DE1960919A1 - Process for graft polymerization - Google Patents
Process for graft polymerizationInfo
- Publication number
- DE1960919A1 DE1960919A1 DE19691960919 DE1960919A DE1960919A1 DE 1960919 A1 DE1960919 A1 DE 1960919A1 DE 19691960919 DE19691960919 DE 19691960919 DE 1960919 A DE1960919 A DE 1960919A DE 1960919 A1 DE1960919 A1 DE 1960919A1
- Authority
- DE
- Germany
- Prior art keywords
- graft polymerization
- graft
- initiator
- concentration
- manganese
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title description 9
- 238000010559 graft polymerization reaction Methods 0.000 title description 6
- 239000003999 initiator Substances 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 235000011007 phosphoric acid Nutrition 0.000 claims description 3
- 230000000977 initiatory effect Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims 1
- 230000010287 polarization Effects 0.000 claims 1
- 239000004753 textile Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 9
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000001603 reducing effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 150000002697 manganese compounds Chemical class 0.000 description 2
- NXYBZKHBQWRTLK-UHFFFAOYSA-B manganese(3+);phosphonato phosphate Chemical compound [Mn+3].[Mn+3].[Mn+3].[Mn+3].[O-]P([O-])(=O)OP([O-])([O-])=O.[O-]P([O-])(=O)OP([O-])([O-])=O.[O-]P([O-])(=O)OP([O-])([O-])=O NXYBZKHBQWRTLK-UHFFFAOYSA-B 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- KVKRSMAXOZCCOG-UHFFFAOYSA-N O.[O-2].[Mn+4].[O-2] Chemical compound O.[O-2].[Mn+4].[O-2] KVKRSMAXOZCCOG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 241001233037 catfish Species 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- MMIPFLVOWGHZQD-UHFFFAOYSA-N manganese(3+) Chemical compound [Mn+3] MMIPFLVOWGHZQD-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000006855 networking Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000009988 textile finishing Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Description
Die Erfindung betrifft ein verfahren zur pfropfpolymerisation · swecks Textilveredlung.The invention relates to a method for graft polymerization swecks textile finishing.
Verodlungeeffekte an textlien, insbesondere an natürlichen Pasoretoffen, ?/erden hauptsächlich chemisch, durch Vernetzungen* Besohichtungen bzw· polynerencinlagerungen sowie duroh Pfropfung, erreicht· Die Pfropfpolymerisation hat sich dabei als vielversprechendes Verfahren herausgestellt,.well so nicht { nur hervorragende Eigenschaften von Synthesefaserstoffen ver- · nittelt, sondern gleichzeitig die Vorteile des pflanzliohen odo.r tierischen Materials aufrechterhalten werden»Verodlungeeffekte to text lien, especially in natural Pasoretoffen? / Ground mainly chemically, by networking * Besohichtungen or · polynerencinlagerungen and reached duroh grafting · The graft polymerization has thereby proved to be a promising method, .well so not {only excellent properties of synthetic fibers comparable · Aids, but at the same time the advantages of the vegetable or animal material are maintained »
pfropfPolymerisationen lassen sich bekannternu.ßon auf verschiedene Art und Welse auslösen. Ala am günstigsten haben eich die oxydativen Methoden erwiesen, anwendbar für alle RUckgratpolynieren mit reduzierenden Eigenschaften» Dabei entstehen duroh Oxydation des vorgelegten polymeren intermediär Maleroradikalo, die die Pfropfpolymerisation radikalisoh polymericierbarer ^onoraörer praktisoh an "Ort und Stelle" einleiten· Unter den dafür geeigneten-Oxydationsmitteln zeigen besonders Manganverbindungen gute Wirkung. Mangan(III)-sulfab, ' Mangan(III)-pyrophosphat, aktiver Braunstein (Mangandioxidhydratf sowie Kallumpormanganut sind als anwendbar bekannt geworden·- Graft polymerizations can be known in various ways Trigger species and catfish. Ala have the cheapest The oxidative methods have been proven to be applicable to everyone Backbone polyning with reducing properties »This creates duroh oxidation of the submitted polymeric intermediate Maleroradikalo, which radikalisoh polymericierbaren the graft polymerisation ^ initiate onoraörer Praktisoh "on the spot" · Among the oxidizing agents suitable for this purpose, manganese compounds in particular have a good effect. Manganese (III) sulfab, ' Manganese (III) pyrophosphate, active manganese dioxide (manganese dioxide hydrate) as well as Kallumpormanganut have become known as applicable -
Obwohl mit den genannten Verbindungen gute, teils sogar ausgezeichnete HQsultato erziolt wurden, ist ihr gemeinsamer Kaohtcil, daß immer vom teuren Kaliumperraanganat ausgegangen werden muß.Although the connections mentioned are good, in some cases even excellent HQsultato is their common one Kaohtcil that always started from the expensive potassium perraanganate must become.
