SU1659422A1 - Method for obtaining polymerization catalyst for styrene polymerization - Google Patents
Method for obtaining polymerization catalyst for styrene polymerization Download PDFInfo
- Publication number
- SU1659422A1 SU1659422A1 SU4111543K SU4111543K SU1659422A1 SU 1659422 A1 SU1659422 A1 SU 1659422A1 SU 4111543 K SU4111543 K SU 4111543K SU 4111543 K SU4111543 K SU 4111543K SU 1659422 A1 SU1659422 A1 SU 1659422A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- polymerization
- styrene
- catalyst
- obtaining
- chloroform
- Prior art date
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims description 3
- 239000002685 polymerization catalyst Substances 0.000 title 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 4
- 239000011541 reaction mixture Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Изобретение относитс к каталитической химии, в частности к получению катализатора полимеризации стирола в массе. С целью улучшени качества целевого продукта безводный трихлорид железа подвергают взаимодействию с бензолом в среде растворител , такого как хлороформ, при 50 - 65°С. При полимеризации стирола в массе врем полимеризации при использовании данного катализатора снижаетс до 30 - 40с.This invention relates to catalytic chemistry, in particular to the preparation of a catalyst for the polymerization of styrene in bulk. In order to improve the quality of the target product, the anhydrous iron trichloride is reacted with benzene in a solvent medium such as chloroform at 50-65 ° C. During the polymerization of styrene in the mass, the polymerization time when using this catalyst is reduced to 30 - 40 s.
Description
Изобретение относитс к способу получени соединени неустановленной структуры , а именно нового катализатора полимеризации стирола в массе, который найдет широкое применение в народном хоз йстве .The invention relates to a method for producing a compound of unidentified structure, namely, a new catalyst for the polymerization of styrene in bulk, which will find wide application in the national economy.
Целью изобретени вл етс улучшение : качества целевого продукта.The aim of the invention is to improve: the quality of the target product.
Пример1.В четырехгорлую колбу емкостью 100 мл, снабженную мешалкой, обратным холодильником, замкнутым скл нкой Тищенко с концентрированной серной кислотой, сообщающейс с устройством дл поглощени хлористого водорода , помещают 25 мл сухого, свободного от спирта технического хлороформа (ГОСТ 20015-74, сорт высший, нестабилизированный ), после чего при работающей мешалке добавл ют 32,4 г безводного трихлорида железа (ГОСТ 11159-76) и 15,7 г (18 мл) бензола (ГОСТ 5.961-70). Реакционную смесь нагревают при перемешивание на вод ной бане. При 50 - 55°С начинаетс выделение хлористого водорода, которое заканчиваетс через 1,5 ч при 64 - 65°С. После охлаждени реакционной смеси до комнатнойExample 1. A 100 ml four-necked flask equipped with a stirrer, a reflux condenser, a closed Tishchenko flask with concentrated sulfuric acid, connected to a device for the absorption of hydrogen chloride, was placed 25 ml of dry, alcohol-free technical chloroform (GOST 20015-74, highest grade , unstabilized), after which 32.4 g of anhydrous iron trichloride (GOST 11159-76) and 15.7 g (18 ml) of benzene (GOST 5.961-70) are added with the stirrer running. The reaction mixture is heated with stirring in a water bath. At 50-55 ° C, release of hydrogen chloride begins, which ends after 1.5 hours at 64-65 ° C. After cooling the reaction mixture to room temperature
температуры водоструйным насосом отсасывают оставшийс хлористый водород. Жидкую фазу реакционной смеси отфильтровывают под вакуумом от твердой через стекл нный фильтр. Осадок на фильтре промывают 30 мл хлороформа. От фильтрата отгон ют хлороформ и при нагревании на вод ной бане в вакууме водоструйного насоса удал ют летучие. Получают 3t г твердого хрупкого продукта, растирающегос в темно-коричневый порошок со средней молекул рной массой 330. Состав продукта: С 46,65; Н 3,42; Fe 16,9; CI32.83.the temperature of the water jet pump sucked the remaining hydrogen chloride. The liquid phase of the reaction mixture is filtered under vacuum from the solid through a glass filter. The filter cake is washed with 30 ml of chloroform. Chloroform is distilled off from the filtrate and, when heated in a water bath in a water jet vacuum, the volatiles are removed. 3t g of a solid brittle product is obtained, triturated into a dark brown powder with an average molecular weight of 330. Product composition: C, 46.65; H 3.42; Fe 16.9; CI32.83.
