Binary titanium alkoxide (VI) compound and its preparing process and application

A technology of titanium dialcohols and titanium compounds, which is applied in the fields of titanium organic compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., and can solve problems such as unreported catalyst synthesis technology

Inactive Publication Date: 2001-12-26
济南齐鲁化纤集团有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a reactor equipped with a stirrer and a distillation device, 25.5 g of tetrabutyl titanate and 124 g of ethylene glycol were added, wherein the molar ratio of titanate to glycol was 0.0375:1.0. Stir to make it react to form a gel, raise the temperature to 130°C, and pass N 2 , and adjust N 2 The flow rate is 0.5L / min·liter reactor, continue to heat up to 197-198°C, stop the reaction when the temperature no longer changes, the reaction time is about 40min, let stand and cool to room temperature, vacuum filter or centrifugal filter, filtrate recovery cycle Use, the solid is washed with industrial ethanol or acetone, decolorized, and dried to obtain a white solid of titanium (VI) ethylene glycol, wherein the Ti content is 25.9%. After it is dispersed in glycol by conventional stirring or ultrasonic vibration, the particles The diameter is 4-19 nanometers, take 5.0g and add it into 100g deionized water, and it will not decompose for at least one day and night.

Embodiment 2

[0023] In a reactor with a stirrer and a distillation device, add 25.5g tetrabutyl titanate, 124g ethylene glycol and 12.75g deionized water, wherein the molar ratio of titanate to glycol is 0.0375: 1.0, Stir to make it react to form a gel, raise the temperature to 130°C, and pass in N 2 and adjust N 2 The flow rate is 1.0L / min. The reactor starts to discharge distillates, and continues to heat up to the boiling point of ethylene glycol at 197-198°C. When the temperature does not change anymore, stop the reaction. The reaction time is about 45min, and it is allowed to stand and cool to room temperature. , the filtrate is recovered and recycled by vacuum filtration, the solid is washed and decolorized with acetone, and dried to obtain a white solid of ethylene glycol titanium with a Ti content of 26.0%. After it is dispersed in glycol by conventional stirring or ultrasonic vibration, the particle size 4-19 nanometers, take 5.0g and add it into 100g deionized water, it will not...

Embodiment 3

[0025] In a reactor with a stirrer and a rectification device, add 0.5g of tetrabutyl titanate and 99.5g of ethylene glycol, wherein the molar ratio of titanate to glycol is 0.0009:1.0, stir to make it react A gel was formed, and when the temperature was raised to 50°C, the solution was transparent, and then the temperature continued to rise to 197-198°C, and the solution remained transparent. After standing and cooling for a whole day and night, there was still no solid matter. Continue to add 0.25g of tetrabutyl titanate and stir. Repeat the above operations, then white solids will be produced, and the solution color is slightly yellow. The solids are obtained by vacuum filtration, washed with industrial ethanol, and dried to obtain a white solid of titanium ethylene glycol. The Ti content is 26.1%. After being dispersed by conventional stirring or ultrasonic vibration, the particle size is 4-19 nanometers. Take 5.0g and add it to 100g deionized water, and it will not decompo...

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Abstract

A binary titanium (VI) alkoxide compound is disclosed, which can be used as high-activity catalyst in esterification, ester exchange and polycondensation reactions. Said compound is prepared from easily hydrolytic Ti (VI) compounds or their hydrolyzed products and diol or hydrous diol through direct reaction to generate gel, regulating temp and pressure of reaction system or introducing inert gasto gradually remove the low-molecular resultants in reaction system, decolouring and drying. Its advantages include simple preparing process, low cost, and the high catalytic activity, optical catalytic performance and anti-hydrolysis nature of said product.

Description

technical field [0001] The invention belongs to the field of highly active catalysts, in particular to the direct reaction of easily hydrolyzed titanium (IV) compounds with dibasic alcohols or water-containing dibasic alcohols to prepare the basic structural unit C n h 2n＋1 o 5 Ti (where n is an even number of 4-12) glycolate titanium (VI) compound, its preparation method and its application as a catalyst for esterification, transesterification and polycondensation reactions. Background technique [0002] As we all know, titanium (IV) esters are an important class of titanium compounds, and are used as catalysts for esterification, transesterification, and polycondensation reactions. However, due to their easy hydrolysis and unstable activity, the polymers formed by catalysis have turbidity. etc., its application is very limited. [0003] Regarding the research on anti-hydrolysis titanium series catalysts, according to Chem. Fibers Int.1999.49(1...

Claims

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Application Information

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IPC IPC(8): B01J31/12C07F7/28
Inventor 曹善文
Owner 济南齐鲁化纤集团有限责任公司
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