CN105669981B - A kind of preparation method of branched chain silicone - Google Patents
A kind of preparation method of branched chain silicone Download PDFInfo
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- CN105669981B CN105669981B CN201410656506.8A CN201410656506A CN105669981B CN 105669981 B CN105669981 B CN 105669981B CN 201410656506 A CN201410656506 A CN 201410656506A CN 105669981 B CN105669981 B CN 105669981B
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Abstract
The invention discloses a kind of preparation methods of branched chain silicone, after siloxanes, silsesquioxane and hexamethyl siloxane are mixed, potassium hydroxide is added, stirring is maintained at 100-150 DEG C, until silsesquioxane is completely dissolved, then end-capping reagent termination reaction is added after being cooled to room temperature, branched chain silicone can be obtained in filtering, distillation.The present invention overcomes the disadvantages of complex process, pollution environment, process repeatability difference in traditional branched chain silicone preparation process, the content of branch in silicone oil also can be accurately controlled simultaneously, by silsesquioxane and hexamethyl siloxane that different content is added, a series of controllable branched chain type silicone oil of viscosity can be prepared, prepared silicone oil has the characteristics that viscosity controllable, low temperature performance well, production cost be low, simple process, traditional silicone oil preparation process can significantly be improved, can be widely applied in aviation and other machinery fields.
Description
Technical field
The present invention relates to a kind of preparation methods of branched chain silicone.
Background technique
Silicone oil, with the oil product that background is widely applied, is widely used in machine-building, cosmetics, instrument and meter as a kind of
In equal fields.Very low use temperature is often required that in machinery field, therefore it is required that used silicone oil has extremely low coagulate
Solid point.For this purpose, the branched structure for introducing certain content in silicone molecule is a kind of general side during synthesizing silicone oil
Method.After introducing branch, the freezing point of silicone oil be can reduce to -70 DEG C hereinafter, meeting the requirement of different machinery.At present
It is generally divided into two-step method during preparing branched chain silicone to be produced: first by methyltriethoxysilane, prestox ring
Tetrasiloxane (D4) react using Loprazolam catalysis with hexamethyl siloxane (MM) prepares the higher silicone oil of branching content,
Then, the silicone oil of the high branching content is carried out reacting under ammonium hydroxide or potassium hydroxide catalysed with D4 preparing finished product silicone oil.
In the process, due to using stepwise reaction, not only complex process, but also there are the strong acid such as Loprazolam in reacting, to environment
It is be easy to cause pollution, in addition, due to using the techniques such as vacuum high-temperature dehydration, holding in the process in current preparation process
It easily causes the raw materials such as D4, MM to be distilled out reaction system with water together, branching content in branched chain silicone is caused to be difficult to control accurately,
In turn result in the unstability of product quality.Therefore, branching content how is accurately controlled, environmental pollution is reduced, simplifies preparation work
Skill is the important channel improved branched chain silicone product quality, expand silicone oil application range.
Summary of the invention
A kind of preparation method for low, simple process branched chain silicone that the purpose of the present invention is to provide production costs.
A kind of preparation method of branched chain silicone, it is characterised in that: mix siloxanes, silsesquioxane and hexamethyl siloxane
After conjunction, potassium hydroxide is added, stirring is maintained at 100-150 DEG C, until silsesquioxane is completely dissolved, is then cooled to room temperature
End-capping reagent is added afterwards and terminates reaction, branched chain silicone can be obtained in filtering, distillation.
The siloxanes be octamethylcy-clotetrasiloxane, aminomethyl phenyl cyclotetrasiloxane, dimethicone, ethyl silicon oil,
Trifluoro propyl methyl-silicone oil or methyl phenyl silicone oil.
The mass ratio of the siloxanes, silsesquioxane and hexamethyl siloxane is 100: 1-5: 0-1.
The silsesquioxane is polymethylsilsesquioxane or poly-phenyl silsesquioxane.
The end-capping reagent is trim,ethylchlorosilane, and the molar ratio with potassium hydroxide is 1:1.
The additional amount of the potassium hydroxide is siloxanes, silsesquioxane and hexamethyl siloxane mixture gross mass
0.01%~5%.
