Organic silicon cooling liquid and preparation method thereof

Abstract

The invention discloses an organic silicon cooling liquid and a preparation method thereof, the chemical structural formula of the organic silicon cooling liquid is shown in the following formula (1), (2), (3) or (4), and the organic silicon cooling liquid is prepared by mixing micro-molecular siloxane containing methoxy or ethyoxyl and a single silicon hydrogen reagent containing long-chain alkyl in a solvent and carrying out condensation reaction under the action of a catalyst. Experimental results show that compared with existing organic silicon cooling liquid, the organic silicon cooling liquid has excellent thermal stability, the overall performance of the organic silicon cooling liquid cannot be affected by low polymers or high polymers generated in the reaction process, and the organic silicon cooling liquid has good repeatability in production; the organic silicon cooling liquid has an exact molecular structure, is a single compound, and can be applied to liquid cooling in the fields of data centers and the like, so that the application range of organic silicon molecules with exact structures is expanded; in addition, the preparation method of the organic silicon cooling liquid is simple in post-treatment and relatively low in energy consumption, so that the organic silicon cooling liquid has a wide application prospect.

Description

Technical Field

[0001] This invention belongs to the field of organosilicon compound synthesis technology, and specifically relates to an organosilicon coolant and its preparation method. Background Technology

[0002] In recent years, with the rapid development of industries such as AI, the liquid cooling market has continued to expand, and the demand for coolant has continued to increase. In order to meet the demand for liquid cooling and at the same time solve the environmental pollution caused by fluorinated coolants, researchers have made continuous efforts to develop a variety of silicone coolants that can be used on a large scale for cooling servers and other scenarios.

[0003] Currently, most published research on the use of siloxanes as cooling media is limited to the polymer field, while research on organosilicon coolants with definite molecular structures is relatively scarce. For example, Chinese patent CN120271827A discloses an organosilicon coolant and its preparation method, the chemical molecular structure of which is as follows: Figure 9 As shown, phenyl groups and long-chain alkyl side chains are introduced into the silicone oil backbone through organic synthesis, disrupting the regularity of the polysiloxane chain and reducing its crystallinity. This alters the molecular structure of the organosilicon coolant, allowing it to remain fluid at lower temperatures (-65°C). Chinese patent CN119462721A discloses an organosilicon coolant and its preparation method, with the following general formula: (CH3)3SiO-[R1 R2SiO] n Si(CH3)3; wherein R1 = 8-16 alkyl groups; R2 = methyl or trimethylsiloxy, n = 1-2. This organosilicon coolant has high flash point, low viscosity, low surface tension, good fluidity, more comprehensive coverage, and better heat dissipation. It also has good compatibility with data center materials and will not cause swelling or other damage to related materials.

[0004] Given that the aforementioned silicone coolants are all mixtures of polysiloxanes, including siloxanes of different molecular weights and structures generated during polymerization, their stability in application is far inferior to that of siloxanes with definite molecular structures. Siloxanes with definite molecular structures (as single compounds) can achieve a more perfect balance of various properties by precisely adjusting the amount of alkyl and silane groups and selectively introducing different types and quantities of organic groups to meet the performance requirements of silicone coolants in specific scenarios. Summary of the Invention

[0005] In view of the problems existing in the background technology, the purpose of this invention is to provide an organosilicon coolant and its preparation method.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] A first aspect of the present invention provides an organosilicon coolant, the chemical structural formula of which is shown in formulas (1), (2), (3) or (4):

[0008]

[0009]

[0010] In the formula, R1 is selected from phenyl or C2-C10 alkyl, R2 is C6-C14 alkyl, and R3 is selected from phenyl, cyclopentyl, cyclohexyl or C6-C14 alkyl.

[0011] The second aspect of the present invention provides a method for preparing the above-mentioned organosilicon coolant, comprising the following steps: mixing a small molecule siloxane containing methoxy or ethoxy groups, a catalyst and a solvent, then adding a monosilane reagent containing a long-chain alkyl group, performing a condensation reaction at room temperature, then adding neutral alumina, continuing stirring, and finally purifying to obtain a small molecule organosilicon coolant containing a long-chain alkyl side chain, referred to as organosilicon coolant.

