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Method for preparing n-eicosane by normal pressure chaining

A technology of n-eicosane and normal pressure, which is applied in the field of preparation of n-eicosane in the normal pressure link, can solve the problems of complex process conditions, high operation risk, low safety factor, etc., and achieve purity and yield improvement, process Simple, Efficiency-Enhancing Effects

Inactive Publication Date: 2011-03-23
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Although the above methods can prepare the corresponding n-alkane monomers, there are certain problems in each method; the first method has relatively complicated process conditions, high requirements for certain equipment and materials, and a large investment scale, which is only applicable to It is suitable for large-scale petrochemical production; the second method is suitable for symmetrical even-numbered alkanes, and the product needs to be repeatedly purified by ether, and the raw materials with a positive octadecyl carbon chain are not easy to obtain; the third and fourth methods are dangerous to operate. It is easy to erupt in the violent reaction of sodium and haloalkane, with low safety factor and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A method for preparing n-eicosane through atmospheric pressure linkage, the steps of preparation are:

[0025] (1) Take brominated n-decane 2211.80g (10mol) for subsequent use;

[0026] (2) Weigh 232.30g (10.1mol) of sodium metal and cut it into small strips with an area of ​​about 1×3cm 2 ,spare;

[0027] (3) Add 50g of n-bromodecane reaction solution and 20g of sodium metal into the reaction kettle, stir and heat up to 80°C, remove the heat source, and rely on the exothermic reaction of n-bromide and sodium metal to maintain the temperature of the reaction system at 120 ℃, continuously dropwise add the remaining n-bromodecane reaction solution and the remaining sodium metal, and keep the reaction system in a slight reflux state. After the addition of the two is completed, raise the temperature to 160 ℃ and keep the temperature for 3 hours;

[0028] (4) 400g 95% ethanol and 1000ml water are added successively in the reactor to precipitate the reactant, separate the o...

Embodiment 2

[0031] A method for preparing n-eicosane through normal pressure linkage, the steps are:

[0032] (1) Take brominated n-decane 2211.80g (10mol) for subsequent use;

[0033] (2) Weigh 232.30g (10.1mol) of sodium metal and cut it into small thin strips with an area of ​​about 1×3cm 2 ,spare;

[0034] (3) Put 50g of n-bromodecane reaction solution and 20g of sodium metal into the reaction kettle, stir and heat up to 80°C, remove the heat source, and rely on the exothermic reaction of n-bromide and sodium metal to maintain the temperature of the reaction system at 130 ℃, continuously drop the remaining n-bromodecane reaction solution and the remaining sodium metal, and keep the reaction system in a slight reflux state. After the addition of the two is completed, control the temperature at 140 ℃ and keep the temperature for 3 hours;

[0035] (4) 400g 95% ethanol and 1000ml water are added successively in the reactor to precipitate the reactant, separate the organic phase, wash th...

Embodiment 3

[0038] A method for preparing n-eicosane through normal pressure linkage, the steps are:

[0039] (1) get brominated n-decane 2211.8g (10mol) for subsequent use;

[0040] (2) Weigh metal sodium 232.30 (10.1mol) and cut it into small thin strips with an area of ​​about 1×3cm 2 ,spare;

[0041] (3) Put 50g of n-bromodecane reaction solution and 20g of sodium metal into the reactor, stir and heat up to 80°C, remove the heat source, and rely on the exothermic reaction of n-bromodecane and sodium metal to maintain the temperature of the reaction system at 140 ℃, continuously dropwise add the remaining n-bromodecane reaction solution and the remaining sodium metal, and keep the reaction system in a slight reflux state. After the addition is complete, control the temperature at 150 ℃ and keep the temperature constant for 3 hours;

[0042] (4) 400g 95% ethanol and 1000ml water are added successively in the reactor to precipitate the reactant, separate the organic phase, wash the org...

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Abstract

The invention relates to a method for preparing n-eicosane by normal pressure chaining, which comprises the following steps of: (1) weighing bromodecane for later use; (2) weighing metal sodium and cutting the metal sodium into small and thin strips for later use; (3) reacting the bromodecane and the metal sodium completely; (4) precipitating and separating an organic phase; (5) obtaining n-eicosane product by distilling, rectifying and passivating. In the preparation method in the invention, strong oxidizers such as concentrated sulfuric acid and acidic potassium permanganate are used for oxidizing unsaturated organic substances and alcoholic impurities to remove impurities, so that the purity of a product is improved; the raw materials for the preparation are fully supplied in the market, the purity and yield of the obtained product both are relatively high, and production efficiency is improved to a certain extent.

Description

technical field [0001] The invention belongs to the field of chemical reagents, in particular to a method for preparing n-eicosane through atmospheric pressure linkage. Background technique [0002] As one of the key components of diesel oil, low-temperature improver and environmentally friendly liquid fuel composition, n-paraffin has been widely used. extremely important role. At present, due to the different sources of n-alkanes, the composition of various n-alkanes is different, resulting in different degrees of differences in products. Therefore, some special n-alkanes monomers are needed to adjust the component distribution ratio of n-alkanes so that Its quality can be guaranteed to the greatest extent. After reviewing domestic and foreign data, the methods for preparing normal alkanes are summarized as follows: [0003] 1. Adopt the mixture of molecular sieve or urea dewaxing n-alkanes, and then conduct segmental freezing to separate n-alkanes monomers. Typical proce...

Claims

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Application Information

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IPC IPC(8): C07C9/22C07C1/26C07C7/148C07C7/171
Inventor 石开丁
Owner TIANJIN CHEM REAGENT RES INST
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