Alkyl silicone oil for immersed cooling medium of data center and preparation method of alkyl silicone oil
By using a micro-reaction continuous flow preparation method, combining plate microchannel reactors and tubular reactors, and controlling reaction conditions, alkyl silicone oil with low Si-H residue was prepared. This solved the problems of low-temperature turbidity and stability of modified silicone oil, and achieved a coolant with high flash point and low viscosity, suitable for applications in a wide range of climatic conditions in data centers.
Patent Information
- Application Number
- CN202511205624.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-27
- Publication Date
- 2025-10-28
- Estimated Expiration
- 2045-08-27
AI Technical Summary
Existing modified silicone oil coolants are prone to turbidity at low temperatures and have high residual Si-H groups, which affects stability and system reliability and cannot meet the application requirements of data centers under a wide range of climatic conditions.
A micro-reaction continuous flow preparation method was adopted, which combines a plate microchannel reactor and a tubular reactor to control the reaction temperature and time. A platinum complex catalyst was used to carry out the hydrosilylation reaction, and combined with activated carbon adsorption decolorization and rotary evaporation treatment to prepare alkyl silicone oil with low Si-H residue.
The prepared alkyl silicone oil is clear and transparent at low temperatures, has a high flash point, low viscosity, and a Si-H residue of less than 0.1 ppm. It is adaptable to a wide range of climatic conditions, improving the stability and reliability of the coolant.
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Figure CN120842580A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of cooling media, and more specifically, to an alkyl silicone oil for immersion cooling media in data centers and a micro-reaction continuous flow preparation method. Background Technology
[0002] One of the core challenges in improving data center energy efficiency lies in significantly reducing energy consumption, with Power Usage Effectiveness (PUE) being a key metric. Traditional air-cooling technologies, due to their high energy consumption and noise levels, struggle to reduce PUE to ideal levels. In contrast, immersion liquid cooling technology, by allowing the fluid cooling medium to directly contact heat-generating equipment such as servers, achieves more efficient heat transfer and has become the most promising solution. This technology can bring the data center's PUE close to the theoretical limit of 1.0, thereby significantly reducing overall energy consumption.
[0003] The core element of immersion liquid cooling is a high-performance fluid cooling medium. Currently, common coolants on the market include fluorinated liquids, mineral oils, and silicone oils, but each has its own significant drawbacks:
[0004] (1) Fluorinated liquids: They usually have a high density and a low boiling point, which may pose safety and environmental challenges.
[0005] (2) Mineral oil: It is inexpensive, but it generally has material compatibility problems (which may cause aging and swelling of seals, coatings, etc.) and poor antioxidant aging performance (short service life, requiring frequent replacement).
[0006] (3) Ordinary silicone oil: Although it has good anti-oxidation and anti-aging properties, its relatively high dielectric constant (which affects electrical insulation performance) often fails to meet the stringent safety and reliability requirements of data center coolant.
[0007] Developing high-performance silicone oil-based cooling media through chemical modification has become a key research focus. Liquid polysiloxanes, also known as silicone oils, are a class of chain-like polysiloxane products with varying degrees of polymerization that remain liquid at room temperature. Their molecular structures can be linear or branched. Silicone oils use a repeating Si-O-Si structure as their main chain, with organic groups (alkyl, phenyl, etc.) attached to the silicon atoms. This unique molecular structure, containing both organic groups and inorganic silica, gives silicone oils the properties of both organic polymers and inorganic compounds, such as heat resistance.
[0008]
[0009] When all R groups are methyl, it is ordinary dimethyl silicone oil; when some or all of the R groups are alkyl, phenyl, or other organic groups, it is called modified silicone oil. Modified silicone oil can be understood as a product in which some of the methyl groups in dimethyl silicone oil are replaced by organic groups or other chain segments.
