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Device and method for producing tri-n-butylamine by extractive rectification heavy component removal

A tri-n-butylamine, extraction and rectification technology, applied in the direction of amino compound purification/separation, organic chemistry, etc., can solve the problem of increased energy consumption of the device, the inability to discharge N-butyl butyramide, and the inability to N-butyl butanamide Eliminate problems such as the production system to achieve the effect of reducing the amount of processing and reducing energy consumption

Active Publication Date: 2019-04-30
ZHEJIANG JIANYE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The applicant's previous patent (ZL 2017100096741, tri-n-butylamine recovery method and the recovery device used) has proposed a method for recovering tri-n-butylamine from the overhead liquid of the stripping tower, and the light impurity IDA in the production system The production system is discharged and tri-n-butylamine is recovered and returned to the production system. However, during the implementation process, as the operating time of the production device increases, the impurity N-butylbutanamide with a higher boiling point continues to accumulate, while the method described in ZL 2017100096741 N-butyl butyramide cannot be discharged from the production system, and it is even more troublesome to find that N-butyl butanamide and tri-n-butylamine have formed an azeotropic system (the mass fractions of N-butyl butanamide and tri-n-butylamine are respectively 3% and 97%), so conventional rectification can't discharge N-butyl butyramide from the production system, the impurity continues to accumulate and affects the purity of product tri-n-butylamine, in order to ensure the quality purity of tri-n-butylamine More than 99.5%, the energy consumption of the whole device is constantly increasing, so it is necessary to develop a new process route to ensure that light and heavy impurities in the device are discharged from the production system at the same time

Method used

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  • Device and method for producing tri-n-butylamine by extractive rectification heavy component removal
  • Device and method for producing tri-n-butylamine by extractive rectification heavy component removal

Examples

Experimental program
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Effect test

example 1

[0050] Example 1, a kind of tri-n-butylamine production device of extracting and rectifying deweighting, consists of fixed bed reactor 1, removing n-butylamine tower 2, removing di-n-butylamine tower 3, tri-n-butylamine removing tower 4, molecule Distillation tower 5, extractive rectification tower 6 and extraction agent regeneration tower 7 are formed;

[0051] The upper part of the fixed-bed reactor 1 is a vaporization chamber, and the lower part is a fixed-bed reaction section, and the vaporization chamber is respectively provided with a raw material liquid inlet 11 and a hydrogen inlet 12;

[0052] The n-butylamine removal tower 2, the di-n-butylamine removal tower 3, the tri-n-butylamine light removal tower 4, the extractive distillation tower 6 and the extraction agent regeneration tower 7 are all rectification towers, and are all provided with a feed inlet, a tower top Distillate port and tower bottom liquid outlet; details are as follows:

[0053] The de-n-butylamine ...

Embodiment 1

[0069] Embodiment 1, using the device described in the above example 1 for the production method of tri-n-butylamine for extracting, rectifying and deweighting, the composition of the mixed raw material liquid is: the concentration of n-butanol is 15%, and the concentration of n-butylamine is 30% , the concentration of di-n-butylamine is 30%, the concentration of N-isobutyl-N, N-di-n-butylamine IDA is 0.1%, the concentration of N-butyl butyramide BBA is 0.1%, and the rest are water; Do the following steps:

[0070] The mixed raw material liquid enters the vaporization chamber of the fixed-bed reactor 1 from the raw material liquid inlet 11, and the temperature in the vaporization chamber is 250°C, so that the above-mentioned raw material liquid is vaporized into a gas; at the same time, hydrogen enters the fixed-bed reactor 1 through the hydrogen gas inlet 12 The vaporization chamber of the above-mentioned vaporized raw material liquid and hydrogen are mixed in the vaporizatio...

Embodiment 2

[0079] Embodiment 2, with respect to embodiment 1, change following parameter:

[0080] The composition of the raw material liquid is: the concentration of n-butanol is 18%, the concentration of n-butylamine is 28%, the concentration of di-n-butylamine is 32%, N-isobutyl-N,N-di-n-butylamine IDA The concentration is 0.15%, the concentration of N-butylbutyramide BBA is 0.08%, and the rest is water;

[0081] Utilize hydrogen to regulate the internal pressure of the fixed-bed reaction section of fixed-bed reactor 1 to 1.1MPa, fixed-bed reaction section arranges the catalyst after activation (the active component in this catalyst is nickel, and carrier is 4A molecular sieve, and active component content is 27%, Activation treatment by hydrogen reduction before use); the reaction temperature in the fixed-bed reactor 1 is controlled at 190°C, and the volume space velocity of the raw material liquid is 0.09h -1 .

[0082] In the n-butylamine removal tower 2, setting tower still temp...

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Abstract

The invention discloses a device for producing tri-n-butylamine by extractive rectification heavy component removal. The device comprises a fixed bed reactor, an n-butylamine removal tower, a di-n-butylamine removal tower, a tri-n-butylamine light component removal tower, a molecular distillation tower, an extractive rectification tower and an extractant regeneration tower; the bottom outlet of the molecular distillation tower, an extractant supplementing pipeline and the tower bottom liquid outlet of the extractant regeneration tower are joined by a cross tee, and then are communicated with the feed port of the extractive rectification tower; the top outlet of the molecular distillation tower is a light impurity outlet, and the tower top distillate port of the extractant regeneration tower is a heavy impurity outlet; and the tower bottle liquid outlet of the tri-n-butylamine light component removal tower is a tri-n-butylamine discharging tube. The present invention also discloses a method for producing tri-n-butylamine by extractive rectification heavy component removal through using the device. Heavy impurities (mainly including N-butylbutyramide) are discharged from the tri-n-butylamine production system in an extractive rectification manner, so the quality of the tri-n-butylamine product is ensured, and the energy consumption of the device is reduced.

Description

technical field [0001] The invention belongs to the field of low-carbon aliphatic amine production, and in particular relates to a tri-n-butylamine production device and process for extracting, rectifying and deweighting. Background technique [0002] Tri-n-butylamine, whose molecular formula is C 12 h 27 N, CAS number: 102-82-9, molecular weight 185.35, boiling point 216.0-217.0°C under normal pressure. Tri-n-butylamine is a colorless or light yellow liquid at normal temperature and pressure. It has a special odor and is weakly alkaline. It is easily soluble in ethanol, ether, etc., and slightly soluble in water. It has a wide range of industrial uses, is an important organic chemical intermediate, and is also an excellent reagent, emulsifier, extractant, insecticide and preservative. [0003] The main production process of tri-n-butylamine, such as figure 1 As shown, the raw material liquid composed of n-butylamine, di-n-butylamine and n-butanol is vaporized in the fix...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/86C07C211/07
CPCC07C209/86C07C211/07
Inventor 沈剑冯烈周国权陈云斌吴为民孙琪张建明杨泽慧
Owner ZHEJIANG JIANYE CHEM
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