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A continuous preparing method and apparatus for cyclohexanedimethanol

A technology for cyclohexanedimethanol and dibutyl phthalate, which is applied in the field of continuous preparation of cyclohexanedimethanol, can solve the problems of complicated separation and purification equipment, low solubility of reaction raw materials, etc., so as to reduce energy consumption and simplify equipment. , the effect of reducing by-products

Active Publication Date: 2017-03-22
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem to be solved by the present invention is to overcome the low solubility of reaction raw materials and complicated separation and purification equipment in the raw material system currently used, especially to overcome the disadvantages caused by the use of different solvents in the two-stage hydrogenation reaction, by selecting suitable catalysts, raw materials and solvents , under the condition that the first-stage hydrogenation product is not separated and purified, the two-stage reactions are connected in series, and the solvent is recycled to realize continuous and efficient production of cyclohexanedimethanol

Method used

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  • A continuous preparing method and apparatus for cyclohexanedimethanol
  • A continuous preparing method and apparatus for cyclohexanedimethanol
  • A continuous preparing method and apparatus for cyclohexanedimethanol

Examples

Experimental program
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Effect test

Embodiment 1

[0069] Raw material preparation:

[0070] Put the metered butanol from the solvent tank into the esterification reaction kettle 2 through the solvent storage tank 1, then put the metered phthalic acid into the esterification reaction kettle, replace the esterification reaction system with nitrogen, and gradually heat up under stirring , as the temperature rises, the pressure of the esterification reaction system gradually reaches 1.0-1.2MPa, butanol and phthalic acid undergo esterification reaction to generate dibutyl phthalate and water, and the by-product water and excess butanol in the reaction system The water-oil phase is separated in the water separator of the esterification system, the lower water phase is slowly discharged, and the total amount of water generated is measured, and the upper oil phase solvent butanol flows into the esterification reactor again. When the discharged water phase reaches the theoretical production amount At that time, it indicates that the e...

Embodiment 2

[0075] Preparation of dibutyl phthalate and dibutyl isophthalate:

[0076] The reaction process and process conditions were the same as in Example 1, and a dibutyl phthalate / butanol solution with a concentration of 22% and a dibutyl isophthalate / butanol solution with a concentration of 20% were obtained respectively.

Embodiment 3

[0078] Hydrogenation reaction of dibutyl terephthalate:

[0079] After the dibutyl terephthalate / butanol solution in the raw material storage tank 3 is pressurized and metered by the high-pressure metering pump 4, it is mixed with the hydrogen from the first-stage hydrogen mass flow control valve 24 and preheated by the first-stage reaction preheater 28 Enter the first-stage reactor 5, carry out the hydrogenation reaction of the benzene ring in the catalyst bed at a certain temperature, pressure, and hydrogen-to-oil ratio, and the generated dibutyl cyclohexanedicarboxylate / butanol solution exits the first-stage reactor 5. The hydrogen from the second-stage hydrogen mass flow control valve 25 is preheated by the second-stage reaction preheater 29, mixed with the first-stage hydrogenation mixture, and enters the second-stage reactor 6. The ester group hydrogenation reaction is carried out at an oil ratio to generate 1, 4-cyclohexanedimethanol, the mixed product of the second-sta...

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Abstract

The invention relates to a continuous preparing method for cyclohexanedimethanol. Dibutyl phthalate is adopted as a raw material and subjected to continuous two-stage catalytic hydrogenation reactions. The method is characterized in that a same solvent is adopted by the two-stage hydrogenation reactions, a first-stage hydrogenation reaction product mixture is directly fed into a second-stage hydrogenation reactor without the need of separation and purification, a target product that is the cyclohexanedimethanol is prepared through regulating conditions of the two-stage hydrogenation processes, and a byproduct that is butanol is adopted as a phthalic acid esterification raw material for preparation of the dibutyl phthalate and is also used in a circulated manner as the solvent for the two-stage hydrogenation reactions. A precious metal supported type catalyst and a transition metal oxide catalyst are respectively adopted by the two-stage hydrogenation reactions. The method has characteristics of a short process, less side products, no intermediate purification equipment and low energy consumption. A cyclic process loop can be formed. The method is suitable for continuous production of the cyclohexanedimethanol.

Description

technical field [0001] The invention relates to a continuous preparation method and device for cyclohexanedimethanol, which adopts two-stage catalytic hydrogenation, and is characterized in that dibutyl phthalate is used as a raw material, butanol is used as a two-stage hydrogenation reaction solvent, and the one-stage hydrogenation product cyclo Dibutyl hexanedicarboxylate is not separated and purified, and the mixed product directly enters the second-stage hydrogenation reactor to generate cyclohexanedimethanol. The two-stage hydrogenation reaction is carried out continuously in series in the process, which has the advantages of short hydrogenation process and high production efficiency. The characteristics of high efficiency and low cost. Background technique [0002] Cyclohexanedimethanol is an alicyclic diol, especially 1,4-cyclohexanedimethanol (CHDM), and the United States and the former Soviet Union carried out its preparation and application research as early as the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/149C07C31/27
CPCC07C29/149C07C67/303C07C69/75C07C31/276
Inventor 王开林张磊司晓郡宁小娟张怀国肖刚李明玉吴俊华李洁
Owner CHINA PETROLEUM & CHEM CORP
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