[0010] The viscosity of silicone oil is less dependent on temperature. At lower temperatures, the polysiloxane chain length shortens, resulting in lower molecular entanglement of the side chain groups. As the temperature gradually increases, the polysiloxane chain lengthens, and the side chain groups form a more compact high-energy configuration, intensifying molecular entanglement and offsetting the increased molecular motion effect. Therefore, the viscosity of flexible polysiloxanes is far less affected by temperature changes than that of fluids with rigid carbon chain molecules.
[0011] Researchers have modified silicone oils to overcome their high dielectric constant while retaining their inherent advantages (such as high thermal stability, low toxicity, and long lifespan), and optimized other key properties (such as viscosity, thermal conductivity, and pour point). However, existing modified silicone oil synthesis methods still face challenges: Chinese patent CN116438502A proposes a method for preparing side-chain alkyl silicone oils and evaluates their basic properties as direct contact coolants. However, the alkyl silicone oils prepared by this patented method have a critical problem—a high content of residual Si-H groups (silicon-hydrogen bonds). Excessive Si-H content may lead to decreased stability of the coolant during long-term use (such as increased risk of oxidation and hydrolysis) or the generation of byproducts, affecting system reliability.
[0012] Existing mature products on the market, such as Dow's DOWSIL™ ICL-1000 Fluid, while offering good overall performance, have an application limitation: this silicone oil coolant becomes cloudy when the ambient temperature is below approximately 25°C. This low-temperature turbidity not only affects visual monitoring but may also indicate potential physical state changes (such as crystallization or precipitation), limiting its application in a wider range of climatic conditions. In conclusion, developing novel modified silicone oil coolants that combine excellent dielectric properties (low dielectric constant), superior long-term stability (low Si-H residue, strong oxidation resistance), a wide operating temperature range (low pour point, no low-temperature turbidity), and good material compatibility is key to promoting the widespread application of immersion liquid cooling technology and achieving ultimate energy efficiency in data centers.
[0013] Based on the above, it is of great significance to develop an alkyl-modified silicone oil and its micro-reaction continuous flow synthesis process.
[0014] The above content is only used to help understand the technical solution of the present invention and does not represent an admission that the above content is prior art. Summary of the Invention
[0015] The primary objective of this invention is to provide an alkyl silicone oil for use as an immersion cooling medium in data centers, which is clear and transparent at low temperatures while still retaining fluidity, has a flash point above 200°C, and a viscosity below 25 mm (at 40°C). 2 / s (cst) can meet more application scenarios. In addition, the present invention also provides a micro-reaction continuous flow preparation method for modified silicone oil, with short reaction time (3~5min), low Si-H bond residue (<0.1ppm), and the silicone oil viscosity can be flexibly adjusted according to market demand.
[0016] This invention first provides an alkyl silicone oil for use as an immersion cooling medium in data centers, the alkyl silicone oil comprising substances with the following molecular structure:
[0017] .
[0018] Where n ranges from 18 to 22, and m is 8 or 10.
[0019] Preferably, when n is constant, the mixing ratio of alkyl silicone oil with m=8 to alkyl silicone oil with m=10 is in the range of (1~4):1.
[0020] Preferably, the alkyl silicone oil is a transparent fluid at -50°C, has a flash point greater than 200°C, and a viscosity less than 20 mm (at 40°C). 2 / s (cst), Si-H residue is less than 0.1ppm.
[0021] This invention also provides a micro-reaction continuous flow preparation method for alkyl silicone oil, comprising the following steps:
[0022] The hydrogen-sealed low-hydrogen-content silicone oil and the olefin and platinum catalyst mixture solution are pumped into the microreactor at a set flow rate and quickly mixed evenly. The mixed material is then transported to a tubular reactor for hydrosilylation reaction to obtain a mixture containing alkyl silicone oil.
[0023] The alkyl silicone oil mixture was subjected to rotary evaporation to obtain alkyl silicone oil.
[0024] The temperature of the microreactor and the tubular reactor is 85~95℃, and the total residence time is 3~5min.
