CN113248720A - Spinnable polycarbosilane and preparation method thereof - Google Patents
Spinnable polycarbosilane and preparation method thereof Download PDFInfo
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- CN113248720A CN113248720A CN202110475414.XA CN202110475414A CN113248720A CN 113248720 A CN113248720 A CN 113248720A CN 202110475414 A CN202110475414 A CN 202110475414A CN 113248720 A CN113248720 A CN 113248720A
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- 229920003257 polycarbosilane Polymers 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 93
- 238000003756 stirring Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 12
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 12
- 238000005336 cracking Methods 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920000555 poly(dimethylsilanediyl) polymer Polymers 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000001723 curing Methods 0.000 claims abstract description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 4
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 4
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 4
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims abstract description 4
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 239000008213 purified water Substances 0.000 claims abstract description 4
- 230000000630 rising effect Effects 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 28
- 230000008569 process Effects 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 claims description 2
- 230000003014 reinforcing effect Effects 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008707 rearrangement Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/11—Stirrers characterised by the configuration of the stirrers
- B01F27/19—Stirrers with two or more mixing elements mounted in sequence on the same axis
- B01F27/191—Stirrers with two or more mixing elements mounted in sequence on the same axis with similar elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/211—Measuring of the operational parameters
- B01F35/2113—Pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/2201—Control or regulation characterised by the type of control technique used
- B01F35/2206—Use of stored recipes for controlling the computer programs, e.g. for manipulation, handling, production or composition in mixing plants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/45—Closures or doors specially adapted for mixing receptacles; Operating mechanisms therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/2805—Mixing plastics, polymer material ingredients, monomers or oligomers
Abstract
The invention relates to a spinnable polycarbosilane and a preparation method thereof, wherein the method comprises the following steps: under the protection of nitrogen, adding an organic solvent and alkali metal into a mixing device for mixing, heating until the alkali metal is molten, adding dimethyldichlorosilane into the molten alkali metal for reaction, and stirring and curing at a high temperature to obtain a reactant; respectively adding purified water and absolute ethyl alcohol into the obtained mixture for cleaning for multiple times to obtain pure polydimethylsilane; reacting for 1-6 hours at the temperature of 100 ℃ and 150 ℃ to perform polycondensation reaction to obtain polydimethylsilane to be treated; and (3) performing pressure maintaining, vacuum pumping, heat preservation, temperature rising and cracking on the vacuum-dried polydimethylsiloxane to obtain a liquid low-molecular cracking product. The invention has excellent fluidity, reduces the branching degree of polycarbosilane, enables the product to have better linear structure, has high fluidity and obviously improves the spinnability.
Description
Technical Field
The invention relates to the technical field of polycarbosilane, in particular to spinnable polycarbosilane and a preparation method thereof.
Background
Polycarbosilane (PCS) is a common, widely used precursor for silicon carbide ceramics. PCS was prepared from Polydimethylsilane (PDMS) by a high temperature rearrangement above 470 ℃. The high-pressure high-temperature rearrangement has higher requirements on equipment, and the normal-pressure high-temperature rearrangement has low synthesis yield and longer production period, thereby leading to higher production cost. Meanwhile, the C/Si ratio in the molecular structure of PCS is 2, the C/Si ratio in the pyrolysis product is about 1.4, and the PCS is rich in carbon, so that the high-temperature oxidation resistance of the PCS is influenced. Hyperbranched polycarbosilane (HBPCS) is widely concerned by researchers due to the characteristics of low viscosity, high ceramic yield, designability of molecular structure and performance and the like, but the commercial application of the material is limited by the high cost.
The existing methods for preparing the spinnable polycarbosilane have the problems of insufficient storage stability or unobvious comprehensive price ratio, and commercial production and application are not realized, so that the improvement is urgently needed.
Disclosure of Invention
The invention aims to provide a preparation method of spinnable polycarbosilane, which has excellent fluidity, reduces the branching degree of polycarbosilane, enables the product to have a better linear structure, has high fluidity and obviously improves the spinnability, and can solve the problems in the background technology.
