CN113214488B - Preparation method of polycarbosilane - Google Patents
Preparation method of polycarbosilane Download PDFInfo
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- CN113214488B CN113214488B CN202110439852.0A CN202110439852A CN113214488B CN 113214488 B CN113214488 B CN 113214488B CN 202110439852 A CN202110439852 A CN 202110439852A CN 113214488 B CN113214488 B CN 113214488B
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- polycarbosilane
- blanking
- box body
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- solid
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C4/00—Crushing or disintegrating by roller mills
- B02C4/02—Crushing or disintegrating by roller mills with two or more rollers
- B02C4/08—Crushing or disintegrating by roller mills with two or more rollers with co-operating corrugated or toothed crushing-rollers
Abstract
The invention provides a preparation method of polycarbosilane, which comprises the following steps: filling inert gas into a reaction kettle, adding metal magnesium, an organic solvent and iodine, dropwise adding chloromethyl chlorosilane into the reaction kettle, and reacting for 3 hours at 25 ℃ to generate a polycarbosilane intermediate; adding a reducing agent, preferably sodium hydride, into the reaction kettle, and reacting for 5 hours at 25 ℃ to generate milky polycarbosilane similar to rubber solid; the polycarbosilane rubber solid generated is subjected to liquid separation, filtration, organic phase washing and drying, the polycarbosilane solid after being heated is discharged after being crushed by the blanking device, and the polycarbosilane solid generated is crushed and guided by the blanking device, so that the problem that a blanking assembly is easy to block in the prior art is solved, the blanking speed can be adjusted according to the production efficiency of material processing equipment, and the reasonable state is achieved.
Description
Technical Field
The invention relates to a preparation method of an organic silicon polymer, in particular to a preparation method of polycarbosilane.
Background
Polycarbosilane (PCS) is an organic precursor that is widely used in the preparation of specialty fibers (e.g., sic fibers) and complex phase ceramics, where sic fibers have the advantages of high strength and hardness, high thermal and oxidation stability, low coefficient of thermal expansion, and low density, and the high temperature stability (chemical, microstructural, and mechanical stability) of sic fibers in inert and oxidizing environments, coupled with their excellent mechanical properties (high fracture strength, stiffness, low creep rate, etc.) make sic fibers the best alternative for producing structural composites with wide applications ranging from heat exchangers and hot gas filters to electrical power production and aerospace mechanical parts, among others.
At present, the sic material directly prepared from polycarbosilane has the defects of insufficient density, low performance, large size of high-temperature grains, reduction of product performance and the like, so that the prepared polycarbosilane material needs to be crushed during blanking, but crushed small polycarbosilane particles are blocked, so that blanking is not smooth, and improvement is urgently needed.
Disclosure of Invention
The invention aims to provide a method for preparing polycarbosilane, which aims to solve the problems in the background technology.
The embodiment of the invention discloses a preparation method of polycarbosilane, which comprises the following steps:
dissolving: filling inert gas into a reaction kettle, wherein the inert gas is preferably nitrogen, adding metal magnesium, an organic solvent and iodine, the organic solvent is preferably benzotrifluoride, dropwise adding chloromethyl chlorosilane into the reaction kettle, and reacting for 3 hours at 25 ℃ to generate a polycarbosilane intermediate;
adding a reducing agent: adding a reducing agent, preferably sodium hydride, into the reaction kettle, and reacting for 5 hours at 25 ℃ to generate milky polycarbosilane similar to rubber solid;
blanking: and (3) carrying out liquid separation, filtration, organic phase washing and drying on the generated polycarbosilane rubber solid, then heating at 200 ℃ for 3 hours to obtain a polycarbosilane solid, and discharging the heated polycarbosilane solid after crushing by a discharging device.
Preferably, the blanking device includes: the material guide assembly is arranged on the support assembly and is used for crushing polycarbosilane solid; and the discharging assembly is connected with the supporting assembly through a spring.
Preferably, the supporting component comprises a supporting frame and a first fixing block, the first fixing block is fixedly mounted on the supporting frame on two sides, and a spring is mounted on one side, close to the discharging component, of the first fixing block.
Preferably, the guide subassembly includes box, driving motor and unloading roller, box fixed mounting is in one side of support frame, unloading roller both sides fixed mounting has the axis of rotation, the axis of rotation rotates to be installed on the box, parallel arrangement has a pair of unloading roller in the box, the one end fixed mounting that the axis of rotation is located the box outside has driven pulleys, the locating piece is installed to the one side of keeping away from driven pulleys outside the box, axis of rotation and locating piece normal running fit, one side that the box was kept away from to the support frame installs driving motor, driving motor's output fixed mounting has driving pulley, driving pulley passes through the drive belt cooperation with driven pulleys.
