Polyorganosiloxane containing silane side chain, and preparation method and application thereof

Abstract

The invention discloses polysiloxane containing a silane side chain as well as a preparation method and application of the polysiloxane, 2, 4, 6, 8-tetramethyl-2, 4, 6, 8-tetravinyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and the like are adopted as raw materials, and are respectively subjected to two-step reaction of ring opening polymerization and hydrosilylation under the action of strong acid and a platinum catalyst, so that the polysiloxane containing the silane side chain is obtained. And the polysiloxane containing the silane side chain is prepared. The polysiloxane containing the silane side chain is applied to liquid cooling for related performance tests, and it is verified that the polysiloxane containing the silane side chain can serve as cooling fluid to be applied to liquid cooling in the fields of data centers and energy storage batteries, so that the range of immersed cooling media is expanded. In addition, the preparation method disclosed by the invention has the characteristics of cheap and easily available raw materials, low preparation cost, simplicity and safety in operation, capability of simply and accurately regulating and controlling the molecular structure and the like, and is suitable for industrial popularization.

Description

Technical Field

[0001] The present invention belongs to the technical field of polyorganosiloxane synthesis, and in particular relates to a polyorganosiloxane containing a silane side chain, a preparation method and an application thereof. Background Art

[0002] In recent years, the development of intensive, green, and efficient data center cooling fluids has become imperative. Polyorganosiloxanes containing side chain groups, as ideal immersion cooling fluids, have great potential for application in data centers and energy storage batteries, such as lithium batteries, where immersion cooling has high cooling fluid requirements.

[0003] Currently, the polyorganosiloxane cooling fluid used in data centers and energy storage batteries (such as lithium batteries) is mainly alkyl-modified silicone oil. Its preparation method mainly starts from hydrogen-containing silicone oil and uses a hydrosilylation reaction to introduce side chains, and the introduced side chains are mainly alkyl side chains. This method of introducing side chains by hydrosilylation using hydrogen-containing silicone oil as the initial raw material often results in residual silicon-hydrogen bonds in the polysiloxane chain segments. The residual silicon-hydrogen bonds will affect the insulation performance of polyorganosiloxane when used as an immersion cooling medium for data centers and energy storage batteries such as lithium batteries for a long time. Summary of the Invention

[0004] In view of the technical problems existing in the background technology, the purpose of the present invention is to provide a polyorganosiloxane containing silane side chains, a preparation method and application thereof.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] The first aspect of the present invention provides a polyorganosiloxane containing a silane side chain, the general chemical structure of which is shown in the following formula (1):

[0007]

[0008] In the formula, R is selected from -Si(CH2CH3)3, -Si(CH3)[OSi(CH3)3]2, -Si(CH3)2OSi(CH3)3 or -Si(CH3)2OSi(CH3)2C p H 2p+1 , m is an integer selected from 4-20, n is an integer selected from 0-20, and p is an integer selected from 6-14.

[0009] The second aspect of the present invention provides a method for preparing the above-mentioned polyorganosiloxane containing silane side chains, comprising the following steps:

[0010] S1. Using 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and octamethylcyclotetrasiloxane as raw materials and hexamethyldisiloxane as a capping agent, a ring-opening reaction is carried out under the catalysis of a strong acid to obtain a polyorganosiloxane containing vinyl groups in the side chain;

[0011] S2. Using the obtained polyorganosiloxane containing vinyl groups in the side chain and a small molecule silicon-hydrogen reagent containing a silicon-hydrogen bond (-Si-H) as raw materials, a silicon-hydrogen addition reaction is carried out under the catalysis of a platinum catalyst to obtain a polyorganosiloxane containing a silane side chain.

[0012] Preferably, in step S1, the amount of the strong acid used is 1-10 wt % of the total mass of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane.

[0013] Preferably, the strong acid is any one of concentrated sulfuric acid, concentrated hydrochloric acid, and trifluoromethanesulfonic acid, more preferably trifluoromethanesulfonic acid.