In order to solve the technical problems, the technical scheme of the preparation method of the spinnable polycarbosilane provided by the invention is as follows:
in a first aspect, the embodiment of the invention discloses a preparation method of spinnable polycarbosilane, which comprises the following steps:
under the protection of nitrogen, adding an organic solvent and alkali metal into a mixing device for mixing, heating until the alkali metal is molten, adding dimethyldichlorosilane into the molten alkali metal for reaction, and stirring and curing at a high temperature to obtain a reactant;
respectively adding purified water and absolute ethyl alcohol into the obtained mixture for cleaning for multiple times to obtain pure polydimethylsilane;
reacting for 1-6 hours at the temperature of 100 ℃ and 150 ℃ to perform polycondensation reaction to obtain polydimethylsilane to be treated;
performing pressure maintaining, vacuum pumping, heat preservation, temperature rising and cracking on the vacuum-dried polydimethylsiloxane to obtain a liquid low-molecular cracking product;
and synthesizing and desolventizing the obtained liquid low-molecular cracking product at high temperature and high pressure to obtain the polycarbosilane.
It is preferred in any preceding scheme, mixing apparatus is including holding subassembly, drive assembly, PLC control module group and hybrid module, drive assembly set up in hold subassembly upper portion, hybrid module set up in hold in the subassembly, just the drive assembly output with the hybrid module input is connected, in order to realize driving hybrid module is in hold the subassembly in mix the stirring to the material, PLC control module group set up in hold on the subassembly, just PLC control module group with drive assembly connects, in order to realize control drive assembly opens or closes.
It is preferred in any one of the above-mentioned schemes, hold the subassembly and include blending tank, lid, supporting leg, water inlet and ejection of compact pipeline, the supporting leg with the blending tank is connected, the blending tank top with the lid is connected, the exhaust duct has on the lid, ejection of compact pipeline one end with the bottom intercommunication of blending tank, the water inlet set up in blending tank one side.
It is preferable in any one of the above schemes that drive assembly includes driving motor, drive shaft and mount pad, the mount pad set up in on the lid, driving motor set up in on the mount pad, the driving motor output with drive shaft one end is connected, the drive shaft other end extends to in the hybrid tank, and with the hybrid assembly connects, the PLC control module group with driving motor connects.
In any one of the above schemes, preferably, the mixing assembly includes a stirring shaft and a stirring blade, one end of the stirring shaft is connected with the other end of the driving shaft, and the stirring blade is disposed on the stirring shaft.
In any one of the above schemes, preferably, the stirring blades are provided in plurality and respectively distributed on the stirring shaft.
In any of the above schemes, preferably, when assembling, the mixing tank is welded with the supporting legs or connected with the supporting legs through screws, the top of the mixing tank is movably connected with the cover body through hinges so as to realize the convenient opening or closing of the cover body, wherein the supporting legs are provided with a plurality of supporting legs and uniformly distributed around the mixing tank, so as to realize the function of supporting the mixing tank, wherein the water inlet is arranged at one side of the mixing tank, so as to realize the communication between the mixing tank and the water inlet, thereby facilitating the water to be discharged into the mixing tank, one end of the discharge pipeline is communicated with the mixing tank, so as to play a role of conveniently discharging materials, when in use, some liquid water is discharged into the mixing tank through the water inlet, then the driving assembly is opened to drive the mixing assembly to work, so that the mixing assembly can mix and stir the materials in the mixing tank, is convenient to use.
It is preferred in any one of the above-mentioned schemes, the PLC control module group includes material collection module, regulation and control module, amplifies module, controller and torque speed sensor, wherein, material collection module is used for gathering the inside material mixing information of blending tank constantly to the material information data that will gather transmits to through amplifying the module the controller, the controller is according to material mixing situation, adjustment driving motor's functioning speed, torque speed sensor gathers constantly the rotational speed of (mixing) shaft, and with the speed data that will gather transmit to through amplifying the module the controller, controller adjustment rotational speed's control offset has constituted the single closed loop control to rotational speed.
In any of the above schemes, preferably, the PLC control module further includes a valve controller and a pressure sensor, the valve controller is disposed on a discharge pipeline and connected with the controller, the pressure sensor is disposed on the exhaust pipeline and connected with the controller.
In any of the above schemes, preferably, the calculation method of the single closed-loop control is as follows:
wherein G isC(s) is the controller transfer function; g2(s) is the amplifier transfer function; h3(s) is a torque revolution speed sensor, H3(s)＝Km2；Km2Is the torque speed sensor gain.
In any of the above solutions, it is preferred that the amplifier transfer function
I is the amplifier output current; u is the amplifier operating voltage.
In a second aspect, the spinnable polycarbosilane is obtained by the preparation method of the spinnable polycarbosilane.
Compared with the prior art, the invention has the beneficial effects that:
1. the product has good fluidity, reduces the branching degree of polycarbosilane, has better linear structure, high fluidity and obviously improved spinnability.
