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A kind of preparation method of highly active tetramethylammonium hydroxide organosilicon alkali gel

A technology of tetramethylammonium hydroxide and ammonium hydroxide, which is applied in the field of silicone rubber, can solve the problems of reduced heat resistance of silicone rubber, difficulty in controlling molecular weight, and reduced catalyst activity, achieving improved thermal stability, high catalytic activity, High ring-opening activity

Active Publication Date: 2020-12-01
中蓝晨光化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if it is used in the synthesis of phenyl silicone rubber raw rubber, it has the disadvantages of inhomogeneous polymerization and difficult molecular weight control.
The remaining water and hydroxyl groups will not only reduce the activity of the catalyst, but also act as a polymerized head agent to reduce the molecular weight of the raw rubber. end, so that the heat resistance of silicone rubber is reduced

Method used

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  • A kind of preparation method of highly active tetramethylammonium hydroxide organosilicon alkali gel
  • A kind of preparation method of highly active tetramethylammonium hydroxide organosilicon alkali gel

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Embodiment 1

[0044] The present embodiment proposes a kind of preparation method of highly active tetramethylammonium hydroxide organosilicon alkali gel, and the method comprises the following steps:

[0045] (1) Weathering: Add 20 parts by weight of tetramethylammonium hydroxide pentahydrate into the flask, while stirring and vacuuming, heat and introduce a small amount of nitrogen flow to make the hydrated tetramethylammonium hydroxide desorb from the crystal water and become free Water Tetramethylammonium Hydroxide;

[0046] (2) Dehydration: add 800 parts by weight of octamethylcyclotetrasiloxane, stir and evacuate to maintain a vacuum degree of -0.08MPa, and at the same time raise the temperature to 80°C to distill out octamethylcyclotetrasiloxane;

[0047] (3) Reaction balance: adjust the nitrogen flow rate to reduce the vacuum degree until no distillate is distilled out, and continue stirring to raise the temperature to 100°C. After the material changes from turbid to colorless, tran...

Embodiment 2

[0050] The present embodiment proposes a kind of preparation method of highly active tetramethylammonium hydroxide organosilicon alkali gel, and the method comprises the following steps:

[0051] (1) Weathering: Add 100 parts by weight of tetramethylammonium hydroxide pentahydrate into the flask, while stirring and evacuating, heat and introduce a small amount of nitrogen flow to make the hydrated tetramethylammonium hydroxide desorb from crystal water and become free Water Tetramethylammonium Hydroxide;

[0052] (2) Dehydration: add 1100 parts by weight of octamethylcyclotetrasiloxane, stir and vacuumize to maintain a vacuum degree of -0.09MPa, and at the same time raise the temperature to 60°C to distill out octamethylcyclotetrasiloxane;

[0053] (3) Reaction balance: adjust the nitrogen flow rate to reduce the vacuum degree until no distillate is distilled out, and continue stirring to raise the temperature to 90°C. After the material changes from turbid to colorless, trans...

Embodiment 3

[0056] The present embodiment proposes a kind of preparation method of highly active tetramethylammonium hydroxide organosilicon alkali gel, and the method comprises the following steps:

[0057] (1) Weathering: Add 60 parts by weight of tetramethylammonium hydroxide pentahydrate into the flask, while stirring and evacuating, heat and introduce a small amount of nitrogen flow to make the hydrated tetramethylammonium hydroxide desorb from crystal water and become free Water Tetramethylammonium Hydroxide;

[0058] (2) Dehydration: add 950 parts by weight of octamethylcyclotetrasiloxane, stir and evacuate to maintain a vacuum degree of -0.085MPa, and at the same time raise the temperature to 70°C to evaporate octamethylcyclotetrasiloxane;

[0059] (3) Reaction balance: adjust the nitrogen flow rate to reduce the vacuum degree until no distillate is distilled out, and continue to stir and heat up to 95°C. After the material changes from turbid to colorless, transparent and viscous...

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Abstract

The invention belongs to the technical field of silicone rubber, and specifically discloses a preparation method of high activity tetramethylammonium hydroxide organosilicon alkali glue. The preparation method comprises the following steps: performing efflorescence treatment on tetramethylammonium hydroxide pentahydrate, adding octamethylcy-clotetrasiloxane, performing dewatering, reaction balancing and cooling, and dropwise adding tetramethyldisiloxane for further removing residual water and hydroxyl groups to obtain high activity alkali glue. The method is simple in operation, and can maximally remove moisture and hydroxyl groups from the alkali glue without introducing other by-products or new impurities. Meanwhile, when the prepared tetramethylammonium hydroxide organosilicon alkali glue is applied to synthesis of crude phenyl silicone rubber, the molecular weight is easier to control, the thermal stability of the silicone rubber is effectively improved, and the requirements of theaerospace field can be better met.

Description

technical field [0001] The invention belongs to the technical field of silicone rubber, and in particular relates to a preparation method of highly active tetramethylammonium hydroxide organosilicon alkali gel. Background technique [0002] Silicone rubber is a kind of highly elastic artificial synthetic material with special properties such as high and low temperature resistance, aging resistance, electrical insulation, low surface energy and radiation resistance. It is widely used in aerospace, electronic appliances, electric power, construction, transportation and other areas of daily life. Especially in the field of aerospace, more types of silicone rubber are required and the requirements are higher. Among them, the high-end material varieties represented by phenyl silicone rubber have become irreplaceable due to their wider temperature resistance range and unique wide temperature range viscoelasticity. [0003] The synthesis route of phenyl silicone rubber is general...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/04
CPCC08G77/04
Inventor 唐小斗谢琴康乃文朱良波
Owner 中蓝晨光化工有限公司