CN109354691A - A kind of preparation method of high ceramic yield Polycarbosilane - Google Patents
A kind of preparation method of high ceramic yield Polycarbosilane Download PDFInfo
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- CN109354691A CN109354691A CN201811354984.8A CN201811354984A CN109354691A CN 109354691 A CN109354691 A CN 109354691A CN 201811354984 A CN201811354984 A CN 201811354984A CN 109354691 A CN109354691 A CN 109354691A
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- polycarbosilane
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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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Abstract
The invention discloses a kind of preparation methods of high ceramic yield Polycarbosilane.This method is dissolved in organic solvent using the compound of solid-state Polycarbosilane and cyano-containing as raw material, under nitrogen or inert gas shielding, catalyst is added and reacts, then removes organic solvent, obtains the Polycarbosilane of cyano-containing.Compared with existing Polycarbosilane modification technology, this method reaction condition is mild, contains cyano in Polycarbosilane obtained, ceramic yield can be significantly improved when thyrite as precursor, therefore have a good application prospect.
Description
Technical field
The invention belongs to silicon carbide precursor preparation technical fields, and in particular to a kind of to prepare high ceramic yield carbon silane
Method.
Background technique
It is precursor for SiC fiber since the Yajima et al. of northeastern Japan university has been started with Polycarbosilane (PCS)
The beginning, organic precursor method conversion method be increasingly becoming prepares SiC fiber and ceramics important method.This method is with organic polymer
Object is precursor, makes its molding using its fusible soluble characteristic, then be allowed to be changed into inorganic ceramic material through high-temperature heat treatment
Method.
Polycarbosilane (PCS) and the Polycarbosilane (PMCS) for containing heterogeneous element (aluminium, iron, zirconium, boron etc.) are silicon carbide fibres
The important precursor of dimension and ceramics.PCS is usually heavy through cracking under 400-500 DEG C, inert gas shielding by polydimethylsiloxane
Row's reaction obtains.PMCS usually is reacted to obtain by PCS with the compound containing heterogeneous element.
Pioneer's volume property is the key factor for influencing final silicon carbide (SiC) fiber and ceramic performance.Pottery with higher
Porcelain yield is an important indicator of precursor.During PCS and PMCS is as polymer pyrolysis ceramics, waved due to low molecular
The pyrolytic reaction of the groups such as hair and Si-H, Si-CH3, usual ceramic yield is lower, 60% or so.Into PCS molecular structure
Its ceramic yield can be effectively improved by introducing potential activity reactive group.With the shape of physical blending or chemical graft such as into PCS
Formula introduces end hydroxy butadiene (HTPB) (aerospace material technique, 1988,2:36-39), divinylbenzene (DVB) (organosilicon
Material, 2002,16 (6): 4-7), methyl ethylene silazane (high-tech communication, 2000,3:83-86), tetramethyl tetravinyl
Tetrasiloxane (organosilicon material, 2011,25 (6): 380-383), dimethyl divinyl silane (organosilicon material, 2015,29
(6): 462-468) etc., improve ceramic yield.Application No. is the Chinese patent of CN201510192549.X disclose it is a kind of high
The synthetic method of ceramic yield Polycarbosilane, it be by molecular weight 500-1500 Polycarbosilane and allyl compound by one
Certainty ratio mixing after, be dissolved in dimethylbenzene, be placed in reaction vessel, be added organolithium reagent, protective gas protection under heat up into
Row reaction, reacts under certain temperature and time, after reaction, is filtered to remove insoluble matter, solvent is evaporated off, and obtains high ceramics
Yield Polycarbosilane.
In the above-mentioned technology modified to PCS, in a manner of physical blending it is modified usually exist be difficult to mix and uniformly poor etc.
Problem, modified usually there are severe reaction conditions in a manner of chemical graft, the deficiencies of reaction temperature is high, and the reaction time is long.