[0025] Preferably, the mixture containing alkyl silicone oil is decolorized before being subjected to rotary evaporation.
[0026] Preferably, the decolorization treatment includes activated carbon adsorption decolorization.
[0027] Preferably, the rotary evaporation process includes vacuum rotary evaporation and / or reduced pressure rotary evaporation.
[0028] Preferably, the microreactor and the tubular reactor control the reaction temperature via an oil bath.
[0029] Preferably, the microreactor is a plate-type microchannel reactor.
[0030] Preferably, the hydrogen content of the low-hydrogen silicone oil is in the range of 0.11%-0.18%, the olefin is one of octene and decene, and the platinum catalyst is a platinum complex catalyst.
[0031] Preferably, the flow rate of the hydrogen-sealed low-hydrogen-content silicone oil is in the range of 100 mL / min to 400 mL / min, the flow rate of the olefin and platinum catalyst mixed solution is in the range of 50 mL / min to 400 mL / min, and the flow rate ratio of the hydrogen-sealed low-hydrogen-content silicone oil to the olefin and platinum catalyst mixed solution is 1:(0.5~1).
[0032] Preferably, the rotary evaporation temperature is 120℃~150℃, and the rotary evaporation time is 2h~6h.
[0033] The beneficial effects of this invention are:
[0034] 1. This invention provides a novel alkyl-modified silicone oil product. While retaining the inherent advantages of silicone oil, it overcomes the shortcoming of excessively high dielectric constant through modification, and has a higher flash point and lower viscosity, which are significantly superior to coolants currently on the market.
[0035] 2. This invention uses a micro-reaction continuous flow system to achieve rapid and efficient mixing of two fluids in a micro-mixer, instantly achieving a uniform reaction environment. The reaction time can be shortened to the minute level, resulting in high production efficiency and reduced usage of platinum complex catalyst.
[0036] The micro-reaction continuous flow system proposed in this invention adopts a combination of "plate microchannel reactor + tubular reactor" based on the characteristics of hydrosilylation reaction, which realizes rapid removal of reaction heat, facilitates monitoring and control of the reaction process, and is easy to scale up to a production scale. Attached Figure Description
[0037] Figure 1 This is a schematic diagram of the process flow for the continuous synthesis of alkyl silicone oil in a microreactor according to an embodiment of the present invention.
[0038] Figure 2 This is the NMR spectrum of the octene-modified silicone oil after post-treatment in Example 1 (the Si-H bond elution peak is at 4.7 ppm, and there is no elution at this position, so the Si-H bond residue can be considered to be 0).
[0039] Figure 3This is the gas chromatogram of the octene-modified silicone oil reaction solution in Example 1 (the conversion rate was calculated based on the octene peak area in the chromatogram using the external standard method).
[0040] Figure 4 The NMR spectrum of the decene-modified silicone oil in Example 1 is shown (the peak position of the Si-H bond is at 4.7 ppm, and there is no peak at this position, so it can be considered that the Si-H bond residue is 0).
[0041] Figure 5 This is the gas chromatogram of the decene-modified silicone oil reaction solution in Example 1 (the conversion rate was calculated based on the decene peak area in the chromatogram using the external standard method).
[0042] Figure 6 These are comparison images of the solution products obtained by mixing octyl-modified silicone oil and decyl-modified silicone oil in Examples 1-3.
[0043] The realization of the objective, functional features and advantages of the present invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation
[0044] To make the objectives, technical solutions, and advantages of the embodiments of this disclosure clearer, the technical solutions of the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this disclosure. Based on the described embodiments of this disclosure, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this disclosure.
[0045] This application discloses an alkyl silicone oil for use as an immersion cooling medium in data centers, the alkyl silicone oil comprising substances with the following molecular structural formula:
[0046] .
[0047] Where n ranges from 18 to 22, and m is 8 or 10; when n is constant, the mixing ratio of alkyl silicone oil with m=8 to alkyl silicone oil with m=10 ranges from 1 to 4:1.