Preferably, the outer side of the blanking roller is uniformly provided with protrusions which are used for increasing the friction force between the polycarbosilane solid and the blanking roller.
Preferably, the top of the box body is fixedly provided with a feeding hopper, the feeding hopper is communicated with the box body, and the bottom of the box body is connected with a blanking hopper.
Preferably, it includes mounting bracket, vibrating motor and row flitch to arrange the material subassembly, mounting bracket both sides fixed mounting has the second fixed block, second fixed block and spring coupling, mounting bracket bottom and side fixed mounting have row flitch, mounting bracket bottom fixed mounting has vibrating motor, row flitch sets up downwards for the support frame slope.
Preferably, a control module is installed on one side, close to the driving motor, of the support frame, and comprises a collecting module, an adjusting module and a temperature monitoring module, wherein the temperature monitoring module is used for collecting the temperatures of the driving motor and the vibrating motor in real time, and when the temperatures of the driving motor and the vibrating motor reach preset temperatures, the temperature monitoring module sends information to the adjusting module in time or transmits the information to the mobile terminal through wireless signals; the collecting module is used for collecting the feeding and the conditions of materials in the reaction kettle in real time and sending collected information to the adjusting module, and the adjusting module adjusts the driving power and the vibration power of the driving motor and the vibration motor according to the received information.
Preferably, the specific optimization method for the optimization work of the adjustment module is as follows: adjusting a parameter K of a moduleP And KIIs most preferred
Design value of
And calculating the running speeds of the driving motor and the vibration motor according to the parameters of the adjusting module, so as to adjust the speeds of the driving motor and the vibration motor.
Compared with the prior art, the feeding device is used for crushing and guiding generated polycarbosilane solids, the problem that a feeding assembly is easy to block in the prior art is solved, and the feeding speed can be adjusted according to the production efficiency of material processing equipment, so that the feeding device reaches a reasonable state.
Drawings
FIG. 1 is a schematic diagram of a process for preparing polycarbosilane according to the present invention.
FIG. 2 is a schematic perspective view of a blanking device in the method for preparing polycarbosilane of the present invention.
FIG. 3 is a bottom view of a blanking device in the method for preparing polycarbosilane of the present invention.
FIG. 4 is a schematic view of a material guiding assembly in a method for preparing polycarbosilane.
FIG. 5 is a schematic view of the interior of a tank in the process for preparing polycarbosilane according to the present invention.
FIG. 6 is a schematic diagram of a control module in the method for preparing polycarbosilane.
Reference numerals:
1-a support assembly, 11-a support frame, 12-a first fixed block, 2-a material guide assembly, 21-a box body, 22-a driving motor, 23-a blanking roller, 24-a driven belt wheel, 25-a rotating shaft, 26-a driving belt, 27-a blanking hopper, 28-a feeding hopper, 29-a positioning block, 3-a material discharge assembly, 31-a mounting frame, 32-a second fixed block, 33-a vibrating motor, 34-a material discharge plate, 4-a spring, 5-a control module, 51-an acquisition module, 52-an adjustment module and 53-a temperature monitoring module.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the description of the present invention, it should be noted that the terms "inside", "outside", "upper", "lower", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or orientations or positional relationships that the products of the present invention conventionally use, which are merely for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, or be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.
Examples
As shown in fig. 1, a method for preparing polycarbosilane is characterized in that chloromethyl chlorosilane is used as a raw material, and the method comprises the following steps:
dissolving: filling inert gas into a reaction kettle, wherein the inert gas can reduce the interference of oxygen and other gases in the air to the reaction process, the inert gas is preferably nitrogen, adding metal magnesium, an organic solvent and iodine, the organic solvent is preferably trifluorotoluene, dropwise adding chloromethyl chlorosilane into the reaction kettle, and reacting for 3 hours at 25 ℃ to generate a polycarbosilane intermediate;
adding a reducing agent: adding a reducing agent, preferably sodium hydride, into the reaction kettle, and reacting for 5 hours at 25 ℃ to generate milky polycarbosilane similar to rubber solid; after the polycarbosilane which generates rubber solid is generated, dilute hydrochloric acid is dripped into the reaction kettle for quenching reaction.
Blanking: and (3) carrying out liquid separation, filtration, organic phase washing and drying on the generated polycarbosilane rubber solid, then heating at 200 ℃ for 3 hours to obtain a polycarbosilane solid, and discharging the heated polycarbosilane solid after crushing by a discharging device.
