CN112538166B - Large-scale production method for ultrasonic-assisted synthesis of polymethylsilane - Google Patents
Large-scale production method for ultrasonic-assisted synthesis of polymethylsilane Download PDFInfo
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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Abstract
The invention discloses a large-scale production method for ultrasonic-assisted synthesis of polymethylsilane, which comprises the following steps: step one, under the protective atmosphere, adding toluene and metal sodium into a reaction kettle; heating to T1 to melt the sodium blocks, stirring, making the sodium blocks into sodium sand, and cooling to T2; dropwise adding the methyldichlorosilane into the reaction kettle for N times to perform reflux reaction; obtaining a reacted liquid; controlling the temperature to be T2 in the dripping process, carrying out the dripping process under the assistance of ultrasound and stirring, stopping the ultrasound after finishing the dripping process each time, heating to T3, and continuously carrying out reflux reaction under stirring, wherein N is more than or equal to 2; and step three, under a protective atmosphere, carrying out centrifugal treatment on the liquid obtained in the step two after the reaction, and carrying out reduced pressure distillation treatment on the liquid obtained by the centrifugal treatment under the protective atmosphere to obtain the polymethylsilane. The reaction temperature of the invention is low, the synthesis yield can reach more than 60 percent, and in a preferred scheme, the synthesis yield is as high as more than 80 percent.
Description
Technical Field
The invention relates to a large-scale production method for ultrasonic-assisted synthesis of polymethylsilane, belonging to the technical field of synthesis of ceramic precursors.
Technical Field
The precursor polysilane is mostly prepared by condensing chlorosilane and sodium by a wurtz method under the stirring condition. The invention relates to the modeling production of polymethylsilanes by ultrasonic law. Under the ultrasonic radiation, chlorosilane and sodium react to generate polysilane with more uniform molecular weight distribution and higher synthesis yield, and the synthesis temperature is lower due to a special working principle and the heat release phenomenon of ultrasonic waves.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the large-scale production method for synthesizing the polymethylsilane under the assistance of the ultrasonic waves, which has the advantages of simple equipment requirement, high safety, higher synthesis yield, low reaction temperature, less volatilization of organic matters and environmental friendliness.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a large-scale production method for synthesizing polymethylsilane by ultrasonic assistance, which comprises the following steps:
step one
Under the protective atmosphere, adding toluene and metal sodium into a reaction kettle; heating to T1 to melt the sodium blocks, stirring, making the sodium blocks into sodium sand, and cooling to T2;
step two
Dropwise adding methyl dichlorosilane into the reaction kettle for N times to perform reflux reaction; obtaining a reacted solution; controlling the temperature to be T2 in the dripping process, carrying out the dripping process under the assistance of ultrasound and stirring, stopping the ultrasound after finishing the dripping process each time, heating to T3, and continuously carrying out reflux reaction under stirring, wherein N is more than or equal to 2;
step three
And (3) centrifuging the reacted liquid obtained in the step two in a protective atmosphere, and carrying out reduced pressure distillation on the centrifuged liquid in the protective atmosphere to obtain the polymethylsilane.
In the invention, the protective atmosphere is preferably nitrogen, and in the practical operation process, the whole reaction system is vacuumized and replaced by nitrogen, the nitrogen replacement achieves that the oxygen content in the reaction system is less than 0.5 percent, wherein the purity of the nitrogen for replacement is 99.999 percent.
Preferably, in the first step, the mass ratio of the toluene to the metallic sodium is 7-10: 1.
in the invention, the purity of the metal sodium is more than or equal to 99 percent and is coin-shaped.
Preferably, in step one, said T1 is 95-105 ℃. At this temperature, it is ensured that the metallic sodium is completely melted.
Preferably, in the step one, the stirring speed is 1200-2000 revolutions, and the stirring time is 20-45 min.
In the invention, the preparation of the sodium sand and the synthesis of the polymethylsilane are in the same reaction kettle, while the sodium sand in the prior art needs to be prepared by adopting other reaction kettles in advance, and the sodium sand needs to be transferred in the synthesis of the polymethylsilane.
In a preferred embodiment, in the first and second steps, the temperature T2 is 50-60 ℃.
In a preferred scheme, the mass ratio of the metal sodium to the methyldichlorosilane is 1: (2.5-3).
Preferably, in the second step, the dropping speed of the methyldichlorosilane is 3-4 Kg/h.
Preferably, in the second step, the ultrasonic frequency is 20KHZ-28 KHZ.
In the invention, the ultrasonic equipment adopts an ultrasonic rod with 3KW power, a top-inserted structure and flange connection, and an ultrasonic transmitting end is 300mm long and is completely immersed below the liquid level.
Preferably, in the step two, the stirring speed is 30-40 r/min in the dropping process.
Preferably, in step two, T3 is 80-90 ℃.
Preferably, in the second step, after each dropwise addition, the reflux reaction is continued under stirring, wherein the stirring speed is 60-80 r/min.
Preferably, in the second step, the time of the reflux reaction after the first to the N-1 th dropwise addition is 2-3h, and the time of the reflux reaction after the N-th dropwise addition is 5-10h, preferably 7-8 h.
In the preferable scheme, in the third step, the temperature of the reduced pressure distillation is 80-105 ℃, and the vacuum degree is 20-10 KPa.
Advantageous effects
The method for producing the polymethylsilane in a modeling manner by the ultrasonic method has the advantages of low synthesis temperature, high synthesis yield, reduction in the treatment of later-stage byproducts, environmental friendliness, good safety and stability and suitability for large-scale production.
Compared with the traditional mechanical stirring wurtz reaction for synthesizing the polymethylsilane, the method has the following main advantages:
1. according to the invention, the ultrasonic wave is used for assisting to synthesize the polymethylsilane, the cavitation effect of the ultrasonic wave is utilized, the activation energy of the reaction is reduced, the reaction temperature is reduced to a large extent, the volatilization of the methyldichlorosilane and the toluene is reduced, the environment is friendly, meanwhile, the ultrasonic wave is beneficial to the falling of sodium chloride from the surface of the sodium sand, the product and the intermediate formed on the surface of the sodium sand are removed in time, the fresh sodium surface is exposed, the contact area of the sodium sand and the dimethyldichlorosilane is increased, and the reaction activity is improved, so that the method is much more efficient than the traditional mechanical stirring wurtz reaction for synthesizing the polymethylsilane;
2. the invention adopts the inserted ultrasonic rods, has simple requirements on equipment, can radiate the whole reaction system only by increasing the number and power of the ultrasonic rods for industrialized expanded production, adds low-speed stirring during ultrasonic treatment, can raise sodium sand without affecting the ultrasonic effect and settling bottom, and ensures the thoroughness of reaction;
3. the invention adopts the mode of alternating ultrasonic method synthesis and low-speed stirring synthesis, namely, during the dropping, the ultrasonic wave is added, and the reflux reaction is carried out only under stirring in the reaction time after the dropping is finished each time, because the cavitation phenomenon of the ultrasonic wave can promote the reaction and simultaneously can decompose the polymerization reaction, therefore, the molecular weight of the polymethylsilane synthesized by the ultrasonic method is smaller, and the conversion rate is lower, therefore, in the dropping process of the invention, the ultrasonic wave is added to improve the reaction activity, and after the dropping is finished each time, the molecular weight of the polymethylsilane can be increased through the short-time low-speed stirring and temperature rise, and the high temperature and the low stirring speed can reduce the solidification of the polymethylsilane, and finally, the synthesis yield can reach more than 60 percent, and in the preferred scheme, the synthesis yield can reach more than 80 percent
4. The polymethylsilane synthesized by the invention is basically straight-chain, has high Si-H activity, a molecular weight of about 1500 and a viscosity of about 200cp.s, is easy to generate a crosslinking reaction with a modifier, is suitable for modifying and adjusting performance, and has very strong plasticity.
