CN109776807A - Polycarbosilane of the dissaving structure containing liquid and preparation method thereof - Google Patents
Polycarbosilane of the dissaving structure containing liquid and preparation method thereof Download PDFInfo
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- CN109776807A CN109776807A CN201910082022.XA CN201910082022A CN109776807A CN 109776807 A CN109776807 A CN 109776807A CN 201910082022 A CN201910082022 A CN 201910082022A CN 109776807 A CN109776807 A CN 109776807A
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Abstract
The present invention relates to Polycarbosilanes of a kind of dissaving structure containing liquid and preparation method thereof.Preparation method mixes later with polydimethylsiloxane comprising steps of prepare a kind of liquid hyperbranched polycarbosilanes first, and finally under the catalytic action of ferrocene, heating and isothermal holding are carried out under atmosphere of inert gases, after cooled to room temperature cross-linking products；Cross-linking products are hydrolyzed, heat and are stirred, are stood later, aqueous top layer substance is collected, obtains final product.Using technical solution provided by the invention, liquid hyperbranched polycarbosilanes are added in common Polycarbosilane and are used, the viscosity of precursor can be reduced, improve its reactivity, finally prepares precursor of good performance.In addition, the present invention also has many advantages, such as that simple process, molecular weight of product are big, self-crosslinking degree is high, ceramic yield is high.
Description
Technical field
The present invention relates to thyrite technical fields, and in particular to a kind of poly- carbon silicon of the dissaving structure containing liquid
Alkane and preparation method thereof.
Background technique
Based on excellent mechanical property and high temperature resistance, silicon carbide fibre is in the high-techs such as aerospace and rocket equipment
Skill field obtains great application.The preparation of silicon carbide fibre is always the key issues that domestic and foreign scholars are concerned about, and pioneer
Preparation is the current method one of most mature using most, technology.Precursor as the key raw material for preparing fiber,
Performance has vital influence to the performance of silicon carbide.Wherein, Polycarbosilane is first as a kind of good silicon carbide fibre
Body is driven, the exemplary steps for preparing silicon carbide fibre include: the melt spinning of precursor, and fiber does not melt processing and fiber
High temperature sintering；However, since to still remain wide molecular weight distribution, large viscosity, spinnability low, miscellaneous for current Polycarbosilane
The disadvantages of matter is more carry out physics, chemical modification to Polycarbosilane, are the mainstream sides of silicon carbide fibre development in international community now
To.
In recent years, the advantages that liquid hyperbranched polycarbosilanes are due to its good physicochemical characteristic and simple preparation process,
Obtain the great attention of domestic and foreign scholars.Liquid hyperbranched polycarbosilanes viscosity is low, good fluidity, and end group contains a large amount of activity
Functional group can design molecular structure as needed, and self-crosslinkable, it is the ideal precursor for preparing Polycarbosilane that ceramic yield is high.
But liquid hyperbranched polycarbosilanes preparation engineering middle-molecular-weihydroxyethyl is uncontrollable, and molecular distribution range is wide, needs to be modified (Cao to it
The synthesis of agreeable liquid hyperbranched polycarbosilanes and ceramic research [D] the National University of Defense Technology, 2012.).
Based on this, providing the novel liquid hyperbranched polycarbosilanes and preparation method thereof of one kind is particularly important.
Summary of the invention
For the defects in the prior art, the present invention is intended to provide a kind of Polycarbosilane of dissaving structure containing liquid and its
Preparation method.Using technical solution provided by the invention, prepare a kind of liquid hyperbranched polycarbosilanes first, later with poly- diformazan
Base silane mixing, finally occurs cross-linking reaction under the catalytic action of ferrocene；Liquid hyperbranched polycarbosilanes are added to
It is used in common Polycarbosilane, the viscosity of precursor can be reduced, improve its reactivity, finally prepare pioneer of good performance
Body.In addition, the present invention also has many advantages, such as that simple process, molecular weight of product are big, self-crosslinking degree is high, ceramic yield is high.
