CN113150286A - Preparation method of polycarbosilane with high silicon-hydrogen content - Google Patents
Preparation method of polycarbosilane with high silicon-hydrogen content Download PDFInfo
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- CN113150286A CN113150286A CN202110439875.1A CN202110439875A CN113150286A CN 113150286 A CN113150286 A CN 113150286A CN 202110439875 A CN202110439875 A CN 202110439875A CN 113150286 A CN113150286 A CN 113150286A
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- 229920003257 polycarbosilane Polymers 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 30
- 239000001257 hydrogen Substances 0.000 title claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 72
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 239000013067 intermediate product Substances 0.000 claims abstract description 33
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000006459 hydrosilylation reaction Methods 0.000 claims abstract description 4
- 239000012280 lithium aluminium hydride Substances 0.000 claims abstract description 4
- -1 lithium aluminum hydride Chemical compound 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000005050 vinyl trichlorosilane Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
- 230000003014 reinforcing effect Effects 0.000 claims description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 14
- 229910010271 silicon carbide Inorganic materials 0.000 description 12
- 239000000835 fiber Substances 0.000 description 8
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 238000004364 calculation method Methods 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- 239000012700 ceramic precursor Substances 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 229920000555 poly(dimethylsilanediyl) polymer Polymers 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G77/60—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 in which all the silicon atoms are connected by linkages other than oxygen atoms
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a preparation method of polycarbosilane with high silicon hydrogen content, which comprises the following steps: adding polycarbosilane and vinyl trichlorosilane into preparation equipment to obtain a first intermediate product through hydrosilylation reaction; adding lithium aluminum hydride into the first intermediate product to prepare a second intermediate product; carrying out solid-liquid separation treatment on the second intermediate product, and removing solids to obtain a third intermediate product; and (3) replacing the first raw material in the step one with the third intermediate product, and sequentially performing the step one, the step two and the step three to prepare the polycarbosilane with high silicon-hydrogen content. The spiral heating pipeline is installed in the preparation equipment, the heating rod heats materials in the reaction equipment, the heating area can be increased by adopting the spiral heating pipeline, the arranged heating rod can heat the spare part of the spiral pipeline, the heating efficiency is improved, and in addition, the heating temperature and the heating time of the spiral heating pipeline and the heating rod are adjusted through the temperature adjusting module, so that the heating is more reasonable.
Description
Technical Field
The invention belongs to the technical field of polycarbosilane production, and particularly relates to a preparation method of polycarbosilane with high silicon hydrogen content.
Background
The polycarbosilane is used as a precursor of the silicon carbide ceramic material, and directly determines the performance of the silicon carbide ceramic material. Polycarbosilane is a kind of high molecular compound, its main chain is composed of silicon and carbon atoms alternatively, the silicon and carbon atoms are connected with hydrogen or organic group, and its molecular chain is linear or branched structure. Polycarbosilane is the most important compound in precursor polymers (advanced polymers) which are newly appeared in the current high-technology new materials, and is mainly used for preparing high-technology ceramic materials of silicon carbide series, wherein silicon carbide fibers are the most representative. One of the major factors in the growing interest in polycarbosilanes research over the years has been their potential for use as silicon carbide precursors, primarily as a continuous ceramic fiber source. Many novel polycarbosilanes are thereby synthesized, either directly or indirectly. However, polycarbosilanes have also become the focus of research in recent years, but this part of the research has not been associated with the development of ceramic precursors. This is because polycarbosilanes are increasingly recognized as a new class of polymers that have potential use in a wide range of applications. Although polycarbosilanes have been synthesized for a long time, only in the 70 s of the 20 th century, the professor of the northeast university of japan, now discovered a new synthesis method and, as a result, produced silicon carbide fibers that could be used for a long period of time at very high temperatures. At present, polycarbosilane is gradually used for preparing new fields of silicon carbide ceramic matrix composite materials and the like besides preparing fibers, and forms a great industry. Currently only japan, china and the united states are available. The way of preparing polycarbosilane by vector island is to adopt dichlorodimethylsilane as an initial raw material, prepare the polydimethylsilane by sodium condensation, and then convert the polydimethylsilane into polycarbosilane at high temperature and high pressure. The molecular weight of the product prepared by the method is 1000-2000, the melting point is about 200 ℃, the product is easy to dissolve in organic solvents such as toluene and the like, and the product has good spinnability.
