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

A technology of methylcyclopentadiene manganese tricarbonyl and steam distillation, which is applied in steam distillation, organic chemistry, chemical instruments and methods, etc., can solve problems such as increased energy consumption, coking of stills, and prolonged operation time, and achieves The effect of saving heat energy, increasing the temperature of return water, and fully mixing materials

Active Publication Date: 2014-07-02
山东东昌精细化工科技有限公司
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] 1. It is necessary to continuously add water to the distillation kettle in the system to supplement the consumption of water, which affects the continuous distillation and prolongs the operation time
[0014] 2. A large amount of steam condensed water is produced during the distillation process. Due to the organic content, organic waste water is formed, which brings great pressure to environmental protection.
[0015] 3. The temperature of steam condensate water can still be close to 100°C, which contains more heat and cannot be recovered, which increases energy consumption
Although the existing steam distillation extraction process can achieve the maximum recovery of MMT, it has all the shortcomings of conventional steam distillation; while the rectification extraction process has the problem of coking in the still

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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
Comparison scheme
Effect test

example 1

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

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

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

[0061] Chromatographic test: the product contains 73.33% of methylcyclopentadiene manganese tricarbonyl (MMT for short), 0.73% of other components CMT, 0.79% of D-MMT, 0.25% of DMCPD, and about 18.8% o...

example 2

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

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

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

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

example 3

[0068] Example 3 Feeding: Methylcyclopentadiene manganese tricarbonyl reaction liquid mixture 1800kg (1400 liters, density is 1.28), because the distilled water of Example 2 is left in the kettle, so only about 1500kg of water is replenished, and the total water volume in the kettle reaches about 3600 kg, add 3kg of defoamer, omit the addition of crude salt and soda ash.

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

[0070] Chromatography 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 ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
densityaaaaaaaaaa
densityaaaaaaaaaa
densityaaaaaaaaaa
Login to view more

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

technical field [0001] The invention relates to a steam distillation device in the field of chemical separation technology and a process for separating and extracting methylcyclopentadiene manganese tricarbonyl (MMT for short) by using the device. Background technique [0002] Steam distillation technology is a common mixture separation technology in the chemical industry. Its basic composition is mainly composed of stills, condensers, oil-water separators, and pipelines and valves connected between the three. The principle of separation is: when water and compounds that are not (or hardly) soluble in water exist together, the vapor pressure of the entire system should be the sum of the vapor pressures of the components according to Dalton's law of partial pressure. That is, P=P A +P B , where P is the total vapor pressure, P A is the vapor pressure of water, P B is the vapor pressure of the water-insoluble compound. The mixture begins to boil when the sum of the vapor...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/38C07F17/00
Inventor 司志华吕家鑫方东海孙海洋
Owner 山东东昌精细化工科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap