CN100575393C - 在氟化乙烯基聚合物填料存在的情况下加工混合物的方法 - Google Patents
在氟化乙烯基聚合物填料存在的情况下加工混合物的方法 Download PDFInfo
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
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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
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/30—Loose or shaped packing elements, e.g. Raschig rings or Berl saddles, for pouring into the apparatus for mass or heat transfer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/30—Details relating to random packing elements
- B01J2219/302—Basic shape of the elements
- B01J2219/30203—Saddle
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/30—Details relating to random packing elements
- B01J2219/302—Basic shape of the elements
- B01J2219/30215—Toroid or ring
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/30—Details relating to random packing elements
- B01J2219/302—Basic shape of the elements
- B01J2219/30257—Wire
- B01J2219/30265—Spiral
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/30—Details relating to random packing elements
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Abstract
本发明涉及在氟化乙烯基聚合物填料存在的情况下加工含有HCl、H2O及硅氧烷的混合物的方法。
Description
技术领域
本发明涉及在氟化乙烯基聚合物填料存在的情况下加工含有HCl、H2O及硅氧烷的混合物的方法。
背景技术
硅油或聚有机硅氧烷是通过环状或直链聚二有机基硅氧烷中间产物的聚合作用制成的，该中间产物是通过二有机基二氯硅烷的水解作用及缩聚作用制得的。盐酸通常用作水解作用所需反应水的来源。水解作用产生的氯化氢与甲醇反应生成氯甲烷，并且再次被用于根据直接合成法的二甲基二氯硅烷的合成。
在此情况下产生含有HCl、H2O及硅氧烷的混合物。例如US3,493,595A及US 5,476,916A描述了从由环状及直链的含氯聚二有机基硅氧烷组成的粗制水解产物制造α，ω-二羟基聚二有机基硅氧烷的方法。为降低氯含量并分离该环状物质，在逆流中用水蒸汽处理该粗制水解产物。这是在装有填料的塔内针对性地加以实施的。此处使用装有陶瓷填料的塔。该陶瓷由硅铝酸盐及选自以下组中的金属的伴生氧化物(Begleitoxiden)组成：钛、铁、钾、钠、钙及镁。例如可使用陶瓷制成的鞍状填料、贝尔鞍状填料、鲍尔环或特殊形状物。
已发现陶瓷在主要的处理条件下容易受到化学侵蚀。尤其是铝及铁在表面附近从复合材料溶出。这造成材料缺陷，并在硅铝酸盐结构内形成空洞、裂痕及裂缝。表面特性发生改变。该填料的机械稳定性降低。该填料容易破碎。提高的量的难分离的填料磨损部分随塔底产物排出。塔的分离效率持续降低。该填料必须每隔2至3年彻底更换。这造成停工以及采购及清理该填料的花费。
形成的铝化合物及铁化合物，如氯化物、氧氯化物及羟基氯化物，在该α，ω-二羟基聚二有机基硅氧烷中保持溶解或悬浮的形式。这些化合物发挥缩合催化剂的作用，并导致该α，ω-二羟基聚二有机基硅氧烷发生非期望的后缩合作用。粘度无法控制地增加。分离出的水使产品变混浊，并且损害其存储稳定性。由于质量不稳定、水含量不稳定以及所含的铝化合物及铁化合物而使得对聚合物的进一步加工变得困难。
发明内容
本发明的目的是提供一种用于加工含有HCl、H2O及硅氧烷的混合物的方法，该方法中的填料更加稳定。
本发明涉及在氟化乙烯基聚合物的填料存在的情况下加工含有HCl、H2O及硅氧烷的混合物的方法。
具体实施方式
在加工含有HCl、H2O及硅氧烷的混合物的主要条件下，该氟化乙烯基聚合物填料具有化学稳定性、机械稳定性及热稳定性。
该氟化乙烯基聚合物可被部分或完全氟化，优选为由通式1的结构单元组成的氟化乙烯基聚合物
-(CR2-CF2)n- (1)，
其中R代表氢或氟。
n的值优选为至少100，特别优选为至少500。
特别优选为聚偏氟乙烯(PVDF)及聚四氟乙烯(PTFE)。
该填料可具有任意的形状，例如环状、螺旋状及鞍状是合适的，它们优选具有中断墙和/或横撑以增加其表面积。特别优选为鲍尔环。