2. Through adopting PLC control module group, can conveniently control the mixture of material, can improve work efficiency, help making its mixture more even.
Drawings
The drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification.
FIG. 1 is a perspective view of a mixing apparatus for a process for producing a spinnable polycarbosilane in accordance with the present invention.
FIG. 2 is another perspective view of a mixing apparatus for the process for producing a spinnable polycarbosilane in accordance with the present invention.
FIG. 3 is a schematic view showing the internal structure of a mixing apparatus for a method of preparing a spinnable polycarbosilane according to the present invention.
The reference numbers in the figures illustrate:
1. a containing assembly; 11. a mixing tank; 12. a cover body; 121. an exhaust duct; 13. supporting legs; 14. a water inlet; 15. a discharge pipeline; 2. a drive assembly; 21. a drive motor; 22. a drive shaft; 23. a mounting seat; 3. a PLC control module; 4. a mixing assembly; 41. a stirring shaft; 42. a stirring blade.
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.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
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.
For better understanding of the above technical solutions, the technical solutions of the present invention will be described in detail below with reference to the drawings and the detailed description of the present invention.
Example 1:
in a first aspect, the embodiment of the invention discloses a preparation method of spinnable polycarbosilane, which comprises the following steps:
under the protection of nitrogen, adding an organic solvent and alkali metal into a mixing device for mixing, heating until the alkali metal is molten, adding dimethyldichlorosilane into the molten alkali metal for reaction, stirring and curing at high temperature to obtain a reactant, and under the protection of nitrogen, the reactant can be more stable in reaction and is not easy to react with other substances, so that the problem that air is not molten and has high oxygen content is avoided;
respectively adding purified water and absolute ethyl alcohol into the obtained mixture for cleaning for multiple times to obtain pure polydimethylsilane;
reacting for 1-6 hours at the temperature of 100 ℃ and 150 ℃ to perform polycondensation reaction to obtain polydimethylsilane to be treated;
performing pressure maintaining, vacuum pumping, heat preservation, temperature rising and cracking on the vacuum-dried polydimethylsiloxane to obtain a liquid low-molecular cracking product;
and synthesizing and desolventizing the obtained liquid low-molecular cracking product at high temperature and high pressure to obtain the polycarbosilane.
Referring to fig. 1 to 3, in the preparation method of the spinnable polycarbosilane according to the embodiment of the present invention, the mixing apparatus includes a holding component 1, a driving component 2, a PLC control module 3, and a mixing component 4, the driving component 2 is disposed on the upper portion of the holding component 1, the mixing component 4 is disposed in the holding component 1, an output end of the driving component 2 is connected to an input end of the mixing component 4, so as to drive the mixing component 4 to mix and stir the materials in the holding component 1, the PLC control module 3 is disposed on the holding component 1, and the PLC control module 3 is connected to the driving component 2, so as to control the opening or closing of the driving component 2.
When using, hold the interior material that is used for holding of subassembly 1, then open drive assembly 2, drive assembly 2 drives mix subassembly 4 begins work, then mixes the material that holds in the subassembly 1, wherein, PLC control module 3 is used for control drive assembly 2 open and close, play the effect of convenient mixture.
Referring to fig. 1 to 3, in the preparation method of the spinnable polycarbosilane according to the embodiment of the present invention, the holding assembly 1 includes a mixing tank 11, a cover 12, support legs 13, a water inlet 14, and a discharge pipe 15, the support legs 13 are connected to the mixing tank 11, the top of the mixing tank 11 is connected to the cover 12, the cover 12 has an exhaust pipe 121, one end of the discharge pipe 15 is communicated with the bottom of the mixing tank 11, and the water inlet 14 is disposed at one side of the mixing tank 11.
When the device is assembled, the mixing tank 11 is welded with the supporting legs 13 or connected by screws, the top of the mixing tank 11 is movably connected with the cover body 12 by hinges to realize that the cover body 12 can be conveniently opened or closed, wherein the supporting legs 13 are provided with a plurality of supporting legs and uniformly distributed around the mixing tank 11 to realize the function of supporting the mixing tank 11, wherein the water inlet 14 is arranged at one side of the mixing tank 11 to realize the communication between the mixing tank 11 and the water inlet 14 so as to conveniently discharge water into the mixing tank 11, one end of the discharging pipeline 15 is communicated with the mixing tank 11 to play a role of conveniently discharging materials, when in use, some liquid water is discharged into the mixing tank 11 through the water inlet 14, then the driving assembly 2 is opened to drive the mixing assembly 4 to work, so that the mixing assembly 4 can mix and stir materials inside the mixing tank 11, is convenient to use.