As shown in fig. 2 and 3, the blanking apparatus includes: the material guide assembly 2 is arranged on the support assembly 1 and is used for crushing polycarbosilane solid, so that the situation that the size of particles of discharged polycarbosilane is different, the compactness and the performance of a sic material are influenced by overlarge polycarbosilane solid, and the performance of a product is greatly reduced by the size of high-temperature grains is avoided; and the discharging component 3 is connected with the supporting component 1 through a spring 4, the discharging component 3 vibrates to discharge polycarbosilane particles discharged by the material guiding component 2, the discharging component shakes under the elastic force action of the spring 4, polycarbosilane materials can be discharged quickly, and the blockage of polycarbosilane in the discharging device can be prevented.
Support assembly 1 includes support frame 11 and first fixed block 12, both sides fixed mounting has first fixed block 12 on support frame 11, and support frame 11 one side interval is provided with two first fixed blocks 12, first fixed block 12 is close to one side of arranging material subassembly 3 and installs spring 4, and spring 4 can provide ascending pulling force to arranging the material subassembly, and support frame 11 can support and fix guide subassembly 2 and row material subassembly 3, guarantees that polycarbosilane does not take place to rock on a large scale and the displacement at unloading in-process unloader, effectively guarantees the stationarity of unloading process.
Be provided with the guide bar in the spring 4, the guide bar with limiting plate sliding fit on the first fixed block 12 can prevent that row's material subassembly 3 from dragging spring 4 downwards, and too big pulling force can make spring 4 lose elastic tension, and the guide bar can protect spring 4 with limiting plate sliding fit.
As shown in fig. 2, 4 and 5, the material guiding assembly 2 includes a box 21, a driving motor 22 and a discharging roller 23, the box 21 is fixedly installed at one side of the supporting frame 11, two sides of the discharging roller 23 are fixedly installed with rotating shafts 25, the rotating shafts 25 are coaxial with the discharging roller 23, the rotating shafts 25 are rotatably installed on the box 21, a pair of discharging rollers 23 are arranged in the box 21 in parallel, one end of the rotating shaft 25 located at the outer side of the box 21 is fixedly installed with a driven pulley 24, one side of the box 21 away from the driven pulley 24 is installed with a positioning block 29, the rotating shafts 25 are rotatably matched with the positioning block 29, the friction and the extrusion between the rotating shafts and the box 21 can be reduced due to the rotating matching of the rotating shafts 25 and the positioning block 29, the discharging roller 23 can be ensured to be kept parallel in the box 21, the driving motor 22 is installed at one side of the supporting frame 11 away from the box 21, the output end fixed mounting of driving motor has the driving pulley, driving pulley and driven pulley 24 pass through drive belt 26 transmission fit, and driven pulley 24 can drive axis of rotation 25 and rotate, drives a blanking roller 23 and at the internal rotation of box 21, can make two blanking roller subtend rolls in the box 21 under the effect of frictional force, can extrude the breakage to the polycarbosilane between the blanking roller 23, and the interval between the blanking roller 23 is the less, and the polycarbosilane granule after the breakage is the less.
During operation, driving motor 22 drives driving pulley and driven pulley 24 transmission coordination, driven pulley 24 drives axis of rotation 25 and rotates around locating piece 29, axis of rotation 25 drives unloading roller 23 and rotates, under the effect of frictional force, the polycarbosilane solid between two unloading rollers 23 is broken under the rotation effect of unloading roller 23, the polycarbosilane of tiny granule falls down from between two unloading rollers 23, make unpowered drive's unloading roller 23 for another unloading roller 23 opposite direction rotation when the polycarbosilane solid falls down, the crushing speed of polycarbosilane can be quickened.
As shown in fig. 4 and 5, the outer side of the discharging roller 23 is uniformly provided with protrusions, the protrusions can increase the friction force between the polycarbosilane solid and the discharging roller 23, the crushing discharging effect can be increased, and the opposite rolling discharging roller 23 can be matched with the protrusions to rapidly crush the polycarbosilane solid above the discharging roller 23 and guide the polycarbosilane solid downwards.
The top fixed mounting of box 21 has loading hopper 28, loading hopper 28 and box 21 intercommunication, loading hopper 28 with between the direct leading-in unloading roller 23 of polycarbosilane solid, can carry out quick breakage to polycarbosilane solid under the effect of pivoted unloading roller 23, the bottom of box 21 is connected with blanking fill 27, and blanking fill 27 can concentrate the direction with the polycarbosilane granule of smashing the whereabouts through unloading roller 23 for polycarbosilane granule concentrates and arranges to in arranging material subassembly 3.
