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Catalyst for decomposition of di-n-butylamine sulfate, preparation method thereof, and method for recovering di-n-butylamine and sulfuric acid

A technology for di-n-butylamine sulfate and n-butylamine sulfate, which is applied in the field of recovering di-n-butylamine and sulfuric acid, can solve the problems of high processing cost, secondary pollution and high energy consumption, achieve good catalytic activity and accelerate decomposition , the effect of large specific surface area

Active Publication Date: 2022-05-17
湖南海利常德农药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, for organic amine wastewater, sodium hydroxide is generally used to adjust the wastewater to strong alkalinity, so that the amines are freed, and then the amines are recovered by liquid separation or distillation, and the SO 4 2- Treated in the form of sodium sulfate, this method requires a large amount of sodium hydroxide, and finally forms sodium sulfate, a salt residue, causing secondary pollution
In addition, if the waste water containing di-n-butylamine sulfate is directly heated and distilled, the existing problems are: high energy consumption and high treatment cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A catalyst for the decomposition of di-n-butylamine sulfate. The catalyst for the decomposition of di-n-butylamine sulfate is essentially a mixture containing mesoporous silica hollow spheres and a template agent, specifically: dodecylamine, polyvinylpyrrolidone, Lauryl alcohol polyoxyethylene ether and polyoxyethylene fatty amine are used as templates, ethyl silicate and 3-(methacryloyloxy)propyltrimethoxysilane are used as silicon sources, and it is prepared after calcining and surface activation.

[0037]In this embodiment, the template is composed of dodecylamine, polyvinylpyrrolidone, polyoxyethylene lauryl ether, and polyoxyethylene fatty amine, and the silicon source is ethyl orthosilicate, 3-(methacryloyloxy)propyltrimethoxy The mass ratio of dodecylamine, polyvinylpyrrolidone, lauryl polyoxyethylene ether, and polyoxyethylene fatty amine is 1:3:1:3, and ethyl orthosilicate, 3-(methacryloyloxy)propyl The mass ratio of trimethoxysilane is 1:2.

[0038] A kind of...

Embodiment 2

[0048] A method for reclaiming di-n-butylamine and sulfuric acid, specifically: reclaiming di-n-butylamine and sulfuric acid from waste water containing di-n-butylamine sulfate, comprising the following steps:

[0049] (1) Decomposition: Add 800g of di-n-butylamine-containing sulfate wastewater into a 1000mL four-necked bottle (this di-n-butylamine-containing sulfate wastewater is prepared by mixing 90g of di-n-butylamine and 710g of sulfuric acid with a mass fraction of 30%) ), add the di-n-butylamine sulfate decomposition catalyst that makes in 0.4g embodiment 1, under the protection of nitrogen, heat up and distill, collect cut, cut pH is carried out real-time monitoring, when cut pH is 10, stop heating At this time, the temperature of the raffinate at the bottom of the still was 125°C, and it was cooled to room temperature under the protection of nitrogen.

[0050] (2) Reclaim di-n-butylamine: the fraction collected after condensation, liquid separation, add 5g of anhydrou...

Embodiment 3

[0053] Investigate the reuse effect of the catalyst for di-n-butylamine sulfate decomposition made in embodiment 1, comprising the following steps:

[0054] (1) Decomposition: Add 800g of waste water containing di-n-butylamine sulfate (same as Example 2) to a 1000mL four-necked bottle, add 0.4g of the catalyst recovered in Example 2 step (3), and heat up under nitrogen protection Distill, collect fractions, monitor the pH of the fractions in real time, stop heating when the pH of the fractions is 10, and the temperature of the raffinate at the bottom of the still is 125°C. Cool to room temperature under nitrogen protection.

[0055] (2) Recover di-n-butylamine: Add 20.0 g of sodium chloride to the fraction collected after condensation, stir to dissolve and separate the liquids, add 5 g of anhydrous sodium sulfate to the upper organic phase, dry, and filter to obtain 88.6 g of di-n-butylamine Amine, the purity of di-n-butylamine is ≥95% by gas phase detection, sodium sulfate i...

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Abstract

The invention discloses a di-n-butylamine sulfate decomposition catalyst, a preparation method thereof and a method for recovering di-n-butylamine and sulfuric acid. The di-n-butylamine sulfate decomposition catalyst is made of laurylamine, polyvinylpyrrolidone, Alcohol polyoxyethylene ether, polyoxyethylene fatty amine as template, ethyl silicate and 3-(methacryloyloxy)propyltrimethoxysilane as silicon source, prepared after calcination and surface activation. The di-n-butylamine sulfate decomposition catalyst of the present invention has the advantages of large specific surface area, good catalytic activity, reusability, etc., and can effectively decompose di-n-butylamine sulfate at a relatively low temperature, so that sulfuric acid and di-n-butylamine can be Realize effective recovery under lower energy consumption, can be widely used in the recovery of sulfuric acid and di-n-butylamine, have higher adaptability and better application prospects, and its preparation method has the advantages of simple process, convenient operation, easy control, and low raw material cost. Low-level advantages, suitable for continuous large-scale mass production, and convenient for industrialized utilization.

Description

technical field [0001] The invention belongs to the field of sewage treatment, and relates to a preparation method of a catalyst for di-n-butylamine sulfate decomposition and a method for recovering di-n-butylamine and sulfuric acid from waste water containing di-n-butylamine sulfate. Background technique [0002] Di-n-butylamine, CAS: 111-92-2, molecular formula C 8 h 19 N, molecular weight 129.24, melting point: -62~-59℃, boiling point: 159~160℃, relative density (water=1): 0.76, colorless liquid with ammonia smell. Often used as a compatibilizer, medicine, pesticide. Intermediates of dyes and fine chemicals. [0003] During the use of di-n-butylamine, sulfuric acid is often used to absorb the tail gas of the workshop and equipment to prevent the pollution caused by the diffusion of di-n-butylamine, and the wastewater containing di-n-butylamine sulfate is formed. At present, for organic amine wastewater, sodium hydroxide is generally used to adjust the wastewater to st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/08B01J35/08B01J35/10B01J37/08C01B17/90C07C209/00B01J37/00C07C211/07
CPCB01J21/08C01B17/905C07C209/00B01J37/0018B01J37/082B01J35/51B01J35/61C07C211/07
Inventor 干兴利秦岳军钟若楠陈灿张海涛马林刘欢张燕曹金艳
Owner 湖南海利常德农药化工有限公司