SU1608193A1 - Method of producing polyacrylamide hydrogel - Google Patents
Method of producing polyacrylamide hydrogel Download PDFInfo
- Publication number
- SU1608193A1 SU1608193A1 SU894674491A SU4674491A SU1608193A1 SU 1608193 A1 SU1608193 A1 SU 1608193A1 SU 894674491 A SU894674491 A SU 894674491A SU 4674491 A SU4674491 A SU 4674491A SU 1608193 A1 SU1608193 A1 SU 1608193A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- chlorophyll
- reducing agent
- mol
- acrylamide
- hydrogel
- Prior art date
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 11
- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title claims description 8
- 229930002875 chlorophyll Natural products 0.000 claims abstract description 14
- 235000019804 chlorophyll Nutrition 0.000 claims abstract description 14
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 claims abstract description 13
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 6
- 230000008961 swelling Effects 0.000 claims abstract description 6
- 241000255789 Bombyx mori Species 0.000 claims abstract description 5
- 239000000499 gel Substances 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000003431 cross linking reagent Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 238000010526 radical polymerization reaction Methods 0.000 claims description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 2
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims 2
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000000284 extract Substances 0.000 abstract description 2
- 238000007334 copolymerization reaction Methods 0.000 abstract 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 15
- 239000000203 mixture Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 210000003608 fece Anatomy 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004160 Ammonium persulphate Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000019395 ammonium persulphate Nutrition 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000001752 chlorophylls and chlorophyllins Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- ZKQFHRVKCYFVCN-UHFFFAOYSA-N ethoxyethane;hexane Chemical compound CCOCC.CCCCCC ZKQFHRVKCYFVCN-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/52—Amides or imides
- C08F20/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F20/56—Acrylamide; Methacrylamide
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Изобретение относитс к химии полимеров и позвол ет получить полиакриламидный гидрогель со степенью набухани 1639-1735 г воды на 1 г гел , что достигаетс радикальной сополимеризацией в водном растворе акриламида, персульфата аммони и хлорофилла из выделений тутового шелкопр да при их мол рном соотношении 1:0, 18:(0,035-0,00035) соответственно. 1 табл.This invention relates to the chemistry of polymers and provides a polyacrylamide hydrogel with a swelling ratio of 1639-1735 g water per g gel, which is achieved by radical copolymerization in aqueous solution of acrylamide, ammonium persulfate and chlorophyll from silkworm extracts at their molar ratio of 1: 0 , 18: (0.035-0,00035), respectively. 1 tab.
Description
Изобретение относитс к химии полимеров , а именно к способу получени полиакриламидного гидрогел , и может быть использовано в медицине, биотехнологии и сельском хоз йстве дл создани в одопоглощающих устройств и средств.The invention relates to the chemistry of polymers, in particular to a method for producing a polyacrylamide hydrogel, and can be used in medicine, biotechnology and agriculture to create self-absorbing devices and devices.
Целью изобретени вл етс повышение водопоглощени гидрогел и упрощение процесса его получени .The aim of the invention is to increase the water absorption of the hydrogel and simplify the process of its preparation.
Пример 1. Получение хлорофилла из выделений тутового шелкопр да .Example 1. Obtaining chlorophyll from secretions of silkworm.
