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Continuous preparation of 1,2-propanediamine catalyst and preparation method thereof

A technology of catalyst and propylenediamine, which is applied in the field of continuous preparation of 1,2-propylenediamine catalyst and its preparation, can solve the problems of difficult continuous production of the catalyst, low industrial application value, and short service life, and achieve significant industrial application value, Excellent catalyst activity and stability

Active Publication Date: 2021-04-13
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the catalysts reported above have the problems of being difficult to be used in continuous production or having low activity and short life, and have low industrial application value.

Method used

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  • Continuous preparation of 1,2-propanediamine catalyst and preparation method thereof
  • Continuous preparation of 1,2-propanediamine catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The present invention is implemented with reference to the following composition by weight percentage:

[0025] 10% Ni, 1.5% Ru, 1.5% Cs, 1.5% Ce, 10% alumina, and the rest is silicon oxide.

[0026] Preparation:

[0027] Make a solution of ethanol and 25% acidic silica sol at a volume ratio of 1:1; add nickel nitrate, ruthenium chloride, cesium nitrate and cerium nitrate to the mixture, add 5 mL of isopropanolamine, and dissolve completely; stand at room temperature 24h; remove the solvent under reduced pressure at 40°C; dry at 100°C for 10h; add alumina and graphite to the obtained solid powder, mix evenly, granulate and shape; roast at 500°C for 4h; The volume space velocity is 600h -1 Hydrogen reduction for 3h.

[0028] Catalytic Performance Evaluation:

[0029] Cool naturally to a temperature of 160°C, at a pressure of 7 MPa, the molar ratio of hydrogen to isopropanolamine is 2:1, the molar ratio of raw material liquid ammonia to isopropanolamine is 12:1, and t...

Embodiment 2

[0031] The present invention is implemented with reference to the following composition by weight percentage:

[0032] 15% Ni, 0.5% Ru, 2.5% Cs, 0.5% La, 15% alumina, and the rest is silicon oxide.

[0033] Preparation:

[0034] Make a solution of methanol and 25% acidic silica sol at a volume ratio of 1:1; add nickel nitrate, ruthenium chloride, cesium nitrate and lanthanum nitrate into the mixture, add 5 mL of isopropanolamine, and dissolve completely; stand at room temperature 16h; remove the solvent under reduced pressure at 40°C; dry at 100°C for 10h; add alumina and graphite to the obtained solid powder, mix evenly, granulate and shape; roast at 500°C for 4h; The volume space velocity is 600h -1 Hydrogen reduction for 3h.

[0035] Catalyst performance evaluation conditions are the same as in Example 1, and the performance remains unchanged after running for 1000h. The results are shown in Table 1.

Embodiment 3

[0037] The present invention is implemented with reference to the following composition by weight percentage:

[0038] 5% Ni, 1.5% Ru, 0.5% Sr, 1.0% La, 8% alumina, and the rest is silicon oxide.

[0039] Preparation:

[0040] Make a solution of ethanol and 25% acidic silica sol at a volume ratio of 1:4; add nickel nitrate, ruthenium chloride, strontium nitrate and lanthanum nitrate to the mixture, add 6 mL of isopropanolamine, and dissolve completely; stand at room temperature 0.5h; remove solvent under reduced pressure at 40°C; dry at 100°C for 10h; add alumina and graphite to the obtained solid powder, mix evenly, granulate and shape; roast at 500°C for 4h; obtain catalyst precursor at 400°C under normal pressure, Take volumetric space velocity as 600h -1 Hydrogen reduction for 3h.

[0041] Catalyst performance evaluation conditions are the same as in Example 1, and the results are shown in Table 1.

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Abstract

The invention relates to a catalyst for continuously preparing 1,2-propylenediamine and a preparation method thereof. The weight percentage of the catalyst involved is: 2-15% Ni, 0.1-1.5% metal M 1 , 0.1~5% additive R 1 , 0.1~2.0% additive R 2 , 8-15% aluminum oxide, the rest is silicon oxide. The preparation method involved comprises making a solution of alcohol and 25% acidic silica sol in a volume ratio of 1:1 to 1:4; mixing nickel nitrate, soluble M 1 Metal salt, R 1 Auxiliary Salt and Auxiliary R 2 Add the precursor to the mixed solution, add isopropanolamine, and dissolve completely; let it stand for 0.5 to 24 hours; remove the solvent under reduced pressure; add alumina and graphite to the dried solid powder, mix evenly, granulate, and shape; roast to obtain the obtained The catalyst precursor; reduction in hydrogen to obtain the catalyst. The catalyst of the invention has good stability, performance is higher than that of the prior art, and has remarkable industrial application value.

Description

technical field [0001] The invention relates to a catalyst for continuously preparing 1,2-propylenediamine and a preparation method thereof, in particular to a reductive amination catalyst and a preparation method for preparing 1,2-propylenediamine from isopropanolamine. [0002] technical background [0003] 1,2-propylenediamine is a very important organic chemical raw material. It has important applications in the fields of organic synthesis, oil passivator, epoxy resin curing accelerator, spandex, modified shellac coatings, etc. Its derivatives can also It is used as a raw material for rubber and paint, as a chelating agent, ore dressing agent, etc. The demand is large, and it mainly depends on imports. [0004] At present, there are two main methods for preparing 1,2-propanediamine. One is to use 1,2-dichloropropane as a raw material to undergo ammonolysis reaction with liquid ammonia to obtain 1,2-propanediamine and hydrogen chloride. Sodium hydroxide is added to neutra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/889B01J23/89C07C209/16C07C211/11
CPCB01J23/8896B01J23/8946C07C209/16C07C211/11
Inventor 吕剑余秦伟王为强张前李江伟袁俊杨建明
Owner XIAN MODERN CHEM RES INST
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