[0048] This alkyl silicone oil is a transparent fluid at -50°C, has a flash point greater than 200°C, a viscosity of less than 20 mm² / s (cst) at 40°C, and a residual SiH content of less than 0.1 ppm.
[0049] A micro-reaction continuous flow preparation method for alkyl silicone oil includes the following steps:
[0050] 1) The hydrogen-sealed low-hydrogen silicone oil stored in storage tank 1 and the olefin and platinum catalyst mixed solution stored in storage tank 2 are pumped into microreactor 5 through metering pump 3 and metering pump 4 at a set flow rate for rapid and uniform mixing. The mixed material is then transported to tubular reactor 6 for hydrosilylation reaction to obtain a mixed liquid containing alkyl silicone oil, which is then stored in storage tank 7.
[0051] 2) The mixture containing alkyl silicone oil is subjected to rotary evaporation to obtain alkyl silicone oil.
[0052] in,
[0053] The temperature of the microreactor and tubular reactor is 85~95℃, and the total residence time is 3~5min.
[0054] Before the mixture containing alkyl silicone oil is subjected to rotary evaporation, a decolorization treatment can also be performed, which includes activated carbon adsorption decolorization, with the amount of activated carbon ranging from 1% to 5% of the mass of the solution to be adsorbed and decolorized.
[0055] Rotary evaporation includes vacuum rotary evaporation and / or reduced pressure rotary evaporation, the purpose of which is to remove low-boiling-point substances and moisture from the reaction solution.
[0056] Microreactors and tubular reactors control the reaction temperature using an oil bath.
[0057] The microreactor is a plate-type microchannel reactor with a liquid holdup of 50-100 mL and a microdispersion scale of 50-200 μm. The inner diameter of the tubular reactor is 6 mm. The plate-type microchannel reactor has heat exchange microchannels on both sides of the reaction channel. Temperature control of the reaction process is achieved using heat transfer oil within the heat exchange microchannels, while the tubular reactor is placed in a constant-temperature oil bath to regulate the reaction temperature.
[0058] The hydrogen content of the low-hydrogen silicone oil ranges from 0.11% to 0.18%, the olefin is either octene or decene, and the platinum catalyst is a platinum complex catalyst. The amount of platinum complex catalyst used ranges from 5 ppm to 10 ppm of the total mass of the hydrogen-containing silicone oil and long-chain olefin.
[0059] The flow rate of the hydrogen-sealed low-hydrogen-content silicone oil is in the range of 100 mL / min to 400 mL / min, and the flow rate of the olefin and platinum catalyst mixed solution is in the range of 50 mL / min to 400 mL / min. The flow rate ratio of the hydrogen-sealed low-hydrogen-content silicone oil to the olefin and platinum catalyst mixed solution is 1:(0.5~1).
[0060] The temperature for rotary evaporation is 120℃~150℃, and the evaporation time is 2h~6h.
[0061] Example 1
[0062] (1) Preparation of octyl modified silicone oil
[0063] 1) Take 500g of hydrogen-containing silicone oil with a hydrogen content of 0.11% and store it in reagent bottle A to form reaction solution A. Take 500g of n-octene and platinum complex catalyst with a concentration of 5ppm and mix them in reagent bottle B to form solution B.
[0064] 2) Reactant solution A and reactant solution B were rapidly mixed in a 50 mL plate microchannel reactor (metering pumps 3 and 4) at flow rates of 100 mL / min and 50 mL / min, respectively. The mixed material was then transferred to a tubular reactor with an inner diameter of 6 mm for hydrosilylation reaction. The reaction was controlled at 85 °C using a heat-conducting oil bath, with a total residence time of 3 min, ultimately yielding a mixture containing octyl-modified silicone oil.
[0065] 3) Add 1% by mass of powdered activated carbon to the mixture containing modified silicone oil collected in the reactor for adsorption and decolorization treatment to obtain a clear and transparent mixed solution.