However, the existing polycarbosilane has low silicon hydrogen content and is difficult to become a raw material of polycarbosilane with high content of heterogeneous elements, and the temperature of the preparation equipment in the prior art is not reasonably controlled, so that the phenomenon of uneven heating is easily caused, and the preparation of polycarbosilane with high silicon hydrogen content is influenced, therefore, a method for preparing polycarbosilane with high silicon hydrogen content is urgently needed.
Disclosure of Invention
The present invention is directed to solving the above problems:
in order to solve the above technical problems, the following technical solutions are now provided:
a preparation method of polycarbosilane with high silicon hydrogen content comprises the following steps:
the method comprises the following steps: obtaining a first intermediate product;
adding polycarbosilane and vinyl trichlorosilane into preparation equipment, and obtaining a first intermediate product through hydrosilylation reaction at the reaction temperature of 20 ℃ for 30 hours;
step two: reducing the obtained first intermediate product to obtain a second intermediate product;
adding lithium aluminum hydride into the first intermediate product, and reacting for 20 hours at the temperature of-20 ℃ to obtain a second intermediate product;
step three: carrying out solid-liquid separation treatment on the second intermediate product, and removing solids to obtain a third intermediate product;
step four: and replacing the first raw material in the first step with the third intermediate product, and sequentially performing the first step, the second step and the third step to obtain the polycarbosilane with high silicon-hydrogen content.
In any of the above schemes, preferably, the solid-liquid separation treatment is at least one of standing for 4-60 h, centrifugal treatment for 100-1000 s and ultrasonic treatment for 5000-10000 s.
In any of the above schemes, preferably, the preparation apparatus includes a support assembly, a reaction assembly, a temperature acquisition module and a temperature adjustment module, the support assembly is connected with the reaction assembly, the temperature acquisition module is disposed in the reaction assembly, and the temperature adjustment module is disposed on the surface of the reaction assembly.
In any of the above schemes, preferably, the support assembly includes a support plate and a transverse reinforcing rod, wherein, the transverse reinforcing rod has at least one, and both ends of the transverse reinforcing rod are connected with the support plate, and the upper end of the support plate is fixedly connected with the reaction assembly.
Preferably in any one of the above schemes, the reaction assembly includes a reaction tank body, both ends of the reaction tank body are in threaded connection with end covers, one end cover is provided with a spiral heating pipeline, a temperature adjusting module is arranged outside the end cover on one side of the spiral heating pipeline, and the other end cover is provided with a heating rod, wherein the heating rod is at least provided with a group, and the surface of the reaction tank body is provided with a feed inlet.
In any of the above schemes, preferably, the temperature acquisition module is disposed in the reaction tank body, and the temperature acquisition module acquires the temperature inside the reaction tank body in real time and sends the acquired temperature data to the temperature adjustment module.
In any of the above schemes, preferably, the temperature adjusting module is arranged on the surface of the end cover on one side of the connecting spiral heating pipeline, and the temperature adjusting module automatically adjusts the temperature of the spiral heating pipeline and the temperature of the heating rod according to a set temperature value, so that the effect of intelligently and accurately controlling the temperature is achieved.
In any of the above schemes, preferably, the temperature adjusting module adjusts and controls the temperature in a following calculation manner, specifically as follows:
obtaining collected temperature data
Wherein t isiThe method comprises the steps of acquiring a furnace temperature value for a single time, wherein n is the acquisition frequency, and t is calculated instantaneous acquired furnace temperature data; and comparing the acquired data t with a temperature control target value, and calculating a temperature deviation delta e (t), wherein delta e (t) is t-t 0.
In any of the above embodiments, preferably, the parameter control of the obtained deviation Δ e (t) is performed by:
wherein k ispIs a proportionality coefficient, kiIs an integral coefficient, kdFor the differential coefficient, it is possible to dynamically adjust the differential coefficient in accordance with the time variation and the detected deviation Δ e (t) of the real-time furnace temperatureActual temperature u (t).
In any of the above aspects, preferably, the method further comprises:
wherein T is the acquisition period, u (T)0) As an initial value of temperature, u (t)i) The temperature change condition after constant temperature and the time required for reaching the temperature are reflected for the target temperature value by adopting the calculation mode, and the accurate adjustment amplitude of the temperature can be realized, the parameter adjustment time is shortened, and the control precision is improved by adopting the adjustment and control method.