As shown in fig. 2 and 3, the discharging assembly 3 includes a mounting frame 31, a vibrating motor 33 and a discharging plate 34, wherein second fixing blocks 32 are fixedly mounted on two sides of the mounting frame 31, the second fixing blocks 32 are connected with springs 4, the discharging plate 34 is fixedly mounted on the upper bottom and the side surface of the mounting frame 31, the vibrating motor 33 is fixedly mounted at the bottom of the mounting frame 31, the vibrating motor 33 can vibrate the mounting frame 31 during operation, the continuous vibration of the mounting frame 31 can enable polycarbosilane particles on the discharging plate 34 to fall rapidly, the springs 4 on one side close to the vibrating motor 33 are longer than the other springs 4 on the same side, so that the discharging plate 34 at the bottom of the mounting frame 31 is arranged obliquely downwards relative to the mounting frame 11, the discharge of the polycarbosilane particle materials is facilitated, the vibrating motor 33 drives the mounting frame 31 to vibrate and simultaneously enable the springs 4 between the mounting frame 31 and the supporting frame 11 to stretch, the blanking speed can be accelerated.
During operation, the little granule of polycarbosilane that falls from blanking hopper 27 falls on blanking plate 34, and vibrating motor 33 vibrates mounting bracket 31, and mounting bracket 31 drives blanking plate 34 and vibrates, and the polycarbosilane granule rolls down fast on the blanking plate 34 that the slope set up, and the amplitude that the blanking plate rocked can be increased to spring 4 when mounting bracket 31 and blanking plate 34 vibrate, through the reducible vibrating motor 33 vibration of the effect of spring 4 to the influence of guide subassembly 2.
As shown in fig. 2 and 6, a control module 5 is installed on one side of the support frame 11 close to the driving motor, the control module includes a collecting module 51, an adjusting module 52 and a temperature monitoring module 53, the temperature monitoring module 53 is used for collecting temperatures of the driving motor 22 and the vibration motor 33 in real time, and when the temperatures of the driving motor 22 and the vibration motor 33 reach preset temperatures, the temperature monitoring module 53 sends information to the adjusting module 52 in time or transmits the information to the mobile terminal through wireless signals; the acquisition module 51 is used for acquiring the conditions of materials in the feeding and reaction kettle in real time and sending acquired information to the adjustment module 52, and the adjustment module 52 adjusts the driving power and the vibration power of the driving motor 22 and the vibration motor 33 according to the received information and adjusts the rotation speed, so that the effect of optimizing the work is achieved.
During operation, temperature monitoring module 53 carries out real-time supervision to the temperature of driving motor 22 and vibrating motor 33 and gives adjustment module 52 with information transmission, adjustment module 52 regulates and control driving motor 22 and vibrating motor 33's slew velocity according to the temperature range of setting for, can guarantee to guarantee machining efficiency in the safety range, collection module 51 carries out information acquisition to material in reation kettle and the loading hopper 28 and sends for adjustment module 52, adjustment module 52 adjusts the slew velocity of driving motor 22 and vibrating motor 33 according to the information of material, can guarantee that the material does not pile up in unloader, temperature monitoring module 53 sends temperature information for mobile terminal, can adjust the material volume in the reation kettle, can guarantee that each link of preparation process can not take place overload operation, guarantee the long-term steady operation of unloader.
The specific optimization method for the optimization work of the adjustment module 52 is as follows: translating the tuning problem of the tuning module 52 parameters into solving KleAnd KPeThe maximum value of the ratio;
thus, the calculation formula is:
order to
，
And
is provided with
，
Thus, therefore, it is
In that
Interval of planar values
There is a maximum value that can be passed
Obtaining, taking reciprocal of the obtained alpha and beta values to obtain the optimal value p of the closed loop pole1=p2=p3=popt=0.5874, and K is obtainedleAnd KPeOf optimum value, i.e.
Wherein p is1、p2And p3Respectively, the closed loop pole of the adjusting module and the parameter K of the adjusting modulePeAnd KIeThe optimum design values for (c) are:
therefore, the running speeds of the driving motor 22 and the vibrating motor 33 can be calculated according to the parameters of the adjusting module, the speeds of the driving motor 22 and the vibrating motor 33 can be adjusted, the working powers of the driving motor 22 and the vibrating motor 33 can be adjusted according to the speed of preparing polycarbosilane, no material accumulation in the blanking device can be ensured, the preparation speed can be ensured, the working temperatures of the driving motor 22 and the vibrating motor 33 can be ensured within a safety range, and the preparation effect can be further optimized.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.