[0066] 4) The decolorized mixed solution was subjected to rotary evaporation at 150°C for 4 hours under reduced pressure to remove low-boiling-point substances and obtain pure olefin-modified silicone oil product.
[0067] Gas chromatography analysis showed that the olefin conversion rate was 99.34%, and the final product contained no long-chain olefin residues. Quantitative NMR analysis showed that the residual Si-H bonds in the hydrogen-containing silicone oil were <0.1 ppm. Visual inspection revealed that the reaction solution was clear and transparent.
[0068] (2) Preparation of decyl modified silicone oil
[0069] 1) Take 500g of hydrogen-containing silicone oil with a hydrogen content of 0.11% and store it in reagent bottle A to form reaction solution A. Take 500g of n-decene and 5ppm of platinum complex catalyst and mix them in reagent bottle B to form solution B.
[0070] 2) Reactant solution A and reactant solution B were rapidly mixed in a 50 mL plate microchannel reactor with a microdispersion scale of 50 μm, pumped at flow rates of 100 mL / min and 50 mL / min respectively. The mixed material was then transferred to a tubular reactor with an inner diameter of 6 mm for hydrosilylation reaction. The reaction was carried out at 85 °C using a heat-conducting oil bath, with a total residence time of 3 min, ultimately yielding a mixture containing octyl-modified silicone oil.
[0071] 3) Add 1% by mass of powdered activated carbon to the mixture containing modified silicone oil collected in the reactor for adsorption and decolorization to obtain a clear and transparent mixed solution.
[0072] 4) The decolorized mixed solution was subjected to reduced pressure rotary evaporation at 150°C for 4 hours to remove low-boiling-point substances, and pure olefin-modified silicone oil product was obtained.
[0073] Gas chromatography analysis showed that the olefin conversion rate was 99.67%, and the final product contained no long-chain olefin residues. Quantitative NMR analysis showed that the residual Si-H bonds in the hydrogen-containing silicone oil were <0.1 ppm. Visual inspection revealed that the reaction solution was clear and transparent.
[0074] (3) Mixed solution preparation
[0075] Octyl-modified silicone oil and decyl-modified silicone oil were mixed at a mass ratio of 1:1, and then relevant indicators were tested.
[0076] Example 2
[0077] (1) Preparation of octyl modified silicone oil
[0078] 1) Take 500g of hydrogen-containing silicone oil with a hydrogen content of 0.18% and store it in reagent bottle A to form reaction solution A. Take 500g of n-octene and 10ppm of platinum complex catalyst and mix them in reagent bottle B to form solution B.
[0079] 2) Reactant solution A and reactant solution B were rapidly mixed in a 100 mL plate microchannel reactor with a microdispersion scale of 200 μm, pumped at flow rates of 400 mL / min and 400 mL / min respectively. The mixed material was then transferred to a tubular reactor with an inner diameter of 6 mm for hydrosilylation reaction. The reaction was carried out at 95 °C using a heat-conducting oil bath, with a total residence time of 5 min, ultimately yielding a mixture containing octyl-modified silicone oil.
[0080] 3) Add 5% by mass of powdered activated carbon to the mixture containing modified silicone oil collected in the reactor for adsorption and decolorization, and obtain a clear and transparent mixed solution.
[0081] 4) The decolorized mixed solution was subjected to reduced pressure rotary evaporation at 120℃ for 6 hours to remove low-boiling-point substances, and pure olefin-modified silicone oil product was obtained.
[0082] Gas chromatography analysis showed that the olefin conversion rate was 99.78%, and the final product contained no long-chain olefin residues. Quantitative NMR analysis showed that the residual Si-H bonds in the hydrogen-containing silicone oil were <0.1 ppm. Visual inspection revealed that the reaction solution was clear and transparent.