除HCl、H2O及硅氧烷以外，经加工的混合物可含有其他具有化学活性的组成分，如链烷醇、氯硅烷及氯烃。甲醇及乙醇作为烷醇，而氯甲烷作为氯烃，通常存在于混合物中。HCl及H2O例如可以稀盐酸、饱和盐酸或在少量H2O存在的情况下的HCl气体的形式存在。硅氧烷例如可以带有诸如-OH及卤素的反应性基团的线链或环状硅氧烷的形式存在。该直链硅氧烷优选为部分带有卤素的α，ω-二羟基聚二有机基硅氧烷。
该方法中主要采用的压力优选为0.1至100巴。该方法优选在70至200℃，特别优选在80至150℃下实施。
含有HCl、H2O及硅氧烷的混合物优选在塔内进行加工。加工方法优选包括提纯步骤，如脱酸作用、从硅氧烷去除卤化物；或蒸馏步骤。
优选的方法是用于制造聚二甲基硅氧烷的方法的部分步骤，其中二甲基二氯硅烷与盐酸中的水反应生成由环状及直链型的含氯聚二甲基硅氧烷及气态氯化氢组成的粗制水解产物。
根据本发明的方法特别优选应用于制造聚二甲基硅氧烷的方法，该方法中，
在第一步骤中，二甲基二氯硅烷与盐酸中的水反应生成由环状及直链型的含氯聚二甲基硅氧烷及气态氯化氢组成的制粗水解产物，及
在第二步骤中，用水蒸汽处理该粗制水解产物以降低氯含量并形成盐酸，
其中，将在该第二步骤中形成的盐酸用于该第一步骤中。
该方法本身已由US 5,476,916A公开。在第二步骤中，可使用由氟化乙烯基聚合物填料填充的塔。
根据本发明的方法同样特别优选应用于制造聚二甲基硅氧烷的方法，该方法中，
在第一步骤中，二有机基二氯硅烷与盐酸中的水反应生成由环状及直链型的含氯聚二有机基硅氧烷及气态氯化氢组成的粗制水解产物，
在第二步骤中，用水蒸汽处理该粗制水解产物以降低氯含量并形成盐酸，其中，将在该第二步骤中形成的盐酸用于该第一步骤中，
在第三步骤中，用水蒸汽处理该具有降低的氯含量的粗制水解产物，以进一步降低氯含量并形成含有盐酸及聚二有机基硅氧烷的酸性水，
其中，将该酸性水分离成不含酸的水及含酸的水，使该含酸的水蒸发，并将所得含酸的水蒸汽用于该第二步骤中。
该方法本身已由DE 199 09 547 A公开。在第二及第三步骤中，可使用由氟化乙烯基聚合物填料填充的塔。
其他优选的方法是：从含有硅氧烷的HCl-酸性水-醇混合物中回收醇的方法。此处优选为蒸馏法，其中使用氟化乙烯基聚合物填料。
从由甲醇及HCl制造氯甲烷时制得的HCl-酸性水-醇混合物回收甲醇的方法是特别优选的。
由用盐酸水解烷氧基硅烷的方法回收醇，尤其是甲醇及乙醇的方法同样是特别优选的。该方法本身已由US 6,069,220A公开。
Claims (4)
1、在氟化的乙烯基聚合物填料存在的情况下加工含有HCl、H2O及硅氧烷的混合物的方法，其中所述氟化的乙烯基聚合物由通式(1)的结构单元组成
-(CR2-CF2)n- (1)，
其中R代表氢或氟，而n的值至少为100。
2、如权利要求1所述的方法，其中所述氟化的乙烯基聚合物选自聚偏氟乙烯(PVDF)及聚四氟乙烯(PTFE)。
3、如权利要求1或2所述的方法，其是在70至200℃下加以实施的。
4、如权利要求1或2所述的方法，其中所述加工包括选自以下组中的提纯步骤：脱酸作用、从硅氧烷去除卤化物以及蒸馏步骤。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102005032947A DE102005032947A1 (de) | 2005-07-14 | 2005-07-14 | Verfahren zur Verarbeitung von Gemischen in Anwesenheit von Füllkörpern aus fluorierten Vinylpolymeren |
| DE102005032947.0 | 2005-07-14 |
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| Publication Number | Publication Date |
|---|---|
| CN1903916A CN1903916A (zh) | 2007-01-31 |
| CN100575393C true CN100575393C (zh) | 2009-12-30 |
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| CN200610105687A Expired - Fee Related CN100575393C (zh) | 2005-07-14 | 2006-07-14 | 在氟化乙烯基聚合物填料存在的情况下加工混合物的方法 |
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| Country | Link |
|---|---|
| US (1) | US7601791B2 (zh) |
| EP (1) | EP1746121B1 (zh) |
| JP (1) | JP2007023281A (zh) |
| KR (1) | KR100791133B1 (zh) |
| CN (1) | CN100575393C (zh) |
| DE (2) | DE102005032947A1 (zh) |
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| DE1645671A1 (de) | 1951-01-28 | 1970-09-24 | Wacker Chemie Gmbh | Verfahren zur Reinigung von Organopolysiloxanoelen |
