CN1056862C - 稳定有机聚硅氧烷的方法 - Google Patents
稳定有机聚硅氧烷的方法 Download PDFInfo
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 17
- 238000009833 condensation Methods 0.000 claims abstract description 11
- 230000005494 condensation Effects 0.000 claims abstract description 11
- 239000003463 adsorbent Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 4
- -1 phosphorus compound Chemical class 0.000 claims description 47
- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical compound OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 claims description 36
- 229910052698 phosphorus Inorganic materials 0.000 claims description 30
- 239000011574 phosphorus Substances 0.000 claims description 30
- 239000002594 sorbent Substances 0.000 claims description 26
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 235000012222 talc Nutrition 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 239000010457 zeolite Substances 0.000 claims description 2
- 238000011067 equilibration Methods 0.000 abstract 1
- 150000003018 phosphorus compounds Chemical class 0.000 abstract 1
- 230000008707 rearrangement Effects 0.000 abstract 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002118 epoxides Chemical class 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000003019 stabilising effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 125000002521 alkyl halide group Chemical group 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008406 cosmetic ingredient Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 125000002769 thiazolinyl group Chemical group 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
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- 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
- C08G77/04—Polysiloxanes
- C08G77/32—Post-polymerisation treatment
- C08G77/34—Purification
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- 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
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
- C10M107/50—Lubricating compositions characterised by the base-material being a macromolecular compound containing silicon