Compared with the prior art, the present invention has the following advantages:
1, the present invention overcomes complex process in traditional branched chain silicone preparation process, pollution environment, process repeatability differences
Disadvantage, while the content of branch in silicone oil also can be accurately controlled, by the way that different amounts of silsesquioxane and hexamethyl silicon is added
Oxygen alkane can prepare a series of controllable branched chain type silicone oil of viscosity.
2, the silicone oil prepared by the present invention has that viscosity is controllable, freezing point is low, low temperature performance well, production cost are low, technique
The features such as simple.
3, the present invention has the characteristics that viscosity is controllable, production cost is low, can substitute traditional preparation process.
Specific embodiment
The present invention will be further explained with reference to the examples below.
Embodiment 1 prepares branched chain silicone with polymethylsilsesquioxane
Octamethylcy-clotetrasiloxane 500g, polymethylsilsesquioxane 8g, hexamethyl siloxane 5g are added in polymeric kettle,
It is uniformly mixed, 2g potassium hydroxide is added, maintain stirring to be allowed to react at 120 DEG C, when methyl silicon sesquialter poly- in polymeric kettle
After oxygen alkane is completely dissolved, it is cooled to room temperature, trim,ethylchlorosilane 3.9g is added, and maintains stirring 1-2 hours, is filtered to remove precipitating
Vacuum distillation obtains silicone oil product afterwards.
Embodiment 2 prepares branched chain silicone with poly-phenyl silsesquioxane
Octamethylcy-clotetrasiloxane 1000g, poly-phenyl silsesquioxane 15g, hexamethyl siloxane are added in polymeric kettle
5g is uniformly mixed, and 4g potassium hydroxide is added, and maintains stirring to be allowed to react at 120 DEG C, when polyphenylene silicon times in polymeric kettle
After half oxygen alkane is completely dissolved, it is cooled to room temperature, trim,ethylchlorosilane 7.8g is added, and maintains stirring 1-2 hours, it is heavy to be filtered to remove
Vacuum distillation obtains silicone oil product behind shallow lake.
Embodiment 3 prepares branched chain silicone with dimethicone
Dimethicone 1200g, polymethylsilsesquioxane 18g are added in polymeric kettle, is uniformly mixed, 4g is added
Potassium hydroxide maintains stirring to be allowed to react at 120 DEG C, after polymethylsilsesquioxane is completely dissolved in polymeric kettle, cooling
To room temperature, trim,ethylchlorosilane 7.8g is added, and maintains stirring 1-2 hours, vacuum distillation obtains silicone oil after being filtered to remove precipitating
Product.
Embodiment 4 prepares branch ethyl silicon oil
Ethyl silicon oil 800g, polymethylsilsesquioxane 13g are added in polymeric kettle, is uniformly mixed, 2g hydrogen is added
Potassium oxide maintains stirring to be allowed to react, after polymethylsilsesquioxane is completely dissolved in polymeric kettle, is cooled at 120 DEG C
Trim,ethylchlorosilane 3.9g is added in room temperature, and maintains stirring 1-2 hours, and vacuum distillation obtains silicone oil production after being filtered to remove precipitating
Product.
Embodiment 5 prepares branched chain methyl phenyl silicone oil
Methyl phenyl silicone oil 1500g, polymethylsilsesquioxane 30g are added in polymeric kettle, is uniformly mixed, is added
4g potassium hydroxide maintains stirring to be allowed to react at 120 DEG C, after polymethylsilsesquioxane is completely dissolved in polymeric kettle, drop
It warms to room temperature, trim,ethylchlorosilane 7.8g is added, and maintain stirring 1-2 hours, vacuum distillation obtains silicon after being filtered to remove precipitating
Oil product.
Embodiment 6 prepares branch trifluoro propyl methyl-silicone oil
Trifluoro propyl methyl-silicone oil 2000g, poly-phenyl silsesquioxane 30g are added in polymeric kettle, is uniformly mixed,
4g potassium hydroxide is added, maintains stirring to be allowed to react at 120 DEG C, when poly-phenyl silsesquioxane is completely dissolved in polymeric kettle
Afterwards, it is cooled to room temperature, trim,ethylchlorosilane 7.8g is added, and maintains stirring 1-2 hours, is evaporated under reduced pressure to after being filtered to remove precipitating
To silicone oil product.
