![]() Method of producing mixed polyethyleneglycol formals
专利摘要:
A fiber preparation containing or consisting of a polyglycol ether mixed formal of the formula R1-(OC2H4)n-OCH2OCH2CH2OR2 in which R1 is a linear or branched alkyl or alkenyl radical of from 8 to 22 carbon atoms, R2 is a linear alkyl radical of from 1 to 4 carbon atoms and n is an integer of from 3 to 30. 公开号:SU1209035A3 申请号:SU803211174 申请日:1980-12-04 公开日:1986-01-30 发明作者:Клебер Рольф;Билленштайн Зигфрид 申请人:Хехст Аг (Фирма); IPC主号:
专利说明:
S1 To the image; T (; Ina refers to the preparation of smoked formals of a yulene glycol of the general formula Rf- (OC ,, H) -OCll2nC H | O - ACi RFC With upnl, oleyl; R. - 0 - C; shkil, p 3-15 , and can (Zyt used in the chemical pro1 1YP1 penny, and formals for finishing fibers Example 1 Into a 2 liter round-bottomed flask equipped with a thermometer and apparatus for removing the process from the cycle, 446 g (1 mol) of the product of interaction with 1 mol of fatty alcohol C with .. 5 mol of ethylene oxide, 410 g (mol di- (methyl glycol) -formal And 3 g of concentrated sulfuric acid and stirred for about 6 hours at. At the same time, very weak nitrogen is passed through. The acidic catalyst particles obtained in the reaction mixture are neutralized with powdered NaOH, Then the excess di (met: ilglycol-formal and the methylglycol formed is distilled off at 100 ° C and a vacuum of 5 mbar. The desired product in the form of an ostak after distillation is freed by filtration from its content of salts. 510 g are obtained (96% of theory) compounds of formula R - (OS „H) gh- pCY20C H40CH, h, and R is a mixture of C | j-C1-alkyl t ruppr which are found in coconut fatty acid. The residual hydroxyl number is 15. The product when is a clear liquid that dissolves easily in cold water, Example 2 In a half-liter with a stirrer, equipped with a thermal meter, J93 g (0.5 mol) of the reaction product between mol of a fatty alcohol with 12-14 carbon atoms with 4 mol of ethylene oxide, 273 g (1; 1 mol) di- (Butyl glycol) -formal and 1 g of chloride ka, 8.2 g of paraformaldehyde (mol) J as well as 1 g at 150 C are stirred for 3 h “At the same time, a very weak stream of nitrogen is passed over the surface, After cooling to 70 ° C, the neutralization catalyst contained in the reaction mixture is caustic soda powder, Excess di- (butnlglycol) - -formal is distilled off under an aqueous 20 mbar at 160 ° C. S3Following after the distillation at the bottom of the final procedure, the filter is released from the salt content; 228 g of the compound of the R formula is obtained - (OC., H) d- OCll ,, where R is C, -, - C,; / --a) kil; The hydroclyable number of the residue is 22, which corresponds to an 86% conversion degree. At 20 ° C, the product is in the form of a gallonic liquid, EXAMPLE 3, a 2-liter flask supplied with a stirrer and a thermomete-metric Cd is placed 460 g (O ,, 5 mol) of the product of the reaction 1 mol oleyl alcohol 15 moles ettpep oxide c (1 p zero) drg- (em Ilglycol) -formal® 8 :, 5 g of paraformaldehyde, Ij35 g of zinc chloride and 1. 35 g and stirred at 15 ° C for 6 hours. The acidic portion of catalysts contained in the reaction mixture is cooled to sodium sulfate, powdered sodium hydroxide, Then an excess of di- (ethyl glycol) - -formal and the formed etushglycol at 100 ° C is distilled off under a vacuum of 5 mbar. The target product in the form of residual Kc. after distillation, it is free from salts containing salts in it. 490 g (96% of theory) of the compounds R- (OC2H ,,) are obtained, g is OCH. ,, H, where R is oleyl - (C, g with -; shkenyl) The product at 20 ° C is a clear liquid 5 easily dissolved in cold water, Example 4 In 1-liter bu with a stirrer equipped with a thermometer j load 350 g (0.64 mol) of the reaction product 1 mol of fatty alcohol C. C 14 with 8 mol of ethylene oxide, 262 1 (1; 6 mol) di (methyl glycol) - -formal 2, 4 g of zinc chloride and 2 g; and stirred for 6 hours. At the same time, a weak stream of nitrogen is passed over the surface. After cooling, the day to 70 ° C is neutralized and then distilled of the beaten (methylglycol) -formal at 160 ° C. under vacuum. 