The standard parts used in the invention can be purchased from the market, the special-shaped parts can be customized according to the description of the specification and the accompanying drawings, the specific connection mode of each part adopts conventional means such as bolts, rivets, welding and the like mature in the prior art, the machines, the parts and equipment adopt conventional models in the prior art, and the circuit connection adopts the conventional connection mode in the prior art, so that the detailed description is omitted.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
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 (1)
1. A method for preparing polycarbosilane is characterized in that chloromethyl chlorosilane is used as a raw material, and the method comprises the following steps
The method comprises the following steps:
dissolving: filling inert gas into a reaction kettle, adding metal magnesium, an organic solvent and iodine, dropwise adding chloromethyl chlorosilane into the reaction kettle, and reacting for 3 hours at 25 ℃ to generate a polycarbosilane intermediate;
adding a reducing agent: adding a reducing agent into the reaction kettle, and reacting for 5 hours at 25 ℃ to generate milky polycarbosilane similar to rubber solid;
blanking: separating, filtering, washing and drying the generated polycarbosilane rubber solid, heating at 200 ℃ for 3 hours to obtain polycarbosilane solid, and crushing the heated polycarbosilane solid by a blanking device and then discharging; the blanking device comprises:
the material guide assembly is arranged on the support assembly and is used for crushing polycarbosilane solid; and
the discharging component is connected with the supporting component through a spring; the supporting assembly comprises a supporting frame and first fixing blocks, the first fixing blocks are fixedly mounted on two sides of the supporting frame, and springs are mounted on one sides, close to the discharging assembly, of the first fixing blocks; the material guide assembly comprises a box body, a driving motor and a blanking roller, the box body is fixedly installed on one side of a support frame, rotating shafts are fixedly installed on two sides of the blanking roller, the rotating shafts are rotatably installed on the box body, a pair of blanking rollers are arranged in parallel in the box body, a driven belt wheel is fixedly installed at one end, located on the outer side of the box body, of each rotating shaft, a positioning block is installed on one side, away from the driven belt wheel, outside the box body, of each rotating shaft, the rotating shafts are in rotating fit with the positioning blocks, the driving motor is installed on one side, away from the box body, of the support frame, the output end of the driving motor is fixedly provided with a driving belt wheel, and the driving belt wheels are in transmission fit with the driven belt wheels through a transmission belt; bulges are uniformly arranged on the outer side of the blanking roller and used for increasing the friction force between polycarbosilane solid and the blanking roller; the top of the box body is fixedly provided with a feeding hopper, the feeding hopper is communicated with the box body, and the bottom of the box body is connected with a blanking hopper; the discharging assembly comprises a mounting frame, a vibrating motor and a discharging plate, wherein second fixed blocks are fixedly mounted on two sides of the mounting frame and connected with springs, the discharging plate is fixedly mounted at the bottom and on the side face of the mounting frame, the vibrating motor is fixedly mounted at the bottom of the mounting frame, and the discharging plate is obliquely arranged downwards relative to the supporting frame; the supporting frame is provided with a control module on one side close to the driving motor, the control module comprises a collecting module, an adjusting module and a temperature monitoring module, the temperature monitoring module is used for collecting the temperatures of the driving motor and the vibrating motor in real time, and when the temperatures of the driving motor and the vibrating motor reach preset temperatures, the temperature monitoring module sends information to the adjusting module in time or transmits the information to the mobile terminal through wireless signals; the collecting module is used for collecting the feeding and the conditions of materials in the reaction kettle in real time and sending collected information to the adjusting module, and the adjusting module adjusts the driving power and the vibration power of the driving motor and the vibration motor according to the received information.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002164A (en) * | 2010-09-14 | 2011-04-06 | 张卫中 | Method for synthesizing ceramic precursor polycarbosilane |
| CN106674528A (en) * | 2016-11-15 | 2017-05-17 | 杭州师范大学 | Preparation method of polycarbosilane |
| CN112062967A (en) * | 2020-08-05 | 2020-12-11 | 福建立亚化学有限公司 | Preparation method of polycarbosilane ceramic precursor material |
Family Cites Families (1)
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| DE102004042531A1 (en) * | 2004-05-03 | 2005-12-15 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Polysilane-polycarbosilane copolymer solutions and low-oxygen ceramic shaped bodies produced therefrom with compositions close to SiC |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002164A (en) * | 2010-09-14 | 2011-04-06 | 张卫中 | Method for synthesizing ceramic precursor polycarbosilane |
| CN106674528A (en) * | 2016-11-15 | 2017-05-17 | 杭州师范大学 | Preparation method of polycarbosilane |
| CN112062967A (en) * | 2020-08-05 | 2020-12-11 | 福建立亚化学有限公司 | Preparation method of polycarbosilane ceramic precursor material |
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