Compared with the prior art, the invention has the beneficial effects that: the spiral heating pipeline is installed in the preparation equipment, the heating rod heats materials in the reaction equipment, the spiral heating pipeline is adopted, the heating area can be increased, the arranged heating rod can heat the spare part of the spiral pipeline, the heating efficiency is improved, in addition, the heating temperature and the heating time of the spiral heating pipeline and the heating rod are adjusted through the temperature adjusting module, the heating is more reasonable, and the preparation of the materials is facilitated.
Drawings
FIG. 1 is a flow chart of temperature acquisition and regulation;
FIG. 2 is a schematic view of the overall structure of the manufacturing apparatus
FIG. 3 is a schematic view of a partial structure of a production apparatus;
FIG. 4 is a schematic view of a spiral heating pipe in the production apparatus;
FIG. 5 is a schematic view showing the structure of a heating rod in the production apparatus;
reference numerals:
1. a support assembly; 101. a support plate; 102. a transverse reinforcing rod;
2. a reaction assembly; 201. a reaction tank body; 202. an end cap; 203. a spiral heating pipe; 204. a heating rod; 205. a feed inlet; 3. a temperature acquisition module; 4. and a temperature adjusting module.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The embodiment of the invention discloses a preparation method of polycarbosilane with high silicon-hydrogen content, which is suitable for the technical field of production of polycarbosilane.
The polycarbosilane is used as a precursor of the silicon carbide ceramic material, and directly determines the performance of the silicon carbide ceramic material. Polycarbosilane is a kind of high molecular compound, its main chain is composed of silicon and carbon atoms alternatively, the silicon and carbon atoms are connected with hydrogen or organic group, and its molecular chain is linear or branched structure. Polycarbosilane is the most important compound in precursor polymers (advanced polymers) which are newly appeared in the current high-technology new materials, and is mainly used for preparing high-technology ceramic materials of silicon carbide series, wherein silicon carbide fibers are the most representative. One of the major factors in the growing interest in polycarbosilanes research over the years has been their potential for use as silicon carbide precursors, primarily as a continuous ceramic fiber source. Many novel polycarbosilanes are thereby synthesized, either directly or indirectly. However, polycarbosilanes have also become the focus of research in recent years, but this part of the research has not been associated with the development of ceramic precursors. This is because polycarbosilanes are increasingly recognized as a new class of polymers that have potential use in a wide range of applications. Although polycarbosilanes have been synthesized for a long time, only in the 70 s of the 20 th century, the professor of the northeast university of japan, now discovered a new synthesis method and, as a result, produced silicon carbide fibers that could be used for a long period of time at very high temperatures. At present, polycarbosilane is gradually used for preparing new fields of silicon carbide ceramic matrix composite materials and the like besides preparing fibers, and forms a great industry.
The spiral heating pipeline is installed in the preparation equipment, the heating rod heats materials in the reaction equipment, the spiral heating pipeline is adopted, the heating area can be increased, the arranged heating rod can heat the spare part of the spiral pipeline, the heating efficiency is improved, in addition, the heating temperature and the heating time of the spiral heating pipeline and the heating rod are adjusted through the temperature adjusting module, the heating is more reasonable, and the preparation of the materials is facilitated.
The preparation method of the polycarbosilane with high silicon hydrogen content comprises the following steps:
the method comprises the following steps: obtaining a first intermediate product;
adding polycarbosilane and vinyl trichlorosilane into preparation equipment to obtain a first intermediate product through hydrosilylation reaction at the reaction temperature of 20 ℃ for 30 hours.
Step two: reducing the obtained first intermediate product to obtain a second intermediate product;
adding lithium aluminum hydride into the first intermediate product, and reacting for 20 hours at the temperature of-20 ℃ to obtain a second intermediate product.
Step three: standing the second intermediate product for 60 hours to realize solid-liquid separation, and removing solids to prepare a third intermediate product;
step four: and replacing the first raw material in the first step with the third intermediate product, and sequentially performing the first step, the second step and the third step to obtain the polycarbosilane with high silicon-hydrogen content.