[0014] Preferably, in step S1, the temperature of the ring-opening reaction is 50-100° C., and the reaction time is 5-12 h.

[0015] Preferably, in step S2, the mass ratio of the polyorganosiloxane containing vinyl groups in the side chain to the small molecule silicon-hydrogen reagent containing one silicon-hydrogen bond (-Si-H) is 1:1.2-3.

[0016] Preferably, in step S2, the temperature of the hydrosilylation reaction is 70-120° C., and the reaction time is 5-18 h.

[0017] Preferably, the small molecule silicon hydride reagent containing one -Si-H bond is one or a combination of two or more of 1,1,1,3,5,5,5-heptamethyltrisiloxane, triethylsilane, pentamethyldisiloxane, and 1,1,3,3-tetramethyl-1-alkyldisiloxane.

[0018] Preferably, the amount of the platinum catalyst used is 0.1-1 wt% of the total mass of the polyorganosiloxane containing vinyl groups in the side chain and the small molecule silicon hydride reagent containing one silicon-hydrogen bond (-Si-H).

[0019] Preferably, the platinum-based catalyst is one or a combination of two or more of chloroplatinic acid, Karstedt catalyst, and Speier catalyst, and is more preferably Karstedt catalyst.

[0020] A third aspect of the present invention provides the use of the above-mentioned polyorganosiloxane containing silane side chains as an (immersion) cooling fluid in liquid cooling in data centers and energy storage battery fields.

[0021] The present invention has the following beneficial effects:

[0022] (1) The present invention uses 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and octamethylcyclotetrasiloxane as raw materials, and prepares a polyorganosiloxane containing silane side chains through a two-step reaction of ring-opening polymerization and then hydrosilylation.

[0023] By using a polyorganosiloxane containing vinyl groups in its side chain and a small molecule silane-hydrogen reagent containing a silicon-hydrogen bond (-Si-H) to carry out a hydrosilylation reaction, different types of silane side chains can be introduced into the obtained polyorganosiloxane.

[0024] By adding an excess of a small molecule silanol containing a single silicon-hydrogen bond (-Si-H) to undergo a hydrosilylation reaction to extend the side chain, the carbon-carbon double bond can be completely reacted. Furthermore, the unreacted small molecule silanol containing a single silicon-hydrogen bond (-Si-H) can be completely removed by vacuum distillation, resulting in no residual silicon-hydrogen bonds in the resulting product, thus preventing residual silicon-hydrogen bonds from affecting the insulating properties of the polyorganosiloxane.

[0025] By adjusting the ratio of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane to octamethylcyclotetrasiloxane and hexamethyldisiloxane, the molecular structure can be simply and precisely controlled.

[0026] (2) The preparation method of the present invention has the advantages of cheap and readily available raw materials, low preparation cost, simple operation and safety.

[0027] (3) By conducting relevant performance tests on the polyorganosiloxane containing silane side chains prepared by the present invention as a cooling fluid in liquid cooling, it was verified that it can be used as a cooling fluid in liquid cooling in data centers and energy storage batteries, thereby expanding the scope of immersion cooling media. Therefore, it has broad application prospects and is suitable for industrial promotion. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0029] Figure 1 is the general chemical structure formula of polyorganosiloxane containing silane side chains;

[0030] Figure 2 The synthetic route of the polyorganosiloxane containing silane side chains provided by the present invention;

[0031] Figure 3 This is the H NMR spectrum of the product 8V obtained in Example 1;

[0032] Figure 4 This is the H NMR spectrum of the product 4V4D obtained in Example 2;

[0033] Figure 5 This is the H NMR spectrum of the product 6V6D obtained in Example 3;

[0034] Figure 6 This is the H NMR spectrum of the product 8V8D obtained in Example 4;

[0035] Figure 7 This is the H NMR spectrum of the product 6V8D obtained in Example 5;

