A centrifugal process for trimethylsilane production

Abstract

The present application relates to a kind of centrifugal methods for trimethylsilane preparation, comprising: trimethylchlorosilane is weighed, it is placed in stirrer, additional reaction solvent is added in stirrer, it is mixed uniformly, and stationary. Again, dimethylamine gas is introduced into stirrer, and catalyst is added. After reaction, product is removed and cooled to room temperature, product is centrifuged using three times centrifugation, respectively, product is placed in centrifuge for first centrifugation, and first centrifugate is obtained, first centrifugate is heated in water bath, and placed in centrifuge for second centrifugation, and second centrifugate is obtained, then second centrifugate is distilled, and the distillate is screened, and purification product is obtained, and purification product is placed in centrifuge again for third centrifugation, and centrifugation product is obtained. The provided method, by three times centrifugation, not only can effectively improve product yield, but also can effectively improve product purity.

Description

Technical Field

[0001] This invention relates to the field of trimethylsilane preparation technology, and more specifically to a centrifugation method for the preparation of trimethylsilane. Background Technology

[0002] Centrifugation is a technique that involves rotating a solution at high speed around an axis, using centrifugal force to cause some components to precipitate while others remain in the supernatant. It is one of the most fundamental experimental procedures in biochemistry. Modern advancements in ultracentrifugation have made the separation of many substances possible, and it can also be used to determine their homogeneity and purity. In the laboratory, centrifugation has become an indispensable experimental tool.

[0003] During the preparation of trimethylsilane, the product is centrifuged. However, the use of a single centrifugation method results in a lack of excellent product yield and high purity, which in turn affects the quality and grade of the prepared trimethylsilane and fails to meet the application requirements.

[0004] In summary, developing a centrifugation method for the preparation of trimethylsilane is a critical issue that urgently needs to be addressed in the field of trimethylsilane preparation technology. Summary of the Invention

[0005] In view of the above-mentioned shortcomings of the existing technology, the present invention provides a centrifugation method for the preparation of trimethylsilane, which can effectively improve the product yield and also effectively improve the product purity.

[0006] To achieve the above objectives, the present invention provides a centrifugation method for the preparation of trimethylsilane, comprising the following steps:

[0007] (1) Weigh trimethylchlorosilane, place it in a stirrer, add the reaction solvent to the stirrer, mix well, and let stand for 30 minutes; wherein, the speed of the stirrer is 20-30 r / min, the stirring time is 8-10 minutes, and the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2.

[0008] (2) Then introduce dimethylamine gas into the stirrer and add a catalyst, and react for 20 minutes;

[0009] (3) Take out the product and cool it to room temperature. Place the product in a centrifuge for the first centrifugation to obtain the first centrifuged product.

[0010] (4) Heat the first centrifuged material in a water bath and place it in a centrifuge for a second centrifugation to obtain the second centrifuged material;

[0011] (5) Distill the second centrifuged product and pass the distillate through a 100-mesh sieve to obtain the purified product;

[0012] (6) Place the purified product in a centrifuge for a third centrifugation to obtain the centrifuged product.

[0013] The present invention is further configured such that, in step (1), before placing trimethylchlorosilane in the stirrer, nitrogen gas is introduced into the stirrer to expel the air inside the stirrer.

[0014] The present invention is further configured such that, in step (1), the reaction solvent is either n-hexane or pseudotrimethylbenzene.

[0015] The present invention is further configured such that, in step (2), the catalyst is any one of ammonium sulfate and n-butyllithium.

[0016] The present invention is further configured such that, in step (3), the centrifugation speed of the first centrifugation is 12000-13000 r / min and the centrifugation time is 12-14 min.

[0017] The present invention is further configured such that, in step (4), the centrifugation speed of the second centrifugation is 8000-9000 r / min and the centrifugation time is 8-10 min.

[0018] The present invention is further configured such that, in step (4), the temperature of the water bath heating is 40-50°C.