The preparation equipment comprises a supporting component 1, a reaction component 2, a temperature acquisition module 3 and a temperature adjustment module 4, wherein the supporting component 1 is connected with the reaction component 2, the temperature acquisition module 3 is arranged in the reaction component 2, and the temperature adjustment module 4 is arranged on the surface of the reaction component 2.
In the preparation method of polycarbosilane with high silicon-hydrogen content, when the preparation method is used, the support component 1 can play a role of supporting the reaction component 2, when the preparation method is used, reactants are added into the reaction tank body 201 through the feed inlet 205 for reaction, when the reactants react, the temperature acquisition module 3 arranged in the reaction tank body 201 acquires reaction temperature data in real time, and then the temperature acquisition module 3 transmits the acquired temperature data to the temperature adjustment module 4.
The supporting assembly 1 comprises supporting plates 101 and transverse reinforcing rods 102, wherein at least one transverse reinforcing rod 102 is arranged, two ends of each transverse reinforcing rod 102 are connected with the supporting plates 101, and the upper ends of the supporting plates 101 are fixedly connected with the reaction assembly 2.
In the preparation method of polycarbosilane with high silicon-hydrogen content according to the embodiment of the invention, two ends of the transverse reinforcing rod 102 are fixedly connected with the supporting plate 101 through welding, so that the supporting function of the supporting plate 101 on the reaction assembly 2 is firmer, and the connecting mode of the supporting plate 101 and the reaction assembly 2 is also welding.
The reaction assembly 2 comprises a reaction tank body 201, the two ends of the reaction tank body 201 are in threaded connection with end covers 202, one side end cover 202 is provided with a spiral heating pipeline 203, the outside of the end cover 202 provided with one side of the spiral heating pipeline 203 is provided with a temperature adjusting module 4, the other side end cover 202 is provided with a heating rod 204, wherein the heating rod 204 is at least provided with a group, and the surface of the reaction tank body 201 is provided with a feed inlet 205.
In the preparation method of polycarbosilane with high silicon-hydrogen content, when the method is used, reactants are added into the reaction tank body 201 through the feed inlet 205 for reaction, when the reactants react, the spiral heating pipeline 203 is adopted, so that the heating area can be increased, the heating time is reduced to a certain extent, the heating rod 204 is inserted between the spiral heating pipelines 203, the heating rod 204 can heat the spare part of the spiral heating pipeline 203, and the spiral heating pipeline 203 and the heating rod 204 are matched with each other, so that the heating is more uniform, the temperature in the reaction tank body 201 is uniform, and the problem of nonuniform heating of the existing equipment is solved.
The temperature acquisition module 3 is arranged in the reaction tank body 201, and the temperature acquisition module 3 acquires the temperature inside the reaction tank body 201 in real time and sends the acquired temperature data to the temperature adjustment module 4.
In the preparation method of polycarbosilane with high silicon-hydrogen content, provided by the embodiment of the invention, the temperature acquisition module 3 is arranged inside the reaction tank body 201, so that the temperature acquisition module 3 can quickly and accurately acquire real-time reaction temperature and transmit the acquired temperature data to the temperature adjustment module 4, and the temperature adjustment module 4 can conveniently adjust the temperature according to actual conditions.
The temperature adjusting module 4 is arranged on the surface of the end cover 202 on one side of the connecting spiral heating pipeline 203, and the temperature adjusting module 4 automatically adjusts the temperature of the spiral heating pipeline 203 and the temperature of the heating rod 204 according to a set temperature value, so that the effect of intelligently and accurately controlling the temperature is achieved.
In the preparation method of polycarbosilane with high silicon-hydrogen content, the temperature adjusting module 4 automatically adjusts the temperature of the spiral heating pipe 203 and the temperature of the heating rod 204 in time according to the set temperature value through the received real-time temperature data, so as to achieve the effect of intelligently and accurately controlling the temperature.