[0083] (2) Preparation of decyl modified silicone oil
[0084] 1) Take 500g of hydrogen-containing silicone oil with a hydrogen content of 0.18% and store it in reagent bottle A to form reaction solution A. Take 500g of n-decene and 10ppm of platinum complex catalyst and mix them in reagent bottle B to form solution B.
[0085] 2) Reactant solution A and reactant solution B were rapidly mixed in a 100 mL plate microchannel reactor with a microdispersion scale of 200 μm, pumped at flow rates of 400 mL / min and 400 mL / min respectively. The mixed material was then transferred to a tubular reactor with an inner diameter of 6 mm for hydrosilylation reaction. The reaction was carried out at 95 °C using a heat-conducting oil bath, with a total residence time of 5 min, ultimately yielding a mixture containing octyl-modified silicone oil.
[0086] 3) Add 5% by mass of powdered activated carbon to the mixture containing modified silicone oil collected in the reactor for adsorption and decolorization, and obtain a clear and transparent mixed solution.
[0087] 4) The decolorized mixed solution was subjected to reduced pressure rotary evaporation at 120℃ for 6 hours to remove low-boiling-point substances, and pure olefin-modified silicone oil product was obtained.
[0088] Gas chromatography analysis showed that the olefin conversion rate was 99.49%, and the final product contained no long-chain olefin residues. Quantitative NMR analysis showed that the residual Si-H bonds in the hydrogen-containing silicone oil were <0.1 ppm. Visual inspection revealed that the reaction solution was clear and transparent.
[0089] (3) Mixed solution preparation
[0090] Octyl-modified silicone oil and decyl-modified silicone oil were mixed at a mass ratio of 2:1, and then relevant indicators were tested.
[0091] Example 3
[0092] (1) Preparation of octyl modified silicone oil
[0093] 1) Take 500g of hydrogen-containing silicone oil with a hydrogen content of 0.14% and store it in reagent bottle A to form reaction solution A. Take 500g of n-octene and 6ppm of platinum complex catalyst and mix them in reagent bottle B to form solution B.
[0094] 2) Reactant solution A and reactant solution B were rapidly mixed in a 100 mL plate microchannel reactor with a microdispersion scale of 200 μm, pumped at flow rates of 400 mL / min and 200 mL / min respectively. The mixed material was then transferred to a tubular reactor with an inner diameter of 6 mm for hydrosilylation reaction. The reaction was carried out at 90 °C using a heat-conducting oil bath, with a total residence time of 4 min, ultimately yielding a mixture containing octyl-modified silicone oil.
[0095] 3) Add 3% by mass of powdered activated carbon to the mixture containing modified silicone oil collected in the reactor for adsorption and decolorization to obtain a clear and transparent mixed solution.
[0096] 4) The decolorized mixed solution was subjected to reduced pressure rotary evaporation at 140℃ for 4 hours to remove low-boiling-point substances, and pure olefin-modified silicone oil product was obtained.
[0097] Gas chromatography analysis showed that the olefin conversion rate was 99.66%, and the final product contained no long-chain olefin residues. Quantitative NMR analysis showed that the residual Si-H bonds in the hydrogen-containing silicone oil were <0.1 ppm. Visual inspection revealed that the reaction solution was clear and transparent.
[0098] (2) Preparation of decyl modified silicone oil
[0099] 1) Take 500g of hydrogen-containing silicone oil with a hydrogen content of 0.14% and store it in reagent bottle A to form reaction solution A. Take 500g of n-decene and 6ppm of platinum complex catalyst and mix them in reagent bottle B to form solution B.
[0100] 2) Reactant solution A and reactant solution B were rapidly mixed in a 100 mL plate microchannel reactor with a microdispersion scale of 200 μm, pumped at flow rates of 400 mL / min and 200 mL / min respectively. The mixed material was then transferred to a tubular reactor with an inner diameter of 6 mm for hydrosilylation reaction. The reaction was carried out at 90 °C using a heat-conducting oil bath, with a total residence time of 4 min, ultimately yielding a mixture containing octyl-modified silicone oil.
