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Preparation method of long-chain alkyl phenyl modified silicone oil

A technology of long-chain alkylphenyl and modified silicon, which is applied in the field of organic silicon, which can solve the problems of incomplete catalyst reaction and dark product color, and achieve the effect of improving dispersion and fully uniform reaction

Active Publication Date: 2020-06-26
郑启波
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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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  • Preparation method of long-chain alkyl phenyl modified silicone oil
  • Preparation method of long-chain alkyl phenyl modified silicone oil
  • Preparation method of long-chain alkyl phenyl modified silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] To prepare Karstedt's 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 1 h;

[0044] (4) The stirred tank was kept warm at 50°C for 1 hour of precipitation.

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

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

[0047] (1) Part of the Karstedt catalyst is added to the reactor;

[0048] (2) Pass α-methylstyrene into the filter column containing neutral alumina under the protection of inert gas and then flow into the reactor, heat up to 70°C, stir for 0.5h, and the stirring speed is 100n / min;

[0049] (3) Drop hydrogen-containing silicone oil with a hydrogen content of 0.5wt% into the reactor for 0.5 hours, s...

Embodiment 2

[0055] To prepare Karstedt's catalyst:

[0056] (1) Add chloroplatinic acid and isopropanol into the stirring tank, and stir 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 1 h;

[0059] (4) The stirred tank was kept warm at 70°C for 1 hour of precipitation.

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

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

[0062] (1) Part of the Karstedt catalyst is added to the reactor;

[0063] (2) Pass α-methylstyrene through a filter column containing neutral alumina under the protection of an inert gas, then flow into the reactor, heat up to 85°C, stir for 1 hour, and the stirring speed is 100n / min;

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

Embodiment 3

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

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

[0072] (1) Part of the Karstedt catalyst is added to the reactor;

[0073] (2) Pass α-methylstyrene through a filter column containing neutral alumina under the protection of an inert gas, then flow into the reactor, heat up to 80°C, stir for 1 hour, and the stirring speed is 100n / min;

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

[0075] (4) add the remaining Karstedt catalyst in the stirred tank in the reactor;

[0076] (5) Pass α-dodecene through a filter column containing neutral alumina under the protection of an inert gas and then flow into the reactor, stir for 2 hours and keep the temperature at 140°C with a stirring speed of 100n / min to obtain a long Alkylpheny...

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Abstract

The invention discloses a preparation method of long-chain alkyl phenyl modified silicone oil. The preparation method comprises the following steps: (1) adding part of a Karstedt catalyst into a reaction kettle; (2) introducing alpha-methylstyrene into a filter column containing neutral aluminum oxide under the protection of inert gas, and enabling the alpha-methylstyrene to flow into a reaction kettle; (3) adding hydrogen-containing silicone oil dropwise into the reaction kettle to obtain phenyl modified silicone oil; (4) adding the residual Karstedt catalyst in a stirring tank into the reaction kettle; and (5) introducing alpha-olefin into the filter column containing neutral aluminum oxide under the protection of inert gas, and then enabling the alpha-olefin to flow into the reaction kettle to obtain the long-chain alkyl phenyl modified silicone oil. The Karstedt catalyst is used for replacing the traditional isopropanol chloroplatinate solution, so that the reaction can be carriedout under the condition of using less catalyst. Meanwhile, the Karstedt catalyst is added for the second time to control the reaction process, so that the product color is prevented from being too dark due to excessive catalyst. The filter column containing neutral aluminum oxide can remove impurities in alpha-methylstyrene and alpha-olefin, so that Si-H bond can react sufficiently, and the conversion rate is increased.

Description

technical field [0001] The invention belongs to the field of organosilicon, and in particular relates to a preparation method of long-chain alkylphenyl modified silicone oil. Background technique [0002] Silicone oils generally refer to linear polysiloxane products that remain liquid at room temperature. It is generally divided into two types: methyl silicone oil and modified silicone oil. The most commonly used silicone oil, organic groups are all methyl, called methyl silicone oil. The organic group can also use other organic groups to replace part of the methyl group, so as to improve certain properties of silicone oil and apply to various purposes. [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. The carbon chain length of the long-chain alkyl group is in the range of 2-17. The long-chain alkyl modified silicone oil not only strengthens the silicon...

Claims

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Application Information

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IPC IPC(8): C08G77/38C08G77/08C08G77/06
CPCC08G77/38C08G77/08C08G77/06
Inventor 郑启波
Owner 郑启波
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