CS195596B1 - Regeneration method for vulcanizing agent for polysiloxane rubbers and mixtures thereof - Google Patents
Regeneration method for vulcanizing agent for polysiloxane rubbers and mixtures thereof Download PDFInfo
- Publication number
- CS195596B1 CS195596B1 CS122978A CS122978A CS195596B1 CS 195596 B1 CS195596 B1 CS 195596B1 CS 122978 A CS122978 A CS 122978A CS 122978 A CS122978 A CS 122978A CS 195596 B1 CS195596 B1 CS 195596B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- amine
- molecular weight
- mixtures
- low molecular
- vulcanizates
- Prior art date
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 22
- -1 polysiloxane Polymers 0.000 title claims abstract description 9
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 6
- 229920001971 elastomer Polymers 0.000 title claims description 9
- 239000005060 rubber Substances 0.000 title claims description 9
- 238000011069 regeneration method Methods 0.000 title description 10
- 239000003795 chemical substances by application Substances 0.000 title description 2
- 150000001412 amines Chemical class 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000945 filler Substances 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 4
- 238000009835 boiling Methods 0.000 claims abstract description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000178 monomer Substances 0.000 claims abstract description 4
- 239000002585 base Substances 0.000 claims abstract description 3
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- 238000004821 distillation Methods 0.000 claims abstract description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 claims abstract description 3
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims 2
- 238000006116 polymerization reaction Methods 0.000 claims 2
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims 1
- 125000000129 anionic group Chemical group 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 230000002779 inactivation Effects 0.000 claims 1
- 230000003472 neutralizing effect Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 238000010992 reflux Methods 0.000 claims 1
- 230000001172 regenerating effect Effects 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000001577 simple distillation Methods 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000000654 additive Substances 0.000 abstract description 5
- 229920002379 silicone rubber Polymers 0.000 abstract description 5
- 239000004945 silicone rubber Substances 0.000 abstract description 5
- 239000007858 starting material Substances 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 abstract 1
- 230000008929 regeneration Effects 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PZIBOVBPVADPBS-UHFFFAOYSA-J S(=O)(=O)([O-])[O-].[Si+4].S(=O)(=O)([O-])[O-] Chemical group S(=O)(=O)([O-])[O-].[Si+4].S(=O)(=O)([O-])[O-] PZIBOVBPVADPBS-UHFFFAOYSA-J 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- DVUVKWLUHXXIHK-UHFFFAOYSA-N tetraazanium;tetrahydroxide Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[OH-].[OH-].[OH-].[OH-] DVUVKWLUHXXIHK-UHFFFAOYSA-N 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/21—Cyclic compounds having at least one ring containing silicon, but no carbon in the ring
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
Description
Vynález, se týká způsobu regenerace vulkanizátů polysiloxanových kaučuků a jejich směsí.. Reggnerací podle vynálezu je možno z vulkanizátů siiHonového kaučuku nebo smmsí silionnového kaučuku s obvyklými přísadami a plnivy získat monomem! sloučeniny vhodné pro přípravu polysilooanů.The invention relates to a process for the regeneration of polysiloxane rubber vulcanizates and mixtures thereof. Regeneration according to the invention can be obtained from monomers of silicone rubber or mixtures of silicone rubber with the usual additives and fillers. compounds suitable for the preparation of polysilooanes.
V současné době se regenerace vulkanizát-ů siikonového kaučuku provádí mechanochrmickým způsobem, kdy získaný·regenerát je přidáván jako přísada do čerstvých si^ss. Dále je známo použití mechanických drtí vulkanizátů jako plniv kaučukových sm sí a jako separačních činidel při výrobě lioovaného zbož i.Currently, regeneration of the silicone rubber vulcanizates is carried out in a mechanochrmic manner, whereby the recovered regenerate is added as an additive to fresh SiS. It is further known to use mechanical crushes of vulcanizates as fillers of rubber mixtures and as release agents in the manufacture of molded articles.
U jmenovaných postupů se nejedná o regeneraci v pravém slova srnslu^to je o znovuzískání čistého polymeru nebo m)n(^mmru) ale o vyuziií odpadu při výrobě siiíonnových pryží. Jedná sr tedy o speciální vyučití získaných rrgonerátů.In the mentioned procedures are not regenerated in the truest srnslu ^ it is the recovery of pure polymer, or m) n (^ mmru) but vyuziií waste in siiíonnových rubber. It is therefore a special teaching acquired rrgoneráty.