375 g of yellowish liquid of low viscosity at 20 C, which corresponds to the formula R- (OS., H) g -OCH., OS, C AISI, where R C.2-0, is alkyl „ The residual hydroxyl number is 19 ,, which corresponds to the degree of grevrev, en 1 the aqueous solution is cloudy at 55 ° C, Example 5 Into a half-liter flask with a stirrer, 270 g (1 mol) of the product of the reaction of 1 mol of Cg fatty alcohol with 3 mol of ethylene oxide, 360 g (2.2 mol of di- (methyl glycol) -fornal and 1.2 g of chloride 16.5 g of paraformaldehyde (0.5 mol) J, as well as 1.2 g of bLPO, at 60 ° C and stirred in 3 hours At the same time, a very weak stream of nitrogen is passed over the surface. After cooling to 70 ° C, the reaction mixture contained in the reaction mixture is neutralized with caustic soda powder. Then the excess di- (methyl glycol) formal is distilled off under a vacuum of 20 mbar at. The final product remaining at the bottom after distillation by filtration is freed from the content of their salts, 340 g of compound of the formula are obtained,). Example 6. A half-liter flask equipped with a stirrer and thermometer was charged with 308 g (0., A mol) of the product of the reaction of 1 mol of Cfj fatty alcohol with 12 mol of ethylene oxide, 164 g (mol) of di- (methyl glycol) -formal and 1 g of zinc chloride and g of paraformaldehyde (0.25 mol), as well as 1 g, and at 150 C are stirred for about 3 hours. At the same time, a very weak stream of nitrogen is passed over the surface, After cooling to 70 ° C, the catalyst components in the reaction mixture are neutralized with catalyst components using sodium hydroxide powder. Then the excess di - (methyl glycol) formal is distilled off at 160 ° C under a vacuum of 15 mbar. The final product remaining in the precipitate by filtration is freed from the contained salts. 326 g of a compound of the formula C j, H - (,) are obtained. Example 7 In a half-liter flask equipped with a stirrer and a thermometer, 336 g (0.35 mol) of the product of the reaction of 1 mol of fatty alcohol with 15 mol of ethylene oxide, 144 g (0s88 mol) di (methyl glycol-formal and 0.95 g of zinc chloride, 5.8 g of paraformaldehyde, and also 0.95 g of LECO j are stirred at 150 ° C for 3 hours. Simultaneously 090354 but they let in a very weak stream of nitrogen, After cooling to 70 ° C, the mixture contained in the reaction mixture is 2 br. Of catalyst is neutralized with caustic soda powder. Then the excess D1g- (methyl glycol) -formal is distilled off at 160 ° C under a vacuum of 20 mbar. The remaining in the flask after distillation is o The inoculated product is freed from the filtration of salts by filtration. 350 g of a compound of the formula R - () ,, are obtained. - ,, where R is C, j2-alkyl, J5 The conditions for the preparation of mixed formulas in Examples 1-7 are tabulated. Example 8, Fiber Finishing 2Q Mixed formals obtained according to the specified examples are applied from an aqueous solution of a concentration of 0.7-1 jO wt.% To a mono-resin made of polyamide-.b and its sliding friction (thread friction 5 metal) after vyuppshani determined in the following way (see drawing) Monofilament 1 comes from the threading through the nitrating device 2, which creates a constant tension of 50 gf, 0 to the first measuring head 3 and from there through the friction element 4 from solid-chrome-plated stainless steel to the second measuring head 5 and from here the monofilament is directed to the thread and accepted by the body 6,. . The dynamic friction coefficient f is obtained from the tension of the thread t (before the friction element 4) and t 0 (after the friction element 4) according to the equation (1 nt - I nt,). about 45 50 where cx, the coverage angle, which is set with a yarn feeder 7 and 8 to 180 ° C. The specified value