CN114249899A - Liquid low-oxygen modified polycarbosilane and preparation method thereof - Google Patents
Liquid low-oxygen modified polycarbosilane and preparation method thereof Download PDFInfo
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- CN114249899A CN114249899A CN202111655670.3A CN202111655670A CN114249899A CN 114249899 A CN114249899 A CN 114249899A CN 202111655670 A CN202111655670 A CN 202111655670A CN 114249899 A CN114249899 A CN 114249899A
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- polycarbosilane
- modified polycarbosilane
- oxygen
- liquid low
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- 229920003257 polycarbosilane Polymers 0.000 title claims abstract description 27
- 239000001301 oxygen Substances 0.000 title claims abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 19
- AWJFCAXSGQLCKK-UHFFFAOYSA-N icosa-1,19-diene Chemical compound C=CCCCCCCCCCCCCCCCCC=C AWJFCAXSGQLCKK-UHFFFAOYSA-N 0.000 claims description 18
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 11
- NPYRNNDTSBRCSK-UHFFFAOYSA-N dichloro(chloromethyl)silane Chemical compound ClC[SiH](Cl)Cl NPYRNNDTSBRCSK-UHFFFAOYSA-N 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 4
- DQEUYIQDSMINEY-UHFFFAOYSA-M magnesium;prop-1-ene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C=C DQEUYIQDSMINEY-UHFFFAOYSA-M 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000007810 chemical reaction solvent Substances 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 10
- -1 ceramic coatings Substances 0.000 abstract description 3
- 229910052573 porcelain Inorganic materials 0.000 abstract description 3
- 238000005524 ceramic coating Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract description 2
- 239000012761 high-performance material Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 26
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- UZNGRHDUJIVHQT-UHFFFAOYSA-M magnesium;prop-1-ene;bromide Chemical compound [Mg+2].[Br-].C[C-]=C UZNGRHDUJIVHQT-UHFFFAOYSA-M 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002431 hydrogen Chemical group 0.000 description 1
- 229910001623 magnesium bromide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- C08G2150/00—Compositions for coatings
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
Abstract
The invention relates to liquid low-oxygen modified polycarbosilane and a preparation method thereof, in particular to a structure shown in a formula (I). The compound shown in the formula (I) with a novel structure is designed and synthesized, has high porcelain yield and low oxygen content, can be used for preparing high-performance materials such as ceramic coatings, fibers and the like, and has wide application.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to liquid low-oxygen modified polycarbosilane and a preparation method thereof.
Background
Polycarbosilane is a kind of high molecular compound, its main chain is composed of silicon and carbon atoms alternatively, the silicon and carbon atoms are connected with hydrogen or organic group, and its molecular chain is linear or branched structure. Polycarbosilane is the most important compound in precursor polymers (advanced polymers) which are newly appeared in a high-technology new material, and is mainly used for preparing high-technology ceramic materials of silicon carbide series. The ceramic material prepared by the polycarbosilane has excellent performances of high modulus, high temperature resistance, corrosion resistance, oxidation resistance, low density and the like, and has wide application in high-technology fields such as advanced aerospace vehicle structural components, high-temperature engines, turbines, nuclear reactor walls, high-temperature sensors and the like. However, there is still a need to develop new polycarbosilanes having low oxygen content and high porcelain yield.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a liquid low-oxygen modified polycarbosilane and a preparation method thereof.
In order to achieve the object of the present invention, one aspect of the present invention provides a liquid low-oxygen modified polycarbosilane having a structure represented by the following formula (I),
wherein R is selected from hydrogen, methyl and ethyl; m is a natural number, preferably, m is a natural number between 1 and 10.
In another aspect, the invention provides a process for the preparation of a compound of formula (I) which is prepared by reacting a polycarbosilane with 1, 19-eicosadiene.
In some preferred embodiments, the present invention provides a method for preparing a compound of formula (I) according to the present invention, wherein the mass ratio of 1, 19-eicosadiene to polycarbosilane is: 1, (0.5-20).