Uvedené nedostatky odstraňuje podle vynálezu způsob regenerace vulkanizátů polysíloxanových kaučuků a jejich směs. Jeho poddtata spočívá v tom, že sr vulkanizáty, výhodně vr formě drti, rozpc^i^šší^;^í v amnech při současném ohřevu aminu až k bodu varu a míchání a za přídavku od jednoho do deseti hrnoH-notních procent hydrooidů alkalických kovů, kvartorních amouóových a fosfoniových bázi, dále se destilací a připadným sníženém tlaku odstraní amin a katalýzou hydrooidů alkalických kovů' vznókkjicí nízkomolceulároí podíly.According to the invention, these processes are overcome by a process for the regeneration of polysiloxane rubber vulcanizates and a mixture thereof. It is based on the fact that vulcanizates, preferably in the form of pulp, are more soluble in amines while heating the amine to the boiling point and stirring and adding from one to ten percent by weight of the alkali metal hydrooids. The quaternary ammonium and phosphonium bases are further removed by distillation and, if necessary, under reduced pressure, the amine and the catalysis of the alkali metal hydrooids giving rise to low molecular weight fractions.
Účinek regenerace podle vynálezu spočívá v získání směsi monommnů z vulkánizátů i oevulкaoizovaoých směsí si lion ového kaučuku, kterou je po úpravě možno použit jako výchozí surovinu pro přípravu polysilooanů. Způsob zároveň umžž^L^Ur regeneraci plniv obsažených v původní smst.. Po vhodné úpravě jsou plniva, znovu pouuitelná.The regeneration effect according to the invention consists in obtaining a mixture of monomones from both vulcanizates and o-vulcanized mixtures of ionic rubber, which after treatment can be used as a starting material for the preparation of polysilooanes. The process also allows the regeneration of the fillers contained in the original mixture. After suitable treatment, the fillers are reusable.
Při regeneraci dochází k chemickému odbourávání pclysiloxanového řetězce vr směsi pllymr-J^P.oiva přísady nebo u neplněného vulkanizátů, popřípadě u nevulkanizlvaných sěěi. Způsob lze poučit pro vulkanizáty perooidické, radiační, polyкondrnzační, a to jednosl^o žkové i dvousloikové a vulkanizáty adični.During the regeneration, the polylysiloxane chain is chemically degraded in the mixture of the pllymr-β-P. additive or in the case of unfilled vulcanizates or in unvulcanized networks. The process can be used for perooid, radiation, polycondensation vulcanizates, both single- and double-stranded and addition vulcanizates.
Podle vynálezu bylo zjištěno, žs vulkanizáty si ooxanových polymerů, •smmsi polymerů s plnivy a běžnými přísadami vr vulkaiúzovaném i nevulkanizovaném stavu sr rozpouštějí v aminech typu:According to the invention, it has been found that vulcanizates dissolve oxox polymers, blends of polymers with fillers and conventional additives in both the vulcanized state and the unvulcanized state with a sol in the amines of the type:
kdrkdr
R1 H H alif.» » » HHR 1 HH aliph. »» HH
R2 H alif. » ’ alif.> >> HHR 2 H aliph. »HIF
R3 alif.’ alif . > > alif.’’» cyklo- feny 1 ___________________________________heoyl_________ alif . » ..........C3 —C 7 alif . > ». C2-C4 a 1 if . » >» ..........ci-c4R3 alif. >> aliph. ´ ´ »cyclopheny 1 ___________________________________heoyl_________ alif. ».......... C3 — C 7 alif. > ». C2-C4 and 1 if. Ci-c4
Rolppožšění v amnech lzs vyssěslit jako nuk keo oi Íoí ^Ьь^-п^ dusíku z aminu na křemík síranového řetězce. Reakce má reverzibilní průběh, po odstranění aminu dojde к obnovení původního charakteru látky.The amalgamation in the amines can be dried out as a nucleate of nitrogen from the amine to the silicon sulfate chain. The reaction is reversible, after removal of the amine the substance is restored to its original character.
Přídavkem hydroxidu alkalického kovu se značně urychlí rozpouštění látky v aminech a dojde zároveň ke vzniku aktivních center na řetězci štěpných produktů, čímž se rozpouštění stane irreverzibilni. Po odstranění aminu nevznikne původní materiál, ale za vhodných podmínek dochází к depolymeraci, která je podporována odstraňováním vznikajících nízkomolekulárních podílu.The addition of an alkali metal hydroxide greatly accelerates the dissolution of the substance in the amines and at the same time the active centers on the fission product chain are formed, thereby rendering the dissolution irreversible. After removal of the amine, the original material is not formed, but under appropriate conditions depolymerization occurs, which is aided by the removal of the resulting low molecular weight fractions.
Získané nízkomo1ekulární podíly lze známým procesem depolymerace v přítomnosti 1 až 2 hmot. % hydrokidu alkalického kovu a za vhodných podmínek převést na monomery, použitelné pr.o přípravu siloxanových polymerů .The low molecular weight fractions obtained may be a known depolymerization process in the presence of 1 to 2 wt. % of an alkali metal hydrocide and, under suitable conditions, converted to monomers useful in the preparation of siloxane polymers.