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Abstract
本发明涉及一种用于稳定有机聚硅氧烷的方法,所述的有机聚硅氧烷含有促进其缩合和/或平衡的磷腈和/或它们的反应产物。为了稳定任何先前已知的含磷腈和/或它们的反应产物的有机聚硅氧烷以防止重排,并防止其分子量的变化以及由此产生的粘度的变化,建议将所说的磷化合物与至少一种非碱性固体吸附剂接触。
Description
本发明涉及一种稳定有机聚硅氧烷的方法,所述的有机聚硅氧烷是在磷腈或它们的反应产物的存在下,借助于含有硅键合的氧的有机硅化合物的缩合和/或平衡制备的,在该方法中,使这些物质与吸附性固体接触。
如果在反应后不钝化或除去磷腈,那么,在作为催化剂的磷腈的存在下,借助于含有硅键合的氧的有机硅化合物的缩合和/或平衡制备的有机聚硅氧烷在储存期间常常改变它们的分子量,并因此改变它们的粘度。例如US-A3398176(1968年8月20日出版,Wacker-Chemie GmbH)披露了借助与叔胺的反应使磷腈钝化,在该专利中所述的磷腈为磷氮氯化物。DE-A3428581(1986年2月13日公开,Wacker-ChemieGmbH)描述了用碱性锂化合物如氢氧化锂或硅氧烷醇锂使采用磷腈制备的有机聚硅氧烷稳定化。DE-A3742069(1989年6月22日公开,Wacker-Chemie GmbH)是描述使用硅氮烷如六甲基二硅氮烷或1,3-二乙烯基-1,1,3,3-四甲基-二硅氮烷使磷腈催化剂钝化的许多专利的一个例子。使用磷腈催化剂制备的有机聚硅氧烷的另一稳定方法是与二价或三价金属的氧化物、氢氧化物或碳酸盐反应,例如与氧化镁反应,该方法披露于DE-A3533028(1987年3月19日公开,Wacker-Chemie GmbH)。EP-B0117503(1987年5月13日出版,Wacker-Chemie GmbH)披露了使用环氧化物使磷腈催化剂钝化。
用于稳定使用磷腈或磷氮氯化物制备的有机聚硅氧烷的所有上述的方法中,均使用了与酸性催化剂反应的化合物。除中性环氧化物以外,这些化合物都是碱性物质。在绝大多数的方法中,磷腈催化剂和钝化剂的反应产物完全或部分保留在有机聚硅氧烷中,只有在DE-A3533028所述的方法中,它们被除去。
本发明提供一种稳定有机聚硅氧烷的方法,该有机硅聚氧烷含有促进其缩合和/或平衡的磷腈和/或它们的反应产物;该方法包括将特定的磷化合物与至少一种非碱性的固体吸附剂接触。
根据本发明的方法,可稳定任何先前已知的含磷腈和/或它们的反应产物的有机聚硅氧烷而防止其重排,并防止其分子量的改变,以及由此产生的粘度的改变。
根据本发明被稳定的有机聚硅氧烷优选具有下述通式:
X(SiR2O)nSiR2X (I)式中,R在每种状态下可相同或不同,并且是H,或SiC键合的、一价的、未取代或取代的烃基,前提条件是每个硅原子至多有一个硅键合的氢原子,
X在每种状态下可相同或不同,并且是羟基,氯或基团-OSiRaR1 3-a,其中R如上定义,R1为通过氧键合至硅上的一价、未取代或取代的烃基,
a为0,1,2或3
n为至少4的整数。
尽管没有被常用的通式所表示,但是,至多5%(摩尔)的二有机硅氧烷单元可被其它硅氧烷替代,而且这些硅氧烷通常只是作为杂质或多或少难免存在的,如RSiO3/2和/或SiO4/2单元,式中R如上定义。
R的例子是烷基如甲基、乙基、正丙基、异丙基、正丁基和仲丁基;烯基如乙烯基和烯丙基;芳基如苯基,烷芳基如甲苯基和二甲苯基;芳烷基如苄基。
一价、取代的烃基R的例子是氰烷基如β-氰乙基;卤烷基如3,3,3-三氟丙基;卤芳基如邻-、间-、和对-氯苯基。
由于它们的便于获得性,因此至少50%的R基团优选甲基,余下的R基团优选乙烯基和/或苯基。此外,还优选存在硅键合的氢。
基团R1的例子为甲氧基、乙氧基和甲氧基亚乙氧基(CH3OCH2CH2O-),和被R取代的苯氧基。
粘度优选为2-10000mm2/s(25℃),特别优选为10-5000mm2/s的有机聚硅氧烷可以被稳定,并防止其发生变化。
本发明的方法对通式(I)中X为卤素或-SiR3,如三甲基甲硅烷基,二甲基乙烯基甲硅烷基或二甲基氢甲硅烷基,或一些X为氢,剩下的X为-SiR3的那些有机聚硅氧烷最为重要。
根据本发明的方法,可以稳定一种类型的有机聚硅氧烷,或至少两种不同类型有机聚硅氧烷的混合物。
存在于根据本发明相对于粘度改变而稳定的有机聚硅氧烷中的磷腈可以是先前可用来促进含硅键合的氧的有机硅化合物缩合和/或平衡的任何磷腈。
这样的磷腈的例子为由2mol PCl5和1mol NH4Cl反应得到的那些,如在US-A3839388(1974年10月1日出版,Wacker-Chemie GmbH)中所披露的,或者是在德国申请号P4317909.6(R.Hager,Wacker-Chemie GmbH;1993年5月28日申请)中描述的那些,或是在DE-A3725377(1989年2月9日公开,Wacker-Chemie GmbH)和德国专利申请号P4317978.9(R.Hager,Wacker-Chemie GmbH,1993年5月28日申请)中披露的含硅磷腈。
