Utilization method of linalool raw product refining raffinate synthesized by 6-methyl-5-heptenyl-2-one

A crude product, linalool technology, applied in the field of utilization of the refined raffinate of the crude product of linalool synthesized from 6-methyl-5-hepten-2-one, to reduce the amount of refined raffinate, improve the utilization value, The effect of reducing pollution

Inactive Publication Date: 2011-03-23
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The invention provides a method for utilizing the refined raffinate of the crude product of linalool synthesized from 6-methyl-5-hepten-2-one, which obtains tetrahydrolinalool from the refined raffinate through processes such as hydrogenation and separation Alcohol, the technical problem to be solved is not only to improve the utilization value of the refined raffinate, but also to reduce the pollution to the environment, so as to make up for the defects in the existing technology

Method used

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  • Utilization method of linalool raw product refining raffinate synthesized by 6-methyl-5-heptenyl-2-one
  • Utilization method of linalool raw product refining raffinate synthesized by 6-methyl-5-heptenyl-2-one
  • Utilization method of linalool raw product refining raffinate synthesized by 6-methyl-5-heptenyl-2-one

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～8

[0025] The test raw material is the refined raffinate of the crude product of linalool synthesized from isoprene by 6-methyl-5-hepten-2-one, which contains 24.9wt% of dihydrolinalool, 46.3 wt% of linalool wt%, dehydrolinalool 0.5wt%, (gas chromatographic analysis, area normalized quantification), others are mainly polymer impurities.

[0026] Place a rectification column in a 0.5L three-neck flask, and carry out rectification of the crude product refining raffinate to remove heavy component impurities. The inner diameter of the rectification column is 25mm, the length of the column is 700mm, and it is filled with φ3mm stainless steel packing. The vacuum of the system is obtained by a 2ZX-4 rotary vane vacuum pump. The feeding amount is 300mL, and the fraction at 80-90°C is collected at the top of the rectification column.

[0027] The rectification operating conditions of Examples 1 to 8 and the corresponding rectification yields are listed in Table 1, wherein the temperature...

Embodiment 9～18

[0032] The 80~90 ℃ cut that embodiment 1~8 rectifying column top collects is mixed, as the raw material of hydrogenation reaction, wherein contains dihydrolinalool 38.4wt%, linalool 59.2wt%, dehydrolinalool 0.6 wt%.

[0033] The hydrogenation reaction is carried out in a 0.5L autoclave with stirring. The raw materials are put into the autoclave, and a catalyst is added. The catalyst is a supported catalyst with activated carbon as a carrier and palladium as an active component. The feeding amount of the raw material is 300mL, the system is replaced three times with 0.5MPa hydrogen, and then filled with hydrogen for hydrogenation reaction.

[0034] The specific hydrogenation process conditions and reaction yields of Examples 9 to 18 are shown in Table 2, wherein the amount of catalyst is based on the total amount of reactants, that is, the amount of hydrogenation reaction; the product content refers to the reaction liquid after the hydrogenation reaction is completed. The mass...

Embodiment 19～28

[0039] The hydrogenated products obtained in Examples 9-18 were cooled and mixed after separating the catalyst, wherein the mass fraction of the product tetrahydrolinalool was 94.0 wt%. The refining of tetrahydrolinalool was carried out by adopting batch rectification process, and refining was carried out in a 0.5L three-necked flask. The three-necked flask is equipped with a rectification column. The inner diameter of the rectification column is 25mm, the length of the column is 700mm, and it is filled with φ3mm stainless steel packing. The theoretical plate number of the rectification column is 16-17 with n-heptane-methylcyclohexane solution. The vacuum of the system is obtained by a 2ZX-4 rotary vane vacuum pump.

[0040] The feeding amount of each embodiment is 300mL.

[0041] First carry out vacuum rectification to remove light component impurities. The pressure at the top of the rectification column is controlled at 0.3-1.4KPa, and the light component impurities are the...

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Abstract

The invention discloses a utilization method of linalool raw product refining raffinate synthesized by 6-methyl-5-heptenyl-2-one, and the raw product refining raffinate comprises the dehydrolinalool, linalool and dihydro linalool. The utilization method comprises the following steps: carrying out the rectification on the raw product refining raffinate to remove the impurities of the heavy components, and collecting the fractions of 80 to 90 DEG C at the the tower top; carrying out the hydrogenation reaction on the collected fractions in the presence of a catalyst; cooling the product of the hydrogenation reaction, separating and recycling the catalyst, rectifying to remove the impurities of the light components, and collecting the fractions of 50 to 80 DEG C at the tower top as the impurities of the light components; performing the rectification by keeping the tower top pressure of the refining column and the tower top temperature of the rectifying column to remove the impurities of the heavy components and collect the refining product of the tetrahydrolinalool, wherein the fractions of 80 to 90 DEG C are collected at the tower top as the refining product of the tetrahydrolinalool, and the raffinate of the rectifying column comprises the impurities of the heavy components. Compared with the existing technologies, the method of the invention enhances the utilization ratio of the refining raffinate, as well as reduces the environmental pollution.

Description

technical field [0001] The invention relates to a method for utilizing the refined raffinate of the crude product synthesized from 6-methyl-5-hepten-2-one, in particular to obtaining tetrahydrogen from the refined raffinate through processes such as hydrogenation and separation. The linalool method. Background technique [0002] The synthesis of linalool by 6-methyl-5-hepten-2-one is to synthesize dehydrolinalool first, and then obtain linalool through selective hydrogenation from dehydrolinalool, so there will be Contains a certain amount of by-product dihydrolinalool and unreacted dehydrolinalool. The selective hydrogenation reaction of dehydrolinalool is shown in the following formula: [0003] [0004] Dehydrolinalool Linalool Dihydrolinalool [0005] To obtain high-purity linalool, the crude product must be subjected to vacuum distillation. During the vacuum distillation process, dihydrolinalool and dehydrolinalool are enriched in the rectification tower still, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/125C07C29/17C07C29/80
CPCY02P20/584
Inventor 翁羽飞郭世卓奚军孙超
Owner CHINA PETROLEUM & CHEM CORP
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