RU2532554C1 - Method of obtaining titanium-containing organometallic caged compound - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: invention relates to obtaining a titanium-containing compound, used as an adsorbent and photocatalyst. Claimed is a method of obtaining the organometallic caged compound of formula Ti₈O₈(OH)₄[O₂C-C₆H₄CO₂]_6. An interaction of terephthalic acid with titanium butoxide in a solvent is realised. The process is carried out at boiling for 6-7 hours under atmospheric pressure.

EFFECT: increased safety and efficiency of the process with an increase of the target product output.

1 dwg, 1 tbl

Description

Introduction

The invention relates to the chemical industry, namely to the production of a titanium-containing organometallic framework compound of the formula Ti ₈ O ₈ (OH) ₄ [O ₂ CC ₆ H ₄ CO ₂ ] ₆ , which can be used in adsorption processes from the liquid phase for wastewater treatment in production organic dyes, and also as a photocatalyst.

State of the art

A known method for producing a titanium-containing organometallic framework compound of the formula Ti ₈ O ₈ (OH) ₄ [O ₂ CC ₆ H ₄ CO ₂ ] ₆ (M. Dan-Hardi, C. Serre, T. Frot, L. Rozes, G. Maurin, C. Sanchez and G. Ferey J. Am. Chem. Soc., 2009, 131, 10857).

The method is implemented as follows. Terephthalic acid and titanium tetraisopropoxide are introduced into a solution containing a mixture of dimethylformamide and methanol (in a volume ratio of 9: 1). Next, the resulting mixture was stirred, placed in an autoclave and kept at a temperature of 150 ° C for 15 hours. Then the reaction mixture is cooled to room temperature, the resulting solid phase is filtered off, washed successively with acetone, dimethylformamide, methanol, and dried at a moderate temperature (190-200 ° C). The product yield is about 56%.

The disadvantages of this method are:

- the use of toxic methanol;

- low efficiency due to:

- the need to use special equipment operating under pressure;

- high energy intensity of the process due to the long duration of the process carried out at high temperature;

- insufficiently high yield of the target product.

SUMMARY OF THE INVENTION

The objective of the invention is to develop a method for producing a titanium-containing organometallic framework compound of the formula Ti ₈ O ₈ (OH) ₄ [O ₂ CC ₆ H ₄ CO ₂ ] ₆ by reacting terephthalic acid with titanium alkoxide in a solvent including dimethylformamide by heating, which would increase safety, efficiency of the process and the yield of the target product.

The problem is solved by a method for producing a titanium-containing organometallic framework compound of the formula Ti ₈ O ₈ (OH) ₄ [O ₂ CC ₆ H ₄ CO ₂ ] ₆ by reacting terephthalic acid with titanium alkoxide in a solvent including dimethylformamide, when heated, in which the process is carried out at atmospheric pressure for 6-7 hours at boiling, titanium butoxide is used as titanium alkoxide, and dimethylformamide is used as solvent including dimethylformamide.

The invention allows:

- increase the safety of the process by eliminating toxic methanol from the synthesis;

- increase the efficiency of the process by eliminating the need to use special expensive equipment operating under pressure, and a significant reduction in energy consumption due to a significant reduction in the duration of the synthesis process;

- get the target product with a higher yield.

Information confirming the possibility of carrying out the invention

To implement the method using the following substances:

dimethylformamide - GOST 20289-74

terephthalic acid - CAS 100-21-0 (Aldrich)

titanium butoxide - CAS 5593-70-4 (Aldrich)

acetone - GOST 2768-84

The method is implemented as follows:

16.6 g (0.1 M) of terephthalic acid are charged into 300 ml of dimethylformamide and the reaction mixture is heated to boiling with stirring. After complete dissolution of the acid, 17 g (0.05 M) of titanium butoxide are added to the solution and the mixture is kept at boiling for 6-7 hours. Then the mixture is cooled to room temperature, the resulting solid phase is filtered off, washed successively with acetone and dimethylformamide and dried at a temperature of 190-200 ° C.

Elemental analysis data:

Calculated for Ti ₈ O ₈ (OH) ₄ [O ₂ CC ₆ H ₄ CO ₂ ] ₆ ,%: C - 36.87, H - 1.80, O - 36.83. Found,%: C - 36.12, H - 1.89, O - 36.43. IR spectrum, ν, cm ^-1 : 3413 (OH), 2918 (CH), 1645, 1585 (C = O), 1401 (C = C).

The purity of the product is confirmed by powder x-ray diffraction. The diffraction pattern of the titanium-containing organometallic framework compound of the formula Ti ₈ O ₈ (OH) ₄ [O ₂ CC ₆ H ₄ CO ₂ ] _{6 is} shown in the figure.

The outputs of the target product during the implementation of the method under various conditions are shown in the table.

Example No. Synthesis time, h The yield of the target product,% one 6 69.8 2 6.5 70.0 3 7 69.9

Claims (1)

A method of obtaining a titanium-containing organometallic framework compound of the formula Ti ₈ O ₈ (OH) ₄ [O ₂ CC ₆ H ₄ CO ₂ ] ₆ by reacting terephthalic acid with titanium alkoxide in a solvent containing dimethylformamide by heating, characterized in that the process is carried out at atmospheric pressure for 6-7 hours at boiling, titanium butoxide is used as titanium alkoxide, and dimethylformamide is used as solvent containing dimethylformamide.

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