[0012] Preferably, the molar ratio of the catalyst to the monosilane reagent containing a long-chain alkyl group is 0.001 to 0.005:1; the catalyst is tris(pentafluorophenyl)borane (B(C6F5)3).

[0013] Preferably, the molar ratio of the monosiloxane containing a long-chain alkyl group to the small molecule siloxane containing a methoxy or ethoxy group is 1.1 to 1.5:1.

[0014] Preferably, the monosiloxane containing a long-chain alkyl group is 1,1,3,3-tetramethyl-1-alkyldisiloxane containing a long-chain alkyl group, wherein the long-chain alkyl group is a C6-C14 alkyl group.

[0015] Preferably, the solvent is one or a combination of two or more of n-hexane, toluene, petroleum ether, and dichloromethane.

[0016] Preferably, the condensation reaction time is 2 to 6 hours.

[0017] Preferably, the continued stirring time is 2 to 4 hours.

[0018] Preferably, the monosilane reagent containing long-chain alkyl groups is added in batches.

[0019] Preferably, the purification process includes: filtering the reaction product and vacuum distillation.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] (1) This invention, through precise molecular structure design, utilizes condensation reactions to prepare organosilicon coolants with branched structures of different types and numbers of functional groups. These organosilicon coolants possess definite molecular structures and are single compounds. Specifically, a small-molecule siloxane containing methoxy or ethoxy groups and a monosilane reagent containing long-chain alkyl groups are mixed in a solvent and subjected to a condensation reaction under the action of a catalyst to prepare a small-molecule organosilicon coolant with long-chain alkyl side chains and a defined structure. Experimental results show that, compared to existing polysiloxanes (which are polymers), this organosilicon coolant exhibits excellent thermal stability and its overall performance is not affected by the formation of oligomers or polymers during the reaction process. It also demonstrates good reproducibility in production.

[0022] (2) The organosilicon coolant with a definite structure provided by the present invention can be used in liquid cooling in data centers and other fields. Its performance is comparable to that of existing polysiloxane (organosilicon coolant), thereby expanding the application range of organosilicon molecules with a definite structure.

[0023] (3) The preparation method of the organosilicon coolant of the present invention has simple post-processing and low energy consumption, and therefore has broad application prospects. Attached Figure Description

[0024] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0025] Figure 1 The chemical structural formula of the organosilicon coolant provided by this invention;

[0026] Figure 2 The 1H NMR spectrum of the organosilicon coolant (sample 1) prepared in Example 1;

[0027] Figure 3 The 1H NMR spectrum of the organosilicon coolant (sample 2) prepared in Example 2;

[0028] Figure 4 The 1H NMR spectrum of the organosilicon coolant (sample 3) prepared in Example 3;

[0029] Figure 5 The 1H NMR spectrum of the organosilicon coolant (sample 4) prepared in Example 4;

[0030] Figure 6 The 1H NMR spectrum of the organosilicon coolant (sample 5) prepared in Example 5;

[0031] Figure 7The 1H NMR spectrum of the organosilicon coolant (sample 6) prepared in Example 6;

[0032] Figure 8 The TG curves are for the organosilicon coolants (samples 1-6) prepared in Examples 1-6.

[0033] Figure 9 The chemical molecular structure of the organosilicon coolant disclosed in the background art is shown below. Detailed Implementation

[0034] In the following description, specific details such as particular system architectures and techniques are set forth for illustrative purposes and not for limitation, in order to provide a thorough understanding of the embodiments of the invention. However, those skilled in the art will understand that the invention may be implemented in other embodiments without these specific details.

[0035] Example 1

[0036] The organosilicon coolant with the chemical structure shown in formula (a) is prepared as follows:

[0037]

[0038] Its synthetic route is as follows:

[0039]

[0040] Specific steps: 17.5 g of 1,8-bis(triethoxysilyl)octane, 0.46 g of tris(pentafluorophenyl)borane, and 50 mL of n-hexane were added to a 500 mL three-necked flask. While stirring at 500 r / min, a mixed solution of 61.2 g of 1,1,3,3-tetramethyl-1-octylsilane and 70 mL of n-hexane was slowly added. After all the solution was added, the mixture was reacted at room temperature for 3 h. After the reaction was complete, neutral alumina was added to the system, and stirring was continued for another 3 h. Finally, the product was obtained by filtration and vacuum distillation, namely the organosilicon cooling liquid with the chemical structure shown in formula (a), designated as sample 1. 1 H NMR spectrum as shown Figure 2 As shown.

