CS197045B1 - Process for preparing dispersion of polyvinylacetate with low wiscosity for surface treatment of glass fibers - Google Patents
Process for preparing dispersion of polyvinylacetate with low wiscosity for surface treatment of glass fibers Download PDFInfo
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- CS197045B1 CS197045B1 CS235378A CS235378A CS197045B1 CS 197045 B1 CS197045 B1 CS 197045B1 CS 235378 A CS235378 A CS 235378A CS 235378 A CS235378 A CS 235378A CS 197045 B1 CS197045 B1 CS 197045B1
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- Prior art keywords
- dispersion
- parts
- glass fibers
- surface treatment
- alkyl
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- 239000006185 dispersion Substances 0.000 title claims description 24
- 239000003365 glass fiber Substances 0.000 title claims description 10
- 229920002689 polyvinyl acetate Polymers 0.000 title claims description 5
- 239000011118 polyvinyl acetate Substances 0.000 title claims description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 238000004381 surface treatment Methods 0.000 title description 4
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 3
- -1 glycol ethers Chemical class 0.000 claims description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000007720 emulsion polymerization reaction Methods 0.000 claims 1
- 150000003014 phosphoric acid esters Chemical class 0.000 claims 1
- 159000000001 potassium salts Chemical class 0.000 claims 1
- 239000000203 mixture Substances 0.000 description 8
- 125000002091 cationic group Chemical group 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000003495 polar organic solvent Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- VYMLCOODZXTLIQ-UHFFFAOYSA-N chromium;2-methylprop-2-enoic acid Chemical class [Cr].CC(=C)C(O)=O VYMLCOODZXTLIQ-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical class [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
Vynález sa týká spósobu přípravy nízkoviskóznoj polyvinylacetátovej disperzie na povrchová úpravu skloněných vlákien.The invention relates to a process for the preparation of a low viscosity polyvinyl acetate dispersion for the treatment of inclined fibers.
Technológia povrchovej úpravy skloněných vlákien kladie na použitú disperziu specifické a vysolconáročné požiadavky. Tieto požiadavlcy vyplývajú zo spósobu použitia disperzie a zo spósobu Salšieho spracovania skleněného vlákna. Pri povrchovej úpravě skleněných vlákien polyvinylacetátové disperzie sa použxvajú ako zložky lubrikačných zmesi spolu s kati onak ti vnytni látkami typu chrómkomplexov kyseliny akrylovej a metakrylovej s katxonaktxvnymi mazadlami, s olektrolytmi a s inými vazbovými prostriedkami. Disperzia musí byt’ odolná voči účinkom uvedených látok. Počas nanášania lubrikačnej zmesi na skleněné vlákno dochádza k styku zmesi s horúcitn vláknom, vplyvom čoho v mieste styku jej teplota prudko stúpne. Ďalším dósledkom styku zmesi s horúcim skleněným vláknom je to, že teplota zmesi v príebehu jej nanášania rastie.The technology of surface treatment of inclined fibers places specific and high-annual requirements on the dispersion used. These requirements result from the use of the dispersion and from the more sophisticated processing of the glass fiber. In the surface treatment of glass fibers, polyvinyl acetate dispersions are used as components of the lubricating compositions together with cationic substances such as acrylic and methacrylic acid chromium complexes with cationic lubricants, with electrolytes and other binding agents. The dispersion must be resistant to the effects of said substances. During application of the lubricant mixture to the glass fiber, the mixture contacts the hot fiber, causing the temperature to rise sharply at the point of contact. A further consequence of contacting the mixture with the hot glass fiber is that the temperature of the mixture increases during application.
