Continuous preparation method of 1,4-butanediol

A technology of butanediol and succinic acid, which is applied in the field of continuous preparation of 1,4-butanediol, can solve problems such as high environmental protection pressure, large environmental pollution, and difference in reaction rate, and achieve the goal of reducing consumption and expanding the scope of use Effect

Active Publication Date: 2020-04-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the shortcomings of the Huntsman/Davy n-butane-maleic anhydride joint process route, the raw materials involved in the production come from fossil raw materials, which have serious environmental pollution and high environmental protection pressure; Under the concentration of methanol, the co-mono...

Method used

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  • Continuous preparation method of 1,4-butanediol
  • Continuous preparation method of 1,4-butanediol
  • Continuous preparation method of 1,4-butanediol

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Succinic acid enters the beating tank from the silo 1 through the metering system. The molar ratio of bio-based succinic acid (calculated as succinic acid, bio-based succinic acid raw material 1) to methanol is 1:4. Slurry made in 2 enters the monoesterification reactor 3 for monoesterification reaction, the temperature is 130°C, the pressure is 3bar, and the residence time is 1hr to obtain succinic acid monoesterification liquid, the conversion rate of succinic acid is 95% .

[0032] The succinic acid monoesterification liquid flow and the maleic acid monoesterification liquid flow (the content of monomethyl maleate is 100%, the same below) from the maleic anhydride monoesterification reactor synthesize a fluid to enter the double esterification reaction Tower 4, the mass of succinic acid monoesterification liquid accounts for 1%, using KC105 maleic anhydride esterification catalyst, and the volume space velocity of esterification liquid flow is 0.7h -1 , methanol vapor...

Embodiment 2

[0035] The molar ratio of methanol to bio-based succinic acid (in terms of succinic acid, bio-based succinic acid raw material 2) is 4:1, and the slurry is beaten in the beating tank and entered into the monoesterification reactor for monoesterification For the reaction, the temperature was 130°C, the pressure was 3 bar, and the residence time was 1 hr to obtain a succinic acid monoesterification liquid, and the conversion rate of succinic acid was 95%. The succinic acid monoesterification liquid flow and the maleic acid monoesterification liquid flow from the maleic anhydride monoesterification reactor are synthesized into one stream and enter the double esterification reaction tower, and the succinic acid monoesterification liquid accounts for 20%. KC105 maleic anhydride esterification catalyst, esterification liquid flow volume space velocity 0.7h -1 , methanol vapor is introduced into the bottom of the tower, and a small amount of methanol is passed into the top of the tow...

Embodiment 3

[0037] The molar ratio of methanol to bio-based succinic acid (in terms of succinic acid, bio-based succinic acid raw material 1) is 4:1, and the slurry is beaten in the beating tank and entered into the esterification reactor for monoesterification reaction , a temperature of 130° C., a pressure of 3 bar, and a residence time of 1 hr to obtain a succinic acid monoesterification liquid, and the conversion rate of succinic acid is 95%. The succinic acid monoesterification liquid flow and the maleic acid monoesterification liquid flow from the maleic anhydride monoesterification reactor are synthesized into one stream and enter the double esterification reaction tower, and the succinic acid monoesterification liquid accounts for 50%. KC105 maleic anhydride esterification catalyst, esterification liquid flow volume space velocity 0.7h -1 , methanol vapor is introduced into the bottom of the tower, and a small amount of methanol is passed into the top of the tower at the same time...

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Abstract

The invention discloses a continuous preparation method of 1,4-butanediol. The method comprises the following steps: carrying out a monoesterification reaction on bio-based succinic acid and methanolto obtain a succinic acid monoesterification liquid containing succinic acid monomethyl ester; mixing with monomethyl maleate to obtain a mixed esterification liquid; feeding into a double esterification reaction tower, and carrying out a double esterification reaction to generate a mixture of dimethyl succinate and dimethyl maleate; feeding the mixture into a hydrogenation reactor, and carrying out a hydrogenation reaction, wherein the the dimethyl maleate in the mixture is hydrogenated to generate dimethyl succinate; and performing a cascade reaction to convert into an intermediate product gamma-butyrolactone, and then generating 1,4-butanediol and tetrahydrofuran. According to the method, the bio-based succinic acid is adopted to partially replace monomethyl maleate to produce 1,4-butanediol, so that the consumption of petroleum chemicals is reduced, and the production cost of 1, 4-butanediol is reduced; and bio-based succinic acid and methanol are subjected to a monoesterificationreaction, and then mixing is performed with monomethyl maleate, so that the mutual influence caused by co-monoesterification of succinic acid and maleic anhydride is avoided.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and relates to a continuous preparation method of 1,4-butanediol. Background technique [0002] 1,4-Butanediol (BDO) is an important basic organic chemical raw material, mainly used in the production of tetrahydrofuran (THF), polybutylene terephthalate (PBT), γ-butyrolactone and polyurethane ( PU). At present, the more advanced BDO production process in the world is the Huntsman / Davy n-butane-maleic anhydride combined process route. More than 25% of the production capacity comes from the maleic anhydride method, and this method is often used in new plants. The method is that butane is oxidized to generate maleic anhydride, maleic anhydride undergoes monoesterification first to generate monomethyl maleate, and monomethyl maleate undergoes double esterification in the esterification tower to generate dimethyl maleate , Dimethyl ester is hydrogenated and catalyzed to produce BDO and other by-produ...

Claims

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Application Information

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IPC IPC(8): C07C29/149C07C31/20C07D307/08
CPCC07C29/149C07D307/08C07C67/08C07C67/303C07D307/33C07C31/207C07C69/40C07C69/60
Inventor 唐建兴仲军实陈志明
Owner CHINA PETROLEUM & CHEM CORP
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