Данные ИК-спектров: 3400,3600 - 3200, 3070, 3970, 3910, 2870, 1650, 1630, 1610, 1585, 1500, 1480, 1450, 1420, 1410, 1360, 1300, 1240, 1190, 1165, 1110, 1090. 1035, 1000. 985, 955, 920. 845, 825, 810, 790, 770, 710,625,615,475.IR spectra data: 3400.3600 - 3200, 3070, 3970, 3910, 2870, 1650, 1630, 1610, 1585, 1500, 1480, 1450, 1420, 1410, 1360, 1300, 1240, 1190, 1165, 1110, 1090 1035, 1000. 985, 955, 920. 845, 825, 810, 790, 770, 710,625,615,475.
Температура начала окислени продукта на воздухе 150°С.The temperature at which the product starts to oxidize in air is 150 ° C.
Полученный продукт был испытан в качестве катализатора полимеризации стирола в массе по сравнению с известным катализатором.The resulting product was tested as a catalyst for the polymerization of styrene in mass in comparison with the known catalyst.
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о N го юabout N go yu
П р и м е р 2. К 20 мл свежеперегнанного стирола, свободного от гидрохинона, добавл ют при перемешивании 20 мг продукта, полученного по примеру 1. Через 7 с (индукционный период) начинаетс полимеризаци с разогреванием системы до закипани полимеризующегос стирола (145°С). Через 30 - 40 с образуетс прозрачный стеклопо- добный полистирол, который раствор ют в бензоле, промывают метанолом и сушат при 40° С и остаточном давлении 10 мм рт.ст, Полученный продукт имеет характеристическую в зкость ц 5,2, выход 98%.EXAMPLE 2 To 20 ml of freshly distilled styrene free of hydroquinone, 20 mg of the product obtained in Example 1 is added with stirring. After 7 seconds (induction period), polymerization begins, heating the system to boil the polymerizing styrene (145 ° WITH). After 30-40 seconds, a clear glass-like polystyrene is formed, which is dissolved in benzene, washed with methanol and dried at 40 ° C and a residual pressure of 10 mm Hg. The resulting product has an intrinsic viscosity of 5.2, yield 98%.
Пример 3. В стекл нную колбу, охлаждаемую водой, помещают стирол, в котором раствор ют комплекс ZnCte в ме- тилметакрилате(содержание ZnCta 18,23 мас.%). Затем при перемешивании добавл ют при 20°С трифторуксусную кислоту в количестве 2% от массы стирола. Реакционную смесь перемешивают 2,5ч, раствор ют в толуоле, высаживают спиртом, получаютExample 3. In a water-cooled glass flask, styrene was placed in which the ZnCte complex was dissolved in methyl methacrylate (ZnCta content 18.23 wt.%). Then, with stirring, trifluoroacetic acid is added at 20 ° C in an amount of 2% by weight of styrene. The reaction mixture is stirred for 2.5 hours, dissolved in toluene, and precipitated with alcohol;
белый порошок, выход 100%, средн мол. масса 62000.white powder, yield 100%, average mol. weight 62,000.
Предлагаемый способ позвол ет получить катализатор, обладающий повышенной активностью по сравнению с известным.The proposed method allows to obtain a catalyst with increased activity compared with the known.
Так, при полимеризации стирола в массе врем полимеризации при использовании предлагаемого катализатора снижаетс So, when polymerization of styrene in the mass, the polymerization time when using the proposed catalyst decreases
до 30 - 40°С по сравнению с известной системой катализатора ZnCte метилметак- рилат + трифторуксуска кислота, при использовании которой общее врем полимеризации составл ет 2,5 ч.up to 30 - 40 ° С in comparison with the well-known ZnCte catalyst system methyl methacrylate + trifluoroacetic acid, using which the total polymerization time is 2.5 hours.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU864111543A SU1659421A1 (en) | 1986-06-19 | 1986-06-19 | Method for obtaining catalyst for dibenzyltoluene synthesis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU1659422A1 true SU1659422A1 (en) | 1991-06-30 |
Family
ID=21254309
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU4111543K SU1659422A1 (en) | 1986-06-19 | 1986-06-19 | Method for obtaining polymerization catalyst for styrene polymerization |
| SU864111543A SU1659421A1 (en) | 1986-06-19 | 1986-06-19 | Method for obtaining catalyst for dibenzyltoluene synthesis |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU864111543A SU1659421A1 (en) | 1986-06-19 | 1986-06-19 | Method for obtaining catalyst for dibenzyltoluene synthesis |
Country Status (1)
| Country | Link |
|---|---|
| SU (2) | SU1659422A1 (en) |
-
1986
- 1986-06-19 SU SU4111543K patent/SU1659422A1/en active
- 1986-06-19 SU SU864111543A patent/SU1659421A1/en active
Non-Patent Citations (1)
| Title |
|---|
| Авторское свидетельство СССР , № 654625, кл. С 08 F 112/08, опублию 1976. * |
Also Published As
| Publication number | Publication date |
|---|---|
| SU1659421A1 (en) | 1991-06-30 |
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