Detailed Description
Example 1
(1) Replacing nitrogen in the whole system until the oxygen content in the system is 0.04 percent;
(2) pumping 350L of methylbenzene into the reaction kettle by a pump;
(3) 32Kg of coin-shaped metal sodium is added into the reaction kettle;
(4) pumping 88Kg of methyl dichlorosilane into the elevated tank by a pump;
(5) heating the reaction kettle to 100 ℃, and preserving the temperature for 30min to completely melt the metal sodium;
(6) starting a high-speed stirrer of the reaction kettle, keeping the rotating speed at 1500 rpm for 30min, stopping high-speed stirring, and cooling to 60 ℃;
(7) starting ultrasound and stirring, adjusting the ultrasound frequency to 20KHZ, adjusting the stirring speed to 40 r/min, and dropwise adding methyl dichlorosilane at the speed of 3 Kg/h;
(8) after dropwise adding for 6h, turning off the ultrasound, stopping dropwise adding, raising the temperature in the reaction kettle to 85 ℃, increasing the stirring speed to 80 r/min, and reacting for 2 h;
(9) reducing the temperature in the kettle to 60 ℃, starting ultrasound with the ultrasonic frequency of 25KHZ, adjusting the stirring speed to 40 r/min, and dropwise adding methyldichlorosilane at the dropping speed of 3 Kg/h;
(10) repeating the operations (8) and (9);
(11) after the last dropwise adding is finished, turning off the ultrasonic wave, raising the temperature in the reaction kettle to 85 ℃, raising the stirring speed to 80 r/min, and reacting for 5 hours;
(12) cooling the reacted liquid to room temperature, and stirring while feeding the liquid into a centrifugal machine for solid-liquid separation;
(13) and (3) feeding the filtrate filtered by the centrifuge into a distillation kettle, maintaining the vacuum degree of 15KPa and the distillation temperature of 90 ℃ to obtain 21.8Kg of product polymethylsilane.
The product yield is as follows: 71.24 percent
Product viscosity: 220cp
The molecular weight of the product is as follows: 1100
Ceramic yield (800 ℃): 30 percent
The product is mainly straight-chain, has high Si-H activity, is easy to generate cross-linking reaction with a modifier, is suitable for modifying and adjusting performance, and has very strong plasticity.
Example 2
(1) Replacing nitrogen in the whole system until the oxygen content in the system is 0.04 percent;
(2) pumping 350L of toluene into the reaction kettle by using a pump;
(3) 32Kg of coin-shaped metal sodium is added into the reaction kettle;
(4) pumping 96Kg of methyl dichlorosilane into the elevated tank by a pump;
(5) heating the reaction kettle to 100 ℃, and preserving the temperature for 30min to completely melt the metal sodium;
(6) starting a high-speed stirrer of the reaction kettle, keeping the rotation speed of 1200 revolutions per minute for 30 minutes, stopping high-speed stirring, and cooling to 50 ℃;
(7) starting ultrasound and stirring, adjusting the ultrasound frequency to 28KHZ, adjusting the stirring speed to 30 r/min, and dropwise adding methyl dichlorosilane at the speed of 3 Kg/h;
(8) after dropwise adding for 6h, turning off the ultrasound, stopping dropwise adding, raising the temperature in the reaction kettle to 90 ℃, increasing the stirring speed to 60 r/min, and reacting for 3 h;
(9) reducing the temperature in the kettle to 50 ℃, starting ultrasound with the ultrasonic frequency of 28KHZ, adjusting the stirring speed to 30 r/min, and dropwise adding methyl dichlorosilane at the dropping speed of 4 Kg/h;
(10) repeating the operations (8) and (9);
(11) after the last dropwise adding is finished, turning off the ultrasonic wave, raising the temperature in the reaction kettle to 90 ℃, raising the stirring speed to 60 revolutions per minute, and reacting for 10 hours;
(12) cooling the reacted liquid to room temperature, and stirring while feeding the liquid into a centrifugal machine for solid-liquid separation;
(13) and (3) feeding the filtrate filtered by the centrifuge into a distillation kettle, maintaining the vacuum degree of 15KPa and the distillation temperature of 90 ℃ to obtain 19.4Kg of product polymethylsilane.
The product yield is as follows: 63.4 percent
Product viscosity: 562cp
The molecular weight of the product is as follows: 800
Ceramic yield (800 ℃): 49 percent.
The product is mainly straight-chain, has high Si-H activity, is easy to generate cross-linking reaction with a modifier, is suitable for modifying and adjusting performance, and has very strong plasticity.