In some preferred embodiments, the invention provides a preparation method of the compound shown in the formula (I), wherein the reaction temperature is 25-115 ℃.
In some preferred embodiments, the present invention provides a method for preparing the compound represented by formula (I), wherein the reaction solvent is toluene, xylene, N-dimethylformamide or tetrahydrofuran.
In some preferred embodiments, the present invention provides a method for preparing the compound represented by formula (I) according to the present invention, which further comprises a process of curing and pyrolysis, wherein the curing process is performed by using a tube furnace, and the curing process is performed by: keeping the temperature at 120 ℃ for 2h, keeping the temperature at 190 ℃ for 2h, keeping the temperature at 210 ℃ for 4h, and keeping the heating rate at 1-5 ℃/min; the curing atmosphere is an inert atmosphere, preferably nitrogen or argon.
In some preferred embodiments, the invention provides a preparation method of the compound shown in the formula (I), wherein the mass ratio of the 1, 19-eicosadiene to the organic solvent is 1 (2-20).
The polycarbosilane is prepared by the following reaction steps:
(1) adding magnesium chips into a tetrahydrofuran solvent which is purified and dried to obtain a mixed system;
(2) mixing tetrahydrofuran and chloromethyl dichlorosilane to obtain a mixed solution;
(3) dropwise adding the mixed solution obtained in the step (2) into the mixed system obtained in the step (1), and stirring at the reaction temperature of-15-80 ℃;
(4) adding allyl magnesium bromide into the reaction product obtained in the step (3).
In the step (1), the mass ratio of the magnesium chips to the tetrahydrofuran is 1 (1-35);
in the step (2), the mass ratio of the chloromethyl dichlorosilane to the tetrahydrofuran is 1 (5-25); the mass ratio of the allyl magnesium bromide to the chloromethyl dichlorosilane is 1 (0.5-20).
Compared with the prior art, the invention has the beneficial effects that:
the compound shown in the formula (I) with a novel structure is designed and synthesized, has high porcelain yield and low oxygen content, can be used for preparing high-performance materials such as ceramic coatings, fibers and the like, and has wide application.
Detailed Description
The following representative examples are intended to better illustrate the present invention and are not intended to limit the scope of the present invention. The materials used in the following examples are all commercially available unless otherwise specified.
Example 1
A constant pressure funnel, a thermometer and a magnetic stirrer are respectively arranged on a 500ml three-necked bottle, and dry nitrogen is introduced to control the flow rate to be about 200ml/min, so as to establish a water-free and oxygen-free system. Respectively adding 7.80g of magnesium chips and 60g of tetrahydrofuran into a three-necked bottle, placing 70g of chloromethyldichlorosilane and 70g of tetrahydrofuran into a constant-pressure funnel, slowly dropwise adding, controlling the temperature to be-10 ℃ in the dropwise adding process, reacting for 3 hours at normal temperature after the dropwise adding is finished, and then heating to 70 ℃ for reacting for 4 hours. The reaction system was cooled to 0 ℃ and 15g of alkenyl magnesium bromide and 110g of tetrahydrofuran were added dropwise. After the dropwise addition, the temperature is raised to 70 ℃ again for reaction for 48 hours, and yellow oily substances are obtained after washing, drying and reduced pressure distillation.
A constant pressure funnel, a thermometer and a magnetic stirrer are respectively arranged on a 500ml three-necked bottle, and dry nitrogen is introduced to control the flow rate to be about 200ml/min, so as to establish a water-free and oxygen-free system. 25g of 1, 19-eicosadiene were added to a three-necked flask, then 110g of xylene were added, the temperature was raised to 50 ℃ with stirring, and the mixture was stirred until the dissolution was complete. Then adding 40g of the yellow oily matter prepared in the previous step, heating to 100 ℃, continuing stirring for reaction for 10 hours, stopping stirring, removing the oil bath, and standing for 10-20 hours. The solvent was pumped off to give the final product.
