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Preparation method of triisopropyl silanol

A technology of triisopropylsilanol and triisopropylsilane, which is applied in the field of preparation of high-purity triisopropylsilanol, can solve the problems of solvent recovery, cumbersome, unsafe oxidants, etc., and achieve simple post-processing, The effect of high yield

Inactive Publication Date: 2016-07-06
SHANGHAI BETTERSYN BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such oxidants are not safe, and the system contains water products, which require extraction or distillation and dehydration steps to obtain products, which is very cumbersome
[0007] 3. It is a good method to use triisopropylsilane as raw material, conventional protic solvents such as methanol, ethanol, and isopropanol as solvent, and add alkali such as potassium hydroxide to hydrolyze, but there are also problems such as solvent recovery.

Method used

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  • Preparation method of triisopropyl silanol
  • Preparation method of triisopropyl silanol
  • Preparation method of triisopropyl silanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of triisopropylsilanol:

[0041] In a 2L four-necked flask equipped with a stirrer, a thermometer and a condenser tube, 250 g (1.58 mol) of triisopropylsilane, 353.9 g (6.32 mol) of KOH, 13.8 g (0.08 mol) of triisopropyl silanol were added under nitrogen protection. mol), the temperature was raised to 70° C., and the reaction was terminated by gas chromatography analysis of the reaction of the raw materials (triisopropylsilane was completely reacted). Cool down to room temperature, and adjust the pH of the reaction system to 6-8 by introducing hydrochloric acid gas. The organic phase was distilled to obtain 271.4 g of triisopropylsilanol (82-85° C. / 15 mmHg fraction), with a yield of 98.5%. Gained triisopropylsilanol analysis, its gas chromatography content 99.1%, gas chromatography result is as follows figure 1 and shown in Table 1. The HNMR identification results of the samples are as follows figure 2 shown.

[0042] Table 1

[0043]

Embodiment 2-10

[0045]Preparation of triisopropylsilanol:

[0046] In embodiment 2-10, the consumption of triisopropyl silane, the kind of alkali, the consumption of alkali, the consumption of triisopropyl silanol, reaction temperature are as shown in table 2, other reaction conditions and aftertreatment process are all with Example 1 is the same. The yield and content of the product obtained by the reaction are shown in Table 2.

[0047] Table 2

[0048]

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Abstract

The invention relates to the field of organic synthesis, particularly a preparation method of high-purity triisopropyl silanol. The preparation method comprises the following step: carrying out reaction on triisopropyl silane (disclosed as Formula II) and an alkali in the presence of a small amount of triisopropyl silanol to generate the triisopropyl silanol (disclosed as Formula I). The preparation method does not generate wastewater or any waste solvent; the after-treatment process is simple; the high-purity triisopropyl silanol can be obtained by simple distillation; the yield is very high; and the purity of the product can reach 99.0% or above.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of high-purity triisopropylsilanol. Background technique [0002] Triisopropylsilanol (Triisopropylsilanol, CASNo.17877-23-5, structural formula shown in formula I), as a new type of composite functional material monomer, is currently mainly used in special antifouling coatings in the shipbuilding industry. Due to its toxicity Low pollution, little pollution, has gradually replaced tin-containing toxic antifouling coatings, in addition, the product has good strength and excellent toughness after cross-linking molding, and has entered the military field to make bulletproof helmets and other It can also be used as an important pharmaceutical intermediate and has broad application prospects. [0003] [0004] The synthetic method of triisopropyl silanol mainly contains 3 classes at present: [0005] 1. Triisopropylchlorosilane (CASNo.13154-24-0) is used as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C07F7/20
CPCC07F7/0836C07F7/20
Inventor 刘伟马钰石强万赵士峰李文龙
Owner SHANGHAI BETTERSYN BIOTECH