CN100545217C - Aqeous suspension of aluminium sesquioxide and polystyrene-maleic anhydride grafting methoxypolyglycol polymer and preparation method thereof - Google Patents
Aqeous suspension of aluminium sesquioxide and polystyrene-maleic anhydride grafting methoxypolyglycol polymer and preparation method thereof Download PDFInfo
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- CN100545217C CN100545217C CNB2007100250755A CN200710025075A CN100545217C CN 100545217 C CN100545217 C CN 100545217C CN B2007100250755 A CNB2007100250755 A CN B2007100250755A CN 200710025075 A CN200710025075 A CN 200710025075A CN 100545217 C CN100545217 C CN 100545217C
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- Prior art keywords
- polystyrene
- maleic anhydride
- suspension
- aluminium sesquioxide
- anhydride grafting
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- 239000000725 suspension Substances 0.000 title claims abstract description 59
- 229920000642 polymer Polymers 0.000 title claims abstract description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 8
- 229920001427 mPEG Polymers 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 230000032050 esterification Effects 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 abstract description 9
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 16
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 230000001105 regulatory effect Effects 0.000 description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 229960000549 4-dimethylaminophenol Drugs 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 4
- 229920002521 macromolecule Polymers 0.000 description 4
- 230000001976 improved effect Effects 0.000 description 2
- -1 metallurgy Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003827 glycol group Chemical group 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses aqeous suspension of a kind of aluminium sesquioxide and polystyrene-maleic anhydride grafting methoxypolyglycol polymer and preparation method thereof.This suspension is made up of aluminium sesquioxide, polystyrene-maleic anhydride grafting methoxypolyglycol polymer, water.Its preparation method is: aluminium sesquioxide and water cooperate by weight percentage, regulate pH value to 9～10 of suspension with the NaOH solution of 0.005～0.03mol/L, add the dispersion agent polystyrene-maleic anhydride grafting methoxypolyglycol polymer then, stir 10～60min and get final product.This suspension has good dispersiveness and mobile, and its preparation method is simple to operate, is easy to realize.
Description
Technical field
The present invention relates to aqeous suspension of a kind of aluminium sesquioxide and preparation method thereof, specifically suspension of aluminium sesquioxide and polystyrene-maleic anhydride grafting methoxypolyglycol polymer and preparation method thereof.
Background technology
At many industrial circles such as chemical industry, coating, papermaking, building, matrix material, metallurgy, medicine and food, disperse to have become to improve the quality of products and performance, raise the efficiency indispensable technique means.At present, all adopt chemical process to realize the dispersion of ultra-fine grain at many industrial sectors.
Macromolecule dispersing agent is compared with the organic molecule dispersion agent with inorganic, have sensitivitys such as the ion in the dispersion system, pH value, temperature little, the stably dispersing good effectiveness.Macromolecule dispersing agent can significantly reduce the viscosity of dispersion system, improves the rheological of dispersion system, makes product processing more easy to operate, saves the energy.Institute's dispersive system stability is high, helps prolonging storage period, reduces and stores loss, does not need the redispersion expense.The adding of macromolecule dispersing agent can improve the solid content of dispersion system, and dispersion system still has good mobility under high solids content, thereby reduces raw materials cost, reduces the wearing and tearing of equipment.Therefore the application of macromolecule dispersing agent in industrial circle is more and more wider.
When the multipolymer that contains the polyoxyethylene glycol side chain is adsorbed on the powder particle surface, side chain adopts the conformation that stretches to form certain thickness three-dimensional barrier, increase the electromotive force on powder particle surface simultaneously, improved interparticle electrostatic repulsion forces, thereby can improve the dispersed and mobile of system.
Summary of the invention
Goal of the invention: technical problem to be solved by this invention provides the aqeous suspension of a kind of dispersiveness and mobile aluminium sesquioxide preferably and polystyrene-maleic anhydride grafting methoxypolyglycol polymer.
Another object of the present invention provides the preparation method of this aqeous suspension.
Technical scheme: the aqeous suspension of aluminium sesquioxide of the present invention and polystyrene-maleic anhydride grafting methoxypolyglycol polymer, this suspension is made up of following material by weight percentage: aluminium sesquioxide is 40～70%, water is 30～60%, and polystyrene-maleic anhydride grafting methoxypolyglycol polymer is 0.1～2.0% of an aluminium sesquioxide weight.
The aqeous suspension preparation method of above-mentioned aluminium sesquioxide and polystyrene-maleic anhydride grafting methoxypolyglycol polymer may further comprise the steps:
1, aluminium sesquioxide and water are cooperated by weight, stir into uniform suspension;
2, regulate pH value to 9～10 of above-mentioned suspension with the NaOH solution of 0.005～0.03mol/L;
3, add polystyrene-maleic anhydride grafting methoxypolyglycol polymer, stir 10～60min.