30g of the product was placed in a ceramic crucible and cured under high purity nitrogen in the following manner: keeping the temperature at 120 ℃ for 2h, keeping the temperature at 190 ℃ for 2h, keeping the temperature at 210 ℃ for 4h, and keeping the heating rate at 1-5 ℃/min to obtain a compact yellow cured substance; the yellow condensate is placed in a high-temperature tube furnace and cracked for 3 hours at 1400 ℃ under high-purity nitrogen to obtain the ceramic, the yield of the ceramic is 92%, and the oxygen content is 0.10%.
Example 2
A constant pressure funnel, a thermometer and a magnetic stirrer are respectively arranged on a 500ml three-necked bottle, and dry nitrogen is introduced to control the flow rate to be about 200ml/min, so as to establish a water-free and oxygen-free system. Respectively adding 7.80g of magnesium chips and 30g of tetrahydrofuran into a three-necked flask, placing 110g of chloromethyldichlorosilane and 90g of tetrahydrofuran into a constant-pressure funnel, slowly dropwise adding, controlling the temperature to be-10 ℃ in the dropwise adding process, reacting for 3 hours at normal temperature after the dropwise adding is finished, and then heating to 70 ℃ for reacting for 4 hours. The reaction system was cooled to 0 ℃ and 13g of isopropenyl magnesium bromide and 85g of tetrahydrofuran were added dropwise. After the dropwise addition, the temperature is raised to 70 ℃ again for reaction for 48 hours, and yellow oily substances are obtained after washing, drying and reduced pressure distillation.
A constant pressure funnel, a thermometer and a magnetic stirrer are respectively arranged on a 500ml three-necked bottle, and dry nitrogen is introduced to control the flow rate to be about 200ml/min, so as to establish a water-free and oxygen-free system. 35g of 1, 19-eicosadiene and then 130g of xylene are added to a three-necked flask, the temperature is raised to 50 ℃ with stirring and the mixture is stirred until the dissolution is complete. Then adding 30g of the yellow oily matter prepared in the previous step, heating to 100 ℃, continuing stirring for reaction for 10 hours, stopping stirring, removing the oil bath, and standing for 10-20 hours. The solvent was pumped off to give the final product.
30g of the product was placed in a ceramic crucible and cured under high purity nitrogen in the following manner: keeping the temperature at 120 ℃ for 2h, keeping the temperature at 190 ℃ for 2h, keeping the temperature at 210 ℃ for 4h, and keeping the heating rate at 1-5 ℃/min to obtain a compact yellow cured substance; the yellow condensate is put into a high-temperature tube furnace and cracked for 3 hours at the temperature of 1400 ℃ under high-purity nitrogen to obtain the ceramic, the ceramic yield is 91 percent, and the oxygen content is 0.15 percent.
Example 3
A constant pressure funnel, a thermometer and a magnetic stirrer are respectively arranged on a 500ml three-necked bottle, and dry nitrogen is introduced to control the flow rate to be about 200ml/min, so as to establish a water-free and oxygen-free system. Respectively adding 7.60g of magnesium chips and 40g of tetrahydrofuran into a three-necked flask, placing 90g of chloromethyldichlorosilane and 105g of tetrahydrofuran into a constant-pressure funnel, slowly dropwise adding, controlling the temperature to be-10 ℃ in the dropwise adding process, reacting at normal temperature for 3 hours after the dropwise adding is finished, and then heating to 70 ℃ for reacting for 4 hours. The reaction system was cooled to 0 ℃ and 16g of isopropenyl magnesium bromide and 95g of tetrahydrofuran were added dropwise. After the dropwise addition, the temperature is raised to 70 ℃ again for reaction for 48 hours, and yellow oily substances are obtained after washing, drying and reduced pressure distillation.