For this purpose, the invention provides the following technical scheme:
In a first aspect, the present invention provides a kind of preparation method of the Polycarbosilane of dissaving structure containing liquid, including following
Step: S1: under atmosphere of inert gases, anhydrous tetrahydro furan is added dropwise in magnesium chips and stirs；S2: by Chloromethyltrichlorosilane
(Cl3SiCH2Cl it) is added drop-wise in the solution that S1 is obtained after mixing with anhydrous tetrahydro furan, heated at constant temperature simultaneously stirs；S3:
Methanol solution is added dropwise in the solution that S2 is obtained, continue heated at constant temperature and stirs；Lithium aluminium hydride reduction (LiAlH is added dropwise later4) solution is simultaneously
Preset time is stirred, is stood；S4: polydimethylsiloxane (PDMS) is distilled, and collects 102~103 DEG C of fractions and drying；
S5: the product that S4 is obtained is mixed with the product that S3 is obtained, and ferrocene is added later, and heat up under atmosphere of inert gases
And isothermal holding, cooled to room temperature obtain cross-linking products；S6: cross-linking products are hydrolyzed, and are heated and are stirred, Zhi Houjing
It sets, collects aqueous top layer substance, obtain final product.
Preferably, in S1: the mass ratio of magnesium chips and tetrahydrofuran is 1:(6~10), mixing time is 0.5~1h；Inertia
Atmosphere selects nitrogen or argon gas, and is preferably first passed through gas in nitrogen or argon gas displacement reaction system, and keep gas stream
Measure 50~100mL/min.
Preferably, in S2: the volume ratio of Chloromethyltrichlorosilane and tetrahydrofuran is 1:(1~3)；Chloromethyltrichlorosilane
Mass ratio with magnesium chips is (6~10): 1；Heating temperature is 60~70 DEG C.
Preferably, in S3: the mass ratio of lithium aluminium hydride reduction, methanol and Chloromethyltrichlorosilane is followed successively by (2~4): (2~3):
1；Heating temperature is 60~80 DEG C, and mixing time is 24~30h；Preset time is 4~6h.
Preferably, in S5: the ratio between product and the product quality of S3 of S4 are (60~80): (10~40)；Ferrocene adds
Enter 1~2% that amount is gross mass；Heating and isothermal holding specifically include: being warming up to 240~260 with the rate of 5~10 DEG C/min
DEG C and keep the temperature 6~8h, with the rate of 5~10 DEG C/min be warming up to 420~460 DEG C and keep the temperature 24~36h；React on inert gas
It is carried out under atmosphere, and controlling inert gas flow is 100~200mL/min, is forced into 0.5~1MPa.
Preferably, in S6: selecting volume ratio is (1~3): 1 dilute hydrochloric acid and the mixed liquor of n-hexane are hydrolyzed, and dilute
The mass percentage concentration of hydrochloric acid is 15%；Heating temperature is 60~80 DEG C, and mixing time is 24~36h.
Preferably, it in preparation method, is heated in oil bath.
Second aspect, using the Polycarbosilane of the dissaving structure provided by the invention containing liquid being prepared.
The Polycarbosilane of the third aspect, the dissaving structure provided by the invention containing liquid is preparing answering in silicon carbide fibre
With.
Above-mentioned technical proposal provided by the invention has the advantage that
(1) applicant has found by numerous studies: using technical solution provided by the invention, it is super to prepare a kind of liquid first
Branching Polycarbosilane, mixes with polydimethylsiloxane later, and cross-linking reaction finally occurs under the catalytic action of ferrocene；It will
Liquid hyperbranched polycarbosilanes, which are added in common Polycarbosilane, to be used, and can be reduced the viscosity of precursor, be improved its reactivity,
Finally prepare precursor of good performance.
(2) preparation method of the Polycarbosilane of the dissaving structure provided by the invention containing liquid, not only simple process, but also
Molecular weight of product is big, self-crosslinking degree is high, ceramic yield is high.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Specific embodiment
The embodiment of technical solution of the present invention will be described in detail below.Following embodiment is only used for clearer
Illustrate technical solution of the present invention, therefore be only used as example, and not intended to limit the protection scope of the present invention.