Wherein, in order to increase the structural strength of the mixing tank 11, a plurality of reinforcing parts 16 can be arranged outside the mixing tank 11, wherein the reinforcing parts 16 can be in the shape of a bar, the reinforcing parts 16 are provided with a plurality of reinforcing parts and uniformly distributed outside the mixing tank 11, wherein, in order to further facilitate the heat dissipation of the mixing tank 11 during the reaction, and in order to save heat sources, the middle part of the reinforcing part 16 can be hollowed to form a bar body with a hollow structure, a water inlet is arranged above the bar body, and a water outlet is arranged below the bar body, so that on one hand, the water inside the bar body can be heated, on the other hand, the inside of the mixing tank 11 can be conveniently cooled, the use is convenient, in order to integrate a plurality of bar bodies, the water inside among the bar bodies can mutually circulate, the plurality of bar bodies can be connected in series or in parallel, therefore, the water bodies in the water-cooling water heater can circulate mutually and can be circulated mutually, and the local overhigh temperature can be avoided.
Referring to fig. 1 to 3, in the preparation method of the spinnable polycarbosilane according to the embodiment of the present invention, the driving assembly 2 includes a driving motor 21, a driving shaft 22 and a mounting seat 23, the mounting seat 23 is disposed on the cover 12, the driving motor 21 is disposed on the mounting seat 23, an output end of the driving motor 21 is connected to one end of the driving shaft 22, the other end of the driving shaft 22 extends into the mixing tank 11 and is connected to the mixing assembly 4, and the PLC control module 3 is connected to the driving motor 21.
When the equipment, mount pad 23 with lid 12 passes through the screw connection, driving motor 21 with mount pad 23 passes through the screw connection, driving motor 21 output with drive shaft 22 one end is connected, can drive shaft 22 rotatory, the drive shaft 22 other end extends to in the blending tank 11, and with mixing component 4 connects, realizes the drive mixing component 4 stirs, PLC control module 3 with driving motor 21 connects, can play control driving motor 21's effect.
Referring to fig. 1 to 3, in the preparation method of the spinnable polycarbosilane according to the embodiment of the present invention, the mixing component 4 includes a stirring shaft 41 and stirring blades 42, one end of the stirring shaft 41 is connected to the other end of the driving shaft 22, the stirring blades 42 are disposed on the stirring shaft 41, and the stirring blades 42 are disposed in plurality and respectively distributed on the stirring shaft 41.
When the equipment, (mixing) shaft 41 one end with the welding of drive shaft 22 other end or through the screw connection, stirring vane 42 pass through the screw with (mixing) shaft 41 is connected, stirring vane 42 is provided with a plurality ofly to evenly distribute respectively in on the (mixing) shaft 41, can be used for making things convenient for the mixed material.
Referring to fig. 1 to 3, in the preparation method of the spinnable polycarbosilane according to the embodiment of the present invention, the PLC control module 3 includes a material collecting module, a regulating module, an amplifying module, a controller, and a torque and rotation speed sensor, where the material collecting module is configured to constantly collect material mixing information inside the mixing tank 11, and transmit collected material information data to the controller through the amplifying module, the controller adjusts an operation speed of the driving motor 21 according to a material mixing condition, the torque and rotation speed sensor constantly collects a rotation speed of the stirring shaft 41, and transmits the collected speed data to the controller through the amplifying module, and the controller adjusts a control compensation amount of the rotation speed to form a single closed-loop control on the rotation speed; the calculation mode of the single closed-loop control is as follows:
wherein G isC(s) is the controller transfer function; g2(s) is the amplifier transfer function; h3(s) is a torque revolution speed sensor, H3(s)＝Km2；Km2Is the torque speed sensor gain; transfer function of the amplifier
I is the amplifier output current; u is the amplifier operating voltage.
In the preparation method of the spinnable polycarbosilane, the rotation speed of the driving motor can be conveniently mastered and regulated through the calculation mode, the use is convenient, and the working efficiency can be improved.
Referring to fig. 1 to 3, in the preparation method of the spinnable polycarbosilane according to the embodiment of the present invention, the PLC control module 3 further includes a valve controller and a pressure sensor, the valve controller is disposed on the discharge pipe 15 and connected to the controller, the pressure sensor is disposed on the exhaust pipe 121 and connected to the controller,
in a second aspect, the spinnable polycarbosilane is obtained by the preparation method of the spinnable polycarbosilane.