Embodiment 7 prepares high viscosity metlyl branching silicone oil
Octamethylcy-clotetrasiloxane 500g, polymethylsilsesquioxane 15g, hexamethyl siloxane are added in polymeric kettle
1g is uniformly mixed, and 2g potassium hydroxide is added, and maintains stirring to be allowed to react at 120 DEG C, when methyl silicon poly- in polymeric kettle times
After half oxygen alkane is completely dissolved, it is cooled to room temperature, trim,ethylchlorosilane 3.9g is added, and maintains stirring 1-2 hours, it is heavy to be filtered to remove
Vacuum distillation obtains silicone oil product behind shallow lake.
Obtained properties of product are as shown in table 1 in above-described embodiment, it can be seen that obtained product has very low
Freezing point, while after adjusting the dosage of hexamethyl siloxane, it can be substantially change the viscosity of silicone oil, while also having very low
Freezing point.
Table 1
。
Claims (5)
1. a kind of preparation method of branched chain silicone, it is characterised in that mix siloxanes, silsesquioxane and hexamethyl siloxane
Afterwards, potassium hydroxide is added, stirring is maintained at 100-150 DEG C, until silsesquioxane is completely dissolved, after being then cooled to room temperature
End-capping reagent is added and terminates reaction, branched chain silicone can be obtained in filtering, distillation；
The end-capping reagent is trim,ethylchlorosilane, and the molar ratio with potassium hydroxide is 1:1.
2. preparation method as described in claim 1, it is characterised in that the siloxanes is octamethylcy-clotetrasiloxane, methylbenzene
Basic ring tetrasiloxane, dimethicone, ethyl silicon oil, trifluoro propyl methyl-silicone oil or methyl phenyl silicone oil.
3. preparation method as described in claim 1, it is characterised in that the siloxanes, silsesquioxane and hexamethyl siloxane
Mass ratio be 100:1-5:0-1.
4. preparation method as described in claim 1, it is characterised in that the silsesquioxane be polymethylsilsesquioxane or
Poly-phenyl silsesquioxane.
5. preparation method as described in claim 1, it is characterised in that the additional amount of the potassium hydroxide is siloxanes, silicon sesquialter
The 0.01%~5% of oxygen alkane and hexamethyl siloxane mixture gross mass.
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| CN201410656506.8A CN105669981B (en) | 2014-11-18 | 2014-11-18 | A kind of preparation method of branched chain silicone |
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| CN201410656506.8A CN105669981B (en) | 2014-11-18 | 2014-11-18 | A kind of preparation method of branched chain silicone |
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| CN105669981B true CN105669981B (en) | 2019-03-29 |
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| CN115386088B (en) * | 2022-10-12 | 2023-06-27 | 中国科学院兰州化学物理研究所 | Fluorine-containing silicone oil and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016384A (en) * | 2007-02-09 | 2007-08-15 | 南京大学 | Method of preparing star-type multi-arm silicon oil |
| CN103289096A (en) * | 2013-01-16 | 2013-09-11 | 杭州师范大学 | Preparation method and application of polyhedral oligomeric silsesquioxane skeleton containing vinyl silicone oil |
| CN104211965A (en) * | 2013-06-03 | 2014-12-17 | 北京化工大学 | Preparation method for net-like methyl phenyl vinyl polysiloxane for LED packaging |
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2014
- 2014-11-18 CN CN201410656506.8A patent/CN105669981B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016384A (en) * | 2007-02-09 | 2007-08-15 | 南京大学 | Method of preparing star-type multi-arm silicon oil |
| CN103289096A (en) * | 2013-01-16 | 2013-09-11 | 杭州师范大学 | Preparation method and application of polyhedral oligomeric silsesquioxane skeleton containing vinyl silicone oil |
| CN104211965A (en) * | 2013-06-03 | 2014-12-17 | 北京化工大学 | Preparation method for net-like methyl phenyl vinyl polysiloxane for LED packaging |
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