[0019] The present invention is further configured such that, in step (5), the distillation temperature is 86-88℃.

[0020] The present invention is further configured such that, in step (6), the centrifugation speed of the third centrifugation is 15000-16000 r / min and the centrifugation time is 20-30 min.

[0021] The present invention is further configured such that, in step (6), the internal temperature of the centrifuge is 35-37°C.

[0022] Compared with known public technologies, the technical solution provided by this invention has the following beneficial effects: The method provided by this invention weighs trimethylchlorosilane, places it in a stirrer, adds a reaction solvent to the stirrer, mixes it evenly, and lets it stand. Then, dimethylamine gas is introduced into the stirrer, and a catalyst is added. After the reaction, the product is taken out and cooled to room temperature. The product is then centrifuged three times: the product is placed in a centrifuge for the first centrifuge to obtain the first centrifuge product; the first centrifuge product is heated in a water bath and placed in a centrifuge for the second centrifuge to obtain the second centrifuge product; the second centrifuge product is then distilled, and the distillate is sieved to obtain the purified product; the purified product is then placed in a centrifuge for the third centrifuge to obtain the centrifuged product. The method provided, through three centrifugations, can not only effectively improve the product yield but also effectively improve the product purity. Attached Figure Description

[0023] Figure 1 This is a statistical diagram illustrating the product yield during performance testing in this invention. Detailed Implementation

[0024] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0025] The present invention will be further described below with reference to embodiments.

[0026] Example 1:

[0027] This invention provides a centrifugation method for the preparation of trimethylsilane, comprising the following steps:

[0028] (1) Weigh out trimethylchlorosilane, place it in a stirrer, add the reaction solvent to the stirrer, mix well, and let stand for 30 minutes.

[0029] The stirrer rotates at 20 r / min for 8 min, and the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2.

[0030] Furthermore, before placing trimethylchlorosilane in the stirrer, nitrogen gas is introduced into the stirrer to expel the air inside.

[0031] The further reaction solvent is n-hexane.

[0032] (2) Then introduce dimethylamine gas into the stirrer and add catalyst, and react for 20 minutes.

[0033] Furthermore, the catalyst is ammonium sulfate.

[0034] (3) Take out the product and cool it to room temperature. Place the product in a centrifuge for the first centrifugation to obtain the first centrifuged product.

[0035] Furthermore, the first centrifugation was performed at a speed of 12,000 r / min for 12 min.

[0036] (4) Heat the first centrifuged material in a water bath and place it in a centrifuge for a second centrifugation to obtain the second centrifuged material.

[0037] Furthermore, the second centrifugation was performed at a speed of 8000 r / min for a time of 8 min.

[0038] Furthermore, the water bath heating temperature is 40℃.

[0039] (5) Distill the second centrifuged product and pass the distillate through a 100-mesh sieve to obtain the purified product.

[0040] Furthermore, the distillation temperature is 86℃.

[0041] (6) Place the purified product in a centrifuge for a third centrifugation to obtain the centrifuged product.

[0042] Furthermore, the third centrifugation was performed at a speed of 15,000 r / min for a time of 20 min.

[0043] Furthermore, the internal temperature of the centrifuge is 35°C.

[0044] Example 2:

[0045] This invention provides a centrifugation method for the preparation of trimethylsilane, comprising the following steps:

[0046] (1) Weigh out trimethylchlorosilane, place it in a stirrer, add the reaction solvent to the stirrer, mix well, and let stand for 30 minutes.

[0047] The stirrer rotates at 25 r / min for 9 min, and the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2.

[0048] Furthermore, before placing trimethylchlorosilane in the stirrer, nitrogen gas is introduced into the stirrer to expel the air inside.

[0049] The further reaction solvent is pseudotrimethylbenzene.

[0050] (2) Then introduce dimethylamine gas into the stirrer and add catalyst, and react for 20 minutes.