The temperature adjusting module 4 adjusts and controls the temperature in the following calculation mode, specifically as follows:
obtaining collected temperature data
Wherein t isiThe method comprises the steps of acquiring a furnace temperature value for a single time, wherein n is the acquisition frequency, and t is calculated instantaneous acquired furnace temperature data; comparing the acquired data t with a temperature control target value, and calculating a temperature deviation delta e (t), wherein delta e (t) is t-t 0; the obtained deviation Δ e (t) is subjected to parameter control by the following method:
wherein k ispIs a proportionality coefficient, kiIs an integral coefficient, kdThe actual temperature u (t) can be dynamically adjusted according to the time change and the detected deviation delta e (t) of the real-time furnace temperature as a differential coefficient;
the preparation method of polycarbosilane with high silicon-hydrogen content in the embodiment of the invention also comprises the following steps:
wherein T is the acquisition period, u (T)0) As an initial value of temperature, u (t)i) The temperature change condition after constant temperature and the time required for reaching the temperature are reflected for the target temperature value by adopting the calculation mode, and the accurate adjustment amplitude of the temperature can be realized, the parameter adjustment time is shortened, and the control precision is improved by adopting the adjustment and control method.
Although the embodiments and examples of the present invention have been described for persons skilled in the art, these embodiments and examples are provided as examples and are not intended to limit the scope of the present invention. These new embodiments can be implemented in other various ways, and various omissions, substitutions, and changes can be made without departing from the spirit of the invention. These embodiments and modifications thereof are included in the scope and gist of the invention, and are included in the invention described in the claims and the equivalent scope thereof.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A preparation method of polycarbosilane with high silicon hydrogen content is characterized by comprising the following steps:
the method comprises the following steps: obtaining a first intermediate product, adding polycarbosilane and vinyl trichlorosilane into preparation equipment, and obtaining the first intermediate product through hydrosilylation reaction at the reaction temperature of 20 ℃ for 30 hours;
step two: reducing the obtained first intermediate product to obtain a second intermediate product, adding lithium aluminum hydride into the first intermediate product, and reacting for 20 hours at the temperature of-20 ℃ to obtain the second intermediate product;
step three: carrying out solid-liquid separation treatment on the second intermediate product, and removing solids to obtain a third intermediate product;
step four: and replacing the first raw material in the first step with the third intermediate product, and sequentially performing the first step, the second step and the third step to obtain the polycarbosilane with high silicon-hydrogen content.
2. The method for preparing polycarbosilane having high silicon-hydrogen content according to claim 1, wherein the solid-liquid separation treatment is at least one of standing, centrifugal treatment or ultrasonic treatment.
3. The method for preparing polycarbosilane with high silicon-hydrogen content according to claim 2, wherein the standing time is 4-60 h, the centrifugal treatment time is 100-1000 s, and the ultrasonic treatment time is 5000-10000 s.
4. The method for preparing polycarbosilane with high silicon hydrogen content according to claim 3, wherein the preparation equipment comprises a support component (1), a reaction component (2), a temperature acquisition module (3) and a temperature adjustment module (4), the support component (1) is connected with the reaction component (2), the temperature acquisition module (3) is arranged in the reaction component (2), and the temperature adjustment module (4) is arranged on the surface of the reaction component (2).
5. The method for preparing polycarbosilane with high silicon hydrogen content according to claim 4, wherein the support assembly (1) comprises a support plate (101) and transverse reinforcing rods (102), wherein at least one transverse reinforcing rod (102) is arranged, two ends of each transverse reinforcing rod (102) are connected with the support plate (101), and the upper end of the support plate (101) is fixedly connected with the reaction assembly (2).
6. The preparation method of polycarbosilane with high silicon-hydrogen content according to claim 5, wherein the reaction assembly (2) comprises a reaction tank body (201), two ends of the reaction tank body (201) are connected with end covers (202) in a threaded manner, one end cover (202) is provided with a spiral heating pipeline (203), a temperature adjusting module (4) is arranged outside the end cover (202) on one side provided with the spiral heating pipeline (203), the other end cover (202) is provided with heating rods (204), wherein at least one group of heating rods (204) is arranged, and a charging opening (205) is arranged on the surface of the reaction tank body (201).
7. The preparation method of polycarbosilane with high silicon-hydrogen content according to claim 6, wherein the temperature acquisition module (3) is arranged in the reaction tank body (201), and the temperature acquisition module (3) acquires the temperature inside the reaction tank body (201) in real time and sends the acquired temperature data to the temperature adjustment module (4).
8. The method for preparing polycarbosilane with high silicon-hydrogen content according to claim 7, wherein the temperature adjusting module (4) is arranged on the surface of the end cover (202) connected with one side of the spiral heating pipeline (203), and the temperature adjusting module (4) automatically adjusts the temperature of the spiral heating pipeline (203) and the temperature of the heating rod (204) according to a set temperature value.
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