation, the pressure in the kettle is 0.09-0.15MPa, the water temperature in the kettle is 110-125℃, and the total steam distillation time is 30 hours. Obtained product 1171kg, product density 1.347g / cm 3 (20°C).

[0070] Chromatographic test: the product contains MMT 89.5%, other components CMT 2.19%, D-MMT 0.71%, DMCPD 2.74%, MCPD 0.81%, heavy components about 2.4%, water 483ppm. Then finally get MMT 1048kg.

[0071] The distillation residue in the kettle was tested, and the residue contained about 2.5% of t...

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Abstract

The invention relates to a circulating steam distillation apparatus and a process for extracting methylcyclopentadienyl manganese tricarbonyl by the aid of the apparatus. The apparatus comprises a distillation kettle, a condenser and an oil and water separator, a heating system and a stirrer are arranged in the distillation kettle, a condensed water overflow pipe is connected between the distillation kettle and the oil and water separator, a lower discharge outlet of the oil and water separator is connected with a liquid seal pipe, and a pressure balancing pipeline is connected among the liquid sealing pipe, the oil and water separator and the condenser. The process includes adjusting the height of the liquid seal pipe and the height of the condensed water overflow pipe; filling materials and water into the distillation kettle; stirring, distilling and cooling the materials; and performing reflux and separation of water and oil by the oil and water separator. The device and the process have the advantages that useful components such as the MMT (methylcyclopentadienyl manganese tricarbonyl) can be recovered to the greatest extent, high methylcyclopentadienyl manganese tricarbonyl recovery rate can be realized, the difficult problem of coking of a distillation kettle used in a traditional rectifying process is avoided, and large quantities of fresh water and energy can be saved as compared with an existing steam distillation process.

Description

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Claims

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Application Information

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Owner 山东东昌精细化工科技有限公司
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