AlOOH catalyst for polyester polycondensation and preparation method thereof

Abstract

The invention relates to an AlOOH catalyst for polyester polycondensation and a preparation method of the AlOOH catalyst. The AlOOH catalyst comprises AlOOH or a mixture of AlOOH and Al2O3. The preparation method of the catalyst comprises the following steps in sequence: uniformly mixing sodium aluminate solution with an additive; adjusting pH; reacting; centrifugally layering; cleaning the obtained solid matter; drying; and grinding, thus obtaining the AlOOH catalyst for polyester polycondensation, wherein the mass ratio of sodium aluminate to the additive is 1: 1 to 2000: 1. The nanometer AlOOH catalyst is simple in preparation method, can be prepared without high temperature condition, and is low in cost, rich in raw material sources, and beneficial for industrial popularization; the catalyst with higher catalyzing activity can be used for preparing polyester; the obtained polyester chip has higher characteristic viscosity; and the catalyst is free of a heavy metal element compound, and is expected to replace an antimony catalyst in the modern polyester industry.

Description

technical field

[0001] The invention belongs to the field of catalysts and preparation thereof, in particular to an AlOOH catalyst for polycondensation of polyester and a preparation method thereof. Background technique

[0002] AlOOH, or written as AlO(OH), is a material with important uses, and can be used as an adsorbent, desiccant, flame retardant, catalyst, and as a precursor for the preparation of alumina.

[0003] Currently AlOOH and Al 2 o 3 The preparation methods include gas phase method, sol-gel method, liquid phase precipitation method, hydrothermal method and so on. However, some of these methods require high temperature and expensive equipment, and some methods require the use of many organic sols, and the operating conditions are relatively harsh. For example, patent CN101182024 reports a preparation method of Γ-AlOOH, which uses inorganic water-soluble aluminum salt as raw material, inorganic alkali or inorganic acid as precipitant, first prepares amorphou...

Examples

Embodiment 1

[0026] Pass the untreated attapulgite through a 200-mesh sieve to remove impurities, weigh 15g, add deionized water to make a suspension with a mass fraction of about 4%, stir for 1 hour, then add 150ml of hydrogen peroxide, and After standing for 30 minutes, the supernatant suspension was decanted to remove the residual impurities in the bottom layer.

[0027] 150 ml of 0.5 mol / L hydrochloric acid was added to the above-mentioned purified suspension, stirred for 1 hour, then sonicated for 30 minutes, and then allowed to stand for 30 minutes. The upper layer suspension was decanted, and after centrifugation, the obtained solid was washed 3 times with deionized water, and finally the washed attapulgite was dried and ground for later use.

[0028] Add 0.2mol / L NaAlO in the flask 2 Solution 250ml, add 0.2g attapulgite, first ultrasonic 30MIN, after fully dispersed, drop 0.5mol / L HCL solution in the flask until the pH value is 7±0.1, and white precipitate appears in the reaction ...

Embodiment 2

[0031] Pass the untreated attapulgite through a 200-mesh sieve to remove impurities, weigh 15g, add deionized water to make a suspension with a mass fraction of about 4%, stir for 1 hour, then add 150ml of hydrogen peroxide, and After standing for 30 minutes, the supernatant suspension was decanted to remove the residual impurities in the bottom layer.

[0032] 150 ml of 0.5 mol / L hydrochloric acid was added to the above-mentioned purified suspension, stirred for 1 hour, then sonicated for 30 minutes, and then allowed to stand for 30 minutes. The upper layer suspension was decanted, and after centrifugation, the obtained solid was washed 3 times with deionized water, and finally the washed attapulgite was dried and ground for later use.

[0033] Add 0.2mol / L NaAlO in the flask 2 Solution 250ml, add 1g of attapulgite, first ultrasonic 30MIN, after fully dispersed, drop 0.5mol / L HCL solution in the flask until the pH value is 7±0.1, and white precipitate appears in the reaction...

Embodiment 3

[0036] Pass the untreated attapulgite through a 200-mesh sieve to remove impurities, weigh 15g, add deionized water to make a suspension with a mass fraction of about 4%, stir for 1 hour, then add 150ml of hydrogen peroxide, and After standing for 30 minutes, the supernatant suspension was decanted to remove the residual impurities in the bottom layer.

