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Purification method of preparing 1,2-propylene glycol by glycerine hydrogenation

A purification method and technology of propylene glycol, applied in 1 field, can solve the problems of low reaction conversion rate of propylene oxide, complicated separation process, many side reactions, etc.

Active Publication Date: 2008-09-10
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
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  • Claims
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Problems solved by technology

Although the direct non-catalytic reaction hydration technology of propylene oxide and water is adopted to avoid the defect of catalytic hydrolysis process with sulfuric acid, the theoretical atom utilization rate is high, but there are many side reactions, the separation process is also complicated, and the reaction conversion rate of propylene oxide is low. Separation energy consumption is high, raw material propylene oxide is expensive

Method used

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  • Purification method of preparing 1,2-propylene glycol by glycerine hydrogenation

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Experimental program
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Embodiment 1

[0023] Using 80% (mass) glycerin aqueous solution as raw material, the catalytic hydrogenation reaction was carried out on a pilot plant, and the composition of the reaction product is shown in Table 1. The analysis uses a gas chromatography capillary separation column, a FID detector, and n-butanol as an internal standard.

[0024] The mass composition (%) of glycerol hydrogenation reaction product of table 1

[0025] water

[0026] According to the five-tower process separation process of the present invention, firstly, the 20kg / h reaction liquid [1] from the hydrogenation reactor is pumped into the dehydration tower [2] to remove water and monohydric alcohol. Under the condition of tower bottom temperature of 130°C, vacuum degree of 75kPa and reflux ratio of 1, 6.5kg / h of the tower top discharge goes to the condenser, part of it is used as reflux, and a part of water (about 4.0kg / h) is used as hydrogenation raw material glycerin thinner. Wastewater containing a...

Embodiment 2

[0043] Using 70% (mass) bio-glycerol as raw material, water as diluent, and catalytic hydrogenation reaction, the composition of the reaction product is shown in Table 7. The analysis uses a gas chromatography capillary separation column, a FID detector, and n-butanol as an internal standard.

[0044] The mass composition (%) of table 7 bioglycerol hydrogenation reaction product

[0045] water

Methanol

ethanol

propanol

Hydroxyacetone

1,2-propanediol

ethylene glycol

Glycerin

42.56

0.26

0.54

0.28

1.03

40.28

1.70

13.30

[0046] Other conditions are carried out by embodiment 1 method. The separation and purification results are shown in Table 8.

[0047] Table 8 Purification results of biological glycerol hydrogenation reaction product (mass composition of overhead material, %)

[0048] Distillation column

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Abstract

The invention relates to a purification method for products of 1, 2-propylene glycol prepared through glycerol hydrogenation. A hydrogenation product contains water, a small amount of monohydric alcohol (methanol, ethanol and propanol), hydroxyacetone, glycol, unconverted glycerol and other compounds; after five steps of vacuum rectification, namely dehydration, light-removing component, heavy-removing component, glycol removal and product refining, are carried out to the reaction products of the composition, the purity of obtained 1, 2-propylene glycol products is greater than 99.9 percent, and the separation yield coefficient of the 1, 2-propylene glycol products is greater than 95 percent; unconverted glycerol and materials containing glycol are sent to a recycling treatment system; light components containing hydroxyacetone and other substances are returned to a reactor as raw material of hydrogenation.

Description

technical field [0001] The invention relates to a method for separating and refining 1,2-propanediol, specifically a method for producing high-purity 1,2-propanediol by rectifying and purifying the reaction product of 1,2-propanediol prepared by catalytic hydrogenation of glycerin. Background technique [0002] 1,2-Propanediol is an important chemical raw material, mainly used in the manufacture of unsaturated polyester, and secondly used as a plasticizer for resins, food additives, tobacco humidifiers and antifreeze agents. At present, the main method for industrial production of 1,2-propanediol is to directly hydrate propylene oxide at 150-160°C, with a residence time of 30 minutes and a pressure of 1.2-1.4 MPa to generate an aqueous solution containing about 16% of 1,2-propanediol. The reaction is to generate dipropylene glycol (DIG) and tripropylene glycol (TPG) and a small amount of glycol with a larger molecular weight, and the reaction product is evaporated and rectif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/74
Inventor 张春雷张庆怀刘书举宁春利刘汉勇袁海英
Owner SHANGHAI HUAYI NEW MATERIAL
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