[0051] Furthermore, the catalyst is n-butyllithium.

[0052] (3) Take out the product and cool it to room temperature. Place the product in a centrifuge for the first centrifugation to obtain the first centrifuged product.

[0053] Furthermore, the first centrifugation was performed at a speed of 12,500 r / min for a time of 13 min.

[0054] (4) Heat the first centrifuged material in a water bath and place it in a centrifuge for a second centrifugation to obtain the second centrifuged material.

[0055] Furthermore, the second centrifugation was performed at a speed of 8500 r / min for a time of 9 min.

[0056] Furthermore, the water bath heating temperature is 45℃.

[0057] (5) Distill the second centrifuged product and pass the distillate through a 100-mesh sieve to obtain the purified product.

[0058] Furthermore, the distillation temperature is 87°C.

[0059] (6) Place the purified product in a centrifuge for a third centrifugation to obtain the centrifuged product.

[0060] Furthermore, the third centrifugation was performed at a speed of 15,500 r / min for a time of 25 min.

[0061] Furthermore, the internal temperature of the centrifuge is 36°C.

[0062] Example 3:

[0063] This invention provides a centrifugation method for the preparation of trimethylsilane, comprising the following steps:

[0064] (1) Weigh out trimethylchlorosilane, place it in a stirrer, add the reaction solvent to the stirrer, mix well, and let stand for 30 minutes.

[0065] The stirrer rotates at 30 r / min for 10 min, and the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2.

[0066] Furthermore, before placing trimethylchlorosilane in the stirrer, nitrogen gas is introduced into the stirrer to expel the air inside.

[0067] The further reaction solvent is n-hexane.

[0068] (2) Then introduce dimethylamine gas into the stirrer and add catalyst, and react for 20 minutes.

[0069] Furthermore, the catalyst is ammonium sulfate.

[0070] (3) Take out the product and cool it to room temperature. Place the product in a centrifuge for the first centrifugation to obtain the first centrifuged product.

[0071] Furthermore, the first centrifugation was performed at a speed of 13,000 r / min for 14 min.

[0072] (4) Heat the first centrifuged material in a water bath and place it in a centrifuge for a second centrifugation to obtain the second centrifuged material.

[0073] Furthermore, the second centrifugation was performed at a speed of 9000 r / min for a time of 10 min.

[0074] Furthermore, the water bath heating temperature is 50°C.

[0075] (5) Distill the second centrifuged product and pass the distillate through a 100-mesh sieve to obtain the purified product.

[0076] Furthermore, the distillation temperature is 88℃.

[0077] (6) Place the purified product in a centrifuge for a third centrifugation to obtain the centrifuged product.

[0078] Furthermore, the third centrifugation was performed at a speed of 16,000 r / min for a time of 30 min.

[0079] Furthermore, the internal temperature of the centrifuge is 37°C.

[0080] Comparative Example 1:

[0081] The centrifugation method for preparing trimethylsilane provided in this embodiment is largely the same as that in Example 1, the main difference being that three centrifugations are not performed. That is, the following steps are used:

[0082] (1) Weigh out trimethylchlorosilane, place it in a stirrer, add the reaction solvent to the stirrer, mix well, and let stand for 30 minutes.

[0083] The stirrer rotates at 20 r / min for 8 min, and the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2.

[0084] Furthermore, before placing trimethylchlorosilane in the stirrer, nitrogen gas is introduced into the stirrer to expel the air inside.

[0085] The further reaction solvent is n-hexane.

[0086] (2) Then introduce dimethylamine gas into the stirrer and add catalyst, and react for 20 minutes.

[0087] Furthermore, the catalyst is ammonium sulfate.

[0088] (3) Remove the product and cool it to room temperature.

