CN1117124C - Antioxidant polysiloxane composition - Google Patents
Antioxidant polysiloxane composition Download PDFInfo
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- CN1117124C CN1117124C CN 99125052 CN99125052A CN1117124C CN 1117124 C CN1117124 C CN 1117124C CN 99125052 CN99125052 CN 99125052 CN 99125052 A CN99125052 A CN 99125052A CN 1117124 C CN1117124 C CN 1117124C
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 38
- -1 polysiloxane Polymers 0.000 title claims abstract description 33
- 239000000203 mixture Substances 0.000 title claims abstract description 24
- 239000003963 antioxidant agent Substances 0.000 title description 4
- 230000003078 antioxidant effect Effects 0.000 title description 3
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 34
- 229920001709 polysilazane Polymers 0.000 claims abstract description 25
- 229920002545 silicone oil Polymers 0.000 claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims abstract description 15
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 15
- 229920002050 silicone resin Polymers 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 239000004945 silicone rubber Substances 0.000 claims description 33
- 229920001971 elastomer Polymers 0.000 claims description 22
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 13
- 239000004519 grease Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical group [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 claims description 2
- 150000002825 nitriles Chemical class 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 229920000260 silastic Polymers 0.000 claims 2
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 claims 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims 1
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 claims 1
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 claims 1
- 239000012716 precipitator Substances 0.000 claims 1
- 239000012808 vapor phase Substances 0.000 claims 1
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 2
- 230000032683 aging Effects 0.000 description 18
- 239000000463 material Substances 0.000 description 9
- 238000004073 vulcanization Methods 0.000 description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 230000004580 weight loss Effects 0.000 description 5
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- KENLFYVFRAQGGV-UHFFFAOYSA-N [Li].[N].[Si] Chemical compound [Li].[N].[Si] KENLFYVFRAQGGV-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 239000004636 vulcanized rubber Substances 0.000 description 2
- WRXCBRHBHGNNQA-UHFFFAOYSA-N (2,4-dichlorobenzoyl) 2,4-dichlorobenzenecarboperoxoate Chemical compound ClC1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1Cl WRXCBRHBHGNNQA-UHFFFAOYSA-N 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 description 1
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- 238000007872 degassing Methods 0.000 description 1
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- SMBQBQBNOXIFSF-UHFFFAOYSA-N dilithium Chemical class [Li][Li] SMBQBQBNOXIFSF-UHFFFAOYSA-N 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229920005560 fluorosilicone rubber Polymers 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
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- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
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Abstract
本发明为一种耐氧化的聚硅氧烷组合物，该组合物以一种含Fe聚硅氮烷作为添加剂，从而提高了聚硅氧烷的抗热氧化性能。提供了一种聚硅氧烷组合物的配方及加入含Fe聚硅氮烷的范围。也可用各种商品的硅油、硅橡胶和硅树脂代替本配方的聚硅氧烷胶料从而提高它们在空气中的耐高温性能。The invention is an oxidation-resistant polysiloxane composition, which uses an Fe-containing polysilazane as an additive, thereby improving the thermal oxidation resistance of the polysiloxane. Provided is a formula of polysiloxane composition and the range of adding Fe-containing polysilazane. Various commercial silicone oils, silicone rubbers and silicone resins can also be used to replace the polysiloxane compound of this formula so as to improve their high temperature resistance in the air.
Description
本发明涉及一种耐氧化的聚硅氧烷组合物，其特征在于以含Fe聚硅氮烷作为聚硅氧烷的添加剂。The invention relates to an oxidation-resistant polysiloxane composition, which is characterized in that Fe-containing polysilazane is used as the polysiloxane additive.
硅橡胶是一种广泛地应用于各个领域的耐高温弹性体，而工农业生产的发展和高新技术的进步对它的耐温性提出了越来越高的要求。硅橡胶主链的热降解和侧基的热氧化是影响其耐温性能的两大因素。我们以前的专利93117929.7和93117921.0发明了一种硅氮聚合物，它可以阻止、延缓硅橡胶的主链降解，从而使室温硫化硅橡胶的耐温性能从200℃左右提高到350℃左右。而要进一步提高硅橡胶在空气中的耐温性能还必须解决侧基的氧化问题，目前最常用的y型Fe2O3已不能满足较高的要求。其它聚硅氧烷，如硅油和硅树脂也存在相似的问题。Silicone rubber is a high-temperature-resistant elastomer widely used in various fields, and the development of industrial and agricultural production and the progress of high-tech have put forward higher and higher requirements for its temperature resistance. The thermal degradation of the main chain of silicone rubber and the thermal oxidation of side groups are two factors that affect its temperature resistance. Our previous patents 93117929.7 and 93117921.0 invented a silicon nitrogen polymer, which can prevent and delay the degradation of the main chain of silicone rubber, thereby increasing the temperature resistance of room temperature vulcanized silicone rubber from about 200°C to about 350°C. In order to further improve the temperature resistance of silicone rubber in air, the problem of side group oxidation must be solved, and the most commonly used y-type Fe 2 O 3 can no longer meet the higher requirements. Similar problems exist with other polysiloxanes, such as silicone oils and silicone resins.