[0036] Figure 8 This is the H NMR spectrum of the product 8V6D obtained in Example 6;

[0037] Figure 9 This is the H NMR spectrum of the product 4V12D obtained in Example 7;

[0038] Figure 10 This is the H NMR spectrum of the product 6V12D obtained in Example 8;

[0039] Figure 11 This is the H NMR spectrum of the product 12V14D obtained in Example 9;

[0040] Figure 12 This is the H NMR spectrum of sample 1 obtained in Example 10;

[0041] Figure 13 This is the H NMR spectrum of sample 2 obtained in Example 11;

[0042] Figure 14 This is the H NMR spectrum of sample 3 obtained in Example 12;

[0043] Figure 15 This is the H NMR spectrum of sample 4 obtained in Example 13;

[0044] Figure 16 This is the H NMR spectrum of sample 5 obtained in Example 14;

[0045] Figure 17 This is the H NMR spectrum of sample 6 obtained in Example 15;

[0046] Figure 18 This is the H NMR spectrum of sample 7 obtained in Example 16;

[0047] Figure 19 This is the H NMR spectrum of sample 8 obtained in Example 17;

[0048] Figure 20The H NMR spectrum of the product obtained in the comparative example. DETAILED DESCRIPTION

[0049] In the following description, specific details such as specific system structures and technologies are provided for the purpose of illustration rather than limitation to facilitate a thorough understanding of the embodiments of the present invention. However, it should be clear to those skilled in the art that the present invention may also be implemented in other embodiments without these specific details.

[0050] Reference Figure 1-2 , to prepare polyorganosiloxanes containing silane side chains, first, using 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and octamethylcyclotetrasiloxane as raw materials to prepare polyorganosiloxanes containing vinyl groups on the side chains, see Examples 1-8; then, the prepared polyorganosiloxanes containing vinyl groups on the side chains are reacted with a small molecule silicon hydrogen reagent containing a silicon-hydrogen bond (-Si-H) to prepare polyorganosiloxanes containing silane side chains, see Examples 9-17.

[0051] Example 1

[0052] 34.3g of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and 8.2g of hexamethyldisiloxane were added to a 250mL three-necked flask, and 2.1g of trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. The mixture was then heated to 50°C and subjected to a ring-opening reaction for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 96.3%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 3 shown.

[0053] Depend on Figure 3 The test results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, denoted as product 8V, and its chemical structure is shown below:

[0054]

[0055] Among them, the average value of m is 8 and n is 0.

[0056] Example 2

[0057] 34.3g 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 29.6g octamethylcyclotetrasiloxane, and 16.2g hexamethyldisiloxane were added to a 250mL three-necked flask, and 4g trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. The mixture was heated to 50°C and reacted for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 97.0%. The obtained product was characterized and obtained 1 HNMR spectrum Figure 4 shown.

[0058] Through Figure 4 The results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, which is denoted as product 4V4D. Its chemical structure is shown below:

[0059]

[0060] Among them, the average value of m is 4, and the average value of n is 4.

[0061] Example 3

[0062] 34.3g 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 29.6g octamethylcyclotetrasiloxane and 9.7g hexamethyldisiloxane were added to a 250mL three-necked flask, and 3.7g trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. Then, the mixture was heated to 50°C and reacted for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 94.3%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 5 shown.

[0063] Through Figure 5 The results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, which is recorded as product 6V6D and has the following chemical structure:

[0064]

[0065] Among them, the average value of m is 6, and the average value of n is 6.

[0066] Example 4

[0067] 68.9g 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 59.3g octamethylcyclotetrasiloxane and 16.2g hexamethyldisiloxane were added to a 250mL three-necked flask, and 7.22g trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. Then, the mixture was heated to 50°C and reacted for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 90.3%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 6 shown.

[0068] Through Figure 6 The results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, which is denoted as product 8V8D. Its chemical structure is shown below:

[0069]

[0070] Among them, the average value of m is 8, and the average value of n is 8.