由磷腈促进的缩合和/或平衡制备的有机聚硅氧烷是否仍含主要地是未改变的磷腈或者主要地是磷腈与硅氧烷、硅氧烷醇或次要成分如水的反应产物,取决于所用磷腈的种类、硅氧烷起始化合物的种类以及反应条件。
这种反应产物的确切的描述通常是不可能的。总的来说,该反应产物具有可与原先所用的磷腈的反应产物相媲美的促进有机聚硅氧烷缩合和/或平衡反应的能力。
含磷腈和同样也促进缩合和/或平衡的它们的反应产物的有机聚硅氧烷的制备通常是已知的,并描述于例如上述的US-A3330388,DE-A4205201(1992年8月27日公开,Dow Corning S.A.),US-A5210129(1993年5月11日出版,Dow Corning S.A.),上面引用的DE-A3625377和德国申请P4317909.6和P4317978.9中。
以包含磷化合物的有机聚硅氧烷的总重量为准,通过本发明的方法稳定的有机聚硅氧烷中磷腈和/或它们的反应产物的含量优选为1-500ppm,特别优选为3-200ppm。
在本发明的方法中,所用的非碱性吸附剂优选活性炭,炭黑,硅胶,漂白土,滑石,玻璃粉和沸石;其中活性炭是特别优选的。
根据本发明所用的吸附剂可是这些吸附剂的一种或多种的混合物。
一旦特定的磷化合物与吸附剂接触,它们对有机硅化合物只有很低的促进其缩合和/或平衡的作用(如果有)。
在本发明的方法中,含有磷化合物并待稳定的有机聚硅氧烷可以各种方法与吸附剂接触。方法A
在该方法中,含有磷化合物并待稳定的有机聚硅氧烷用吸附剂进行处理,例如通过搅拌将吸附剂和有机聚硅氧烧混合,优选是均匀混合,随后将载有磷化合物的吸附剂从有机聚硅氧烷中分离出来。
待稳定的有机聚硅氧烷与吸附剂的接触时间,即从添加吸附剂至载有磷化合物的吸附剂被分离出来的时间优选为5分钟至5小时,特别优选从10分钟至3小时。
载有磷化合物的吸附剂最好通过过滤或离心分离而分离出来。
以该方式处理的有机聚硅氧烷基本上完全不含磷腈和它们的反应产物。
在此所用的吸附剂的粒径优选为1μm-5mm,特别优选为20μm至1mm。根据本发明所用的吸附剂的比表面积以BET方法测量优选至少为104m2/kg,特别优选至少为105m2/kg。
在本发明的方法A中,以含有磷化合物的有机聚硅氧烷的总重量为基准,吸附剂的用量优选为0.005-5%(重量),特别优选为0.01-2%(重量)。
本发明的方法A优选在0-200℃、特别是室温至120℃和优选900-1100hPa压力的条件下进行。然而,使用更高或更低的压力也是可能的。方法B
在该方法中,将含有磷化合物并待稳定的有机聚硅氧烷通过一过滤床进行过滤,该床含有吸附剂或被吸附剂覆盖。以该方法处理的有机聚硅氧烷同样也不含磷腈组份。
在该方法中使用的吸附剂可是任何上述的吸附剂。
过滤床上的吸附剂量优选为0.01-10g/m2,特别优选为0.1至5g/m2。
在本发明的方法B中,以含有磷化合物的有机聚硅氧烷的总重量为准,所用的过滤床优选含有0.01-5%(重量)的吸附剂,特别优选为0.05-2%(重量)。
本发明的方法B优选为在0-200℃、特别是室温至120℃进行。
本发明的方法即方法A和方法B两种方法具有很大的优点,也就是在不用与磷腈反应的碱性物质或其它物质的情况下,可以以简单和温和的方式从有机聚硅氧烷中基本上完全除去磷腈和同样也促进有机聚硅氧烷缩合和/或平衡的它们的反应产物。本发明的稳定方法还有一个优点就是在吸附剂作用下,有机聚硅氧烷不发生任何变化。
根据本发明稳定的有机聚硅氧烷可用于通过已知方法稳定的有机聚硅氧烷能用的所有场合,如个人护理用品和化妆品配料,作为螺纹润滑剂(thread lubricants),用于制备有机聚硅氧烷弹性体,和生产防粘涂料。此外,根据本发明稳定的有机聚硅氧烷适用于例如用于电工技术中作为变压器油,电绝缘油以及电绝缘硅橡胶的原始材料。
在下面的例子中,除非另有说明,所有的份数和百分数均以重量计,下面的例子在环境压力即约1000hPa和室温即约20℃,或在室温混合反应物不另外加热或冷却时建立起的温度进行。
下面给出的所有粘度为25℃时的粘度。实施例1
于155℃将208g(1mol)PCl5和26.7g(0.5mol)在160ml 1,2,3-三氯丙烷中的NH4Cl的混合物搅拌5小时。冷却至室温后,将7.5ml水在2小时内计量加入淡黄色溶液中。随后,在最高100℃和1hPa的压力除去挥发性组份。剩下的残余物为95g黄棕色油状液体,其密度为1.8g/ml,主要由化合物PCl3=N-PCl2=N-PCl2O和PCl3=N(-PCl2=N)2-PCl2O组成。为了能准确测量所用的少量成分,制备在醋酸乙酯中该磷腈混合物的10%的浓溶液。
在装有搅拌器的烧瓶中,将240g粘度为25mm2/s的α,ω-双(三甲基甲硅烷氧基)聚甲基氢硅氧烷和100g粘度为350mm2/s的α,ω-双(三甲基甲硅烷氧基)聚二甲基硅氧烷于120℃与0.35ml上述的磷腈溶液混合,并在此温度搅拌10分钟。