CN99/25051-6公开了我们的“含Fe聚硅氮烷及其合成方法”专利申请，该申请提供了含Fe聚硅氮烷的结构及其合成方法。CN99/25051-6 discloses our patent application "Fe-containing polysilazane and its synthesis method", which provides the structure of Fe-containing polysilazane and its synthesis method.
本发明的目的是以该含Fe聚硅氮烷作为聚硅氧烷的的抗氧化添加剂，由于它与聚硅氧烷的相容性优于Fe2O3，因而抗氧效果更佳，又含有硅氮烷结构，可降低其热失重，从而大幅度地提高硅橡胶在空气中的耐温性能。同时，它也可作为抗氧添加剂而应用于其它有机硅高分子(如硅油、硅树脂等)。The object of the present invention is to use this Fe-containing polysilazane as the antioxidant additive of polysiloxane, because its compatibility with polysiloxane is better than Fe 2 O 3 , thus the antioxidative effect is better, and Containing silazane structure can reduce its thermal weight loss, thus greatly improving the temperature resistance of silicone rubber in air. At the same time, it can also be used as an antioxidant additive for other silicone polymers (such as silicone oil, silicone resin, etc.).
本发明的内容是在硅油、硅橡胶和硅树脂聚硅氧烷中添加一种含Fe聚硅氮烷，作为其抗氧化添加剂和提高其抗主链降解性能，从而提高其在空气中的耐温性能。该聚硅氧烷组合物的组份和含量如下(重量份)：The content of the present invention is to add a kind of Fe-containing polysilazane in silicone oil, silicone rubber and silicone resin polysiloxane, as its antioxidant additive and improve its resistance to main chain degradation performance, thereby improving its resistance in air temperature performance. The components and content of the polysiloxane composition are as follows (parts by weight):
聚硅氧烷胶料 100
含Fe聚硅氮烷 0.1--15，较佳为0.5-5；所述聚硅氧烷胶料可为各种商品硅油、硅橡胶及其混炼胶和硅树脂。The polysilazane containing Fe 0.1--15, preferably 0.5-5; the polysiloxane rubber can be various commercial silicone oil, silicone rubber and its compound rubber, and silicone resin.
所述含Fe聚硅氮烷的通式为(A)和(B)：
所述的硅油为粘度300-100000CP的甲基硅油、苯基硅油、乙烯基硅油或氟硅油。The silicone oil is methyl silicone oil, phenyl silicone oil, vinyl silicone oil or fluorosilicone oil with a viscosity of 300-100000CP.
所述的硅橡胶胶料具有以下组份和含量(重量份)：Described silicone rubber compound has following composition and content (weight part):
硅橡胶生胶 100Silicone raw rubber 100
气相法SiO2 10-40Gas phase method SiO 2 10-40
沉淀法SiO2 0-60Precipitation SiO 2 0-60
催化剂 0-2Catalyst 0-2
交联剂或硫化剂 0.3-6
所述的硅橡胶生胶为分子量为1-80万的含氢硅油、羟基硅油、二甲基硅橡胶、甲基乙烯基硅橡胶、甲基苯基硅橡胶、氟硅橡胶或腈硅橡胶。催化剂为有机锡类催化剂或铂催化剂。交联剂为Si(OEt)4或KH-CL交联剂。硫化剂为过氧化苯甲酰、2，4-二氯过氧化苯甲酰、过苯甲酸叔丁酯、过氧化二异丙苯、过氧化二叔丁基或2，5-二甲基-2，5-二叔丁基过氧化己烷。硅脂为锂基硅脂，白炭黑硅脂或炭黑硅脂。The silicone rubber raw rubber is hydrogen-containing silicone oil, hydroxyl silicone oil, dimethyl silicone rubber, methyl vinyl silicone rubber, methylphenyl silicone rubber, fluorosilicone rubber or nitrile silicone rubber with a molecular weight of 1-800,000. The catalyst is an organotin catalyst or a platinum catalyst. The crosslinking agent is Si(OEt) 4 or KH-CL crosslinking agent. The vulcanizing agent is benzoyl peroxide, 2,4-dichlorobenzoyl peroxide, tert-butyl perbenzoate, dicumyl peroxide, di-tert-butyl peroxide or 2,5-dimethyl- 2,5-Di-tert-butylperoxyhexane. The silicone grease is lithium-based silicone grease, white carbon black silicone grease or carbon black silicone grease.