[0101] 3) Add 3% by mass of powdered activated carbon to the mixture containing modified silicone oil collected in the reactor for adsorption and decolorization to obtain a clear and transparent mixed solution.
[0102] 4) The decolorized mixed solution was subjected to reduced pressure rotary evaporation at 140℃ for 4 hours to remove low-boiling-point substances, and pure olefin-modified silicone oil product was obtained.
[0103] Gas chromatography analysis showed that the olefin conversion rate was 99.23%, and the final product contained no long-chain olefin residues. Quantitative NMR analysis showed that the residual Si-H bonds in the hydrogen-containing silicone oil were <0.1 ppm. Visual inspection revealed that the reaction solution was clear and transparent.
[0104] (3) Mixed solution preparation
[0105] Octyl modified silicone oil and decyl modified silicone oil were mixed at a mass ratio of 4:1, and then relevant index tests were conducted. The test results are shown in Table 1.
[0106] Table 1. Indicators of the compound products from Examples 1-3
[0107]
Claims
1. An alkyl silicone oil for use as an immersion cooling medium in data centers, characterized in that, The alkyl silicone oil includes substances with the following molecular structure (I): Formula (I), Where n ranges from 18 to 22, and m is 8 or 10.
2. The alkyl silicone oil according to claim 1, characterized in that, When n is constant, the mixing ratio of alkyl silicone oil with m=8 to alkyl silicone oil with m=10 is in the range of (1~4):
1.
3. The alkyl silicone oil according to claim 2, characterized in that, The alkyl silicone oil is a transparent fluid at -50°C, has a flash point greater than 200°C, a viscosity of less than 20 mm² / s at 40°C, and a residual SiH content of less than 0.1 ppm.
4. A micro-reaction continuous flow preparation method for alkyl silicone oil, characterized in that, The steps include: 1) The hydrogen-sealed low-hydrogen-content silicone oil and the olefin and platinum catalyst mixture solution are pumped into the microreactor at a set flow rate and mixed quickly and evenly. The mixed material is then transported to a tubular reactor for hydrosilylation reaction to obtain a mixture containing alkyl silicone oil. 2) The mixture containing alkyl silicone oil is subjected to rotary evaporation to obtain alkyl silicone oil.
5. The method according to claim 4, characterized in that, The temperature of the microreactor and the tubular reactor is 85~95℃, and the total residence time is 3~5min.
6. The method according to claim 5, characterized in that, Before the mixture containing alkyl silicone oil is subjected to rotary evaporation, it is decolorized.
7. The method according to claim 6, characterized in that, The decolorization process includes activated carbon adsorption decolorization.
8. The method according to claim 4, characterized in that, The rotary evaporation process includes vacuum rotary evaporation and / or reduced pressure rotary evaporation.
9. The method according to claim 4, characterized in that, The reaction temperatures of the microreactor and the tubular reactor are controlled by an oil bath.
10. The method according to claim 4, characterized in that, The microreactor is a plate-type microchannel reactor.
11. The method according to claim 4, characterized in that, The hydrogen content of the low-hydrogen silicone oil ranges from 0.11% to 0.18%, the olefin is one of octene and decene, and the platinum catalyst is a platinum complex catalyst.
12. The method according to claim 4, characterized in that, The flow rate of the hydrogen-sealed low-hydrogen-content silicone oil is in the range of 100 mL / min to 400 mL / min, the flow rate of the olefin and platinum catalyst mixed solution is in the range of 50 mL / min to 400 mL / min, and the flow rate ratio of the hydrogen-sealed low-hydrogen-content silicone oil to the olefin and platinum catalyst mixed solution is 1:(0.5~1).
13. The method according to claim 4, characterized in that, The rotary evaporation treatment is carried out at a temperature of 120℃~150℃ for 2h~6h.
Citation Information
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