[0089] Comparative Example 2:

[0090] The centrifugation method for preparing trimethylsilane provided in this embodiment is largely the same as that in Example 1, the main difference being that only the first centrifugation is used. That is, the following steps are employed:

[0091] (1) Weigh out trimethylchlorosilane, place it in a stirrer, add the reaction solvent to the stirrer, mix well, and let stand for 30 minutes.

[0092] The stirrer rotates at 20 r / min for 8 min, and the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2.

[0093] Furthermore, before placing trimethylchlorosilane in the stirrer, nitrogen gas is introduced into the stirrer to expel the air inside. The reaction solvent is n-hexane.

[0094] (2) Then introduce dimethylamine gas into the stirrer and add catalyst, and react for 20 minutes.

[0095] Furthermore, the catalyst is ammonium sulfate.

[0096] (3) Take out the product and cool it to room temperature. Place the product in a centrifuge and centrifuge to obtain centrifuged material.

[0097] Comparative Example 3:

[0098] The centrifugation method for preparing trimethylsilane provided in this embodiment is largely the same as that in Example 1, the main difference being that only a second centrifugation is used. That is, the following steps are employed:

[0099] (1) Weigh out trimethylchlorosilane, place it in a stirrer, add the reaction solvent to the stirrer, mix well, and let stand for 30 minutes.

[0100] The stirrer rotates at 20 r / min for 8 min, and the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2.

[0101] Furthermore, before placing trimethylchlorosilane in the stirrer, nitrogen gas is introduced into the stirrer to expel the air inside. The reaction solvent is n-hexane.

[0102] (2) Then introduce dimethylamine gas into the stirrer and add catalyst, and react for 20 minutes.

[0103] Furthermore, the catalyst is ammonium sulfate.

[0104] (3) Take out the product and cool it to room temperature. Place the product in a centrifuge and centrifuge to obtain centrifuged material.

[0105] Furthermore, the centrifugation speed was 8000 r / min, and the centrifugation time was 8 min. The water bath heating temperature was 40℃.

[0106] Comparative Example 4:

[0107] The centrifugation method for preparing trimethylsilane provided in this embodiment is largely the same as that in Example 1, the main difference being that only a third centrifugation is used. That is, the following steps are employed:

[0108] (1) Weigh out trimethylchlorosilane, place it in a stirrer, add the reaction solvent to the stirrer, mix well, and let stand for 30 minutes.

[0109] The stirrer rotates at 20 r / min for 8 min, and the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2.

[0110] Furthermore, before placing trimethylchlorosilane in the stirrer, nitrogen gas is introduced into the stirrer to expel the air inside. The reaction solvent is n-hexane.

[0111] (2) Then introduce dimethylamine gas into the stirrer and add catalyst, and react for 20 minutes.

[0112] Furthermore, the catalyst is ammonium sulfate.

[0113] (3) Remove the product and cool it to room temperature. Then place the product in a centrifuge to centrifuge and obtain the centrifuged product.

[0114] Furthermore, the centrifuge speed was 15000 r / min, and the centrifugation time was 20 min. The internal temperature of the centrifuge was 35℃.

[0115] Performance testing:

[0116] Trimethylsilane was prepared by centrifugation according to the methods of Examples 1, 2 and 3, and was used as Experiment 1, Experiment 2 and Experiment 3, respectively. Trimethylsilane was then prepared by centrifugation according to the methods of Comparative Examples 1, 2, 3 and 4, and was used as Control 1, Control 2, Control 3 and Control 4, respectively.

[0117] 1) The test data are recorded in Table 1 according to the product yield of each group after preparing trimethylsilane.

[0118] Table 1: Product Yield Records for Each Group

[0119] Group n Product yield (%) Experiment 1 Group 6 91.55 Experiment 2 group 6 90.86 Experimental Group 3 6 90.59 Control Group 1 6 70.24 Control group 2 6 74.82 Control group 3 6 76.71 Control group 4 6 71.22

[0120] As shown in Table 1 and Figure 1 As shown, compared with the experimental groups (experimental groups 1, 2, 3, and 3), the product yield of the experimental groups (control groups 1, 2, and 3) was significantly higher than that of the control groups (control group 1, control group 2, control group 3, and control group 4) (p < 0.05), while the product yield difference among the experimental groups was not significant (p > 0.05). The method provided by this invention can effectively improve the product yield through three centrifugations.