[0037] 150 ml of 0.5 mol / L hydrochloric acid was added to the above-mentioned purified suspension, stirred for 1 hour, then sonicated for 30 minutes, and then allowed to stand for 30 minutes. The upper layer suspension was decanted, and after centrifugation, the obtained solid was washed 3 times with deionized water, and finally the washed attapulgite was dried and ground for later use.

[0038] Add 0.2mol / L NaAlO in the flask 2Solution 250ml, add 0.1g attapulgite, first ultrasonic 30MIN, after fully dispersed, drop 0.5mol / L HCL solution in the flask until the pH value is 7±0.1, and white precipitate appears in the reaction s...

technical field

[0001] The invention belongs to the field of catalysts and preparation thereof, in particular to an AlOOH catalyst for polycondensation of polyester and a preparation method thereof. Background technique

[0002] AlOOH, or written as AlO(OH), is a material with important uses, and can be used as an adsorbent, desiccant, flame retardant, catalyst, and as a precursor for the preparation of alumina.

[0003] Currently AlOOH and Al 2 o 3 The preparation methods include gas phase method, sol-gel method, liquid phase precipitation method, hydrothermal method and so on. However, some of these methods require high temperature and expensive equipment, and some methods require the use of many organic sols, and the operating conditions are relatively harsh. For example, patent CN101182024 reports a preparation method of Γ-AlOOH, which uses inorganic water-soluble aluminum salt as raw material, inorganic alkali or inorganic acid as precipitant, first prepares amorphou...

Examples

Embodiment 1

[0026] Pass the untreated attapulgite through a 200-mesh sieve to remove impurities, weigh 15g, add deionized water to make a suspension with a mass fraction of about 4%, stir for 1 hour, then add 150ml of hydrogen peroxide, and After standing for 30 minutes, the supernatant suspension was decanted to remove the residual impurities in the bottom layer.

[0027] 150 ml of 0.5 mol / L hydrochloric acid was added to the above-mentioned purified suspension, stirred for 1 hour, then sonicated for 30 minutes, and then allowed to stand for 30 minutes. The upper layer suspension was decanted, and after centrifugation, the obtained solid was washed 3 times with deionized water, and finally the washed attapulgite was dried and ground for later use.

[0028] Add 0.2mol / L NaAlO in the flask 2 Solution 250ml, add 0.2g attapulgite, first ultrasonic 30MIN, after fully dispersed, drop 0.5mol / L HCL solution in the flask until the pH value is 7±0.1, and white precipitate appears in the reaction ...

Embodiment 2

[0031] Pass the untreated attapulgite through a 200-mesh sieve to remove impurities, weigh 15g, add deionized water to make a suspension with a mass fraction of about 4%, stir for 1 hour, then add 150ml of hydrogen peroxide, and After standing for 30 minutes, the supernatant suspension was decanted to remove the residual impurities in the bottom layer.

[0032] 150 ml of 0.5 mol / L hydrochloric acid was added to the above-mentioned purified suspension, stirred for 1 hour, then sonicated for 30 minutes, and then allowed to stand for 30 minutes. The upper layer suspension was decanted, and after centrifugation, the obtained solid was washed 3 times with deionized water, and finally the washed attapulgite was dried and ground for later use.

[0033] Add 0.2mol / L NaAlO in the flask 2 Solution 250ml, add 1g of attapulgite, first ultrasonic 30MIN, after fully dispersed, drop 0.5mol / L HCL solution in the flask until the pH value is 7±0.1, and white precipitate appears in the reaction...

Embodiment 3

[0036] Pass the untreated attapulgite through a 200-mesh sieve to remove impurities, weigh 15g, add deionized water to make a suspension with a mass fraction of about 4%, stir for 1 hour, then add 150ml of hydrogen peroxide, and After standing for 30 minutes, the supernatant suspension was decanted to remove the residual impurities in the bottom layer.

[0037] 150 ml of 0.5 mol / L hydrochloric acid was added to the above-mentioned purified suspension, stirred for 1 hour, then sonicated for 30 minutes, and then allowed to stand for 30 minutes. The upper layer suspension was decanted, and after centrifugation, the obtained solid was washed 3 times with deionized water, and finally the washed attapulgite was dried and ground for later use.

[0038] Add 0.2mol / L NaAlO in the flask 2Solution 250ml, add 0.1g attapulgite, first ultrasonic 30MIN, after fully dispersed, drop 0.5mol / L HCL solution in the flask until the pH value is 7±0.1, and white precipitate appears in the reaction s...

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