Summary of the invention
Technical purpose of the invention is the problem low for ceramic yield existing for above-mentioned Polycarbosilane, is provided a kind of new
The method for preparing high ceramic yield Polycarbosilane, compared with existing Polycarbosilane modification technology, this method has reaction condition temperature
The advantages that high with product ceramic yield.
To realize the above-mentioned technical purpose, the technical scheme adopted by the invention is as follows: a kind of high ceramic yield Polycarbosilane
Preparation method, it is characterized in that: organic solvent is dissolved in, in nitrogen using the compound of solid-state Polycarbosilane and cyano-containing as raw material
Or under inert gas shielding, catalyst is added and reacts, then removes organic solvent, obtains the Polycarbosilane of cyano-containing.
In the present invention, the Polycarbosilane is to contain CH in molecular structure3SiHCH2The compound of structural unit, at room temperature
In solid-state.The Polycarbosilane is also possible to the Polycarbosilane containing heterogeneous element, and the heterogeneous element is unlimited, including aluminium, iron,
One or more of titanium, zirconium, cobalt, nickel, boron, lanthanum, yttrium, niobium etc..
In the present invention, contain unsaturated alkyl in the compound of the cyano-containing.The compound of the cyano-containing include but
It is not limited to one of acrylonitrile, methacrylonitrile, butene nitrile, allyl acetonitrile, cyanoacetylene, hydroxyl terminated butadiene acrylonitrile copolymer or several
Kind.
In the present invention, the catalyst is preferably Si―H addition reaction type catalyst or free radical type catalyst.The silicon hydrogen
Add-on type catalyst is unlimited, including chloroplatinic acid, chloroplatinic acid-amine, Karstedt catalyst, Wilkinson catalyst, Rh2
(OAc)4、RhH(CO)(PPh3)3、[(C4H6)2RhCl]2、Cu2One or more of O/TMEDA etc..The free radical type is urged
Agent is unlimited, including azodiisobutyronitrile, azobisisoheptonitrile, azo-bis-iso-dimethyl, dibenzoyl peroxide, peroxide
Change lauroyl, acetyl peroxide, dioctanoyl peroxide, peroxidized t-butyl perbenzoate, cumyl peroxide, di-t-butyl mistake
One or more of oxide, persulfate etc..
The present invention, the organic solvent is unlimited, including benzene,toluene,xylene, tetrahydrofuran, carbon tetrachloride, hexamethylene,
One or more of n-hexane, pentane, normal heptane.
Preferably, reaction temperature is 20 DEG C -150 DEG C, more preferably 40 DEG C -80 DEG C.
Preferably, the reaction time is 2h-20h.
Preferably, the cyano-containing compound accounts for the 1%-50% of Polycarbosilane quality.
Preferably, the catalyst accounts for the 0.01%-20% of cyano-containing compound quality.
Compared with the modification technology of existing Polycarbosilane, method of the invention has reaction condition mild, simple and easy,
By containing cyano in the modified Polycarbosilane of this method, can significantly be mentioned as precursor for when thyrite
High ceramic yield, therefore have a good application prospect.
Detailed description of the invention
Fig. 1 is the FTIR spectrogram of PCS-CN01 obtained in the embodiment of the present invention 1.
Fig. 2 is TG curve of the PCS-CN01 obtained and unmodified PCS in nitrogen atmosphere in the embodiment of the present invention 1
Figure.
Specific embodiment
Below with reference to embodiment, present invention is further described in detail with attached drawing, it should be pointed out that reality as described below
It applies example to be intended to convenient for the understanding of the present invention, and does not play any restriction effect to it.
Embodiment 1:
It takes the Polycarbosilane (PCS) of 20g to be dissolved in the tetrahydrofuran (THF) of 30g, 100ml is added after dissolving completely and burns
In bottle, acrylonitrile 2g is added, under nitrogen protection, rhodium-containing compound Si―H addition reaction type catalyst 0.001g is added, it then will be anti-
System is answered to be warming up to 60 DEG C of reaction 5h.Finally, THF is removed in a manner of being evaporated under reduced pressure, cyano-containing Polycarbosilane PCS- is obtained
CN01。
Fig. 1 is the FTIR spectrogram of PCS-CN01 obtained above.2240cm in figure-1There is the apparent peak-C ≡ N in place, and
2100cm-1The Si-H and 1245cm at place-1The intensity rate for locating Si-CH3 is 0.88, and original PCS, i.e., unmodified before reaction
The ratio of PCS is 0.94, illustrates that cyano is introduced into PCS molecule.