Wherein polystyrene-maleic anhydride grafting methoxypolyglycol polymer makes as follows: with polystyrene-maleic anhydride and 1: 1 in molar ratio～2: 1 stirring and dissolving of methoxy poly (ethylene glycol) in solvent, and it is 5～15% that polystyrene-maleic anhydride and methoxy poly (ethylene glycol) amount to weight percent, the weight percent of solvent is 85～95%, under 20～30 ℃, add 4-(dimethylamino) pyridine, the mol ratio of its add-on and methoxy poly (ethylene glycol) is 0.05: 1～1: 1, esterification 12～72 hours; Reaction product is added in the ether, separates out throw out; Filter drying.Solvent described in the preparation method of polystyrene-maleic anhydride grafting methoxypolyglycol polymer is methylene dichloride, tetrahydrofuran (THF), perhaps 2: 1 by volume mixed solvent of methylene dichloride and tetrahydrofuran (THF).
Table 1 has provided polystyrene-maleic anhydride grafting methoxypolyglycol polymer (SMA-g-MPEO) consumption to aluminium sesquioxide (Al
2O
3) influence of zeta-potential of aqeous suspension.The SMA-g-MPEO that adds is adsorbed on Al
2O
3Particle surface has changed the particle surface charge property, and the zeta-potential of aqeous suspension is from the occasion of changing negative value into.The absolute value of zeta-potential improves with the increase of SMA-g-MPEO consumption.
Table 1SMA-g-MPEO
*Consumption is to the influence of zeta-potential
| The SMA-g-MPEO consumption (accounts for Al 2O 3wt％) | 0 | 0.3 | 0.6 | 1.0 | 1.5 |
| Zeta-potential (mV) | 6.11 | -8.37 | -18.06 | -22.31 | -26.43 |
*The MPEO number-average molecular weight is 750
With Al
2O
3Aqeous suspension is compared, Al
2O
3With the Al in the aqeous suspension of SMA-g-MPEO
2O
3Median size reduce (table 2).Along with the SMA-g-MPEO consumption increases, Al
2O
3Median size diminish (table 3).
Table 2Al
2O
3Al in the aqeous suspension
2O
3Median size
| Sample | Do not contain dispersion agent | SMA-g-MPEO * | SMA-g-MPEO ** |
| Particle diameter (μ m) | 1.29 | 0.94 | 0.87 |
*The MPEO number-average molecular weight is 200;
*The number-average molecular weight of MPEO is 2000
Table 3SMA-g-MPEO
*Consumption is to Al
2O
3Al in the aqeous suspension
2O
3The influence of median size
| The SMA-g-MPEO consumption (accounts for Al 2O 3wt％) | 0 | 0.3 | 0.6 | 1.0 | 1.5 |
| Median size (μ m) | 1.29 | 0.98 | 0.86 | 0.79 | 0.71 |
*The MPEO number-average molecular weight is 750
Al when not adding SMA-g-MPEO
2O
3Particle accumulation, system viscosity big (referring to Fig. 2); System viscosity reduces (referring to Fig. 3 and Fig. 4) after adding SMA-g-MPEO.Be adsorbed on Al
2O
3Sterically hindered and the Coulomb repulsion improved effect of the SMA-g-MPEO of particle surface the dispersiveness of system, thereby cause system viscosity to reduce.
Beneficial effect: Al provided by the present invention
2O
3Have dispersiveness and mobile preferably with the aqeous suspension of SMA-g-MPEO, and its preparation method is simple to operate, is easy to realize.
Description of drawings
Fig. 1 is Al
2O
3The infrared spectrum of (a) back (b) before the absorption SMA-g-MPEO.Among the b figure, 3450cm
-1The absorption peak corresponding to-OH stretching vibration at place is obviously strengthened; At 2927cm
-1And 2860cm
-1The absorption peak at place is corresponding to the asymmetric and symmetrical stretching vibration of C-H, 1727cm
-1The absorption peak at place is corresponding to C=O stretching vibration, 1394cm
-1The absorption peak at place corresponds respectively to the flexural vibration of C-H, 1106cm
-1The absorption peak at place is corresponding to the C-O-C stretching vibration on the branched chair polymacrogol.Infrared analysis is the result show, polystyrene-maleic anhydride grafting methoxypolyglycol polymer is adsorbed on A1
2O
3Particle surface.
Fig. 2 is A1
2O
3The apparent viscosity of aqeous suspension.This suspension consist of A1
2O
360wt%, water 40wt%.
Fig. 3 is A1
2O
3The apparent viscosity of the aqeous suspension of/SMA-g-MPEO200 (200 is the number-average molecular weight of MPEO).This suspension consist of Al
2O
360wt%, water 40wt%, SMA-g-MPEO200 are Al
2O
30.3wt%.
