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Preparation method of complex metal oxide modified titanium dioxide type solid acid and catalytic synthesis method of polytetrahydrofuran ether using same

A technology of polytetrahydrofuran ether and solid acid catalyst, which is applied in the field of catalytic synthesis of polytetrahydrofuran ether, can solve the problems of high cost and achieve the effects of high space-time efficiency, short time and high activity

Inactive Publication Date: 2014-04-30
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] U.S.4120930 discloses the use of Nafion's fluorosulfonic acid polymer as a catalyst for polymerizing tetrahydrofuran, but its cost is high

Method used

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  • Preparation method of complex metal oxide modified titanium dioxide type solid acid and catalytic synthesis method of polytetrahydrofuran ether using same
  • Preparation method of complex metal oxide modified titanium dioxide type solid acid and catalytic synthesis method of polytetrahydrofuran ether using same
  • Preparation method of complex metal oxide modified titanium dioxide type solid acid and catalytic synthesis method of polytetrahydrofuran ether using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Dissolve titanium tetrachloride in deionized water, add ammonia water dropwise at 20°C, and adjust the pH to 9-11. Settled at 20°C for 20 hours and filtered under reduced pressure. The filter cake was washed with deionized water to contain no chloride ions, dried, and passed through a 200-mesh sieve to obtain white titanium hydroxide powder.

[0043] Dissolve 4g of ammonium molybdate in 20ml (1mol / L) of sulfuric acid, add 10g of titanium hydroxide, then add 0.35g of nickel sulfate, and stir for 4 hours. Heat and concentrate in a box-type resistance furnace until there is no liquid, and bake at 600°C for 3 hours to obtain a solid acid catalyst.

[0044] Tetrahydrofuran and solid acid catalyst were added into the flask according to the mass ratio of 10:1, and epichlorohydrin was added according to 0.1% of the mass of tetrahydrofuran. The temperature was controlled at 10°C for 48 hours. Add 30ml of toluene to the product, filter, and distill the toluene from the filtrate ...

Embodiment 2

[0048] Dissolve 4g of ammonium molybdate in 20ml (1mol / L) of sulfuric acid, add 10g of titanium hydroxide, then add 0.76g of sodium tungstate, and stir for 4 hours. Heat and concentrate in a box-type resistance furnace until there is no liquid, and bake at 550°C for 3 hours to obtain a solid acid catalyst.

[0049] Tetrahydrofuran and solid acid catalyst were added into the flask according to the mass ratio of 10:1, and epichlorohydrin was added according to 0.1% of the mass of tetrahydrofuran. The temperature was controlled at 10°C for 48 hours. The product was filtered and the yield was 72.6%.

Embodiment 3

[0051] Dissolve 4g of ammonium molybdate in 20ml (1mol / L) of sulfuric acid, add 10g of titanium hydroxide, then add 0.18g of nickel sulfate, 0.38g of sodium tungstate, and stir for 4 hours. Heat and concentrate in a box-type resistance furnace until there is no liquid, and bake at 600°C for 3 hours to obtain a solid acid catalyst.

[0052] Tetrahydrofuran and solid acid catalyst were added into the flask according to the mass ratio of 10:1, and epichlorohydrin was added according to 0.1% of the mass of tetrahydrofuran. The temperature was controlled at 15°C for 36 hours. Add 30ml of toluene to the product, filter, and distill the toluene from the filtrate to obtain polytetrahydrofuran ether. The yield was 74.5%.

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Abstract

The invention discloses a preparation method of a complex metal oxide modified titanium dioxide type solid acid and a catalytic synthesis method of polytetrahydrofuran ether using the same. With the catalyst, the metal ions form a complex oxide on the surface of titanium dioxide through a roasting mode. The catalyst is used for modifying molybdenum oxide and the oxides of the metals of the 4th, 5th and 6th periods on the surface of titanium dioxide, including the lanthanide series. The temperature of the polymerization reaction is 10-50 DEG C, and the conversion rate of the polytetrahydrofuran ether is 50-80%. The catalyst prepared by the method disclosed by the invention avoids equipment corrosion caused by the catalysis of traditional protonic acid catalyst, does not generate a great quantity of wastewater neutralizing acid liquid, and reduces environmental pollution; and moreover, the catalyst can be repeatedly used, and the production cost is lowered.

Description

technical field [0001] The invention relates to a method for modifying titanium dioxide with a composite metal oxide and preparing it into a solid acid, and also relates to a method for catalyzing and synthesizing polytetrahydrofuran ether with the prepared solid acid. Background technique [0002] Polytetrahydrofuran ether has a soft chain structure and is an important intermediate for preparing polyurethane elastic fibers and polyether elastic materials. Polytetrahydrofuran ether can improve the cold resistance, water resistance and flexibility of elastomers. In recent years, spandex, the main downstream product of domestic polytetrahydrofuran ether, has developed rapidly, and the demand for polytetrahydrofuran ether has increased. Therefore, it is imminent to improve the conversion rate and space-time efficiency of the polymerization reaction, reduce the production cost and improve the product quality. [0003] The polymerization of THF is usually a cationic-catalyzed ri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/20
Inventor 杨大伟魏鑫王传宇毕然陈欣硕
Owner DALIAN POLYTECHNIC UNIVERSITY
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