[0121] 2) The test data for the product purity after preparing trimethylsilane in each group are recorded in Table 2.

[0122] Table 2: Product Purity Record Sheet for Each Group

[0123] Group n Product purity (%) Experiment 1 Group 10 97.21 Experiment 2 group 10 98.05 Experimental Group 3 10 97.54 Control Group 1 10 65.67 Control group 2 10 67.39 Control group 3 10 68.58 Control group 4 10 69.31

[0124] As shown in Table 2, compared with control group 1, the product purity of control groups 2, 3, and 4 was improved, but the improvement was not significant (p > 0.05). Compared with the experimental groups (experimental groups 1, 2, 3, and 3), the product purity of the experimental groups (control groups 1, 2, 3, and 4) was significantly higher (p < 0.05), while the product purity differences among the experimental groups were not significant (p > 0.05). The method provided by this invention can effectively improve product purity through three centrifugations.

[0125] The method provided by this invention involves weighing trimethylchlorosilane, placing it in a stirrer, adding a reaction solvent to the stirrer, mixing thoroughly, and allowing it to stand. Then, dimethylamine gas is introduced into the stirrer, and a catalyst is added. After the reaction, the product is removed and cooled to room temperature. The product is then centrifuged three times: first, the product is centrifuged in a centrifuge to obtain a first centrifuge sample; second, the first centrifuge sample is heated in a water bath and centrifuged again to obtain a second centrifuge sample; third, the second centrifuge sample is distilled, and the distillate is sieved to obtain a purified product; finally, the purified product is centrifuged a third time to obtain a centrifuged product. This method, through three centrifugations, not only effectively improves the product yield but also effectively improves the product purity.

[0126] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions will not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A centrifugal process for trimethylsilane production, characterized by, The method comprises the following steps: (1) weigh trimethylchlorosilane, and place it in a stirrer, then add a reaction solvent into the stirrer, mix uniformly, and stand still for 30 min; The rotation speed of the stirrer is 20-30 r / min, and the stirring time is 8-10 min; the mass ratio of trimethylchlorosilane to the reaction solvent is 1:2; (2) then, introduce dimethylamine gas into the stirrer, and add a catalyst, and react for 20 min; The catalyst is any one of ammonium sulfate and n-butyllithium; (3) take out the product, cool it to room temperature, place it in a centrifuge for first centrifugation, and obtain a first centrifugate; The rotation speed of the first centrifugation is 12000-13000 r / min, and the centrifugation time is 12-14 min; (4) water-bath heat the first centrifugate, and place it in a centrifuge for second centrifugation, and obtain a second centrifugate; The rotation speed of the second centrifugation is 8000-9000 r / min, and the centrifugation time is 8-10 min; The water-bath heating temperature is 40-50 ℃; (5) distill the second centrifugate, pass the distillate through a 100-mesh sieve, and obtain a purified product; The distillation temperature is 86-88 ℃; (6) place the purified product in a centrifuge again for third centrifugation, and obtain a centrifugate; The rotation speed of the third centrifugation is 15000-16000 r / min, and the centrifugation time is 20-30 min; The internal temperature of the centrifuge is 35-37 ℃.

2. A centrifugation process for trimethylsilane production according to claim 1, characterized in that, In step (1), before placing trimethylchlorosilane in the stirrer, introduce nitrogen gas into the stirrer to expel air in the stirrer.

3. A centrifugal process for trimethylsilane production according to claim 1, characterized in that, In step (1), the reaction solvent is any one of n-hexane and cymene.

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