100 г выделений тутового шелкопр да (ВТШ) экстрагируют 400-500 мл ацетона в течение 3-5 ч. Экстракт фильтруют и после упаривани получают 5 г пасты, которую подвергают колоночной хроматографии на силика- геле в колонке (35x200 мм), использу в качестве элюирующей смеси следующие системы: петролейньй эфир - диэтиловый эфир (10:1), петролей- ный эфир - диэтиловый эфир (5:1), петролейный эфир - диэтиловьй эфир . (1:1), ацетон. Контроль за очисткой хлорофилла осуществл ют методом ТСХ на пластинках Silufol в системе гек- сан - диэтиловый эфир (1:1). Фракции , содержащие целевой продукт, объедин ют, упаривают до суха и получают продукт, содержащий смесь хлорофиллов а и Ь. Структуру хлорофилла подтверждают спектроскопическим методом (диэтиловый эфир) Ад,о1 (нм): 410,430, 533,578,615,662. Содержание хлорофилла в ВТШ 4,2%.100 g of silkworm excreta (HTS) are extracted with 400-500 ml of acetone for 3-5 hours. The extract is filtered and after evaporation 5 g of paste is obtained, which is subjected to column chromatography on silica gel in a column (35x200 mm), using The following systems are eluting mixtures: petroleum ether - diethyl ether (10: 1), petroleum ether - diethyl ether (5: 1), petroleum ether - diethyl ether. (1: 1), acetone. Monitoring of chlorophyll purification was performed by TLC on Silufol plates in the hexane-diethyl ether (1: 1) system. The fractions containing the desired product are combined, evaporated to dryness and a product is obtained containing a mixture of chlorophylls a and b. The structure of chlorophyll is confirmed by a spectroscopic method (diethyl ether) Hell, o1 (nm): 410.430, 533.578.615.662. Chlorophyll content in HTS is 4.2%.
П р и м е р 2. Получение полиакриламидного гидрогел .PRI mme R 2. Obtaining polyacrylamide hydrogel.
К 12 мл 6М водного раствора акрил- амида (АА) прикапывают 0,2 мл 210 М этанолового раствора хлорофилла приTo 12 ml of a 6M aqueous solution of acrylamide (AA) was added dropwise 0.2 ml of a 210 M ethanolic solution of chlorophyll at
о:)about:)
оabout
0000
со соwith so
посто нном перемешивании. Затем приливают 3 мл раствора персульфата аммони (ПСА) концентрации 1,. Смесь медленно нагревают до при нормальном давлении в течение 8 мин. После остывани реакционную смесь промьшают 10 мин проточной водой и выдерживают в избытке 10%-ного водного раствора щелочи. Продукт реакции ме санически измельчают и сушат при в течение 7 ч. Выход гидрогел 70%. Мол рное соотношение АА:персульфат аммони : хлорофилл составл ет 1:0,18:0,035.constant stirring. Then 3 ml of ammonium persulphate (PSA) solution of concentration 1, is poured. The mixture is slowly heated to normal pressure for 8 minutes. After cooling, the reaction mixture is washed with running water for 10 minutes and kept in an excess of 10% aqueous alkali solution. The reaction product is micronized and dried at 7 hours. Hydrogel yield 70%. The molar ratio of AA: ammonium persulfate: chlorophyll is 1: 0.18: 0.035.
Дл определени водопоглощени гидрогелей используют и гравиметрический метод. Навеску сухогополимера помещают в дистиллированную воду и пйсле равновесного набухани удал ют избыток жидкости фильтрацией, а набухший гель взвешивают. Степень набухани определ ют по формулеThe gravimetric method is also used to determine the water absorption of hydrogels. A portion of the dry polymer was placed in distilled water and, after equilibrium swelling, excess liquid was removed by filtration, and the swollen gel was weighed. The degree of swelling is determined by the formula
W ll Масса сухого гел ТгТW ll Dry GtTT Mass
Дл данного примера величина W составила 1660.For this example, the value of W was 1660.
10ten
Данные по примерам 3 и 4 и сравнительным примерам 5 и 6 приведены вThe data for examples 3 and 4 and comparative examples 5 and 6 are given in
таблице.the table.
Таким образом, изобретение позвол ет получить полиакриламидный гель с высокой набухаемостью по упрощенной технологии (без сшивающего агента , без удалени кислорода из мономерной смеси).Thus, the invention makes it possible to obtain a high swelling polyacrylamide gel according to a simplified technology (without a crosslinking agent, without removing oxygen from the monomer mixture).
