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A kind of preparation method of long-chain alkyl phenyl modified silicone oil

A long-chain alkyl phenyl, modified silicon technology, applied in the field of silicone, can solve the problems of incomplete catalyst reaction, dark product color, etc., and achieve the effect of improving dispersion and fully and uniform reaction.

Active Publication Date: 2022-08-02
ZHEJIANG QUZHOU ZHENGBANG ORGANOSILICON CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method simplifies the steps, it is prone to incomplete reaction when there is less catalyst, and the product will be too dark when there is more catalyst.

Method used

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  • A kind of preparation method of long-chain alkyl phenyl modified silicone oil
  • A kind of preparation method of long-chain alkyl phenyl modified silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] To formulate Karstedt catalyst:

[0041] (1) Add chloroplatinic acid and isopropanol into the stirring tank, and stir at room temperature for 0.5h;

[0042] (2) Add sodium bicarbonate, heat up to 50°C, and stir for 0.5h;

[0043] (3) Add 1,3-divinyltetramethyldisiloxane and stir for 1h;

[0044] (4) Precipitation in the stirring tank at 50°C for 1h.

[0045] Wherein, the mass ratio of chloroplatinic acid: isopropanol: sodium bicarbonate: 1,3-divinyltetramethyldisiloxane is 1:50:25:25.

[0046] Preparation of long-chain alkyl phenyl modified silicone oil:

[0047] (1) adding part of Karstedt catalyst to the reactor;

[0048] (2) Under the protection of inert gas, α-methylstyrene was passed into the filter column containing neutral alumina and then flowed into the reaction kettle, heated to 70°C, stirred for 0.5h, and the stirring speed was 100n / min;

[0049] (3) dropping hydrogen-containing silicone oil with a hydrogen content of 0.5wt% into the reaction kettle, the...

Embodiment 2

[0055] To formulate Karstedt catalyst:

[0056] (1) Chloroplatinic acid and isopropanol were added to the stirring tank, and stirred at room temperature for 1 hour;

[0057] (2) Add sodium bicarbonate, heat up to 75°C, and stir for 1h;

[0058] (3) Add 1,3-divinyltetramethyldisiloxane and stir for 1h;

[0059] (4) Precipitate at 70°C for 1h in a stirring tank.

[0060] Wherein, the mass ratio of chloroplatinic acid: isopropanol: sodium bicarbonate: 1,3-divinyltetramethyldisiloxane is 1:100:30:30.

[0061] Preparation of long-chain alkyl phenyl modified silicone oil:

[0062] (1) adding part of Karstedt catalyst to the reactor;

[0063] (2) Under the protection of inert gas, α-methylstyrene was passed into the filter column containing neutral alumina and then flowed into the reaction kettle, heated to 85°C, stirred for 1h, and the stirring speed was 100n / min;

[0064] (3) drop the hydrogen-containing silicone oil with a hydrogen content of 1wt% into the reaction kettle, drop...

Embodiment 3

[0070] The Karstedt catalyst was formulated as in Example 2.

[0071] Preparation of long-chain alkyl phenyl modified silicone oil:

[0072] (1) adding part of Karstedt catalyst to the reactor;

[0073] (2) Under the protection of inert gas, α-methylstyrene was passed into the filter column containing neutral alumina and then flowed into the reaction kettle, heated to 80°C, stirred for 1h, and the stirring speed was 100n / min;

[0074] (3) drop the hydrogen-containing silicone oil with a hydrogen content of 1wt% into the reaction kettle, dropwise for 1 h, stir for 2 h while the reaction temperature rises to 110°C, to obtain phenyl modified silicone oil;

[0075] (4) adding the remaining Karstedt catalyst in the stirred tank in the reaction kettle;

[0076] (5) Under the protection of inert gas, α-dodecene was passed into the filter column containing neutral alumina and then flowed into the reaction kettle, stirred for 2 hours and kept the temperature at 140 ° C, stirring spee...

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PUM

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Abstract

The invention discloses a preparation method of long-chain alkyl phenyl modified silicone oil, which comprises the following steps: (1) adding a part of Karstedt catalyst to a reaction kettle; (3) drop the hydrogen-containing silicone oil into the reactor to obtain phenyl-modified silicone oil; (4) add the remaining catalyst in the stirring tank in the reactor; (5) add the α-olefin After passing through a filter column containing neutral alumina, it flows into the reactor to obtain long-chain alkyl phenyl modified silicone oil. Using Karstedt's catalyst instead of traditional chloroplatinic acid in isopropanol allows the reaction to proceed with less catalyst. At the same time, the reaction process is controlled by adding catalyst twice to prevent the product from being too dark due to too much catalyst.

Description

technical field [0001] The invention belongs to the field of organic silicon, and in particular relates to a preparation method of long-chain alkyl phenyl modified silicone oil. Background technique [0002] Silicone oils generally refer to linear polysiloxane products that remain liquid at room temperature. Generally divided into two categories: methyl silicone oil and modified silicone oil. The most commonly used silicone oil, all organic groups are methyl, called methyl silicone oil. The organic group can also use other organic groups to replace part of the methyl group to improve certain properties of the silicone oil and apply to various uses. [0003] Long-chain alkyl modified silicone oil refers to the replacement of some methyl groups by long-chain carbon hydrocarbon groups in ordinary dimethyl silicone oil, and the carbon chain length of long-chain alkyl groups is in the range of 2-17. Long-chain alkyl modified silicone oil not only strengthens the silicone oil T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/08C08G77/06
CPCC08G77/38C08G77/08C08G77/06
Inventor 郑启波
Owner ZHEJIANG QUZHOU ZHENGBANG ORGANOSILICON CO LTD
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