[0071] Example 5

[0072] 25.9g 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 29.6g octamethylcyclotetrasiloxane, and 8.1g hexamethyldisiloxane were added to a 250mL three-necked flask, and 3.1g trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. Then, the mixture was heated to 50°C and reacted for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 90.7%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 7 shown.

[0073] Through Figure 7 The results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, which is recorded as product 6V8D and has the following chemical structure:

[0074]

[0075] Among them, the average value of m is 6, and the average value of n is 8.

[0076] Example 6

[0077] 68.9g 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 44.5g octamethylcyclotetrasiloxane and 16.2g hexamethyldisiloxane were added to a 250mL three-necked flask, and 6.39g trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. Then, the mixture was heated to 50°C and reacted for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 98.3%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 8 shown.

[0078] Through Figure 8 The results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, which is recorded as product 8V6D. Its chemical structure is as follows:

[0079]

[0080] Among them, the average value of m is 8, and the average value of n is 6.

[0081] Example 7

[0082] 20g 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 51.6g octamethylcyclotetrasiloxane and 9.4g hexamethyldisiloxane were added to a 250mL three-necked flask, and 4.05g trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. Then, the mixture was heated to 50°C and reacted for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 96.4%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 9 shown.

[0083] Through Figure 9 The results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, which is recorded as product 4V12D and has the following chemical structure:

[0084]

[0085] Among them, the average value of m is 4, and the average value of n is 12.

[0086] Example 8

[0087] 34.4g 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 59.3g octamethylcyclotetrasiloxane and 10.8g hexamethyldisiloxane were added to a 250mL three-necked flask, and 10.8g trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. Then, the mixture was heated to 50°C and reacted for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 96.3%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 10 shown.

[0088] Through Figure 10 The results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, which is recorded as product 6V12D and has the following chemical structure:

[0089]

[0090] Among them, the average value of m is 6, and the average value of n is 12.

[0091] Example 9

[0092] 34.4g 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 34.5g octamethylcyclotetrasiloxane and 5.4g hexamethyldisiloxane were added to a 250mL three-necked flask, and 3.7g trifluoromethanesulfonic acid was added thereto at a stirring speed of 300r / min. Then, the mixture was heated to 50°C and reacted for 8h. After the reaction was completed, excess sodium carbonate was added to neutralize the trifluoromethanesulfonic acid, and the product was obtained by filtration and vacuum distillation with a yield of 97.5%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 11 shown.

[0093] Through Figure 11 The results show that the product obtained in this example is a polyorganosiloxane with vinyl side chains, denoted as product 12V14D, and its chemical structure is shown below:

[0094]

[0095] Among them, the average value of m is 12, and the average value of n is 14.

[0096] Example 10

[0097] Weigh 40g of product 4V4D and add it to a 250mL three-necked flask. Add 200μL of xylene solution with a 2% Karstedt catalyst content. Slowly add 66.5g of 1,1,1,3,5,5,5-heptamethyltrisiloxane to the flask at room temperature and heat to 80°C for 12h. After the reaction is completed, add activated carbon and diatomaceous earth and stir for 2h to adsorb the catalyst. Finally, filter and remove excess silicon hydrogen reagent by vacuum distillation to obtain the product with a yield of 95.5%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 12 shown.

[0098] Through Figure 12 The results show that the product obtained in this example is a polyorganosiloxane with a silane side chain, which is recorded as Sample 1 and has the following chemical structure:

[0099]

[0100] Among them, R is -Si(CH3)[OSi(CH3)3]2, the average value of m is 4, and the average value of n is 4.

[0101] Example 11

[0102] Weigh 40g of product 4V4D into a 250mL three-necked flask, add 200μL of xylene solution containing 2% Karstedt catalyst, slowly add 34.3g of triethylsilane into the flask at room temperature, heat to 80℃ and react for 12h. After the reaction is completed, add activated carbon and diatomaceous earth and stir for 2h to adsorb the catalyst. Finally, filter and remove excess silicon hydrogen reagent by vacuum distillation to obtain the product with a yield of 95.5%. The obtained product was characterized and obtained 1 HNMR spectrum Figure 13 shown.