for dynamic friction (friction between a thread and a metal) is the average of the measured values at removal speed 25 and 100 m / min, Get1-shy. dynamic values friction factors (f) are respectively, for mixed formals in the examples: - 0.205-0.270; 2 0 ,, 210--0,280; 4 - 0.225-0.280, Friction factor for monofilament decorated with well-known mixed form S. 12090356 fleM no to the prototype of the Cd-C formula, - As can be seen from the examples, the proposing () - is the mixed formulas that are more effective - 0.240-0.310, i.e. much higher. us for finishing than known. Compiled by A, Gorchev Editor M. Nedoluzhenko Tekhred AO Kikemezey Proofreader L, Patay 310/61 Circulation 471 Subscription VNIISH State Committee of the USSR for inventions and discoveries 1130359 Moscow, Zh-35, Raushsk nab., 4/5 Branch GOSH Patent, Uzhgorod, st. Project, 4
权利要求:
Claims (1) [1] METHOD FOR PRODUCING : MIXED FORMALS OF POLYETHYLENE GLYCOL of the general formula R r (OC z n 4 ) n —OCH z OC 2 H 4 OP ^, where R 4 is C g —C 22 alkyl, oleyl; R is C, C 4 alkyl; η “3-15, which consists in the fact that 0.35-1.0 mol of oxyethylates of fatty alcohol of the General formula R, - (0C 2 H 4 ) n -0H, where Rj and η have the indicated meanings, are reacted with 0.88-2.5 mol of di— (alkyl glycol) —formals of the general formula ch 2 (oc 2 h 4 or 2 ) 2 , where R has the indicated mass value at 150-160 C in the presence of 0.3-0.5 wt.% of a mixture of sulfuric acid reagents or a mixture of zinc chloride with phosphinic acid when they are. a mass ratio of 1: 1 - 2: 1 as a catalyst, followed by cooling the reaction mixture to 70-100 C, neutralizing the catalyst with sodium hydroxide, distilling unreacted di— - (alkyl glycol) -formals from 100-160 ° C under a vacuum of 15-20 mbar and department - ι | pouring the target product from those formed during the neutralization of salts by filtration; 00 cl I 209035
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同族专利:
公开号 | 公开日 IT7921156D0|1979-03-20| GB2017100B|1982-07-14| FR2420594A1|1979-10-19| DE2812443A1|1979-10-04| SU1222200A3|1986-03-30| US4294990A|1981-10-13| FR2420594B1|1982-07-16| GB2017100A|1979-10-03| MX150393A|1984-04-30| JPS6151069B2|1986-11-07| IT1112962B|1986-01-20| JPS54134198A|1979-10-18| DE2812443C2|1982-12-02|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 DE1594906A1|1966-05-11|1970-05-27|Boehme Chem Fab Kg|Process for preparing and oiling fully synthetic and cellulose ester threads| US3926816A|1970-05-22|1975-12-16|Goulston Co George A|Textile fiber lubricants| US3997450A|1972-04-10|1976-12-14|Fiber Industries, Inc.|Synthetic fibers of enhanced processability| JPS50101693A|1974-01-18|1975-08-12| DE2523588C2|1975-05-28|1983-11-10|Hoechst Ag, 6230 Frankfurt|Polyglycol ether mixed formals and their use as caustic alkali-resistant wetting agents, detergents and cleaning agents|DE3018149A1|1980-05-12|1981-11-19|Henkel KGaA, 4000 Düsseldorf|USE OF ALKYLPOLYGLYKOLETHERMAL FORMAL FOR FOAM PREVENTION| DE3018135A1|1980-05-12|1981-11-19|Henkel KGaA, 4000 Düsseldorf|METHOD FOR PRODUCING POLYGLYKOLETHERMAL FORMALS AND NEW POLYGLYKOLETHERMAL FORMALS| JPS5789668A|1980-11-19|1982-06-04|Unitika Ltd|Production of polyester fiber having good adhesiveness with rubbers| US4408084A|1981-01-09|1983-10-04|Basf Wyandotte Corporation|Non-ionic surfactants containing acetal groups| JPS6260510B2|1984-04-06|1987-12-16|Takemoto Oil & Fat Co Ltd| DE3701303A1|1987-01-17|1988-07-28|Hoechst Ag|POLYALCOXY THERMAL FORMAL| JPH038378U|1989-06-09|1991-01-25| TW225562B|1991-10-15|1994-06-21|Hoechst Ag| EP0538714B2|1991-10-19|1999-09-01|Clariant GmbH|Biodegradable fibers treating agent| WO1994026463A1|1993-05-18|1994-11-24|Jack Douglas Ward|Powered stand for rotating workpieces|
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申请号 | 申请日 | 专利标题 DE19782812443|DE2812443C2|1978-03-22|1978-03-22|Polyglycol ether thermal formals and their use as fiber finishes| 相关专利
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