CN102408343A - Method for synthesizing tetra-n-propylamine bromide - Google Patents

Abstract

In the production process of HZSM-5 catalyst in industry, in order to generate nanoparticles and prevent the nanoparticles from aggregating and growing, it is necessary to add a template agent tetra-n-propylamine bromide, but tetra-n-propylamine bromide still needs to be imported in China, which brings inconvenience to the catalyst industry. The present invention studies a method for synthesizing tetra-n-propylamine bromide using 1-n-propane bromide and tri-n-propylamine. Using the process, when the molar ratio of reactants is 1:1, react in a solution such as acetonitrile at 80 degrees for 22 hours, stand, filter, and dry to obtain a light yellow product with a purity of more than 99%, and the yield can reach up to 93%.

Description

A kind of method of synthesizing tetra-n-propylamine bromide

technical field

The invention relates to the field of industrially preparing HZSM-5 catalysts, in particular to a method for obtaining uniform nano-aluminum silicate particles by using tetra-n-propylamine bromide as a template in the process of industrially synthesizing the HZSM-5 catalysts. In addition, tetra-n-propylamine bromide can also be used as surfactant; solvent; intermediate; hair conditioner active ingredient; antistatic agent; washing detergent; fabric paper softener; phase transfer catalyst; bactericide; disinfectant; Slimicide; Algaecide; Emulsifier; Pigment dispersant, etc.

Background technique

As a big country in oil production and processing, my country needs to consume hundreds of millions of tons of catalysts every year. Improving the production technology of catalysts and producing catalysts with small particle size and narrow particle size distribution can prolong the service life of catalysts to a certain extent. HZSM-5 is a catalyst widely used in the petroleum industry, but due to the need for templates to control particle size and prevent particle aggregation, templates still need to be imported, so the production of HZSM-5 catalysts is limited, and product prices continue to rise. Not only for production, but also for the scientific research department to import the templating agent tripropylamine bromide from the United States or India when carrying out scientific research experiments. It is imminent to find an efficient method for synthesizing tetra-n-propylamine bromide.

Contents of the invention

Aiming at the difficulties in the current HZSM-5 production process, the invention provides a method for synthesizing tetra-n-propylamine bromide with high yield and high purity by utilizing 1-bromo-n-propane and tripropylamine.

Use 1-bromo-n-propane and tripropylamine to mix in a solvent such as diformamide, and stir vigorously under heating to increase the reaction speed. After reacting for a certain period of time, let the solution stand still, filter out the crystalline yellow or light yellow precipitate, and after drying, it will be n-tetrapropylamine bromide.

Description of drawings

See Infrared Spectrum in Attachment

Detailed ways

Example 1

A three-necked flask is used as a reaction vessel, and a thermometer, a stirring paddle, and a reflux condensing device are respectively installed in the three-necked flask; an electric stirrer is used for stirring; an electric heating mantle with a thermocouple is used for heating, and the reaction temperature is set and controlled. 1-Bromo-n-propane and tri-n-propylamine are respectively measured at a molar ratio of 1:1, and a certain proportion of solvent is added, and the solvent is selected from acetonitrile, formamide, and dimethylformamide. First, add the tri-n-propylamine solution into the three-necked flask, then slowly add the 1-bromo-n-propane solution into the flask with strong stirring, and continue to react at 70-130 degrees for 8-22 Hours, the reaction is complete when no stratification occurs in the liquid layer. Stop heating, take out the three-necked flask and let it stand for a few days. After the precipitation is complete, filter, wash, and dry to obtain n-tetrapropylamine bromide with a yield of 63%.

Example 2

Use an inert atmosphere to prevent bromine ions from being oxidized to generate bromine. Other steps are the same as example 1 [007] to obtain n-tetrapropylamine bromide with a purity of 99.9%, and the yield reaches 87%.

Example 3

The use of 1-bromo-n-propanetri-n-propylamine with a molar ratio of 1.2: 1, other steps are the same as Example 2 [008], the product purity obtained is the same as Example 2 [009], and the productive rate is increased to 93%.

Example 4

Use industrial grade reagent, other same example 3 [010], the product productive rate that obtains is the same as example 3 [010], and purity reaches more than 99%.

Example 5

Expand reagent consumption to 50 liters, other with example 4 [012], obtain productive rate and purity with example 4 [012].

Claims (8)

1. template that is used to prepare the HZSM-5 catalyzer; Can also be used for other purposes such as tensio-active agent, washing composition, sterilant; It is characterized in that: (1) can effectively prevent aggregation of particles in preparation HZSM-5 process, these particles can not be grown up, and remains nano particle size; (2) these bromination four n-propyl amine are unstable in air, and the tendency of decomposition is arranged;

2. according to the right 1 said bromination four n-propyl amine that obtain, it is characterized in that being prone to distillation;

3. according to the right 1 said bromination four n-propyl amine that obtain, it is characterized in that and sealing to preserve;

4. according to the right 1 said bromination four n-propyl amine that obtain, it is characterized in that preferably preserving at the inert atmosphere lower seal;

5. according to the right 1 said bromination four n-propyl amine that obtain, it is characterized in that and to be sucked by human body, can cause and have sore throat;

6. according to the right 1 said bromination four n-propyl amine that obtain, it is characterized in that arriving pale yellow powder for white;

7. according to the right 1 said bromination four n-propyl amine that obtain, it is characterized in that product purity is high, more than 99.9%;

8. according to the right 1 said bromination four n-propyl amine that obtain, it is characterized in that product yield is high, more than 93%.

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