[0103] Through Figure 13 The results show that the product obtained in this example is a polyorganosiloxane with a silane side chain, which is recorded as Sample 2 and has the following chemical structure:

[0104]

[0105] Among them, R is -Si(CH2CH3)3, the average value of m is 4, and the average value of n is 4.

[0106] Example 12

[0107] Weigh 50g of product 8V8D into a 250mL three-necked flask, add 200μL of xylene solution with a 2% Karstedt catalyst content, slowly add 77g of 1,1,1,3,5,5,5-heptamethyltrisiloxane into the flask at room temperature, heat to 80°C and react for 12h. After the reaction is completed, add activated carbon and diatomaceous earth and stir for 2h to adsorb the catalyst. Finally, filter and remove excess silicon hydrogen reagent by vacuum distillation to obtain the product with a yield of 93.8%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 14 shown.

[0108] Through Figure 14 The results show that the product obtained in this example is a polyorganosiloxane with silane side chains, which is recorded as Sample 3. Its chemical structure is shown below:

[0109]

[0110] Among them, R is -Si(CH3)[OSi(CH3)3]2, the average value of m is 8, and the average value of n is 8.

[0111] Example 13

[0112] Weigh 50g of product 6V8D and add it to a 250mL three-necked flask. Add 200μL of xylene solution with a 2% Karstedt catalyst content. Slowly add 36.5g of triethylsilane to the flask at room temperature and heat to 80°C for 12h. After the reaction is completed, add activated carbon and diatomaceous earth and stir for 2h to adsorb the catalyst. Finally, filter and remove excess silicon hydrogen reagent by vacuum distillation to obtain the product with a yield of 90.5%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 15 shown.

[0113] Through Figure 15 The results show that the product obtained in this example is a polyorganosiloxane with a silane side chain, which is recorded as Sample 4 and has the following chemical structure:

[0114]

[0115] Among them, R is -Si(CH2CH3)3, the average value of m is 6, and the average value of n is 8.

[0116] Example 14

[0117] Weigh 50g of product 4V12D and add it to a 250mL three-necked flask. Add 200μL of xylene solution with a 2% Karstedt catalyst content. Slowly add 45.4g of 1,1,1,3,5,5,5-heptamethyltrisiloxane to the flask at room temperature and heat to 80°C for 12h. After the reaction is completed, add activated carbon and diatomaceous earth and stir for 2h to adsorb the catalyst. Finally, filter and remove excess silicon hydrogen reagent by vacuum distillation to obtain the product with a yield of 98.4%. The obtained product was characterized and obtained 1 HNMR spectrum Figure 16 shown.

[0118] Through Figure 16 The results show that the product obtained in this example is a polyorganosiloxane with a silane side chain, which is recorded as Sample 5. Its chemical structure is shown below:

[0119]

[0120] Among them, R is -Si(CH3)[OSi(CH3)3]2, the average value of m is 4, and the average value of n is 12.

[0121] Example 15

[0122] Weigh 35g of product 12V14D and add it to a 250mL three-necked flask. Add 200μL of xylene solution with a 2% Karstedt catalyst content. Slowly add 47.2g of 1,1,1,3,5,5,5-heptamethyltrisiloxane to the flask at room temperature and heat to 80°C for 12h. After the reaction is completed, add activated carbon and diatomaceous earth and stir for 2h to adsorb the catalyst. Finally, filter and remove excess silicon hydrogen reagent by vacuum distillation to obtain the product with a yield of 92.8%. The obtained product was characterized and obtained 1 HNMR spectrum Figure 17 shown.

