Preparation method of titanium tetraisopropoxide

A technology of titanium tetraisopropoxide and isopropanol, which is applied in the field of preparation of titanium tetraisopropoxide, can solve the problems that the purity is not easy to meet the requirements, is not suitable for large-scale production, and has complicated operation procedures, and is convenient for large-scale production and application. , The requirements of equipment are reduced, and the operation process is simple.

Active Publication Date: 2020-11-13
苏州欣溪源新材料科技有限公司
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Problems solved by technology

[0006]2. Stir TiCl4 and isopropanol in toluene evenly, and pass ammonia gas (NH3), after filtering, the solvent and by-products are distilled off to obtain the target product; this method has high raw material cost, low yield, generally about 60%, and the purity is difficult to meet the requirements. In addition, this method involves high-pressure ammonia, once Leakage will cause serious safety accidents, and this method requires high equipment and is not suitable for large-scale production;
[0007]3. Titanium metal is selected as the cathode and anode poles. Through the characteristic anode method, tetrapropylammonium bromide is selected as the conductive salt. By dissolving the titanium metal anode, the cathode A reduction reaction occurs to prepare isopropyl acid; this method has higher purity, but it takes a long time, the operation process is complicated, and the cost is high

Method used

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  • Preparation method of titanium tetraisopropoxide
  • Preparation method of titanium tetraisopropoxide

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[0030] The embodiment of the present invention provides a kind of preparation method of titanium tetraisopropoxide, comprises the steps:

[0031] Mixing solvent, titanium tetrachloride and isopropanol to prepare a mixed reaction system;

[0032] Dialkylamine is added into the mixed reaction system for reaction, and the obtained reactant is processed to prepare the titanium tetraisopropoxide.

[0033] The reaction principle of the preparation method of above-mentioned titanium tetraisopropoxide can be expressed as follows by chemical equation (taking diethylamine as example):

[0034] TiCl 4 +4iPrOH+4HNEt 2 →Ti(OiPr) 4 +4NEt 2 h 2 · Cl

[0035] The inventor found by accident in the process of studying the process scheme of titanium tetraisopropoxide that replacing traditional ammonia with dialkylamine can better match the reaction process of titanium tetrachloride and isopropanol. The carrying out of the reaction of titanium tetrachloride and isopropanol, the hydrochlori...

Embodiment 1

[0048] Present embodiment is a kind of preparation method of titanium tetraisopropoxide, and the steps are as follows:

[0049] (1) Under the protection of nitrogen, the TiCl 4 (151.2g, 0.8mol) and isopropanol (192g, 3.2mol) were stirred evenly in n-hexane (1L), and placed in a low-temperature cold bath at 0°C;

[0050] (2) Add diethylamine (351g, 4.8mol) dropwise to the reaction system of step (1), which takes 30min, that is, the addition rate of said diethylamine is 9.6mol / h;

[0051] (3) After the reaction system of step (2) continued to react for 1 hour, under the protection of nitrogen, suction filtration was obtained to obtain the filtrate, and the solvent was distilled off under reduced pressure at 30° C. to obtain 216 g of crude product, with a yield of 95%;

[0052] (4) Purify the filtrate by distillation under a vacuum of 0.1 Torr, collect fractions at 62 to 65° C., and obtain titanium tetraisopropoxide (193 g, 0.68 mol) with a yield of 85%, which is a colorless tra...

Embodiment 2

[0055] This embodiment is a preparation method of titanium tetraisopropoxide, the steps of which are basically the same as those in Example 1, the main difference being that the amount of diethylamine added dropwise in step (2) is 234 g, 3.2 mol.

[0056] The specific technical scheme is as follows:

[0057] (1) Under the protection of nitrogen, the TiCl 4 (151.2g, 0.8mol) and isopropanol (192g, 3.2mol) were stirred evenly in n-hexane (1L), and placed in a low-temperature cold bath at 0°C;

[0058] (2) Add diethylamine (234g, 3.2mol) dropwise to the reaction system of step (1), which takes 20min, that is, the addition rate of said diethylamine is 9.6mol / h;

[0059] (3) After the reaction system of step (2) continued to react for 1 hour, under the protection of nitrogen, suction filtration was performed to obtain the filtrate, and the solvent was distilled off under reduced pressure at 30° C. to obtain 200 g of crude product with a yield of 88%;

[0060] (4) Distill and purif...

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Abstract

The invention relates to a preparation method of titanium tetraisopropoxide. The preparation method comprises the following steps: mixing a solvent, titanium tetrachloride and isopropanol to prepare amixed reaction system; and adding dialkylamine into the mixed reaction system to react, and carrying out aftertreatment on the obtained reactant to prepare the titanium tetraisopropoxide. The preparation method comprises the following steps: taking titanium tetrachloride and isopropanol as raw materials and adding dialkylamine into the mixed reaction system, wherein the dialkylamine can effectively absorb HCl generated by the reaction of the mixed reaction system, the reaction is promoted, meanwhile, impurities can be prevented from being generated, the high-purity titanium tetraisopropoxidecan be prepared through simple post-treatment, and the yield is high.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of titanium tetraisopropoxide. Background technique [0002] Titanium tetraisopropoxide, also known as tetrapropoxy titanium, tetraisopropoxide titanate or (tetra) isopropyl titanate, English name: Titanium tetraisopropanolate, CAS No. 546-68-9, its molecular structure is as follows Formula (1) shown. Titanium tetraisopropoxide has a wide range of uses in industry, the most important ones are: 1. Catalyst for transesterification and condensation reactions in organic synthesis; 2. Titanium tetraisopropoxide of electronic grade purity in atomic layer deposition process (ALD) can be used as a precursor material to provide a titanium source. [0003] [0004] There are three commonly used synthesis methods of titanium tetraisopropoxide: [0005] 1. Add TiCl 4 Stir evenly with isopropanol in toluene, heat to reflux, and distill under reduced pres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28
CPCC07F7/28
Inventor 陈鹏宇刘迪柯靖
Owner 苏州欣溪源新材料科技有限公司
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