其合成方法和步骤如下：Its synthetic method and steps are as follows:
(1)制备硅氮烷的锂盐(1) Preparation of lithium salt of silazane
将硅氮烷(带2～4个NH)与丁基锂在N2保护下，在有机溶剂中搅拌进行反应。反应完成后，减压除溶剂，然后用正己烷进行洗涤1～4次，减压抽干得到硅氮锂盐。根据硅氮烷与丁基锂的反应比例，可以得到二锂盐、三锂盐或四锂盐。Silazane (with 2 to 4 NH) and butyllithium are reacted with stirring in an organic solvent under the protection of N 2 . After the reaction is completed, the solvent is removed under reduced pressure, and then washed with n-hexane for 1 to 4 times, and dried under reduced pressure to obtain silicon nitrogen lithium salt. According to the reaction ratio of silazane and butyllithium, dilithium salt, trilithium salt or tetralithium salt can be obtained.
(2)合成含Fe聚硅氮烷(2) Synthesis of Fe-containing polysilazane
将上述步骤得到的硅氮锂盐与FeX3或FeX2(X＝Cl，Br)在有机溶剂中进行缩聚反应。FeX3和FeX2与硅氮锂盐的官能团摩尔比控制在1∶0.5～3，反应温度为-30～145℃，反应时间为0.5～24小时。反应完成后，砂芯过滤并洗涤1～5次，至滤液基本无色，合并滤液，蒸馏除溶剂，稍加热减压抽干，即得到聚硅氮烷，可为液体，半固体，硬脆固体。The lithium silicon nitrogen salt obtained in the above steps is subjected to polycondensation reaction with FeX 3 or FeX 2 (X=Cl, Br) in an organic solvent. The functional group molar ratio of FeX 3 and FeX 2 to silicon nitrogen lithium salt is controlled at 1:0.5-3, the reaction temperature is -30-145°C, and the reaction time is 0.5-24 hours. After the reaction is completed, the sand core is filtered and washed 1 to 5 times until the filtrate is basically colorless, the filtrate is combined, the solvent is distilled off, and the polysilazane is obtained after a little heating and vacuum drying, which can be liquid, semi-solid, hard and brittle solid.
本发明的配方工艺：Formula technology of the present invention:
在100份的上述聚硅氧烷胶料中加入0.1--15份含Fe聚硅氮烷，然后按各自聚硅氧烷胶料通用的加工方法，如调匀脱气、混炼等。Add 0.1--15 parts of Fe-containing polysilazane to 100 parts of the above-mentioned polysiloxane rubber, and then follow the common processing methods for each polysiloxane rubber, such as mixing thoroughly, degassing, mixing, etc.
本发明耐氧化的聚硅氧烷组合物经空气中高温热老化，测定其老化失重、凝胶时间或老化前后的力学性能变化，见表1、表2，可见具有良好的抗氧化性能。The oxidation-resistant polysiloxane composition of the present invention is subjected to high-temperature thermal aging in the air, and its aging weight loss, gel time, or changes in mechanical properties before and after aging are measured. See Table 1 and Table 2. It can be seen that it has good oxidation resistance.
表1、凝胶时间与添加剂的关系
表2、老化失重与时间的关系
实施例1(对比例)Embodiment 1 (comparative example)
在玻璃样品皿(直径35mm)中加入厚度为3mm的300CP的107甲基硅油，然后于300℃老化箱中鼓风老化，测定其凝胶时间和热失重。其结果如表1和表2所示。Add 300CP 107 methyl silicone oil with a thickness of 3mm into a glass sample dish (diameter 35mm), then air-blast aging in a 300°C aging box, and measure its gel time and thermal weight loss. The results are shown in Table 1 and Table 2.