[0123] Through Figure 17 The results show that the product obtained in this example is a polyorganosiloxane with a silane side chain, which is recorded as Sample 6 and has the following chemical structure:

[0124]

[0125] Among them, R is -Si(CH3)[OSi(CH3)3]2, the average value of m is 12, and the average value of n is 14.

[0126] Example 16

[0127] Weigh 50g of product 6V12D into a 250mL three-necked flask, add 200μL of xylene solution with a 2% Karstedt catalyst content, slowly add 56.7g of 1,1,1,3,5,5,5-heptamethyltrisiloxane into the flask at room temperature, heat to 80°C and react for 12h. After the reaction is completed, add activated carbon and diatomaceous earth and stir for 2h to adsorb the catalyst. Finally, filter and remove excess silicon hydrogen reagent by vacuum distillation to obtain the product with a yield of 90.5%. The obtained product was characterized and obtained 1 HNMR spectrum Figure 18 shown.

[0128] Through Figure 18 The results show that the product obtained in this example is a polyorganosiloxane with silane side chains, which is recorded as Sample 7. Its chemical structure is shown below:

[0129]

[0130] Among them, R is -Si(CH3)[OSi(CH3)3]2, the average value of m is 6, and the average value of n is 12.

[0131] Example 17

[0132] Weigh 30g of product 4V4D and add it to a 250mL three-necked flask. Add 60μL of xylene solution with a 2% Karstedt catalyst content. Slowly add 45g of 1,1,3,3-tetramethyl-1-hexyldisiloxane to the flask at room temperature and heat to 80°C for 12h. After the reaction is completed, add activated carbon and diatomaceous earth and stir for 2h to adsorb the catalyst. Finally, filter and distill under reduced pressure to remove excess silicon hydrogen reagent to obtain the product with a yield of 90.6%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 19 shown.

[0133] Through Figure 19 The results show that the product obtained in this example is a polyorganosiloxane with a silane side chain, which is recorded as Sample 8 and has the following chemical structure:

[0134]

[0135] Where R is -Si(CH3)2OSi(CH3)2C6H 13 , the average value of m is 4, and the average value of n is 4.

[0136] Comparative Example 1

[0137] 40g of hydrogenated silicone oil (hydrogen content 1.55%) and 50mL of n-hexane were mixed and added to a round-bottom flask. A mixed solution of 50mL of n-hexane, 200μL of xylene solution containing 2% Karstedt catalyst and 80g (excess) of 1-hexene was added in batches at a stirring speed of 300r / min. The temperature was raised to 80°C and the reaction was carried out for 12h. After the reaction was completed, activated carbon and diatomaceous earth were added and stirred for 2h to adsorb the catalyst. Finally, alkyl side chain polyorganosiloxane was obtained by filtration and vacuum distillation with a yield of 95.5%. The obtained product was characterized and obtained 1 H NMR spectrum Figure 20 shown.

[0138] Through Figure 20 The results show that the product is an alkyl side chain polysiloxane, but there are residual silicon hydrogen, which indicates that even if the olefin is excessive, the silicon hydrogen is still difficult to react completely.

[0139] Test Example 1

[0140] Silicon hydrogen residual test

[0141] With reference to the method in the "T / FSI 102-2023" standard, the silicon hydride (-Si-H) content of the obtained samples 1-8 and the product obtained in Comparative Example 1 was tested. The results are shown in Table 1.

[0142] Table 1

[0143]

[0144] As can be seen from Table 1, the present invention successfully prepares a polyorganosiloxane product containing a silane side chain by first performing ring-opening polymerization of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane with octamethylcyclotetrasiloxane and hexamethyldisiloxane, and then performing hydrosilylation using a small molecule silane hydride reagent containing a silicon-hydrogen bond (-Si-H). The small molecule silane hydride reagent can be completely removed by reduced pressure distillation, so that no silicon-hydrogen bonds remain in the product.