ФормуForm
ла изобретени la invention
Способ получени полиакриламидно- 5 го гидрогел путем радикальной полимеризации акриламида в водном растворе под действием окислительно-восстановительной системы персульфат аммони - аминосодержащий восстано- 2Q витель, отличающийс тем, что, с целью повышени водопоглощени гидрогел и упрощени процесса его получени , в качестве аминосо- держащего восстановител используют 25 хлорофилл из выделений тутового шелкопр да и процесс провод т при мол рном соотношении акриламид: персульфат аммони : хлорофилл, равном 1:0,18:0,035-0,00035.The method of producing a polyacrylamide-5 hydrogel by radical polymerization of acrylamide in an aqueous solution under the action of the redox system ammonium persulfate - an amine containing reducing agent 2Q, characterized in that, in order to increase the water absorption of the hydrogel and simplify its preparation, as an amino-containing the reducing agent uses 25 chlorophyll from silkworm excreta and the process is carried out at a molar ratio of acrylamide: ammonium persulfate: chlorophyll, equal to 1: 0.18: 0.035-0,00035.
Данные по примерам 3 и 4 и сравнительным примерам 5 и 6 приведены вThe data for examples 3 and 4 and comparative examples 5 and 6 are given in
таблице.the table.
Таким образом, изобретение позвол ет получить полиакриламидный гель с высокой набухаемостью по упрощенной технологии (без сшивающего агента , без удалени кислорода из мономерной смеси).Thus, the invention makes it possible to obtain a high swelling polyacrylamide gel according to a simplified technology (without a crosslinking agent, without removing oxygen from the monomer mixture).
ФормуForm
ла изобретени la invention
Г „Т п.п-метиленоисакриламид и в качестве восстановител - ,и,и ,н -тетраметилэтилендиамнны в количестве 0,. G „T pp-methylenoisacrylamide and as a reducing agent -, and, and, n-tetramethylethylenediamine in the amount of 0 ,.
В качестве восстановител использованы метабисульфит натри и ионы 0,5-10 моль.Sodium metabisulfite and ions of 0.5-10 mol were used as a reducing agent.
количествquantities
количествеquantity
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU894674491A SU1608193A1 (en) | 1989-04-04 | 1989-04-04 | Method of producing polyacrylamide hydrogel |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU894674491A SU1608193A1 (en) | 1989-04-04 | 1989-04-04 | Method of producing polyacrylamide hydrogel |
Publications (1)
Publication Number | Publication Date |
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SU1608193A1 true SU1608193A1 (en) | 1990-11-23 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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SU894674491A SU1608193A1 (en) | 1989-04-04 | 1989-04-04 | Method of producing polyacrylamide hydrogel |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7186419B2 (en) | 2000-08-25 | 2007-03-06 | Contura Sa | Polyacrylamide hydrogel for arthritis |
US7678146B2 (en) | 2000-08-25 | 2010-03-16 | Contura A/S | Polyacrylamide hydrogel and its use as an endoprosthesis |
-
1989
- 1989-04-04 SU SU894674491A patent/SU1608193A1/en active
Non-Patent Citations (1)
Title |
---|
Маурер Г. Диск-электрофорез: Теори и практика электрофореза в полиакриламидном геле. - М.: Мир, 1971, с.14. Патент US № 4473689, кл. С 08 F 20/56, опублик. 1979. * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7186419B2 (en) | 2000-08-25 | 2007-03-06 | Contura Sa | Polyacrylamide hydrogel for arthritis |
US7678146B2 (en) | 2000-08-25 | 2010-03-16 | Contura A/S | Polyacrylamide hydrogel and its use as an endoprosthesis |
US7780958B2 (en) | 2000-08-25 | 2010-08-24 | Contura Sa | Polyacrylamide hydrogel for the treatment of incontinence and vesicouretal reflux |
US7790194B2 (en) | 2000-08-25 | 2010-09-07 | Contura A/S | Polyacrylamide hydrogel as a soft tissue filler endoprosthesis |
US7935361B2 (en) | 2000-08-25 | 2011-05-03 | Contura A/S | Polyacrylamide hydrogel as a soft tissue filler endoprosthesis |
US8216561B2 (en) | 2000-08-25 | 2012-07-10 | Contura A/S | Polyacrylamide hydrogel for the treatment of incontinence and vesicouretal reflex |
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