Dar Erfindung liegt die Aufgabe zugrunde, die Initiierung der pfrcrpfpolynerlsatlon auf BückgratpOlymeren mit reduzierenden Eigenschaften duroh olne möglichst billige Manganverbindun/· au en.'iügliohen»The object of the invention is the initiation the pfrcrpfpolynerlsatlon on backbone polymers with reducing Properties without the cheapest possible manganese compound / · au en.'iügliohen »
009851/204Ä009851 / 204Ä
BADBATH
Ka nur do gefunden, darJ die pfropfpolymerisation auf reduzierend wirkenden Polymeren sehr gut mit n;*türliohe;;if in— aktiven Braunstein ausgelöst werden kann, wenn dieser zuvor duroh Erhitzen.mit Orthophosphorsäure au wasserlöslichem, violetten Mangan(III)-pyrophosphat aufgeschlossen-wird· Der folgende. tPfropfproaeß ist in flüssiger oder gasförmiger Phase ausführbar.Ka only do found because r J graft polymerization very well with n on reducing action polymers; * türliohe ;; i f can be triggered in-active manganese dioxide, if this previously duroh Erhitzen.mit orthophosphoric acid au water soluble violet manganese (III) - Pyrophosphate is digested · The following. tPfropfproaeß can be carried out in the liquid or gaseous phase.
Duroh Verwendung des crflndungsgeiaäQen Initiators wird eine Verbilligung dos Verfahrens erreicht. Die als AiifsciilußsAuro eingesetzte Orfchöphoaphorsäure. dient außerdem gleichzeitig zur Einstellung de ο erforderlichen definierten pll-V/ertes beiThe use of the appropriate initiator becomes one The process has become cheaper. The as AiifsciilusssAuro Orfchöphoaphoric acid used. also serves at the same time for setting the ο required defined pll-values
«
Durchführung der Pfropfreaktion»«
Carrying out the grafting reaction »
. Die Kühe der Pfrop&usbeuten naoh diesem Verfahren ist eine Funktion der RGaktlonsbedinguiigen, also der Säurekonsentration, laitlatorkonsentration, Temperatur/ Motioaerkonzentratlon und Realctlonsäeit für Reaktionen la flüssiger Pha3e sowie Säurekonaentrati'on, Initlatorkonaentration, Behandlungsdauer mit dem saure'h Initiator bad sowie dessen Temperatur und Bedaiapfungs— dauer für Reaktionen in der. Gasphase» Diese Reaktionsbedingungen sind mehr oder vjeniger von der Art des vorgelegten Polymeren und dem zu pfropfpolymerisierenden Bionomeren abliängiß, d.h. das Optimum der einzelnen parameter hinsiohtlioh maximaler pfropfauabeuten lot von Reaktion zu Reaktion verschieden. Für Reaktionen in flüssiger !»hase gilt, daß mit steigender Säure— konzentration und auoh Mangankonaentration ein Kaximum in den Pfrop5iuabeuten durohlaufen wird und dafl sieb, mit Erhöhung der Monomerkonaentratlon und Boliandlun^sdauer die Pfropfausbeuten erhöhen*- Die Beliandlungstemperatur richtet sich naoh deni verwendeten Monomeren V/aHaerunlösllcho flonoiaere werden in Gegen— \zart eines Emul hiermit tele oder eines vermittelnden !,öeu mittels eingesetzt» Für Reaktionen In der Gaspbxise gelten löge Bedingungen; jedoch sind solche Prozesse Im allgemeinen weniger chemikalien-.und Eeitaufwendig.. The cows of the grafts after this procedure is one Function of the RGaktlonsbedinguiiigen, i.e. the acid concentration, laitlator concentration, temperature / motor concentration and Realctlonsäeit for reactions la liquid phase as well as acid concentration, Initiator concentration, duration of treatment with the acidic initiator bath as well as its temperature and demand duration for reactions in the. Gas phase »These reaction conditions are more or less of the type of polymer presented and the bionomer to be graft polymerized, i.e. the optimum of the individual parameters in terms of maximum Grafts vary from reaction to reaction. For Reactions in liquid form: with increasing acidity, concentration and manganese concentration a maximum in the The grafting will run through and sieve, with an increase in the Monomer concentration and bolus duration determine the graft yields increase * - The exposure temperature depends on the type of coating used Monomers V / aHaerunlösllcho flonoiaere are in counter- \ tender of an emul herewith tele or a mediating!, öeu by means of »For reactions in the gas practice apply put conditions; however, such processes are general less chemical and time consuming.
