Supported catalyst for synthesizing polyether amine, preparation method and application

A supported catalyst and polyetheramine technology, which is applied in the fields of synthesis, preparation and supported catalysts of polyetheramine, can solve the problems of reduced reaction selectivity, broadened molecular weight distribution, and polyether chain scission, and achieves inhibition of metal nitrides. The effect of forming, low cost and less load

Pending Publication Date: 2022-03-15
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing preparation process of polyetheramine, the polyether chain often breaks, resulting in a broadening of the molecular weight distribution and a decrease in reaction selectivity, thereby affecting its performance in downstream applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Dissolve 49.3g of nickel nitrate hexahydrate, 11.7g of copper nitrate hexahydrate, 5.2g of ammonium molybdate tetrahydrate, and 15.5g of cerium nitrate hexahydrate in 82mL of deionized water, heat up to 60°C and stir for 0.5h to obtain a metal salt solution ; Then pour the above metal salt solution and 82.1g spherical γ-alumina into a rotary evaporator, heat up to 45 degrees Celsius and rotate for 0.5h, stop rotating and let stand for 0.5h; then after fully adsorbed, heat up to 90 degrees Celsius Vacuum dehydration for 1h, then take out the impregnated carrier and put it into a muffle furnace, gradually raise the temperature to 420°C, roast for 5h in the air atmosphere, cool down; finally take out the roasted carrier and put it in a tube furnace The temperature was gradually raised to 450° C. in a hydrogen flow per minute, and after reduction for 8 hours, a supported catalyst A containing 10wt% Ni, 2.5wt% Cu, 0.4wt% Mo and 5wt% Ce was obtained.

Embodiment 2

[0065] Dissolve 49.3g of nickel nitrate hexahydrate, 11.7g of copper nitrate hexahydrate, 5.2g of ammonium molybdate tetrahydrate, and 15.5g of cerium nitrate hexahydrate in 82mL of deionized water, heat up to 60°C and stir for 0.5h to obtain a metal salt solution ; Then pour the above metal salt solution and 82.1g of amorphous silica into a rotary evaporator, heat up to 45 degrees Celsius, rotate for 0.5h, stop rotating and let stand for 0.5h; then after fully adsorbed, heat up to 90°C Vacuum dehydration for 1 hour, then take out the impregnated carrier and put it into a muffle furnace, gradually raise the temperature to 420°C, roast it in an air atmosphere for 5 hours, and cool it; Gradually raise the temperature to 450°C in a hydrogen flow, and after reduction for 8 hours, a supported catalyst B containing 10wt% Ni, 2.5wt% Cu, 0.4wt% Mo and 5wt% Ce was obtained.

Embodiment 3

[0067] First, potassium hydroxide is dissolved in deionized water to prepare potassium hydroxide solution; at the same time, 440g of magnesium nitrate and 200g of aluminum nitrate are dissolved in deionized water, and the solution is heated at 50°C for a period of time; then, under stirring and heating, the 6mol / L potassium hydroxide solution was slowly added dropwise to the nitrate solution to obtain a white paste-like precipitate; then reflux at 80°C for 1 hour to obtain a crystallized precipitate, which was filtered and washed to obtain a magnesium-aluminum composite oxide Finally, the above precursor was put into a muffle furnace and fired at 700°C for 5 hours to obtain a magnesium-aluminum composite oxide carrier.

[0068] Dissolve 49.3g of nickel nitrate hexahydrate, 11.7g of copper nitrate hexahydrate, 5.2g of ammonium molybdate tetrahydrate, and 15.5g of cerium nitrate hexahydrate in 82mL of deionized water, and raise the temperature to 60°C and stir for 0.5h to obtain ...

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Abstract

The invention relates to a supported catalyst for synthesizing polyether amine as well as a preparation method and application thereof.According to the supported catalyst, metal Mo and CeO2 are introduced into active components Ni and Cu, and through cooperation of Ni, Cu and Mo, CeO2 and Ni form more active sites, so that the supported catalyst has high reaction activity and selectivity, and the catalyst is suitable for synthesis of polyether amine. When the supported catalyst is used for synthesizing polyether amine, the amination efficiency and selectivity of polyether polyol can be greatly improved, polyether amine with light color and narrower molecular weight distribution is prepared, the cost of the catalyst can be reduced, the process conditions are relatively mild, the defect of low reaction activity of a nickel-based catalyst in synthesis of small-molecular polyether amine is overcome, and the method is suitable for industrial production. Good industrial application prospects are realized.

Description

technical field [0001] The invention belongs to the technical field of organic polymers, and in particular relates to a supported catalyst for synthesizing polyetheramine, a preparation method and an application. Background technique [0002] Polyether amine is a kind of compound with polyether structure backbone as the main chain and terminal active functional group as amine group. The special molecular structure endows polyetheramine with excellent comprehensive properties, making it widely used in the synthesis of polyurethane and polyurea, especially in the curing agent of epoxy resin. At present, there are commercial polyetheramines with a molecular weight of 230-5000, including monoamine, diamine, and triamine polyetheramines. [0003] The existing synthesis methods of polyether amines are mainly divided into leaving group method, hydrolysis method, nitro capping method, polyether nitrile alkylation and catalytic reductive amination method. [0004] (1) Leaving group...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/887C07C213/02C07C217/50C08G65/325
CPCB01J23/8871C07C213/02C08G65/3255C07C217/50C08G65/269B01J23/002B01J23/83B01J23/888B01J35/1019B01J35/1061B01J21/04B01J21/06B01J21/10B01J23/10B01J23/885B01J2523/17B01J2523/22B01J2523/31B01J2523/3712B01J2523/41B01J2523/47B01J2523/68
Inventor 王知王新荣王胜利赵世聪
Owner ZHEJIANG HUANGMA TECH
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