Experimental method in following embodiments is unless otherwise specified conventional method.Examination as used in the following examples
Material is tested, is to be commercially available from conventional reagent shop unless otherwise specified.Quantitative test in following embodiment, is all provided with
Three repeated experiments are set, data are the average value or mean+SD of three repeated experiments.
The present invention provides a kind of preparation method of the Polycarbosilane of dissaving structure containing liquid, comprising the following steps:
S1: it will be passed through high pure nitrogen or argon gas after three-necked flask drying, replaces gas in flask, and keep gas flow 50
~100mL/min；Magnesium chips is added, anhydrous tetrahydro furan, 0.5~1h of uniform stirring are added dropwise later.Wherein, magnesium chips and tetrahydrofuran
Mass ratio be 1:(6~10).
S2: by Chloromethyltrichlorosilane (Cl3SiCH2Cl it) is added drop-wise to three-necked flask after mixing with anhydrous tetrahydro furan
In, flask is placed in oil bath pan, is heated to 60~70 DEG C of constant temperature oil baths and is stirred.Wherein, Chloromethyltrichlorosilane and tetrahydro furan
The volume ratio muttered is 1:(1~3), the mass ratio of Chloromethyltrichlorosilane and magnesium chips is (6~10): 1.
S3: being added dropwise methanol solution in the solution that S2 is obtained, and keeps 60~80 DEG C of oil bath temperatures constant, stirs 24~30h；
Continue that lithium aluminium hydride reduction (LiAlH is added dropwise later4) solution, it is stood after stirring 4~6h.Wherein, lithium aluminium hydride reduction, methanol and chloromethyl three
The mass ratio of chlorosilane is followed successively by (2~4): (2~3): 1.
S4: polydimethylsiloxane is distilled, and collects 102~103 DEG C of fractions and drying.
S5: the product that S4 is obtained being mixed with the product that S3 is obtained, ferrocene is added later, is passed through inert gas, and control
Flow processed is 100~200mL/min, is forced into 0.5~1MPa, is warming up to 240~260 DEG C simultaneously with the rate of 5~10 DEG C/min
6~8h is kept the temperature, be warming up to 420~460 DEG C with the rate of 5~10 DEG C/min and keeps the temperature 24~36h, cooled to room temperature obtains
Cross-linking products.Wherein, the ratio between product quality of the product of S4 and S3 is (60~80): (10~40)；The additional amount of ferrocene is
The 1~2% of gross mass.
S6: cross-linking products being put into the mixed liquor of 15% dilute hydrochloric acid and n-hexane and be hydrolyzed, 60~80 DEG C of oil baths, after
24~36h of continuous stirring, stands, isolates aqueous top layer substance, obtain final product.Wherein, the volume of dilute hydrochloric acid and n-hexane
Than for (1~3): 1.
It is illustrated With reference to embodiment:
Embodiment one
The present embodiment provides a kind of preparation methods of the Polycarbosilane of dissaving structure containing liquid, comprising the following steps:
S1: a three-necked flask is taken, is passed through gas in high pure nitrogen displacement flask thereto after dry, and keep gas stream
Measure 50mL/min；Magnesium chips is added into three-necked flask, anhydrous tetrahydro furan, uniform stirring 1h is added dropwise.Wherein, magnesium chips and tetrahydro furan
The mass ratio muttered is 1:8.
S2: by Chloromethyltrichlorosilane (Cl3SiCH2Cl it) is added drop-wise to three-necked flask after mixing with anhydrous tetrahydro furan
In, three-necked flask is placed in oil bath pan, is heated to 70 DEG C of constant temperature oil baths and is stirred.Wherein, Chloromethyltrichlorosilane and tetrahydro furan
The volume ratio muttered is 1:1, and the mass ratio of Chloromethyltrichlorosilane and magnesium chips is 6:1.
S3: being added dropwise methanol solution in the solution that S2 is obtained, and keeps 70 DEG C of oil bath temperatures constant, stirs 30h；Continue later
Lithium aluminium hydride reduction (LiAlH is added dropwise4) solution, it is stood after stirring 6h.Wherein, the matter of lithium aluminium hydride reduction, methanol and Chloromethyltrichlorosilane
Amount ratio is followed successively by 4:2:1.
