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Octamethyl octasilsesquioxane and its preparation method and application

A technology of octamethyloctasilsesquioxane and tetramethyltetrahydrocyclotetrasiloxane, which is applied in the field of preparation of octamethyloctasilsesquioxane, can solve the problem of low POSS yield and affecting performance , high production cost and other issues, to achieve the effect of mild reaction conditions, good reaction selectivity and low production cost

Active Publication Date: 2019-06-21
SHENZHEN TAIKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because of this, there are at least the following three deficiencies in the trichlorosilane hydrolysis condensation method: (1) a large amount of reaction medium must be used, which seriously affects the productivity of the product and limits the production capacity of the equipment; (2) trichlorosilane hydrolysis The yield of POSS prepared by condensation method is low, and the yield is often about 8%~10% in the common preparation process report; The POSS cage structure is not always formed, and a large amount of insoluble and infusible large molecular weight cross-linked products are also generated due to the condensation polymerization reaction between different silanol molecules, and these by-products are difficult to remove from POSS
Make POSS products impure and affect their performance
The above shortcomings make POSS poor in quality, high in production cost, and difficult to produce large quantities of products with limited equipment, thus severely limiting the scope of application of POSS as an excellent heat-resistant material.

Method used

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  • Octamethyl octasilsesquioxane and its preparation method and application
  • Octamethyl octasilsesquioxane and its preparation method and application
  • Octamethyl octasilsesquioxane and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] catalytic hydrolysis

[0031] In a four-necked flask equipped with a reflux condenser, mechanical stirring and heating device, drop into 100 grams of acetone, 0.5 grams of 5% Pd / C catalyst and 12 grams of buffer solution (0.65 grams of NaH 2 PO 4 ·H 2 O was prepared by adding 40 g of 0.1 mol / L NaOH aqueous solution), cooled to 5°C in an ice-water bath, and slowly added 24.5 g of tetramethyltetrahydrocyclotetrasiloxane dropwise, and the drop was completed in 30 minutes. After the addition, the reaction was carried out for 30 minutes, and the temperature was raised to 25° C. to continue the reaction for 3 hours. After the reaction is finished, the Pd / C is suction-filtered, and the Pd / C that is suction-filtered can be recycled. The obtained filtrate is the hydrolysis product tetramethyltetrahydroxycyclotetrasiloxane, and the filtrate does not need to be separated and directly enters the next step of reaction.

[0032] condensation

[0033] Transfer 120 grams of the ab...

Embodiment 2

[0036] catalytic hydrolysis

[0037] In a four-necked flask equipped with a reflux condenser, mechanical stirring and heating device, drop into 120 grams of acetone, 1.0 grams of 5% Pd / C catalyst and 12 grams of buffer solution (0.8 grams of NaH 2 PO 4 ·H 2 O was prepared by adding 40 grams of 0.1 mol / L NaOH aqueous solution), cooled in an ice-water bath at about 2°C, and slowly added 25.0 grams of tetramethyltetrahydrocyclotetrasiloxane dropwise, and the drop was completed in 45 minutes. After the addition was completed, the reaction was carried out for 45 minutes, and the temperature was raised to 28° C. to continue the reaction for 5 hours. After the reaction is finished, the Pd / C is suction-filtered, and the obtained filtrate does not need to be separated, and directly enters the next step of the reaction.

[0038] condensation

[0039] Transfer 121.3 grams of the filtrate of the above-mentioned hydrolyzate tetramethyltetrahydroxycyclotetrasiloxane to a four-necked flask...

Embodiment 3

[0042] catalytic hydrolysis

[0043] In the four-necked flask equipped with reflux condenser, mechanical stirring and heating device, drop into 100 grams of butanone, 0.9 grams of 5% Pd / C catalyst and 12 grams of buffer solution (0.8 grams of NaH 2 PO 4 ·H 2 O was prepared by adding 40 g of 0.1 mol / L NaOH aqueous solution), cooled to 4°C in an ice-water bath, and slowly added 24.4 g of tetramethyltetrahydrocyclotetrasiloxane dropwise for 40 minutes. After the addition, the reaction was carried out for 50 minutes, and the temperature was raised to 25° C. to continue the reaction for 3 hours. After the reaction is finished, the Pd / C is suction-filtered to obtain a filtrate, and the filtrate does not need to be separated, and directly enters the next step of the reaction.

[0044] condensation

[0045] Transfer 118.6 grams of the above-mentioned filtrate to a four-necked flask, assemble a reflux condenser, mechanical stirring and heating device, add 2.1 grams of tris(pentaflu...

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PUM

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Abstract

The invention discloses octamethylsilsesquioxane and a preparation method and application thereof. With tetramethyl tetralin cyclotetrasiloxane being a raw material, the octamethylsilsesquioxane is prepared through catalytic hydrolysis and a condensation reaction. Cyclosiloxane is used as a raw material, in this way, reaction conditions are mild, no hydrogen chloride gas is released, and operation environment is good. Tri(pentafluorophenyl)borane is utilized for a catalytic reaction, selectivity is good, in this way, the yield is high, cost is low, and production efficiency is high. The preparation technology of the octamethylsilsesquioxane is simple, the raw materials are easy to obtain, industrial production, application and popularization are easy, and a foundation is laid for preparation of a large amount of POSS and expanded application of POSS as a heat-resisting material and a modifying agent.

Description

technical field [0001] The invention relates to a preparation method of octamethyloctasilsesquioxane (POSS), which belongs to the field of organosilicon materials and fine chemicals. Background technique [0002] Octamethyloctasilsesquioxane (POSS) is an organic-inorganic hybrid material. Because of its elemental composition close to that of inorganic silicate and the performance characteristics of organosilicon, POSS has great potential in modifying polymers. big advantage. For example, the introduction of octamethyloctasilsesquioxane as a bridging group into polymers through chemical bonding can increase the glass transition temperature of the product and increase the hardness and modulus of the material. Improve the thermal stability of the product and improve the flame retardant performance of the polymer. POSS can also be mixed into polymer materials as an additive, and the heat-resistant nature of octamethyloctasilsesquioxane can be used to improve the high-temperatu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/04C08G77/08
CPCC08G77/045C08G77/08
Inventor 傅筠
Owner SHENZHEN TAIKE TECH