Fig. 2 is thermogravimetric (TG) curve graph of PCS-CN01 obtained above and unmodified PCS in a nitrogen atmosphere.It can
To see, unmodified PCS only has 47% in 1000 DEG C of ceramic yield, and the ceramic yield of PCS-CN01 is 86%, ceramics
Yield is significantly increased.
Embodiment 2:
It takes the Polycarbosilane (PCS) same as Example 1 of 20g to be dissolved in the dimethylbenzene of 30g, is added after dissolving completely
In 100ml flask, acrylonitrile 3g is added, under nitrogen protection, azodiisobutyronitrile catalyst 0.2g is added, then by reactant
System is warming up to 65 DEG C of reaction 8h.Finally, dimethylbenzene is removed in a manner of being evaporated under reduced pressure, cyano-containing Polycarbosilane PCS- is obtained
CN02。
It is same as Example 1, according to the FTIR spectrogram of PCS-CN02 obtained above it can be concluded that cyano is introduced into PCS points
In son.
It is same as Example 1, PCS-CN02 obtained above and unmodified PCS are subjected to thermogravimetric in a nitrogen atmosphere
(TG) it analyzes, the ceramic yield for obtaining PCS-CN02 is 75%, is significantly increased compared to PCS.
Embodiment 3:
It takes the polyaluminocarbosilane (PACS) of 25g to be dissolved in the dimethylbenzene of 30g, 100ml flask is added after dissolving completely
In, methacrylonitrile 2g is added, under nitrogen protection, azodiisobutyronitrile catalyst 0.2g is added, then by reaction system liter
Temperature is to 70 DEG C of reaction 5h.Finally, dimethylbenzene is removed in a manner of being evaporated under reduced pressure, cyano-containing polyaluminocarbosilane PACS-CN03 is obtained.
It is same as Example 1, according to the FTIR spectrogram of PACS-CN03 obtained above it can be concluded that cyano is introduced into PCS
In molecule.
It is same as Example 1, PACS-CN03 obtained above and unmodified PACS are subjected to heat in a nitrogen atmosphere
Weight (TG) analysis, the ceramic yield for obtaining PACS and PACS-CN03 is respectively 55% and 78%, compares PACS, PACS-CN03's
Ceramic yield is significantly increased.
Embodiment 4:
It takes the iron content Polycarbosilane (PFCS) of 25g to be dissolved in the n-hexane of 30g, 100ml flask is added after dissolving completely
In, methacrylonitrile 2.5g is added, under nitrogen protection, dibenzoyl peroxide catalyst 0.3g is added, then by reactant
System is warming up to 65 DEG C of reaction 6h.N-hexane is removed in a manner of being evaporated under reduced pressure, obtains cyano-containing Polyferrocarbosilane PFCS-CN04.
It is same as Example 1, according to the FTIR spectrogram of PFCS-CN04 obtained above it can be concluded that cyano is introduced into PFCS
In molecule.
It is same as Example 1, PFCS-CN03 obtained above and unmodified PFCS are subjected to heat in a nitrogen atmosphere
Weight (TG) analysis, the ceramic yield for obtaining PFCS and PFCS-CN04 is respectively 58% and 80%, compares PFCS, PFCS-CN04
Ceramic yield be significantly increased.