实施例2(对比例)Embodiment 2 (comparative example)
在玻璃样品皿(直径35mm)中加入厚度为3mm的300CP107甲基硅油100份及5份Fe2O3，搅拌混匀后，于300℃老化箱中鼓风老化，测定其凝胶时间和热失重。其结果如表1和表2所示。Add 100 parts of 300CP107 methyl silicone oil and 5 parts of Fe 2 O 3 with a thickness of 3 mm into a glass sample dish (diameter 35 mm), stir and mix well, then age in a 300°C aging box with air blast, and measure its gel time and heat weightlessness. The results are shown in Table 1 and Table 2.
实施例3Example 3
在玻璃样品皿(直径35mm)中加入厚度为3mm的300CP107甲基硅油100份及5份含Fe聚硅氮烷，搅拌混匀后，于300℃老化箱中鼓风老化，测定其凝胶时间和热失重。其结果如表1和表2所示。Add 100 parts of 300CP107 methyl silicone oil with a thickness of 3mm and 5 parts of Fe-containing polysilazane into a glass sample dish (35mm in diameter), stir and mix well, then age in a 300°C aging box to measure its gel time and heat loss. The results are shown in Table 1 and Table 2.
从表1可以看出，实施例3含Fe聚硅氮烷的抗氧化效果比Fe2O3要好得多，它明显延长了甲基硅油的凝胶时间；同时从表2可以看出，实施例3的老化失重也比实施例2和1要低。As can be seen from Table 1, the antioxidant effect of the Fe-containing polysilazane in Example 3 is much better than Fe 2 O 3 , and it obviously prolongs the gel time of methyl silicone oil; as can be seen from Table 2 simultaneously, the implementation The aging weight loss of Example 3 is also lower than that of Examples 2 and 1.
实施例4(对比例)Embodiment 4 (comparative example)
将15g气相法SiO2、30gCaCO3加入到100g107胶中在捏合机捏炼1.5小时，取出后在三辊筒炼胶机上混炼2次，得到的胶料在135℃的烘箱中烘3小时，冷却后再回炼2次得到硅橡胶胶料A。Add 15g of gas-phase SiO 2 and 30g of CaCO 3 into 100g of 107 rubber and knead in a kneader for 1.5 hours, take it out and knead twice on a three-roller rubber mixer, and bake the obtained rubber in an oven at 135°C for 3 hours. After cooling, it was milled back twice to obtain the silicone rubber material A.
在烧杯中称入100份硅橡胶胶料A和5份Fe2O3，混匀后再混炼1次，加入Si(OEt)41份，然后到入到聚四副氟乙烯摸具中，硫化后得到约2mm厚的硫化胶片，然后切成哑里铃状试片。将试片于300℃老化箱中鼓风老化，测定其力学性能。Weigh 100 parts of silicone rubber material A and 5 parts of Fe 2 O 3 into a beaker, mix well and knead again, add 1 part of Si(OEt) 4 , and then put it into a polytetrafluoroethylene mold , After vulcanization, a vulcanized film about 2mm thick is obtained, and then cut into dumbbell-shaped test pieces. The test pieces were aged in a 300°C aging box to determine their mechanical properties.
实施例5Example 5
将15g气相法SiO2、30gCaCO3加入到100g107胶中在捏合机捏炼1.5小时，取出后在三辊筒炼胶机上混炼2次，得到的胶料在135℃的烘箱中烘3小时，冷却后再回炼2次得到硅橡胶胶料A。Add 15g of gas-phase SiO 2 and 30g of CaCO 3 into 100g of 107 rubber and knead in a kneader for 1.5 hours, take it out and knead twice on a three-roller rubber mixer, and bake the obtained rubber in an oven at 135°C for 3 hours. After cooling, it was milled back twice to obtain the silicone rubber material A.
在烧杯中称入100份硅橡胶胶料A和5份含Fe聚硅氮烷，混匀后，再混炼1次，加入Si(OEt)41份，然后到入到聚四副氟乙烯摸具中，硫化后得到约2mm厚的硫化胶片，然后切成哑里铃状试片。将试片于300℃老化箱中鼓风老化，测定其力学性能。Weigh 100 parts of silicone rubber compound A and 5 parts of Fe-containing polysilazane into a beaker, mix well, then knead again, add 1 part of Si(OEt) 4 , and then add polytetrafluoroethylene In the mould, after vulcanization, a vulcanized film with a thickness of about 2mm is obtained, and then cut into dumbbell-shaped test pieces. The test pieces were aged in a 300°C aging box to determine their mechanical properties.