| US3478886A (en) * | 1967-03-31 | 1969-11-18 | Atomic Energy Commission | Graft-copolymer column support material for liquid-liquid partition chromatography |
| US3577266A (en) * | 1969-01-13 | 1971-05-04 | Du Pont | Superficially porous chromatographic packing with sulfonated fluoropolymer coating |
| DE2521742C3 (de) * | 1975-05-15 | 1978-12-21 | Wacker-Chemie Gmbh, 8000 Muenchen | Verfahren zur Herstellung von Organosiloxanen |
| US4448981A (en) * | 1983-05-13 | 1984-05-15 | General Electric Company | Method of making organosiloxanes and alkyl halides from dialkyldialkoxysilanes |
| US4576763A (en) | 1984-06-27 | 1986-03-18 | Nutter Dale E | Packings for gas-liquid contact apparatus |
| US5766565A (en) * | 1993-01-21 | 1998-06-16 | Dow Corning Corporation | Purification of hydrochloric acid |
| DE4343033A1 (de) | 1993-12-16 | 1995-06-29 | Wacker Chemie Gmbh | Verfahren zur Herstellung von Polydimethylsiloxanen |
| DE19800023A1 (de) | 1998-01-02 | 1999-07-08 | Huels Silicone Gmbh | Kontinuierliches Verfahren zur Herstellung von Polyorganosiloxanen |
| DE19909547A1 (de) | 1999-03-04 | 2000-09-07 | Wacker Chemie Gmbh | Abwasserfreie Herstellung von Polydiorganosiloxanen |
| US6372022B1 (en) | 2000-08-10 | 2002-04-16 | Air Liquide America Corporation | Ionic purifier |
-
2005
- 2005-07-14 DE DE102005032947A patent/DE102005032947A1/de not_active Withdrawn
-
2006
- 2006-05-24 DE DE502006001014T patent/DE502006001014D1/de active Active
- 2006-05-24 EP EP06010750A patent/EP1746121B1/de not_active Expired - Fee Related
- 2006-07-04 KR KR1020060062434A patent/KR100791133B1/ko not_active IP Right Cessation
- 2006-07-05 US US11/481,113 patent/US7601791B2/en not_active Expired - Fee Related
- 2006-07-13 JP JP2006192843A patent/JP2007023281A/ja active Pending
- 2006-07-14 CN CN200610105687A patent/CN100575393C/zh not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| US7601791B2 (en) | 2009-10-13 |
| DE502006001014D1 (de) | 2008-08-14 |
| KR20070009396A (ko) | 2007-01-18 |
| US20070015891A1 (en) | 2007-01-18 |
| EP1746121B1 (de) | 2008-07-02 |
| DE102005032947A1 (de) | 2006-08-24 |
| EP1746121A1 (de) | 2007-01-24 |
| JP2007023281A (ja) | 2007-02-01 |
| CN1903916A (zh) | 2007-01-31 |
| KR100791133B1 (ko) | 2008-01-02 |
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