Embodiment 5:
It takes the Polycarbosilane containing zirconium (PZCS) of 30g to be dissolved in the tetrahydrofuran of 40g, 200ml is added after dissolving completely and burns
In bottle, methacrylonitrile 3.5g is added, under nitrogen protection, chloroplatinic acid-amine catalyst 0.05g is added, then by reaction system
70 DEG C are warming up to, stops reaction after reacting 5h.Tetrahydrofuran is removed in a manner of being evaporated under reduced pressure, obtains the poly- zirconium carbon silane of cyano-containing
PZCS-CN05。
It is same as Example 1, according to the FTIR spectrogram of PZCS-CN05 obtained above it can be concluded that cyano is introduced into PZCS
In molecule.
It is same as Example 1, PZCS-CN03 obtained above and unmodified PZCS are subjected to heat in a nitrogen atmosphere
Weight (TG) analysis, the ceramic yield for obtaining PZCS and PZCS-CN05 is respectively 54% and 76%, compares PZCS, PZCS-CN05
Ceramic yield be significantly increased.
Embodiment 6:
The present embodiment is substantially the same manner as Example 1, except that replacing acrylonitrile with butene nitrile.
It is same as Example 1, according to the FTIR spectrogram of the poly- zirconium carbon silane of cyano-containing obtained above it can be concluded that cyano quilt
It is introduced into PCS molecule.
It is same as Example 1, in a nitrogen atmosphere by the poly- zirconium carbon silane of cyano-containing obtained above and unmodified PCS
Thermogravimetric (TG) analysis is carried out, is obtained compared with unmodified PCS, the ceramic yield of the poly- zirconium carbon silane of cyano-containing is significantly increased.
Embodiment 7:
The present embodiment is substantially the same manner as Example 1, except that replacing acrylonitrile with cyanoacetylene.
It is same as Example 1, according to the FTIR spectrogram of the poly- zirconium carbon silane of cyano-containing obtained above it can be concluded that cyano quilt
It is introduced into PCS molecule.
It is same as Example 1, in a nitrogen atmosphere by the poly- zirconium carbon silane of cyano-containing obtained above and unmodified PCS
Thermogravimetric (TG) analysis is carried out, is obtained compared with unmodified PCS, the ceramic yield of the poly- zirconium carbon silane of cyano-containing is significantly increased.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention,
Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high ceramic yield Polycarbosilane, it is characterized in that: with the chemical combination of solid-state Polycarbosilane and cyano-containing
Object is raw material, is dissolved in organic solvent, under nitrogen or inert gas shielding, catalyst is added and reacts, then removal has
Solvent obtains the Polycarbosilane of cyano-containing；
The compound of the cyano-containing contains unsaturated alkyl.
2. the preparation method of high ceramic yield Polycarbosilane as described in claim 1, it is characterized in that: the Polycarbosilane packet
Containing heterogeneous element；
Preferably, the heterogeneous element includes one or more of aluminium, iron, titanium, zirconium, cobalt, nickel, boron, lanthanum, yttrium, niobium.
3. the preparation method of high ceramic yield Polycarbosilane as described in claim 1, it is characterized in that: the chemical combination of the cyano-containing
Object includes one of acrylonitrile, methacrylonitrile, butene nitrile, allyl acetonitrile, cyanoacetylene, hydroxyl terminated butadiene acrylonitrile copolymer or several
Kind.
4. the preparation method of high ceramic yield Polycarbosilane as described in claim 1, it is characterized in that: the catalyst is silicon
Hydrogen add-on type catalyst or free radical type catalyst.
5. the preparation method of high ceramic yield Polycarbosilane as claimed in claim 4, it is characterized in that: the Si―H addition reaction type
Catalyst includes chloroplatinic acid, chloroplatinic acid-amine, Karstedt catalyst, Wilkinson catalyst, Rh2(OAc)4、RhH(CO)
(PPh3)3、[(C4H6)2RhCl]2、Cu2One or more of O/TMEDA；
Preferably, the free radical type catalyst includes azodiisobutyronitrile, azobisisoheptonitrile, two isobutyric acid two of azo
Methyl esters, dibenzoyl peroxide, dilauroyl peroxide, acetyl peroxide, dioctanoyl peroxide, peroxidized t-butyl perbenzoate,
One or more of cumyl peroxide, di-tert-butyl peroxide, persulfate.