S4: polydimethylsiloxane is distilled, and collects 102 DEG C of fractions and drying.
S5: the product that S4 is obtained being mixed with the product that S3 is obtained, ferrocene is added later, is passed through inert gas, and control
Flow processed is 100mL/min, is forced into 0.5MPa, is warming up to 240 DEG C with the rate of 5 DEG C/min and keeps the temperature 8h, with 10 DEG C/min
Rate be warming up to 460 DEG C and keep the temperature 30h, cooled to room temperature obtains cross-linking products.Wherein, the product of the product of S4 and S3
Mass ratio is 71:32；The additional amount of ferrocene is the 1% of gross mass.
S6: cross-linking products being put into the mixed liquor of 15% dilute hydrochloric acid and n-hexane and be hydrolyzed, and 80 DEG C of oil baths continue to stir
It mixes for 24 hours, stands, isolate aqueous top layer substance, obtain the Polycarbosilane of final product dissaving structure containing liquid.Wherein, dilute
The volume ratio of hydrochloric acid and n-hexane is 1:1.
Polycarbosilane manufactured in the present embodiment, average molecular weight 2780, ceramic yield 91%.
Embodiment two
The present embodiment provides a kind of preparation methods of the Polycarbosilane of dissaving structure containing liquid, comprising the following steps:
S1: a three-necked flask is taken, is passed through gas in high-purity argon gas displacement flask after dry thereto, replaces gas in flask
Body, and keep gas flow 80mL/min；Magnesium chips is added, anhydrous tetrahydro furan, uniform stirring 1h are added dropwise later.Wherein, magnesium chips
Mass ratio with tetrahydrofuran is 1:7.
S2: by Chloromethyltrichlorosilane (Cl3SiCH2Cl it) is added drop-wise to three-necked flask after mixing with anhydrous tetrahydro furan
In, three-necked flask is placed in oil bath pan, is heated to 65 DEG C of constant temperature oil baths and is stirred.Wherein, Chloromethyltrichlorosilane and tetrahydro furan
The volume ratio muttered is 1:2, and the mass ratio of Chloromethyltrichlorosilane and magnesium chips is 9:1.
S3: being added dropwise methanol solution in the solution that S2 is obtained, and keeps 80 DEG C of oil bath temperatures constant, stirs 30h；Continue later
Lithium aluminium hydride reduction (LiAlH is added dropwise4) solution, it is stood after stirring 5h.Wherein, the matter of lithium aluminium hydride reduction, methanol and Chloromethyltrichlorosilane
Amount ratio is followed successively by 2:3:1.
S4: polydimethylsiloxane is distilled, and collects 103 DEG C of fractions and drying.
S5: the product that S4 is obtained being mixed with the product that S3 is obtained, ferrocene is added later, is passed through inert gas, and control
Flow processed is 50mL/min, is forced into 1MPa, is warming up to 255 DEG C with the rate of 8 DEG C/min and keeps the temperature 8h, with the speed of 6 DEG C/min
Rate is warming up to 435 DEG C and keeps the temperature 26h, and cooled to room temperature obtains cross-linking products.Wherein, the product quality of the product of S4 and S3
The ratio between be 68:37；The additional amount of ferrocene is the 1.5% of gross mass.
S6: cross-linking products being put into the mixed liquor of 15% dilute hydrochloric acid and n-hexane and be hydrolyzed, and 80 DEG C of oil baths continue to stir
30h is mixed, is stood, is isolated aqueous top layer substance, obtain the Polycarbosilane of final product dissaving structure containing liquid.Wherein, dilute
The volume ratio of hydrochloric acid and n-hexane is 3:1.
Polycarbosilane manufactured in the present embodiment, average molecular weight 3230, ceramic yield 88%.
Certainly, prepared by the case where being enumerated in addition to embodiment one and embodiment two, the weight percent of other raw material components
Each condition and parameter in journey etc. are also possible.