[0145] Performance Characterization

[0146] According to the standard "T / SHSIC 0202-2023", the prepared samples 1-8 were tested for relevant properties in liquid cooling (dielectric constant (AC frequency of 1 kHz), volume resistivity (90°C), dielectric loss factor (90°C), and kinematic viscosity (40°C). The test results are shown in Table 2 below.

[0147] Table 2

[0148]

[0149] As can be seen from the results in Table 2, the polyorganosiloxane containing silane side chains provided by the present invention can be used as an (immersion) cooling fluid in liquid cooling in data centers and energy storage batteries (such as lithium batteries), thereby expanding the scope of immersion cooling media.

[0150] The present invention is not limited to the above-mentioned specific implementation methods. Various changes made by ordinary technicians in this field based on the above-mentioned concept without creative work are all within the scope of protection of the present invention.

Claims

1. A polyorganosiloxane containing silane side chains, characterized in that: Its chemical structure is shown in the following formula (1): In the formula, R is selected from -Si(CH2CH3)3, -Si(CH3)[OSi(CH3)3]2, -Si(CH3)2OSi(CH3)3 or -Si(CH3)2OSi(CH3)2C p H 2p+1 , m is an integer selected from 4-20, n is an integer selected from 0-20, and p is an integer selected from 6-14.

2. A method for preparing a polyorganosiloxane containing silane side chains according to claim 1, characterized in that: The following steps are involved: S1. Using 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and octamethylcyclotetrasiloxane as raw materials and hexamethyldisiloxane as a capping agent, a ring-opening reaction is carried out under the catalysis of a strong acid to obtain a polyorganosiloxane containing vinyl groups in the side chain; S2. Using the obtained polyorganosiloxane containing vinyl groups in the side chain and a small molecule silicon-hydrogen reagent containing one silicon-hydrogen bond as raw materials, a silicon-hydrogen addition reaction is carried out under the catalysis of a platinum catalyst to obtain a polyorganosiloxane containing a silane side chain.

3. The method for preparing a polyorganosiloxane containing a silane side chain according to claim 2, wherein: In step S1, the amount of the strong acid used is 1-10 wt % of the total mass of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane.

4. The method for preparing a polyorganosiloxane containing a silane side chain according to claim 2, wherein: The strong acid is any one of concentrated sulfuric acid, concentrated hydrochloric acid, and trifluoromethanesulfonic acid.

5. The method for preparing polyorganosiloxane containing silane side chains according to claim 2, wherein: In step S1, the temperature of the ring-opening reaction is 50-100° C., and the reaction time is 5-12 h.

6. The method for preparing polyorganosiloxane containing silane side chains according to claim 2, wherein: In step S2, the mass ratio of the polyorganosiloxane containing vinyl groups in the side chain to the small molecule silicon-hydrogen reagent containing one silicon-hydrogen bond is 1:1.2-3.

7. The method for preparing polyorganosiloxane containing silane side chains according to claim 2, characterized in that: The amount of the platinum catalyst used is 0.1-1 wt% of the total mass of the polyorganosiloxane containing vinyl groups on the side chain and the small molecule silicon-hydrogen reagent containing one silicon-hydrogen bond.

8. The method for preparing polyorganosiloxane containing silane side chains according to claim 2, wherein: In step S2, the temperature of the hydrosilylation reaction is 70-120° C., and the reaction time is 5-18 hours.

9. The method for preparing polyorganosiloxane containing silane side chains according to claim 2, wherein: The small molecule silicon hydride reagent containing one -Si-H bond is one or a combination of two or more of 1,1,1,3,5,5,5-heptamethyltrisiloxane, triethylsilane, pentamethyldisiloxane, and 1,1,3,3-tetramethyl-1-alkyldisiloxane; the platinum-based catalyst is one or a combination of two or more of chloroplatinic acid, Karstedt catalyst, and Speier catalyst.

10. Use of the polyorganosiloxane containing silane side chains as claimed in claim 1 as a cooling fluid in liquid cooling in data centers and energy storage batteries.

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