Výtěžek nízkomo1eku1árních podílů vzniklých regenerací se pohybuje v závislosti na účinnosti chemicko-inženýrského procesu v rozmezí 70 až -85 % hm. , počítáno na původní obsah polymeru.Depending on the efficiency of the chemical engineering process, the yield of the low-molecular-weight fractions produced by the regeneration is in the range of 70 to -85% by weight. calculated on the original polymer content.
Amin použitý к regeneraci je recyklován v plném rozs ahu.The amine used for regeneration is fully recycled.
Způsob podle vynálezu je dále blíže popsán na příkladu provedení.The process according to the invention is described in more detail below by way of example.
Příklad g plněného polykondenzačního vulkanizátu ve formě drti bylo smícháno se 750 g di-n-buty1 aminu ve vytápěné reakční nádobě, opatřené účinným míchadlem, teploměrem a hlavou rektífikační kolony. «Směs byla zahřívána na teplotu bodu varu aminu při současném míchání. Zároveň bylo přidáno 2,5 hm.% tetráme ty1amoniumhydroxidu, čímž se podstatně zkrátila doba rozpouštění vulkani zátu.Example g of filled polycondensation vulcanizate in the form of pulp was mixed with 750 g of di-n-butyl amine in a heated reaction vessel equipped with an efficient stirrer, a thermometer and a head of the rectifying column. The mixture was heated to the boiling point of the amine with stirring. At the same time, 2.5 wt.% Of tetra-ammonium hydroxide was added, substantially reducing the dissolution time of the vulcanization.
Po dokonalém rozpuštění bylo přidánoAfter complete dissolution was added
Claims (1)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS122978A CS195596B1 (en) | 1978-02-27 | 1978-02-27 | Regeneration method for vulcanizing agent for polysiloxane rubbers and mixtures thereof |
| GB7849821A GB2015550B (en) | 1978-02-27 | 1978-12-22 | Reclamation of siloxanes |
| FR7900813A FR2418249A1 (en) | 1978-02-27 | 1979-01-12 | PROCESS FOR REGENERATION OF VULCANIZED POLYSILOXANE RUBBERS AND THEIR MIXTURES |
| DE19792901698 DE2901698A1 (en) | 1978-02-27 | 1979-01-17 | PROCESS FOR THE REGENERATION OF POLYSILOXANE RUBBER VOLCANIZATIONS AND THEIR MIXTURES |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS122978A CS195596B1 (en) | 1978-02-27 | 1978-02-27 | Regeneration method for vulcanizing agent for polysiloxane rubbers and mixtures thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS195596B1 true CS195596B1 (en) | 1980-02-29 |
Family
ID=5346162
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS122978A CS195596B1 (en) | 1978-02-27 | 1978-02-27 | Regeneration method for vulcanizing agent for polysiloxane rubbers and mixtures thereof |
Country Status (4)
| Country | Link |
|---|---|
| CS (1) | CS195596B1 (en) |
| DE (1) | DE2901698A1 (en) |
| FR (1) | FR2418249A1 (en) |
| GB (1) | GB2015550B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5504235A (en) * | 1994-06-15 | 1996-04-02 | Kanegafuchi Chemical Industry Co., Ltd. | Method for decomposing polysiloxane |
| FR2733988B1 (en) * | 1995-05-11 | 1997-08-01 | Rhone Poulenc Chimie | PROCESS FOR THE MANUFACTURE OF CYCLOSILOXANES BY DEPOLYMERIZATION OF POLYSILOXANES |
| DE19521009A1 (en) * | 1995-06-08 | 1996-12-12 | Wacker Chemie Gmbh | Continuous thermal degradation of organopolysiloxanes |
| NL1003475C2 (en) * | 1996-07-01 | 1998-01-12 | Rhone Poulenc Chimie | Cyclic poly-di:organo-siloxane cpds. for prodn. of silicone(s) |
| DE102005033063B3 (en) | 2005-07-15 | 2007-01-25 | Cht R. Beitlich Gmbh | Remove the silicone coating from coated fabrics and airbags |
| CN109651427B (en) * | 2019-01-10 | 2021-07-02 | 枣阳市金鹏化工有限公司 | Waste silica gel cracking process |
-
1978
- 1978-02-27 CS CS122978A patent/CS195596B1/en unknown
- 1978-12-22 GB GB7849821A patent/GB2015550B/en not_active Expired
-
1979
- 1979-01-12 FR FR7900813A patent/FR2418249A1/en active Granted
- 1979-01-17 DE DE19792901698 patent/DE2901698A1/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| GB2015550B (en) | 1983-01-19 |
| GB2015550A (en) | 1979-09-12 |
| DE2901698A1 (en) | 1979-09-06 |
| FR2418249B3 (en) | 1981-10-02 |
| FR2418249A1 (en) | 1979-09-21 |
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