009851/2ΟΛΑ ßADOR,SfNAL009851 / 2ΟΛΑ ßADOR, Sf NAL
19C091919C0919
DiG iir.chxol^eiulcm Daisplwle dionen dor Veranschaullchung de3 Verfahren^, ohne ca darauf zu beschränken·DiG iir.chxol ^ eiulcm Daisplwle dion dor eviction de3 procedure ^ without restricting ca
Bereitung d*>rPreparation d *> r
Ι ιmΙ ιm
'250 r.ig Braunstein werden mit 2,5 ml kons* Orthophosphorsäure bis sum vollständigen Auflösen erhitzt* Haoh kurzzeitiger Abkühlung gibt man cum violetten Heald;ionsgemlsch unter Umrühren 5 al ctest· H0O- und erhitzt nochmals zwecks vollständiger Lösung· Sodann v/lrd mit dest· IUO auf 100 ml Gesamtvolumen verdünnt.'250 r.ig Braunstein are heated with 2.5 ml of cons * orthophosphoric acid to completely dissolve sum * Haoh brief cooling gives you cum violet Heald; ionsgemlsch stirring 5 al ctest · H 0 O and heated again for complete solution then · v / lrd diluted to 100 ml total volume with dist.IUO.
Beispiel_1; "' 'Example 1; "''
Zv. 100 ml Initiatorlösung gibt man 7 g Acrylamid und oa· 1 g Polyamid-6· Dieses Reaktionssystera wird 3 std» lang bei 6o C gehalten» Man beendet nun die Reaktion durch Zugabe einer fjpatelspitae Natriumsulfit, wäscht das Pfropf produkt sorgfältig und-trooknet bis aur Gewichtskonstanz· * Gewiohtsaunahme: 29,8# Zv. 7 g of acrylamide and 1 g of polyamide-6 are added to 100 ml of initiator solution. This reaction system is kept at 6o C. for 3 hours Weight constancy * Weight gain: 29.8 #
Boispiel g; .Boig g; .
Etwa 2 g einer Baumwollprobe werden 5 min bei 600C^mIt 100 ml Initiatorin sung behandelt» (Jas IniMatorbad kann anschließend noch etliche Male verwendet "werden,) iisn drückt danach die Probe kurz aus und bedampft sie 15 min lang mit Acrylnitril*About 2 g of a cotton sample for 5 min at 60 0 C ^ with 100 ml of initiator solution treated "(Jas IniMatorbad can then even a number of times used" are) iisn then pushes the sample from short and steamed for 15 minutes with acrylonitrile *
^ Dann wird mit reichlich V.'asser gewaschen, evtl· noch anhoftender Initiator mit Sohv/efliger Säure beseitigt, erneut gewaschen und bis zur Göwiohtskonstanz getrocknet»·- .. .^ Then it is washed with copious amounts of water, possibly even better Eliminated initiator with solid acid, washed again and dried to Göwiohts constancy »· - ...
. GewichtSKunahme : 72,5 'n . Weight increase: 72.5 'n
009851/204A009851 / 204A
' BAD ORIGINAL'BAD ORIGINAL
Claims (1)
Braunstein verwendet wird, der zuvor mit OrthophospHorsäure . aufgeschlossen worden ist· - · .Ancestors for the graft polarization of textile fibers with realizing properties in liquid or gaseous form! ' Phase by initiation with Maugan (III) -pyrophosphafc > characterized in that as .Initiator natural, inactive
Mangestone is used previously with orthophosphoric acid. has been unlocked · - ·.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DD14003669 | 1969-05-23 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1960919A1 true DE1960919A1 (en) | 1970-12-17 |
Family
ID=5481255
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19691960919 Pending DE1960919A1 (en) | 1969-05-23 | 1969-12-04 | Process for graft polymerization |
Country Status (4)
| Country | Link |
|---|---|
| CH (2) | CH531085A (en) |
| DE (1) | DE1960919A1 (en) |
| FR (1) | FR2043625A7 (en) |
| GB (1) | GB1241281A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115650195A (en) * | 2022-12-15 | 2023-01-31 | 北京林立新能源有限公司 | Method for preparing manganese phosphate from tetravalent manganese |
-
1969
- 1969-12-04 DE DE19691960919 patent/DE1960919A1/en active Pending
-
1970
- 1970-01-05 GB GB45870A patent/GB1241281A/en not_active Expired
- 1970-01-15 CH CH54470A patent/CH531085A/en unknown
- 1970-01-15 CH CH54470D patent/CH54470A4/xx unknown
- 1970-03-03 FR FR7007616A patent/FR2043625A7/fr not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115650195A (en) * | 2022-12-15 | 2023-01-31 | 北京林立新能源有限公司 | Method for preparing manganese phosphate from tetravalent manganese |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2043625A7 (en) | 1971-02-19 |
| CH54470A4 (en) | 1972-08-15 |
| GB1241281A (en) | 1971-08-04 |
| CH531085A (en) | 1972-11-30 |
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