冷却至室温后,将1g比表面积(根据BET)为800m2/g的活性炭(由Merck-Schuchardt以“activated carbon,pure”的牌号市售)搅拌入该反应混合物中。从加入活性炭起30分钟后,通过直径为6.5cm的多孔玻璃过滤该混合物。如此得到的有机聚硅氧烷是无色、澄清的油,粘度为35mm2/s,并有平均成分Me3Si[OSiMe2]35[OSiMeH]150SiMe3。该产物呈中性,并且甚至在180℃加热1小时其粘度仍不改变。
为了测量磷含量,于80℃将100g有机聚硅氧烷与100ml去离子水剧烈混合1小时。然后将两相分离,通过ICP(原子发射光谱学)分析水相。磷含量在检测极限0.2mg/kg测试物质以下。因此,在该产物中不存在任何磷化合物。实施例2
将1000g粘度约120mm2/s的α,ω-二羟基聚二甲基硅氧烷和125g粘度为30mm2/s的α,ω-二乙烯基聚二甲基硅氧烷的混合物于120℃与0.15ml实施例1所述的磷腈溶液混合。随后将反应器的压力降至1hPa,并在这些条件下将该混合物搅拌30分钟。移去热源并将反应器的压力再调至大气压。
一旦该反应混合物冷却至约50℃,就通过直径为6.5cm和每平方厘米过滤面积用约0.1g比表面积(根据BET)为800m2/g的活性炭(由Merck-Schuchardt以“activated carbon,pure”的牌号市售)覆盖的多孔玻璃进行过滤。滤液为α,ω-二乙烯基聚二甲基硅氧烷,粘度为880mm2/s。该产物为澄清的中性物质,在180℃加热1小时其粘度不改变。
然后使用实施例1所述的步骤,通过ICP测定磷含量。该测量表明,磷含量低于0.2mg/kg测试物质。因此已完全除去了磷腈和它们的反应产物。实施例3
在装有搅拌器的烧瓶中,将1200g粘度为25mm2/s的α,ω-双(三甲基甲硅烷氧基)聚甲基氢硅氧烷和500g粘度为350mm2/s的α,ω-双(三甲基甲硅烷氧基)聚二甲基硅氧烷于120℃与175ml实施例1所述的磷腈溶液混合,并在此温度将该混合物搅拌10分钟。
冷却至室温后,将平均组成为Me3Si[OSiMe2]35[OSiMeH]150SiMe3的如此得到的有机聚硅氧烷分四份,每份300g,通过直径为6.5cm并事先用1g比表面积(根据BET)为800m2/g的活性炭(由Merck-Schuchardt以“activated carbon,pure”的牌号市售)覆盖的多孔玻璃进行过滤。
每份都过滤后,测定各份的磷含量和酸含量。结果列于表1。使用实施例1所述的步骤借助于ICP光谱学测定磷含量(以ppm计,即每公斤硅氧烷中磷的毫克数)。通过用NaOH溶液滴定来测定酸含量,该值(以ppm计,即mg HCl/kg硅氧烷)由下式计算出,
表1
份 | 酸含量(ppm) | 磷含量(ppm) |
1234 | 001.62.2 | <0.2<0.21.21.7 |
在实施例3所选择的条件下,1g活性炭足以完全或至少几乎完全除去多于600g有机聚硅氧烷中的磷腈或它们的反应产物。实施例4
使用实施例3所述的步骤,将1200g α,ω-双(三甲基甲硅烷氧基)聚甲基氢硅氧烷,500g α,ω-双(三甲基甲硅烷氧基)聚二甲基硅氧烷和1.75ml磷腈溶液的反应重复三次,并将三批产物结合。将平均组成为Me3Si[OSiMe2]35[OSiMeH]150SiMe3的如此得到的有机聚硅氧烷分五份每份500g通过含活性炭的直径为14cm的深床过滤器进行过滤(由Seitz以“SeitzTiefenfilter AKS4-14D”的牌号市售)。
每份都过滤后,如实施例3所述,测定各部分的磷含量和酸含量。结果列于表2。
表2
份 | 酸含量(ppm) | 磷含量(ppm) |
12345 | 00001.8 | <0.2<0.2<0.2<0.21.4 |
在实施例4所选择的条件下,在2000g硅氧烷的滤液中检测不到任何的磷组分,在2500g时仅检测到痕量的酸和磷。
Claims (6)
1、一种用于稳定有机聚硅氧烷的方法,该有机聚硅氧烷含有促进其缩合和/或平衡的磷腈和/或它们的反应产物,该有机聚硅氧烷具有下面通式
X(SiR2O)nSiR2X (I)式中,R在每种状态下可相同或不同,并且是H,或SiC键合的、一价的、未取代或取代的烃基,前提条件是每个硅原子至多有一个硅键合的氢原子,
X在每种状态下可相同或不同,并且是羟基,氯或基团-OSiRaR1 3-a,其中R如上定义,R1为通过氧键合至硅上的一价、未取代或取代的烃基,
a为0,1,2或3,
n为至少4的整数,该方法包括将所述的磷化合物与至少一种非碱性的固体吸附剂接触,其中所用的非碱性吸附剂为活性炭,炭黑,硅胶,漂白土,滑石,玻璃粉和沸石。
2、如权利要求1的方法,其中所用的非碱性吸附剂为活性炭。
3、如权利要求1的方法,其中,将含有磷化合物并待稳定的有机聚硅氧烷用吸附剂处理,然后从有机聚硅氧烷中分离出载有磷化合物的吸附剂。
4、如权利要求3的方法,其中,以含有磷化合物的有机聚硅氧烷的总重量为准,吸附剂的用量为0.005-5%(重量)。