[0041] Example 2

[0042] The organosilicon coolant with the chemical structure shown in formula (b) is prepared as follows:

[0043]

[0044] Specific steps: 12g of 1,2-bis(triethoxysilyl)ethane, 0.46g of tris(pentafluorophenyl)borane, and 50mL of n-hexane were added to a 500mL three-necked flask. While stirring at 500r / min, a mixed solution of 93.8g of 1,1,3,3-tetramethyl-1-dodecylsilane and 90mL of n-hexane was slowly added. After all the solution was added, the mixture was reacted at room temperature for 3 hours. After the reaction was complete, neutral alumina was added to the system, and stirring was continued for another 3 hours. Finally, the product was obtained by filtration and vacuum distillation, namely, an organosilicon coolant with the chemical structure shown in formula (b), designated as sample 2. 1 H NMR spectrum as shown Figure 3 As shown.

[0045] Example 3

[0046] The organosilicon coolant with the chemical structure shown in formula (c) is prepared as follows:

[0047]

[0048] Specific steps: 20g of 1,4-bis(triethoxysilyl)benzene, 0.46g of tris(pentafluorophenyl)borane, and 50mL of n-hexane were added to a 500mL three-necked flask. While stirring at 500r / min, a mixed solution of 94g of 1,1,3,3-tetramethyl-1-dodecylsilane and 90mL of n-hexane was slowly added. After all the solution was added, the mixture was reacted at room temperature for 3 hours. After the reaction was complete, neutral alumina was added to the system, and stirring was continued for another 3 hours. Finally, the product was obtained by filtration and vacuum distillation, namely, an organosilicon coolant with the chemical structure shown in formula (c), designated as sample 3. 1 H NMR spectrum as shown Figure 4 As shown.

[0049] Example 4

[0050] The organosilicon coolant with the chemical structure shown in formula (d) is prepared as follows:

[0051]

[0052] Specific steps: 24g of phenyltriethoxysilane, 0.46g of tris(pentafluorophenyl)borane, and 50mL of n-hexane were added to a 500mL three-necked flask. While stirring at 500r / min, a mixed solution of 96g of 1,1,3,3-tetramethyl-1-dodecylsilane and 90mL of n-hexane was slowly added. After all the solution was added, the mixture was reacted at room temperature for 3 hours. After the reaction was complete, neutral alumina was added to the system, and stirring was continued for another 3 hours. Finally, the product was obtained by filtration and vacuum distillation, namely, an organosilicon coolant with the chemical structure shown in formula (d), designated as sample 4. 1 H NMR spectrum as shown Figure 5As shown.

[0053] Example 5

[0054] The organosilicon coolant with the chemical structure shown in formula (e) is prepared as follows:

[0055]

[0056] Specific steps: 24.2 g of tetrakis(2-(diethoxy(methyl)silyl)ethyl)dimethylsilyl)silane, 0.46 g of tris(pentafluorophenyl)borane, and 50 mL of n-hexane were added to a 500 mL three-necked flask. While stirring at 500 rpm, a mixed solution of 52.4 g of 1,1,3,3-tetramethyl-1-octylsilane and 60 mL of n-hexane was slowly added. After all the solution was added, the mixture was reacted at room temperature for 3 hours. After the reaction was complete, neutral alumina was added to the system, and stirring was continued for another 3 hours. Finally, the product was obtained by filtration and vacuum distillation, namely, an organosilicon coolant with the chemical structure shown in formula (e), designated as sample 5. 1 H NMR spectrum as shown Figure 6 As shown.

[0057] Example 6

[0058] The organosilicon coolant with the chemical structure shown in formula (f) is prepared as follows:

[0059]

[0060] Specific steps: 22g of 2,4,6,8-tetra[2-(diethoxymethylsilyl)ethyl]-2,4,6,8-tetramethylcyclotetrasiloxane, 0.46g of tris(pentafluorophenyl)borane, and 50mL of n-hexane were added to a 500mL three-necked flask. While stirring at 500r / min, a mixed solution of 52.4g of 1,1,3,3-tetramethyl-1-octylsilane and 60mL of n-hexane was slowly added. After all the solution was added, the mixture was reacted at room temperature for 3 hours. After the reaction was complete, neutral alumina was added to the system, and stirring was continued for another 3 hours. Finally, the mixture was filtered and distilled under reduced pressure to obtain the target product, an organosilicon coolant with the chemical structure shown in formula (f), designated as sample 7. 1 H NMR spectrum as shown Figure 7 As shown.

