Method for separating and purifying diisopropylamine from crude isopropamide

A technology for diisopropylamine and isopropylamine, applied in the field of chemical synthesis, can solve the problems of low diisopropylamine conversion rate, low production cost, low production process conversion rate, and high production cost, achieve energy saving and material consumption, and simple reactant composition , the effect of reducing production time

Inactive Publication Date: 2017-12-29
ANHUI HAOYUAN CHEM IND GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for separating and purifying diisopropylamine from crude isopropylamine, which has the advantages of high conversion rate of diisopropylamine and low production cost, and solves the problems of low conversion rate and high production cost of the existing production process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 70g of Hβ zeolite (SiO2 / Al2O3 molecular ratio is 30) to 250ml of 0.2M KCL solution, carry out ion exchange at a temperature of 95°C, the exchange time is 2.0h: then filter and wash until there is no C1; Dry at 60°C for 4.0h, 110°C for 4.0h; then mix with 10g of aluminum hydroxide powder, add nitric acid and deionized water, knead and extrude on the extruder, and the addition of nitric acid will account for 0.5w of the dry material %, the amount of deionized water added is subject to kneading and extruding. The bar-shaped catalyst was dried at 110°C for 4.0h, and then calcined at 550°C in a muffle furnace for 4.0h to obtain the K / Hβ zeolite-Al2O3 catalyst, which contained 0.9w% potassium, 92.8w% Hβ zeolite, and the balance was Y- Al2O3, the catalyst number is PA-1.

Embodiment 2

[0013] Add 70g of Hβ zeolite (SiO2 / Al2O3 molecular ratio is 42) to 250ml of 0.2M KCL solution, carry out ion exchange at a temperature of 95°C, and the exchange time is 2.5h: then filter and wash until there is no C1; Repeat the ion exchange once, the conditions are the same as the first time: dry at 50°C for 4.0h, 100°C for 4.0h; then mix with 20g of aluminum hydroxide powder, add nitric acid and deionized water, knead and extrude on the extruder, The addition of nitric acid will account for 1.0w% of the dry material, and the amount of deionized water added is subject to kneading and extruding. The strip-shaped catalyst was dried at 50°C for 4.0h, at 110°C for 4.0h, and then calcined in a muffle furnace at 450°C for 8.0h to obtain a K / Hβ zeolite-Al2O3 catalyst, which contained 1.6w% potassium and 85.8w% Hβ zeolite %, the balance is Y-Al2O3, and the catalyst number is PA-2.

Embodiment 3

[0015] Add 70g of Hβ zeolite (SiO2 / Al2O3 molecular ratio is 66) to 250ml of 0.2M KCL solution, carry out ion exchange at a temperature of 95°C, and the exchange time is 2.5h: then filter and wash until there is no C1; Repeat the ion exchange once, the conditions are the same as the first time: dry at 60°C for 8.0h, 110°C for 8.0h; then mix with 20g of aluminum hydroxide powder, add nitric acid and deionized water, knead and extrude on the extrusion machine, The addition of nitric acid will account for 2.0w% of the dry material, and the amount of deionized water added is subject to kneading and extruding. The strip-shaped catalyst was dried at 50°C for 4.0h, at 110°C for 4.0h, and then calcined in a muffle furnace at 550°C for 12.0h to obtain a K / Hβ zeolite-Al2O3 catalyst, which contained 1.6w% potassium and 85.8w% Hβ zeolite %, the balance is Y-Al2O3, and the catalyst number is PA-3.

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Abstract

The invention discloses a method for separating and purifying diisopropylamine from crude isopropamide. The method comprises the following steps: by taking isopropamide as a raw material and taking K/Hbeta zeolite-Al2O3 as a catalyst, compounding diisopropylamine. The conditions for compounding diisopropylamine from isopropamide are as follows: the reaction temperature is 200-300 DEG C, the pressure is from normal pressure to 0.5MPa and the airspeed is 0.2-1.5h. According to the invention, isopropamide is taken as the raw material for continuously compounding diisopropylamine, the original compounding process is simplified, the conversion rate is high, the selectivity is high, the reactant composition is simple, the production time is shortened, the energy is saved, the material consumption is lowered and the production cost is greatly lowered.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a method for separating and purifying diisopropylamine from crude isopropylamine. Background technique [0002] Diisopropylamine is a colorless and transparent liquid, soluble in water, soluble in most organic solvents, volatile liquid with ammonia odor, colorless liquid, with ammonia odor, volatile, strongly alkaline, soluble in water , ethanol and most organic solvents, relative density 0.722, boiling point 84°C, freezing point -96.3°C, refractive index 1.3924, flash point -6°C, flammable, low toxicity, median lethal dose 770mg / kg, corrosive, diisotropic Propylamine is an important organic synthesis intermediate, used as rubber accelerator, pharmaceutical intermediate pesticide herbicide, surfactant, etc., used in the production of dyes, mineral flotation agents, emulsifiers and intermediates of fine chemicals, widely used It is used in the production of rubber accelerators, medi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/02C07C211/06B01J29/70
CPCC07C209/02B01J29/7007C07C211/06
Inventor 凡殿才高玉磊王卫峰张海生吴珍汉张浩
Owner ANHUI HAOYUAN CHEM IND GRP
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