Compared with the prior art, the invention has the beneficial effects that:
the product has good fluidity, reduces the branching degree of polycarbosilane, has better linear structure, high fluidity and obviously improved spinnability.
Through adopting PLC control module group, can conveniently control the mixture of material, can improve work efficiency, help making its mixture more even.
Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of spinnable polycarbosilane is characterized in that: the method comprises the following steps:
under the protection of nitrogen, adding an organic solvent and alkali metal into a mixing device for mixing, heating until the alkali metal is molten, adding dimethyldichlorosilane into the molten alkali metal for reaction, and stirring and curing at a high temperature to obtain a reactant;
respectively adding purified water and absolute ethyl alcohol into the obtained mixture for cleaning for multiple times to obtain pure polydimethylsilane;
reacting for 1-6 hours at the temperature of 100 ℃ and 150 ℃ to perform polycondensation reaction to obtain polydimethylsilane to be treated;
performing pressure maintaining, vacuum pumping, heat preservation, temperature rising and cracking on the vacuum-dried polydimethylsiloxane to obtain a liquid low-molecular cracking product;
and synthesizing and desolventizing the obtained liquid low-molecular cracking product at high temperature and high pressure to obtain the polycarbosilane.
2. The process for producing a spinnable polycarbosilane as claimed in claim 2, wherein: mixing apparatus is including holding subassembly (1), drive assembly (2), PLC control module group (3) and hybrid module (4), drive assembly (2) set up in hold subassembly (1) upper portion, hybrid module (4) set up in hold in subassembly (1), just drive assembly (2) output with hybrid module (4) input is connected, in order to realize driving hybrid module (4) are in hold in subassembly (1) and mix the stirring to the material, PLC control module group (3) set up in hold on subassembly (1), just PLC control module group (3) with drive assembly (2) are connected, in order to realize control opening or closing of drive assembly (2).
3. The process for producing a spinnable polycarbosilane as claimed in claim 2, wherein: hold subassembly (1) including blending tank (11), lid (12), supporting leg (13), water inlet (14) and ejection of compact pipeline (15), supporting leg (13) with blending tank (11) are connected, blending tank (11) top with lid (12) are connected, exhaust duct (121) have on lid (12), ejection of compact pipeline (15) one end with the bottom intercommunication of blending tank (11), water inlet (14) set up in blending tank (11) one side.
4. The process for producing a spinnable polycarbosilane as claimed in claim 3, wherein: drive assembly (2) include driving motor (21), drive shaft (22) and mount pad (23), mount pad (23) set up in on lid (12), driving motor (21) set up in on mount pad (23), driving motor (21) output with drive shaft (22) one end is connected, the drive shaft (22) other end extends to in blending tank (11), and with blending unit (4) are connected, PLC control module (3) with driving motor (21) are connected.
5. The process for producing a spinnable polycarbosilane as claimed in claim 4, wherein: the mixing assembly (4) comprises a mixing shaft (41) and mixing blades (42), one end of the mixing shaft (41) is connected with the other end of the driving shaft (22), and the mixing blades (42) are arranged on the mixing shaft (41).
6. The process for producing a spinnable polycarbosilane as claimed in claim 5, wherein: the stirring blades (42) are arranged in a plurality and are respectively distributed on the stirring shaft (41).
7. The process for producing a spinnable polycarbosilane as claimed in claim 6, wherein: PLC control module group (3) include material collection module, regulation and control module, enlarge module, controller and torque speed sensor, wherein, material collection module is used for gathering the inside material mixing information of blending tank (11) constantly to the material information data that will gather transmits to through enlarging the module the controller, the running speed of adjustment driving motor (21) is according to the material mixing situation to the controller, torque speed sensor gathers constantly the rotational speed of (mixing) shaft (41) to the speed data that will gather transmits to through enlarging the module the controller, controller adjustment rotational speed's control offset has constituted the single closed loop control to rotational speed.
8. The process for producing a spinnable polycarbosilane as claimed in claim 7, wherein: the PLC control module (3) further comprises a valve controller and a pressure sensor, the valve controller is arranged on a discharging pipeline (15), the valve controller is connected with the controller, the pressure sensor is arranged on the exhaust pipeline (121), and the pressure sensor is connected with the controller.
9. Spinnable polycarbosilanes obtainable by the process of any one of claims 1 to 8.
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