Using technical solution provided by the invention, prepare a kind of liquid hyperbranched polycarbosilanes first, later with poly- diformazan
Base silane mixing, finally occurs cross-linking reaction under the catalytic action of ferrocene；Liquid hyperbranched polycarbosilanes are added to
It is used in common Polycarbosilane, the viscosity of precursor can be reduced, improve its reactivity, finally prepare pioneer of good performance
Body.In addition, the present invention also has many advantages, such as that simple process, molecular weight of product are big, self-crosslinking degree is high, ceramic yield is high.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (9)
1. a kind of preparation method of the Polycarbosilane of dissaving structure containing liquid, which comprises the following steps:
S1: under atmosphere of inert gases, anhydrous tetrahydro furan is added dropwise in magnesium chips and stirs；
S2: Chloromethyltrichlorosilane and anhydrous tetrahydro furan are added drop-wise to after mixing in the solution that the S1 is obtained, constant temperature
It heats and stirs；
S3: being added dropwise methanol solution in the solution that the S2 is obtained, and continues heated at constant temperature and stirs；It is molten that lithium aluminium hydride reduction is added dropwise later
Liquid simultaneously stirs preset time, stands；
S4: polydimethylsiloxane is distilled, and collects 102~103 DEG C of fractions and drying；
S5: the product that the S4 is obtained is mixed with the obtained product of the S3, ferrocene is added later, and in inert gas atmosphere
Heating is carried out under enclosing and isothermal holding, cooled to room temperature obtain cross-linking products；
S6: the cross-linking products are hydrolyzed, and are heated and are stirred, stand later, are collected aqueous top layer substance, are finally produced
Object.
2. the preparation method of the Polycarbosilane of the dissaving structure according to claim 1 containing liquid, it is characterised in that:
In the S1:
The mass ratio of magnesium chips and tetrahydrofuran is 1:(6~10), mixing time is 0.5~1h；Atmosphere of inert gases selects nitrogen
Or argon gas, and it is preferably first passed through gas in nitrogen or argon gas displacement reaction system, and keep 50~100mL/min of gas flow.
3. the preparation method of the Polycarbosilane of the dissaving structure according to claim 1 containing liquid, it is characterised in that:
In the S2:
The volume ratio of Chloromethyltrichlorosilane and tetrahydrofuran is 1:(1~3)；The mass ratio of Chloromethyltrichlorosilane and magnesium chips is
(6~10): 1；Heating temperature is 60~70 DEG C.
4. the preparation method of the Polycarbosilane of the dissaving structure according to claim 1 containing liquid, it is characterised in that:
In the S3:
The mass ratio of lithium aluminium hydride reduction, methanol and Chloromethyltrichlorosilane is followed successively by (2~4): (2~3): 1；Heating temperature be 60~
80 DEG C, mixing time is 24~30h；The preset time is 4~6h.
5. the preparation method of the Polycarbosilane of the dissaving structure according to claim 1 containing liquid, it is characterised in that:
In the S5:
The ratio between product quality of the product of the S4 and the S3 is (60~80): (10~40)；The additional amount of ferrocene is total
The 1~2% of quality；The heating and isothermal holding specifically include: being warming up to 240~260 DEG C simultaneously with the rate of 5~10 DEG C/min
6~8h is kept the temperature, be warming up to 420~460 DEG C with the rate of 5~10 DEG C/min and keeps the temperature 24~36h；React on atmosphere of inert gases
Lower progress, and controlling inert gas flow is 100~200mL/min, is forced into 0.5~1MPa.
6. the preparation method of the Polycarbosilane of the dissaving structure according to claim 1 containing liquid, it is characterised in that:
In the S6:
Selecting volume ratio is (1~3): 1 dilute hydrochloric acid and the mixed liquor of n-hexane are hydrolyzed, and the quality percentage of dilute hydrochloric acid is dense
Degree is 15%；Heating temperature is 60~80 DEG C, and mixing time is 24~36h.
7. the preparation method of the Polycarbosilane of described in any item dissaving structures containing liquid according to claim 1~6, feature
It is:
In the preparation method, heated in oil bath.
8. the Polycarbosilane for the dissaving structure containing liquid that any one the method is prepared according to claim 1~7.
9. the Polycarbosilane of the dissaving structure according to any one of claims 8 containing liquid is preparing the application in silicon carbide fibre.
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