Z uvedených dóvodov sa požaduje odolnost’ disperzie voči ostatným zložlcám lubrikačnej zmesi aj pri zvýšenej teplote. Požiadavko odolnosti voči kationaktívnym látkám pri teplote 70 až 80 °C výhovujú disperzie připravené použitím kationaktivnych emulgátorov a to buS samotných, alebo v kombinácii s neionogénnytni emulgátormi a ochrannými koloidmi. Disperzie připravené použitím anionaktívnych emulgátorov uvedenoj požiadavke v plnej miere nevýhovuju, zrážajú sa už pri nižšej teplote. Po povrchovej úpravo skleněné vlákno sa suší priFor these reasons, the dispersion's resistance to other components of the lubricating composition is required at elevated temperature. The requirement for resistance to cationic substances at 70 to 80 ° C is met by dispersions prepared using cationic emulsifiers, either alone or in combination with nonionic emulsifiers and protective colloids. Dispersions prepared using anionic emulsifiers do not fully satisfy this requirement, they precipitate at a lower temperature. After finishing the glass fiber is dried at
197 045197 045
7 O 4 5 teplote 120 až 140 °C. Film polymóru na vlákno musí odolávat’ účinkom uvedenej teploty bez změny farby. Náročnějšío technologie fialšleho spracovania skleněného vlákna požadujú dokonalú rozpustnost’ filmu připraveného z disporzie v nepolárných organických rozpúšťadlách aj po joho vystavení vyššie uvedenému tepelnému namáhaniu, pričom rýchlosť rozpúšťania má byť čo najvačšia. Uvedeným požiadavkám nevyhovujú filmy připravené z disperzi! obsaljujúcich ochranné koloidy. Tieto filmy pri teplote sušenia žltnú a rýchlosť ich rozpúšťania nedosahuje požadované hodnoty. Disperzie připravené použitím kombinácie anionaktívnyoh emulgátorov s neionogónnymi, poskytujú filmy odolné voči teplotám sušenia vlákna. Rýchlosť rozpúšťania týchto filmov v nepolárných organických rozpúšťadlách vyhovuje požiadavkám. Nedosif tatkom týchto disperzi! z hl’adiska ich použitia na povrchovú úpravu skleněných vlókien je ich nizka odolnost’ voči kationaktivnym zložkám lubrikačných zmes! za horúoa.The temperature is 120 to 140 ° C. The polymer film on the fiber must withstand the effect of the specified temperature without discoloration. More sophisticated glass fiber processing technologies require perfect dissolution of the film prepared from dispersion in non-polar organic solvents, even after being subjected to the aforementioned thermal stresses, the dissolution rate being as high as possible. Films prepared from dispersions do not meet these requirements! containing protective colloids. These films turn yellow at the drying temperature and do not reach the desired dissolution rate. Dispersions prepared using a combination of anionic emulsifiers with nonionic ones provide films resistant to fiber drying temperatures. The dissolution rate of these films in non-polar organic solvents complies with the requirements. Do not disperse these dispersions! in terms of their use for the surface treatment of glass fibers, their low resistance to the cationic components of the lubricant mixtures! za horúoa.
Uvedený nodostatok odstraňuje předložený vynález. Spósob prlpravy nízkoviskóznoj polyvinylaoetátovej disperzie podl’a uvedeného vynálezu spočívá v emulznej polymerizácii vinylaeetátu použitím 20 až 120 hmotnostných (hm.) dielov alkylpolyotylónglykoléteru obsáhujúcoho alkyl C12 až C^g a 18 až 60 molov etylonoxidu na mól alkylu a z 1 až 17 hm. dielov sodných a/alobo draselných soli estorov kyseliny fosforečnoj s alkylpolyotylénglykolétermi obsahujúcimi alkyl C1Q až a 3 až 12 molov etylénoxidu na mól alkylu, na 1 000 hm. dielov vinylacetátu.The above removes the present invention. The process for preparing the low viscosity polyvinyl acetate dispersion according to the invention consists in emulsifying polymerization of vinyl acetate using 20 to 120 parts by weight of an alkyl poly (polyol) glycol ether containing from C 12 to C 18 alkyl and from 18 to 60 moles of etylon oxide per mole of alkyl. parts of a sodium / potassium salt of aluminum foil of fosforečnoj eStore alkylpolyotylénglykolétermi containing a C alkyl, and Q1 and 3 to 12 moles of ethylene oxide per mole of alkyl per 1000 wt. parts of vinyl acetate.
Disperzia připravená podl’a předloženého vynálezu vykazuje sušinu 50 až 60 % hm., viskozitu 20 až 100 m Pa.s, pH v rozmedzí 2,5 až 3,5 obsah zbytkového vinylacetátu maximálně 1 % hmot. Je mrazuvzdorná do -7 °C. Účinkom kationaktivnych látok typu chrómkomplcxov kyseliny metakrylovej /obchodného názvu Spolapret VA/ odolává pri 80 °C počas hodin boz změny. Film připravený z disperzie je lesklý, hladký, na povrchu nelopivý. Po tepolnom namáhaní pri 130 °C počas 3 hodin nevykazuje farebnú změnu a je dokonalo rozpustný v styréne, pričom rýchlosť rozpúšťania je v rozsahu 85Ο až 1 150 g/m hod.The dispersion prepared according to the present invention has a dry matter content of 50 to 60% by weight, a viscosity of 20 to 100 mPa.s, a pH in the range of 2.5 to 3.5, a residual vinyl acetate content of at most 1% by weight. It is hardy to -7 ° C. Cationic methacrylic acid-type cationic agents (trade name Spolapret VA) resist boz changes at 80 ° C for hours. The film prepared from the dispersion is glossy, smooth, non-stick on the surface. After thermal stress at 130 ° C for 3 hours it does not show a color change and is completely soluble in styrene, with a dissolution rate ranging from 85Ο to 1150 g / m hr.
Disporzia připravená podl’a námi navrhovaného Spósobu spina všetky nároky kladené technológiou povrchovej úpravy skleněných vlákien. Vyniká zvlášť vysokou odolnosťou voči kationaktivnym látkám v teplotnoj oblasti 70 až 95 °C.The dispersion prepared according to our proposed method of spin all the demands of the glass fiber coating technology. It has a particularly high resistance to cationic substances in the temperature range of 70 to 95 ° C.
