Preparation method and application of primaquine-terminated polyether catalyst prepared through static bed catalytic hydrogenation

A technology of primary amino polyether and terminal primary amino polyether, which is applied in the field of fixed bed synthesis of primary amino terminal polyether and the preparation of high-efficiency catalysts, can solve the problem of not too high selection, increased production time and production cost, and increased equipment Investment and other issues, to achieve the effect of reducing production time, eliminating the purification process, and reducing equipment investment

Inactive Publication Date: 2016-10-26
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In recent years, due to the better advantages of the fixed bed continuous method, such as good reaction selectivity, high conversion rate, less environmental pollution, and convenient post-treatment, etc., most of the current preparations of primary amino-terminated polyethers use this type of continuous method. The catalyst mainly adopts Ni-Cu-Cr series catalyst and its improved body such as adding a small amount of elements such as lanthanum to improve its overall performance, but its selection is often not too high, and the reaction data of the original particle size catalyst is generally about 90%. If you want to get a high The primary amino-terminated polyether with low purity and low molecular weight often needs to set up a special purification process, which not only increases the equipment investment, but also increases the production time and production cost, and its production efficiency needs to be further improved

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0021] Co-precipitate 2.0M magnesium sulfate and aluminum sulfate solution (magnesium-aluminum ratio is 2.2:1.0) and 2.0M sodium carbonate at 40°C to prepare magnesium-aluminum spinel for Ni-Cu-Cr-MgAl 2 o 4 Catalyst preparation. The loading metal content (reduced state) is: nickel 50%, copper 30%, chromium 5%, MgAl 2 o 4 The addition amount is 1.0%, the concentration of the metal nitrate solution is 0.5mol / L, and the precipitant Na 2 CO 3 0.5mol / L, co-precipitation reaction occurs at 40°C, aged at 60°C for 30 minutes, suction filtration and washing are performed in sequence, and the carrier Al is selected 2 o 3 The content is 15%, dried for 10 hours after suction filtration, granulated by grinding, and calcined at 350°C for 2 hours, and finally the calcined catalyst is pressed into tablets to obtain granular catalyst 1.

Embodiment 2

[0023] Co-precipitate 1.0M magnesium nitrate and aluminum nitrate solution (magnesium-aluminum ratio is 2:1) with 0.5M potassium bicarbonate at 60°C to prepare magnesium-aluminum spinel for Ni-Cu-Cr-MgAl 2 o 4 Catalyst preparation. The loading metal content (reduced state) is: nickel 80%, copper 5%, chromium 1%, MgAl 2 o 4 The addition amount is 3.0%, the concentration of the metal nitrate solution is 1mol / L, and the precipitant K 2 CO 3 1mol / L, the precipitation temperature is 60°C, aging at 70°C for 30min, suction filtration and washing in sequence, and the carrier SiO 2 The content is 10%, dried for 10 hours after suction filtration, granulated by grinding, and calcined at 300°C for 2 hours, and finally the calcined catalyst is pressed into tablets to obtain granular catalyst 2.

Embodiment 3

[0025] Co-precipitate 0.5M magnesium chloride and aluminum chloride solution (magnesium-aluminum ratio is 0.8:1) and 1.0M potassium carbonate at 80°C to prepare magnesium-aluminum spinel for Ni-Cu-Cr-MgAl 2 o 4 Catalyst preparation. Co-precipitate with potassium carbonate at 80°C to prepare magnesium-aluminum spinel, which is used for the preparation of Ni-Cu-Cr catalyst. The loading metal content (reduced state) is: nickel 20%, copper 20%, chromium 10%, MgAl 2 o 4 The addition amount is 3.0%, the concentration of the metal nitrate solution is 2mol / L, and the precipitant Na 2 CO 3 2mol / L, co-precipitation reaction occurs at 80°C, aged at 80°C for 30min, suction filtration and washing are performed in sequence, and the carrier Al is selected 2 o 3 The amount is 50%, dried for 10 hours after suction filtration, granulated by grinding, and calcined at 400°C for 2 hours, and finally the calcined catalyst is pressed into tablets to obtain granular catalyst 3.

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Abstract

The invention discloses a catalyst preparation method for improving selectivity of primaquine-terminated polyether prepared through hydroxyl-terminated polyether static bed catalytic hydrogenation and a method for selectively and continuously producing primaquine-terminated polyether. An Ni-Cu-Cr-MgAl2O4 catalyst is prepared through a coprecipitation method, an original-size catalyst is adopted for producing low molecular weight primaquine-terminated polyether in a static bed reactor, polyether polyol, hydrogen and liquid ammonia are adopted as raw materials, the self-prepared Ni-Cu-Cr-MgAl2O4 catalyst is adopted, the materials are continuously subjected to an ammoniation catalytic reaction through the static bed reactor at the temperature of 180 DEG C to 260 DEG C and the pressure of 4.0 MPa to 8.0 MPa, low molecular weight primaquine-terminated polyether can be obtained through gas-liquid separation, the conversion rate of the obtained primaquine-based polyether product is larger than or equal to 90.0%, and the primaquine selectivity is larger than or equal to 95.0%. The continuous process production technology is adopted, the selectivity of low molecular weight primaquine-terminated polyether can be improved, therefore, product aftertreatment is simplified, the quality of the low molecular weight primaquine-terminated polyether product is improved, and the production efficiency is improved.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to a production method for synthesizing a primary amino-terminated polyether by a fixed bed method and a preparation method for a high-efficiency catalyst. Background technique [0002] Amino-terminated polyether, also known as polyether amine, is a kind of polyalkylene oxide compound whose molecular main chain is polyether skeleton, and the terminal active functional group is primary amine or primary amine group. Due to the active nature of the terminal amine group, it can react with a variety of groups, so it is widely used, especially in modern industrial fields, such as epoxy resin curing agent, polyurethane (polyurea) material, surfactant, ion exchanger wait. According to the molecular weight, the number of functional groups, and the types of amine groups, there are a variety of products in the market, such as monoamines, diamines, and triamines. In particular,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/86C07C215/08C07C213/06C08G65/325C08G65/48
CPCB01J23/868B01J23/002B01J2523/00C07C213/06C08G65/3255C08G65/48C08G2650/50
Inventor 朱凯吴永忠魏星
Owner NANJING FORESTRY UNIV
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