Preparation method of C12 tertiary alkyl primary amine

A technology of tertiary alkyl primary amines and propylene tetramers, which is applied in the field of compound preparation, can solve the problems of cumbersome production methods, high cost, and difficult wastewater treatment, and achieve the goals of reducing unit consumption, reducing pollution, and reducing the total amount of wastewater Effect

Active Publication Date: 2022-03-29
潍坊滨海石油化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although CN1223254A and CN105051002A have been improved on this, the production method is too loaded down with trivial details, need to carry out two-step reaction, described two-step reaction is still based on Ritter reaction as principle, and Ritter reaction is carried out under sulfuric acid catalysis, after the first step reaction , Sulfuric acid continues to provide an acidic environment for the second hydrolysis reaction, and sulfuric acid is not separated, which leads to the need to consume excessive alkaline compounds to neutralize sulfuric acid, and will produce a large amount of alkaline wastewater containing various cations and anions. Wastewater treatment is difficult and costly

Method used

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  • Preparation method of C12 tertiary alkyl primary amine
  • Preparation method of C12 tertiary alkyl primary amine
  • Preparation method of C12 tertiary alkyl primary amine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add organic raw materials and hydrogen cyanide dropwise and keep warm

[0030] Weigh 100g of propylene tetramer (purity above 99%) in the reaction vessel, add 95g of 80% sulfuric acid solution (newly prepared or re-coated) dropwise to the reaction vessel through the constant pressure dropping funnel, about 1min Finally, add 18.5g of hydrogen cyanide into the reaction vessel through a constant-pressure dropping funnel, control the cooling temperature and dropping speed, and ensure that the temperature of the reaction solution is below 30°C;

[0031] The dropping speed of sulfuric acid solution and hydrogen cyanide is set, and the dropwise addition can basically be completed at the same time. After the dropwise addition, the temperature is stepped up, and the temperature is kept at 30°C, 40°C, and 50°C for 1 hour respectively.

[0032] (2) Hydrolysis, extraction, separation

[0033] After the heat preservation is over, add 100g of water to the reaction solution, stir...

Embodiment 2

[0037] (1) Add organic raw materials and hydrogen cyanide dropwise and keep warm

[0038] Weigh 100g of propylene tetramer (purity above 99%) in the reaction vessel, add 112g of 80% sulfuric acid solution (newly prepared or returned) dropwise to the reaction vessel through the constant pressure dropping funnel, about 1min Finally, add 18.5g of hydrogen cyanide into the reaction vessel through a constant pressure dropping funnel, control the cooling temperature and the dropping speed, and ensure that the temperature of the reaction solution is below 30°C;

[0039] The dropping speed of sulfuric acid solution and hydrogen cyanide is set, and the dropwise addition can basically be completed at the same time. After the dropwise addition, the temperature is stepped up, and the temperature is kept at 25°C, 35°C, and 60°C for 2 hours each.

[0040] (2) Hydrolysis, extraction, separation

[0041] After the heat preservation is over, add 100g of water to the reaction solution, stir at...

Embodiment 3

[0045] (1) Add organic raw materials and hydrogen cyanide dropwise and keep warm

[0046] Weigh 100g of propylene tetramer (purity above 99%) in the reaction vessel, add 76g of 80% sulfuric acid solution (newly prepared or returned) dropwise to the reaction vessel through the constant pressure dropping funnel, about 1min Finally, add 18.5g of hydrogen cyanide into the reaction vessel through a constant pressure dropping funnel, control the cooling temperature and the dropping speed, and ensure that the temperature of the reaction solution is below 30°C;

[0047] The dropping speed of sulfuric acid solution and hydrogen cyanide is set, and the dropwise addition can basically be completed at the same time. After the dropwise addition, the temperature is stepped up, and the temperature is kept at 30°C, 40°C, and 70°C for 1.5h each.

[0048] (2) Hydrolysis, extraction, separation

[0049] After the heat preservation is over, add 100g of water to the reaction solution, stir at 95°C ...

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Abstract

The invention belongs to the technical field of compound preparation, and particularly relates to a preparation method of C12 tertiary alkyl primary amine, which comprises the following steps: (1) dropwise adding and carrying out heat preservation reaction; (2) hydrolysis, extraction and separation; and (3) alkaline hydrolysis rectification. The intermediate product generated by the reaction is separated through an extraction separation method, the sulfuric acid solution added in the first step is recycled, the recycling amount of the sulfuric acid solution can reach 70% or above of the original amount, the alkaline hydrolysis reaction is carried out under the alkaline condition, and due to the fact that most sulfuric acid is extracted and separated out, the product quality is improved. Therefore, the amount of alkali required for neutralizing sulfuric acid can be reduced, the reduced amount is about 50% of the original amount of alkali, the unit consumption of acid and alkali can be reduced, the total amount of wastewater can be reduced by more than 75%, the unit consumption is reduced, and the cost is saved.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, in particular to a preparation method of C12 tertiary alkyl primary amine. Background technique [0002] C12 tertiary alkyl primary amine is a kind of aliphatic primary amine with multi-branched alkyl, the nitrogen atom in the amino group is connected with a tertiary carbon functional group to form a tertiary alkyl structure. This substance has unique chemical and physical properties, and its main use is as an additive for high-grade fuel and lubricating oil. [0003] The preparation method of the tertiary alkyl primary amine is based on the principle of the famous Ritter reaction, and its chemical reaction process is known. The current mature process is to react organic raw materials with cyanide under acidic conditions to generate intermediate products. This organic raw material is a multi-carbon linear alkyl olefin with isobutenyl or a branched olefin compound as a raw material, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C209/84C07C211/08C07C239/22
CPCC07C209/00C07C209/84C07C239/22C07C211/08
Inventor 林小鹏徐登清彭辉郑作深王龙富赵伟张伟周连宗
Owner 潍坊滨海石油化工有限公司
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