Example 3
(14) Replacing nitrogen in the whole system until the oxygen content in the system is 0.04 percent;
(15) pumping 350L of toluene into the reaction kettle by using a pump;
(16) 32Kg of coin-shaped metal sodium is added into the reaction kettle;
(17) pumping 80Kg of methyl dichlorosilane into the elevated tank by a pump;
(18) heating the reaction kettle to 100 ℃, and preserving the temperature for 30min to completely melt the metal sodium;
(19) starting a high-speed stirrer of the reaction kettle, keeping the rotating speed at 2000 rpm for 20min, stopping high-speed stirring, and cooling to 55 ℃;
(20) starting ultrasound and stirring, adjusting the ultrasound frequency to 25KHZ, adjusting the stirring speed to 35 r/min, and dropwise adding methyl dichlorosilane at the speed of 3.5 Kg/h;
(21) after dropwise adding for 6h, turning off the ultrasound, stopping dropwise adding, raising the temperature in the reaction kettle to 80 ℃, increasing the stirring speed to 70 r/min, and reacting for 3 h;
(22) cooling the temperature in the kettle to 55 ℃, starting ultrasound with the ultrasonic frequency of 25KHZ, adjusting the stirring speed to 35 r/min, and dropwise adding methyl dichlorosilane at the dropping speed of 3.5 Kg/h;
(23) repeating the operations (8) and (9);
(24) after the last dropwise adding is finished, turning off the ultrasonic wave, raising the temperature in the reaction kettle to 80 ℃, raising the stirring speed to 70 r/min, and reacting for 8 hours;
(25) cooling the reacted liquid to room temperature, and stirring while feeding the liquid into a centrifugal machine for solid-liquid separation;
(26) and (3) feeding the filtrate filtered by the centrifuge into a distillation kettle, maintaining the vacuum degree of 15KPa and the distillation temperature of 90 ℃, and obtaining 24.5Kg of the product polymethylsilane.
The product yield is as follows: 80.07 percent
Product viscosity: 250cp
The molecular weight of the product is as follows: 1200
Ceramic yield (800 ℃): 35 percent of
The product is mainly straight-chain, has high Si-H activity, is easy to generate cross-linking reaction with a modifier, is suitable for modifying and adjusting performance, and has very strong plasticity.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the scope of the present invention.
Comparative example 1
The other conditions are the same as example 3, except that the reaction ultrasound is turned on all the time from the dropwise addition, 18Kg of the product polymethylsilane is obtained:
the product yield is as follows: 58.82 percent
Product viscosity: 90cp
The molecular weight of the product is as follows: 600
Ceramic yield (800 ℃): 17 percent of
The product is mainly straight-chain, the molecular weight is lower than that of the example, the Si-H activity is too high, the product is extremely unstable in the air and generates heat when exposed to the air, and the product is dipped in absorbent cotton at normal temperature and immediately self-ignites in the air.
Comparative example 2
The other conditions are the same as the example 3, only stirring and ultrasound are started in the dropping process, however, as the temperature in the dropping process is lower than that in the prior art, the dropping is started in the dropping process, the reaction basically does not occur or occurs very slowly, the concentration of the unreacted methyldichlorosilane is higher and higher along with the dropping, and after a certain amount of the unreacted methyldichlorosilane is accumulated, the reaction suddenly and violently occurs, a large amount of heat is released, a sudden polymerization kettle is flushed, and potential safety hazards exist.
The dropping temperature is adjusted to 80 ℃ in the prior art, only stirring and no ultrasound are started in the dropping process, the reaction can be carried out stably, and 13Kg of polymethylsilane is finally obtained:
the product yield is as follows: 42.48 percent
Product viscosity: 270cp
The molecular weight of the product is as follows: 1300
Ceramic yield (800 ℃): 40 percent.
The product properties were essentially the same as in the examples.
Comparative example 3
The other conditions are the same as the example 3, except that the stirring speed is 70 r/min during the dropping process, and the product, namely the polymethyl silane, is 12 Kg:
the product yield is as follows: 39.21 percent
Product viscosity: 630cp
The molecular weight of the product is as follows: 680
Ceramic yield (800 ℃): and 55 percent.
The product has increased branching, higher viscosity than the examples, lower molecular weight and activity than the examples, but lower Si-H activity than the examples, and lower modification adjustment performance than the examples.