5、如权利要求1的方法,其中,通过含吸附剂或覆盖有吸附剂的过滤床,过滤含有磷化合物并待稳定的有机聚硅氧烷。
6、如权利要求5的方法,其中,以含有磷化合物的有机聚硅氧烷的总重量为准,使用的过滤床含有0.01-5%(重量)的吸附剂。
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GB9103666D0 (en) * | 1991-02-21 | 1991-04-10 | Dow Corning Sa | Method of making organopolysiloxanes |
GB9105372D0 (en) | 1991-03-14 | 1991-05-01 | Dow Corning Sa | Method of making siloxane compositions |
DE4317978A1 (de) * | 1993-05-28 | 1994-12-01 | Wacker Chemie Gmbh | Organosiliciumreste aufweisende Phosphazene, Verfahren zu deren Herstellung und deren Verwendung |
DE4317909A1 (de) * | 1993-05-28 | 1994-12-01 | Wacker Chemie Gmbh | Verfahren zum Kondensieren und/oder Äquilibrieren von Organosiliciumverbindungen |
-
1994
- 1994-06-29 DE DE4422813A patent/DE4422813A1/de not_active Withdrawn
-
1995
- 1995-06-22 ES ES95109671T patent/ES2105821T3/es not_active Expired - Lifetime
- 1995-06-22 DE DE59500527T patent/DE59500527D1/de not_active Expired - Fee Related
- 1995-06-22 EP EP95109671A patent/EP0692513B1/de not_active Expired - Lifetime
- 1995-06-29 CN CN95107722A patent/CN1056862C/zh not_active Expired - Fee Related
- 1995-06-29 JP JP7164122A patent/JP2716680B2/ja not_active Expired - Lifetime
-
1996
- 1996-10-04 US US08/726,850 patent/US5621061A/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3441353A1 (de) * | 1984-11-13 | 1986-05-22 | Licentia Patent-Verwaltungs-Gmbh, 6000 Frankfurt | Verfahren zur reinigung von siliconoel |
DE3533028A1 (de) * | 1985-09-16 | 1987-03-19 | Wacker Chemie Gmbh | Verfahren zum stabilisieren von organopolysiloxanen |
EP0311766A2 (de) * | 1987-08-14 | 1989-04-19 | Wacker-Chemie Gmbh | Herstellung und Weiterverarbeitung von Mischungen mit einem hohen Anteil an Organo-cyclosiloxanen |
Also Published As
Publication number | Publication date |
---|---|
JP2716680B2 (ja) | 1998-02-18 |
EP0692513A1 (de) | 1996-01-17 |
US5621061A (en) | 1997-04-15 |
JPH0848877A (ja) | 1996-02-20 |
ES2105821T3 (es) | 1997-10-16 |
CN1115767A (zh) | 1996-01-31 |
DE59500527D1 (de) | 1997-09-25 |
DE4422813A1 (de) | 1996-01-04 |
EP0692513B1 (de) | 1997-08-20 |
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