[0061] Performance Characterization

[0062] (1) Thermal stability test

[0063] The thermal stability of samples 1-6 prepared in Examples 1-6 was tested in air using a thermogravimetric analyzer. The results are shown in the figure. Figure 8 .

[0064] Depend on Figure 8The results show that samples 1-6 can maintain good thermal stability below 200℃ and have a wide range of applications. Therefore, they will not have thermal decomposition problems during conventional cooling.

[0065] (2) Relevant performance tests (appearance, odor, volume resistivity, dielectric loss factor, specific heat capacity)

[0066] According to the standard T / SHSIC 0202-2023, relevant performance tests were conducted on samples 1-6 in liquid cooling, and the results are shown in Table 1.

[0067] Table 1

[0068] performance Appearance below 25℃ odor Volume resistivity at 90℃ 90℃ dielectric loss Specific heat capacity at 40℃ Sample 1 Colorless and transparent Tasteless <![CDATA[0.2×10 10 ]]> 0.05569 1.88 Sample 2 Colorless and transparent Tasteless <![CDATA[1.68×10 10 ]]> 0.02365 1.83 Sample 3 Colorless and transparent Tasteless <![CDATA[2.37×10 10 ]]> 0.01535 1.90 Sample 4 Colorless and transparent Tasteless <![CDATA[1.61×10 10 ]]> 0.03890 1.75 Sample 5 Colorless and transparent Tasteless <![CDATA[0.19×10 10 ]]> 0.01362 1.76 Sample 6 Colorless and transparent Tasteless <![CDATA[1.32×10 10 ]]> 0.01398 1.65

[0069] As shown in Table 1, the organosilicon coolant provided by this invention can be used as a (immersion) cooling fluid in liquid cooling in fields such as data centers, thereby expanding the application range of organosilicon molecules with definite structures and enriching the types of coolants.

[0070] This invention is not limited to the specific embodiments described above. Any modifications made by those skilled in the art based on the above concept without creative effort are within the scope of protection of this invention.

Claims

1. An organosilicon coolant, characterized in that, The chemical structural formula of the organosilicon coolant is shown in formulas (1), (2), (3), or (4) below: In the formula, R1 is selected from phenyl or C2-C10 alkyl, R2 is C6-C14 alkyl, and R3 is selected from phenyl, cyclopentyl, cyclohexyl or C6-C14 alkyl.

2. A method for preparing the organosilicon coolant as described in claim 1, characterized in that, The process includes the following steps: mixing a small molecule siloxane containing methoxy or ethoxy groups, a catalyst, and a solvent; then adding a monosilane reagent containing a long-chain alkyl group; carrying out a condensation reaction at room temperature; then adding neutral alumina; continuing stirring; and finally purifying the mixture to obtain an organosilicon coolant.

3. The method for preparing the organosilicon coolant according to claim 1, characterized in that, The molar ratio of the catalyst to the monosilane reagent containing long-chain alkyl groups is 0.001 to 0.005:1; the catalyst is B(C6F5)3.

4. The method for preparing the organosilicon coolant according to claim 1, characterized in that, The molar ratio of the monosiloxane containing long-chain alkyl groups to the small molecule siloxane containing methoxy or ethoxy groups is 1.1 to 1.5:

1.

5. The method for preparing the organosilicon coolant according to claim 1, characterized in that, The monosiloxane containing long-chain alkyl groups is 1,1,3,3-tetramethyl-1-alkyldisiloxane containing long-chain alkyl groups, wherein the long-chain alkyl groups are C6 to C14 alkyl groups.

6. The method for preparing the organosilicon coolant according to claim 1, characterized in that, The condensation reaction time is 2 to 6 hours.

7. The method for preparing the organosilicon coolant according to claim 1, characterized in that, The solvent is one or a combination of two or more of the following: n-hexane, toluene, petroleum ether, and dichloromethane.

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