Claims (8)
1. A large-scale production method for ultrasonic-assisted synthesis of polymethylsilane is characterized by comprising the following steps: the method comprises the following steps:
step one
Under the protective atmosphere, adding toluene and metal sodium into a reaction kettle; heating to T1 to melt the sodium blocks, stirring, making the sodium blocks into sodium sand, and cooling to T2; the T1 is 95-105 ℃; the T2 is 50-60 ℃;
step two
Dropwise adding methyl dichlorosilane into the reaction kettle for N times to perform reflux reaction; obtaining a reacted liquid; controlling the temperature to be T2 in the dripping process, and carrying out the dripping process with the assistance of ultrasound and stirring, wherein the stirring speed is 30-40 r/min in the dripping process; stopping ultrasound after each dropwise addition is finished, heating to T3, and continuously carrying out reflux reaction under stirring, wherein N is more than or equal to 2; the T2 is 50-60 ℃; t3 is 80-90 ℃; the ultrasonic frequency is 20KHZ-28 KHZ;
step three
And (3) under a protective atmosphere, centrifuging the liquid obtained in the second step after the reaction, and carrying out reduced pressure distillation treatment on the centrifuged liquid under the protective atmosphere to obtain the polymethylsilane.
2. The method for mass production of polymethylsilane of ultrasonic-assisted synthesis as claimed in claim 1, wherein: in the first step, the mass ratio of the toluene to the metal sodium is 7-10: 1.
3. the method for mass production of polymethylsilane of ultrasonic-assisted synthesis as claimed in claim 1, wherein: in the first step, the stirring speed is 1200-.
4. The method for mass production of polymethylsilane of ultrasonic-assisted synthesis as claimed in claim 1, wherein: the mass ratio of the metal sodium to the methyl dichlorosilane is 1: 2.5-3.
5. The method for mass production of polymethylsilane of ultrasonic-assisted synthesis as claimed in claim 1, wherein: in the second step, the dropping speed of the methyl dichlorosilane is 3-4 Kg/h.
6. The method for mass production of polymethylsilane of ultrasonic-assisted synthesis as claimed in claim 1, wherein: and in the second step, after each dropwise addition is finished, continuously carrying out reflux reaction under stirring at the speed of 60-80 revolutions per minute.
7. The method for mass production of polymethylsilane of ultrasonic-assisted synthesis as claimed in claim 1, wherein: in the second step, the time of reflux reaction after the first time to the Nth-1 th dropwise adding is 2-3h, and the time of reflux reaction after the Nth dropwise adding is 5-10 h.
8. The method for mass production of polymethylsilane of ultrasonic-assisted synthesis as claimed in claim 1, wherein: in the third step, the temperature of the reduced pressure distillation is 80-105 ℃, and the vacuum degree is 20-10 KPa.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62241926A (en) * | 1986-04-14 | 1987-10-22 | Katsumi Yoshino | Production of polysilane |
| US6020447A (en) * | 1996-03-29 | 2000-02-01 | Massachusetts Institute Of Technology | Sonichemical synthesis of silicon carbide precursors and methods for preparation thereof |
| US6989428B1 (en) * | 2002-03-22 | 2006-01-24 | University Of Massachusetts | Methods of preparing polysilynes |
| CN101024694A (en) * | 2007-03-29 | 2007-08-29 | 上海大学 | Method for synthesizing polysilane containing two bonds |
| CN103755849A (en) * | 2014-02-24 | 2014-04-30 | 哈尔滨理工大学 | Carbon nanotube-polysilane-organic high-molecular composite material and preparation method thereof |
| CN109400886A (en) * | 2018-11-28 | 2019-03-01 | 湖北科技学院 | A kind of ultrasonic radiation preparation method of liquid Polycarbosilane |
-
2020
- 2020-12-11 CN CN202011446869.0A patent/CN112538166B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62241926A (en) * | 1986-04-14 | 1987-10-22 | Katsumi Yoshino | Production of polysilane |
| US6020447A (en) * | 1996-03-29 | 2000-02-01 | Massachusetts Institute Of Technology | Sonichemical synthesis of silicon carbide precursors and methods for preparation thereof |
| US6989428B1 (en) * | 2002-03-22 | 2006-01-24 | University Of Massachusetts | Methods of preparing polysilynes |
| CN101024694A (en) * | 2007-03-29 | 2007-08-29 | 上海大学 | Method for synthesizing polysilane containing two bonds |
| CN103755849A (en) * | 2014-02-24 | 2014-04-30 | 哈尔滨理工大学 | Carbon nanotube-polysilane-organic high-molecular composite material and preparation method thereof |
| CN109400886A (en) * | 2018-11-28 | 2019-03-01 | 湖北科技学院 | A kind of ultrasonic radiation preparation method of liquid Polycarbosilane |
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