6. the preparation method of high ceramic yield Polycarbosilane as described in claim 1, it is characterized in that: the organic solvent packet
Include one or more of benzene,toluene,xylene, tetrahydrofuran, carbon tetrachloride, hexamethylene, n-hexane, pentane, normal heptane.
7. the preparation method of high ceramic yield Polycarbosilane as described in claim 1, it is characterized in that: reaction temperature be 20 DEG C-
150 DEG C, preferably 40 DEG C -80 DEG C.
8. the preparation method of high ceramic yield Polycarbosilane as described in claim 1, it is characterized in that: the reaction time is 2h-
20h。
9. the preparation method of the high ceramic yield Polycarbosilane as described in any claim in claim 1 to 8, feature
Be: the compound of the cyano-containing accounts for the 1%-50% of Polycarbosilane quality.
10. the preparation method of the high ceramic yield Polycarbosilane as described in any claim in claim 1 to 8, feature
Be: the catalyst accounts for the 0.01%-20% of the compound quality of cyano-containing.
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Cited By (7)
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| CN112126064A (en) * | 2020-09-24 | 2020-12-25 | 长沙科航特种织造有限公司 | Preparation method of novel solid silicon carbide ceramic precursor |
| CN112300397A (en) * | 2020-11-05 | 2021-02-02 | 江西信达航科新材料科技有限公司 | High-performance polycarbosilane and preparation method thereof |
| CN113274965A (en) * | 2021-04-29 | 2021-08-20 | 福建立亚化学有限公司 | Preparation method of polycarbosilane with high ceramic yield |
| CN114015058A (en) * | 2021-10-28 | 2022-02-08 | 福建立亚化学有限公司 | High-conversion-rate ceramic precursor polycarbosilane material and preparation method thereof |
| CN114249899A (en) * | 2021-12-30 | 2022-03-29 | 江西信达航科新材料科技有限公司 | Liquid low-oxygen modified polycarbosilane and preparation method thereof |
| CN115305011A (en) * | 2022-08-08 | 2022-11-08 | 中电化合物半导体有限公司 | Preparation method and application of polishing material |
| CN115573056A (en) * | 2022-09-27 | 2023-01-06 | 宁波杭州湾新材料研究院 | Low-oxygen silicon carbide fiber and preparation method thereof |
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| CN112126064A (en) * | 2020-09-24 | 2020-12-25 | 长沙科航特种织造有限公司 | Preparation method of novel solid silicon carbide ceramic precursor |
| CN112126064B (en) * | 2020-09-24 | 2022-04-05 | 宁波曙翔新材料股份有限公司 | Preparation method of solid silicon carbide ceramic precursor |
| CN112300397A (en) * | 2020-11-05 | 2021-02-02 | 江西信达航科新材料科技有限公司 | High-performance polycarbosilane and preparation method thereof |
| CN113274965A (en) * | 2021-04-29 | 2021-08-20 | 福建立亚化学有限公司 | Preparation method of polycarbosilane with high ceramic yield |
| CN114015058A (en) * | 2021-10-28 | 2022-02-08 | 福建立亚化学有限公司 | High-conversion-rate ceramic precursor polycarbosilane material and preparation method thereof |
| CN114249899A (en) * | 2021-12-30 | 2022-03-29 | 江西信达航科新材料科技有限公司 | Liquid low-oxygen modified polycarbosilane and preparation method thereof |
| CN115305011A (en) * | 2022-08-08 | 2022-11-08 | 中电化合物半导体有限公司 | Preparation method and application of polishing material |
| CN115305011B (en) * | 2022-08-08 | 2023-11-28 | 中电化合物半导体有限公司 | Preparation method and application of polishing material |
| CN115573056A (en) * | 2022-09-27 | 2023-01-06 | 宁波杭州湾新材料研究院 | Low-oxygen silicon carbide fiber and preparation method thereof |
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