实施例6Example 6
将15g气相法SiO2、30gCaCO3加入到100g107胶中在捏合机捏炼1.5小时，取出后在三辊筒炼胶机上混炼2次，得到的胶料在135℃的烘箱中烘3小时，冷却后再回炼2次得到硅橡胶胶料A。Add 15g of gas-phase SiO 2 and 30g of CaCO 3 into 100g of 107 rubber and knead in a kneader for 1.5 hours, take it out and knead twice on a three-roller rubber mixer, and bake the obtained rubber in an oven at 135°C for 3 hours. After cooling, it was milled back twice to obtain the silicone rubber material A.
在烧杯中称入100份硅橡胶胶料A和5份含Fe聚硅氮烷，混匀后，再混炼1次，加入KH-CL5份，然后到入到聚四副氟乙烯摸具中，硫化后得到约2mm厚的硫化胶片，然后切成哑里铃状试片。将试片于300℃老化箱中鼓风老化，测定其力学性能。Weigh 100 parts of silicone rubber material A and 5 parts of Fe-containing polysilazane into a beaker, mix well, then knead once more, add 5 parts of KH-CL, and then put it into the polytetrafluoroethylene mold , After vulcanization, a vulcanized film about 2mm thick is obtained, and then cut into dumbbell-shaped test pieces. The test pieces were aged in a 300°C aging box to determine their mechanical properties.
实施例7Example 7
将15g气相法SiO2、30gCaCO3加入到100g108胶中在捏合机捏炼1.5小时，取出后在三辊筒炼胶机上混炼2次，得到的胶料在135℃的烘箱中烘3小时，冷却后再回炼2次得到硅橡胶胶料A。Add 15g of gas-phase SiO 2 and 30g of CaCO 3 to 100g of 108 rubber and knead in a kneader for 1.5 hours, take it out and knead twice on a three-roller rubber mixer, and bake the obtained rubber in an oven at 135°C for 3 hours. After cooling, it was milled back twice to obtain the silicone rubber material A.
在烧杯中称入100份硅橡胶胶料A和5份含Fe聚硅氮烷，混匀后，再混炼1次，加入KH-CL5份，然后到入到聚四副氟乙烯摸具中，硫化后得到约2mm厚的硫化胶片，然后切成哑里铃状试片。将试片于300℃老化箱中鼓风老化，测定其力学性能。Weigh 100 parts of silicone rubber material A and 5 parts of Fe-containing polysilazane into a beaker, mix well, then knead once more, add 5 parts of KH-CL, and then put it into the polytetrafluoroethylene mold , After vulcanization, a vulcanized film about 2mm thick is obtained, and then cut into dumbbell-shaped test pieces. The test pieces were aged in a 300°C aging box to determine their mechanical properties.
实施例8Example 8
将15g气相法SiO2、30gCaCO3加入到100g氟硅胶中在捏合机捏炼1.5小时，取出后在三辊筒炼胶机上混炼2次，得到的胶料在135℃的烘箱中烘3小时，冷却后再回炼2次得到硅橡胶胶料A。Add 15g gas-phase SiO 2 and 30g CaCO 3 into 100g fluorosilica gel and knead in a kneader for 1.5 hours, take it out and knead twice on a three-roller rubber mixer, and bake the obtained rubber in an oven at 135°C for 3 hours , and then re-milled twice to obtain silicone rubber material A after cooling.
在烧杯中称入100份硅橡胶胶料A和5份含Fe聚硅氮烷，混匀后，再混炼1次，加入KH-CL5份，然后到入到聚四副氟乙烯摸具中，硫化后得到约2mm厚的硫化胶片，然后切成哑里铃状试片。将试片于300℃老化箱中鼓风老化，测定其力学性能。Weigh 100 parts of silicone rubber material A and 5 parts of Fe-containing polysilazane into a beaker, mix well, then knead once more, add 5 parts of KH-CL, and then put it into the polytetrafluoroethylene mold , After vulcanization, a vulcanized film about 2mm thick is obtained, and then cut into dumbbell-shaped test pieces. The test pieces were aged in a 300°C aging box to determine their mechanical properties.