A constant pressure funnel, a thermometer and a magnetic stirrer are respectively arranged on a 500ml three-necked bottle, and dry nitrogen is introduced to control the flow rate to be about 200ml/min, so as to establish a water-free and oxygen-free system. 20g of 1, 19-eicosadiene were added to a three-necked flask, 85g of xylene were then added, the temperature was raised to 50 ℃ with stirring, and the mixture was stirred until complete dissolution. Then adding 45g of the yellow oily substance prepared in the step, heating to 100 ℃, continuing stirring for reaction for 10 hours, stopping stirring, removing the oil bath, and standing for 10-20 hours. The solvent was pumped off to give the final product.
30g of the product was placed in a ceramic crucible and cured under high purity nitrogen in the following manner: keeping the temperature at 120 ℃ for 2h, keeping the temperature at 190 ℃ for 2h, keeping the temperature at 210 ℃ for 4h, and keeping the heating rate at 1-5 ℃/min to obtain a compact yellow cured substance; the yellow condensate is placed in a high-temperature tube furnace and cracked for 3 hours at the temperature of 1400 ℃ under high-purity nitrogen to obtain the ceramic, the ceramic yield is 89%, and the oxygen content is 0.11%.
Although the present invention has been described in detail above, those skilled in the art will appreciate that various modifications and changes can be made to the present invention without departing from the spirit and scope of the invention. The scope of the invention is not to be limited by the above detailed description but is only limited by the claims.
Claims (10)
1. A liquid low-oxygen modified polycarbosilane is characterized in that the liquid low-oxygen modified polycarbosilane has a structure shown in the following formula (I),
wherein R is selected from hydrogen, methyl and ethyl; m is a natural number.
2. The method for preparing liquid low-oxygen modified polycarbosilane according to claim 1, wherein m is a natural number between 1 and 10.
3. A method for preparing the liquid modified polycarbosilane with low oxygen content according to claim 1, which is characterized in that the polycarbosilane is prepared by reacting 1, 19-eicosadiene.
4. The method for preparing the liquid low-oxygen modified polycarbosilane according to claim 3, wherein the mass ratio of the 1, 19-eicosadiene to the polycarbosilane is 1 (0.5-20).
5. The method for preparing the liquid low-oxygen modified polycarbosilane according to claim 3, wherein the reaction temperature is 25-115 ℃.
6. The method for preparing a liquid low oxygen modified polycarbosilane as claimed in claim 3, wherein the reaction solvent is toluene, xylene, N-dimethylformamide or tetrahydrofuran.
7. The method for preparing the liquid low-oxygen modified polycarbosilane according to claim 3, wherein the mass ratio of the 1, 19-eicosadiene to the organic solvent is 1 (2-20).
8. The method for preparing liquid modified polycarbosilane with low oxygen content as claimed in claims 3-7, wherein the polycarbosilane is prepared by the following reaction steps:
(1) adding magnesium chips into a tetrahydrofuran solvent which is purified and dried to obtain a mixed system;
(2) mixing tetrahydrofuran and chloromethyl dichlorosilane to obtain a mixed solution;
(3) dropwise adding the mixed solution obtained in the step (2) into the mixed system obtained in the step (1), and stirring at the reaction temperature of-15-80 ℃;
(4) adding allyl magnesium bromide into the reaction product obtained in the step (3).
9. The method for preparing the liquid low-oxygen modified polycarbosilane according to claim 8, wherein the mass ratio of the magnesium chips to the tetrahydrofuran in the step (1) is 1 (1-35).
10. The method for preparing the liquid low-oxygen modified polycarbosilane according to claim 8, wherein in the step (2), the mass ratio of the chloromethyldichlorosilane to the tetrahydrofuran is 1 (5-25); the mass ratio of the allyl magnesium bromide to the chloromethyl dichlorosilane is 1 (0.5-20).
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| CN202111655670.3A CN114249899A (en) | 2021-12-30 | 2021-12-30 | Liquid low-oxygen modified polycarbosilane and preparation method thereof |
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