Příklad 1 $Example 1 $
V štvorhrdlej 1,5 litrovoj sulfonačnej baňke opatrenej rámovým miešadlom, spatným chladičom, teplomorom a prívodom monoméru sa pripravi vodná fáza pozostávajúca z 367 hm. dielov vody, z 27,5 hm. dielov alkylpolyotylónglykoléteru /obchodného názvu Slovasol 2^30/ a z 5,7 hm. dielov sodnej soli estorov kyseliny fosforečnéj s alkylpolyetylónglykolétermi /obchodného názvu Slovafos 1/, ktorá sa vyhřeje na 70 °C. Pri tejto teploto sa přidá 1,5 hm. dielu peroxodvojsíranu draselného a sa zahájí rovnoměrné dávkováni© 500 hm. diolov vinylacetátu, ktoré trvá 220minút pri 75 °C. Po skončení dávkovania vinylacetátu teplota disperzie sa udržuje pri 75 °C ešte fialšichΛ0 minút. Po tojto dobo disperzia sa vychladí. Připravená disperzia má nasledovné vlastnosti: sušina 58,5 % hm., viskozita 80 m Pa.s, priemerná veHsoeť častíc 5^0 nm. Teplota zrážania s chrómkomploxom kyseliny metakrylovejAn aqueous phase consisting of 367 wt.% Was prepared in a four-necked 1.5 liter sulfonation flask equipped with a frame stirrer, a reflux condenser, a thermometer and a monomer feed. parts of water, from 27.5 wt. parts by weight of alkyl poly (ethylene glycol ether) (trade name Slovasol 2? 30) and from 5.7 wt. parts of the sodium salt of phosphoric acid esters with alkylpolyethylene glycol ethers (trade name Slovafos 1), which is heated to 70 ° C. At this temperature, 1.5 wt. % of potassium peroxydisulphate and a uniform dosage of 500 wt. diols of vinyl acetate which lasted 220 minutes at 75 ° C. After the vinyl acetate dosing is complete, the dispersion temperature is maintained at 75 ° C for a further violet of 0 minutes. After this time the dispersion is cooled. The prepared dispersion has the following properties: dry matter 58.5 wt.%, Viscosity 80 mPa.s, average particle size 50 nm. Precipitation temperature with methacrylic acid chromocloxlo
197 045 obchodného názvu Spolapret VA je 85 °C. Film připravený z disperzio odolává účinkom teploty 130 °C 3 hodiny bez farebnej změny. Rýchlost’ rozpúsťania Filmu v styréne jc 1 000 g/m2 hod.197 045 of the trade name Spolapret VA is 85 ° C. The film prepared from the dispersion is resistant to coloring at 130 ° C for 3 hours. Film dissolution rate in styrene is 1000 g / m 2 hr.
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Přiklad 2Example 2
V aparatúre popísaněj v příklade 1 sa připraví vodná fáza nasledovného zloženia:In the apparatus described in Example 1, an aqueous phase of the following composition is prepared:
410 hm. dielov vody, 27,5 hm. dielov Slovasolu 24-30 a 5,5 hm. dielov Slovafosu 1. Vodná fáza sa vyhřeje na 68 °C. Pri tejto teplote sa přidá 1,5 hm. dielu peroxodvojsíranu draselného a pristúpi sa ku kontlnuálnemu dávkovaniu 500 hm. dielov vinylacetátu. Dávlcovanie trvá 260 minút, počas dávkovania reakčná teplota sa udržuje v rozsahu 73 až 77 °C. Po skon čení dávkovania monoméru sa uskutočni doreagovanie počas 60 minút pri 75 °C. Po tejto době disperzia sa vychladí.410 wt. parts of water, 27.5 wt. parts of Slovasol 24-30 and 5.5 wt. parts of Slovafos 1. The aqueous phase is heated to 68 ° C. At this temperature, 1.5 wt. % of potassium peroxodisulphate and a continuous dosage of 500 wt. parts of vinyl acetate. Dosing takes 260 minutes while maintaining the reaction temperature in the range of 73-77 ° C during dosing. After the monomer dosing is complete, the reaction is carried out for 60 minutes at 75 ° C. After this time, the dispersion is cooled.
Vlastnosti disperzie sa líšia od hodnot Uvedených v příklade 1 v obsahu sušiny á v priemernej velkosti častíc, ktoré sú 56,0 Jo hm. a 356 nm.The dispersion properties differ from the values given in Example 1 in the dry matter content and in the average particle size, which are 56.0% by weight. and 356 nm.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS235378A CS197045B1 (en) | 1978-04-11 | 1978-04-11 | Process for preparing dispersion of polyvinylacetate with low wiscosity for surface treatment of glass fibers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS235378A CS197045B1 (en) | 1978-04-11 | 1978-04-11 | Process for preparing dispersion of polyvinylacetate with low wiscosity for surface treatment of glass fibers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS197045B1 true CS197045B1 (en) | 1980-04-30 |
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ID=5360428
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS235378A CS197045B1 (en) | 1978-04-11 | 1978-04-11 | Process for preparing dispersion of polyvinylacetate with low wiscosity for surface treatment of glass fibers |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS197045B1 (en) |
-
1978
- 1978-04-11 CS CS235378A patent/CS197045B1/en unknown
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