实施例9Example 9
将3g Ph2Si(OH)2、25g气相法SiO2、60gCaCO3和5份含Fe聚硅氮烷加入到100g甲基乙烯基硅橡胶中混炼，加入过氧化苯甲酰2份再混炼，在硫化机上硫化。硫化后得到约2mm厚的硫化胶片，然后切成哑里铃状试片。将试片于300℃老化箱中鼓风老化，测定其力学性能。Add 3g Ph 2 Si(OH) 2 , 25g gas phase SiO 2 , 60g CaCO 3 and 5 parts of Fe-containing polysilazane to 100g of methyl vinyl silicone rubber for mixing, add 2 parts of benzoyl peroxide and mix again Refined and vulcanized on a vulcanizing machine. After vulcanization, a vulcanized film with a thickness of about 2 mm is obtained, and then cut into dumbbell-shaped test pieces. The test pieces were aged in a 300°C aging box to determine their mechanical properties.
实施例10Example 10
将3g Ph2Si(OH)2、25g气相法SiO2、60gCaCO3和1份含Fe聚硅氮烷加入到100g甲基乙烯基硅橡胶中混炼，加入2，4-二氯过氧化苯甲酰2份再混炼，在硫化机上硫化。硫化后得到约2mm厚的硫化胶片，然后切成哑里铃状试片。将试片于300℃老化箱中鼓风老化，测定其力学性能。Add 3g Ph 2 Si(OH) 2 , 25g gas phase SiO 2 , 60g CaCO 3 and 1 part of Fe-containing polysilazane to 100g methyl vinyl silicone rubber for mixing, add 2,4-dichloroperoxybenzene 2 parts of formyl are mixed again and vulcanized on a vulcanizing machine. After vulcanization, a vulcanized rubber sheet with a thickness of about 2 mm is obtained, and then cut into dumbbell-shaped test pieces. The test pieces were aged in a 300°C aging box to determine their mechanical properties.
实施例11Example 11
将3g Ph2Si(OH)2、25g气相法SiO2、60gCaCO3和1份含Fe聚硅氮烷加入到100g甲基乙烯基硅橡胶中混炼，加入2，4-二氧过氧化苯甲酰2份再混炼，在硫化机上硫化。硫化后得到约2mm厚的硫化胶片，然后切成哑里铃状试片。将试片于300℃老化箱中鼓风老化，测定其力学性能。Add 3g Ph 2 Si(OH) 2 , 25g gas-phase SiO 2 , 60g CaCO 3 and 1 part of Fe-containing polysilazane to 100g methyl vinyl silicone rubber for mixing, add 2,4-dioxoxybenzene 2 parts of formyl are mixed again and vulcanized on a vulcanizing machine. After vulcanization, a vulcanized rubber sheet with a thickness of about 2 mm is obtained, and then cut into dumbbell-shaped test pieces. The test pieces were aged in a 300°C aging box to determine their mechanical properties.
实施例12Example 12
将20g气相法SiO2、10g硬脂酸锂和1份含Fe聚硅氮烷加入到100g甲基硅油中在捏合、混炼制成硅脂。将试片于300℃老化箱中鼓风老化，测定其滴点、蒸发量与析油量。Add 20g of gas phase SiO 2 , 10g of lithium stearate and 1 part of Fe-containing polysilazane to 100g of methyl silicone oil and knead and knead to make silicone grease. The test piece was aged in a 300°C aging box with air blowing, and its dropping point, evaporation and oil separation were measured.
Claims (8)
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| CN 99125052 CN1117124C (en) | 1999-11-25 | 1999-11-25 | Antioxidant polysiloxane composition |
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| CN104312169A (en) * | 2014-09-19 | 2015-01-28 | 天长市荣盛有机硅科技有限公司 | Corrosion resistant silicone rubber material and preparation method thereof |
| CN104725879B (en) * | 2015-03-19 | 2017-08-04 | 山东大学 | A kind of ablation-resistant organosilicon compound and its preparation method and application |
| CN105622943B (en) * | 2016-03-24 | 2018-06-05 | 山东大学 | A kind of synthesis of the high molecular weight silicone of while nitrile group-containing and vinyl and the preparation method of additional hot vulcanized nitrile silicone rubber |
| CN106146853B (en) * | 2016-06-30 | 2019-09-27 | 东莞市贝特利新材料有限公司 | LED liquid casting glue heat-resistant agent and preparation method thereof |
| CN110128999A (en) * | 2019-05-15 | 2019-08-16 | 华成新材料（惠州）有限公司 | A kind of fire-retardant bonded adhesives of one-component additional organosilicon and preparation method thereof |
| CN112375389A (en) * | 2020-10-21 | 2021-02-19 | 佛山科学技术学院 | High-temperature-resistant silicon rubber and preparation method and application thereof |
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