Fig. 4 is Al
2O
3The apparent viscosity of the aqeous suspension of/SMA-g-MPEO750 (750 is the number-average molecular weight of MPEO).This suspension consist of Al
2O
360wt%, water 40wt%, SMA-g-MPEO750 are Al
2O
30.3wt%.
Embodiment
Below by embodiment the present invention is specifically described, be necessary to be pointed out that at this, following examples only are used for the present invention is further specified, and can not be interpreted as limiting the scope of the invention.
Embodiment 1:
Add 8.1g SMA in the reaction flask of 250mL, the 4.0g molecular weight is 200 MPEO and 109ml methylene dichloride, stirs it is dissolved fully, and 25 ℃ add 1.22gDMAP, reaction 48h down; Be added in the ether, separate out throw out, filter, be drying to obtain SMA-g-MPEO200.
With Al
2O
3With water by weight mark be that 40% and 60% ratio cooperates, stir into uniform suspension, with the pH value to 9 that the NaOH solution of 0.005mol/L is regulated suspension, adding accounts for Al
2O
3The SMA-g-MPEO200 of weight 0.8% stirs 10min, obtains Al
2O
3The aqeous suspension of/SMA-g-MPEO200.
Embodiment 2:
Add 4.0g SMA in the reaction flask of 250mL, the 7.5g molecular weight is 750 MPEO and 103ml methylene dichloride, stirs it is dissolved fully, and 25 ℃ add 0.61g DMAP, reaction 48h down; Be added in the ether, separate out throw out, filter, be drying to obtain SMA-g-MPEO750.
With Al
2O
3With water by weight mark be that 60% and 40% ratio cooperates, stir into uniform suspension, with the pH value to 9.5 that the NaOH solution of 0.01mol/L is regulated suspension, adding accounts for Al
2O
3The SMA-g-MPEO750 of weight 1.0% stirs 20min, obtains Al
2O
3The aqeous suspension of/SMA-g-MPEO750.
Embodiment 3:
Add 2.5g SMA in the reaction flask of 250mL, the 12.4g molecular weight is 2000 MPEO and 134ml methylene dichloride, stirs it is dissolved fully, adds 0.38g DMAP, and 25 ℃ are reacted 48h down; Be added in the ether, separate out throw out, filter, be drying to obtain SMA-g-MPEO2000.
With Al
2O
3With water by weight mark be that 60% and 40% ratio cooperates, stir into uniform suspension, with the pH value to 9.7 that the NaOH solution of 0.02mol/L is regulated suspension, adding accounts for Al
2O
3The SMA-g-MPEO2000 of weight 0.1% stirs 50min, obtains Al
2O
3The aqeous suspension of/SMA-g-MPEO2000.
Embodiment 4:
With embodiment 2 described methods, different is with Al
2O
3With water by weight mark be that 65% and 35% ratio cooperates, stir into uniform suspension, with the pH value to 10 that the NaOH solution of 0.03mol/L is regulated suspension, adding accounts for Al
2O
3The SMA-g-MPEO750 of weight 0.5% stirs 30min, obtains Al
2O
3The aqeous suspension of/SMA-g-MPEO750.
Embodiment 5:
With embodiment 3 described methods, different is with Al
2O
3With water by weight mark be that 70% and 30% ratio cooperates, stir into uniform suspension, with the pH value to 9.5 that the NaOH solution of 0.01mol/L is regulated suspension, adding accounts for Al
2O
3The SMA-g-MPEO2000 of weight 2.0% stirs 60min, obtains Al
2O
3The aqeous suspension of/SMA-g-MPEO2000.
Embodiment 6:
Add 2.5g SMA in the reaction flask of 250mL, the 9.3g molecular weight is 750 MPEO and 107ml methylene dichloride, stirs it is dissolved fully, adds 0.75g DMAP, and 25 ℃ are reacted 60h down; Be added in the ether, separate out throw out, filter, be drying to obtain SMA-g-MPEO750.
With Al
2O
3With water by weight mark be that 50% and 50% ratio cooperates, stir into uniform suspension, with the pH value to 9.6 that the NaOH solution of 0.01mol/L is regulated suspension, adding accounts for Al
2O
3The SMA-g-MPEO750 of weight 1.2% stirs 15min, obtains Al
2O
3Aqeous suspension with SMA-g-MPEO750.
Embodiment 7:
Add 2.5g SMA in the reaction flask of 250mL, the 9.3g molecular weight is 750 MPEO and 106ml tetrahydrofuran (THF), stirs and makes its dissolving, adds 0.76g DMAP, and 25 ℃ are reacted 48h down; Be added in the ether, separate out throw out, filter, be drying to obtain SMA-g-MPEO750.
With Al
2O
3With water by weight mark be that 60% and 40% ratio cooperates, stir into uniform suspension, with the pH value to 9.4 that the NaOH solution of 0.01mol/L is regulated suspension, adding accounts for Al
2O
3The SMA-g-MPEO750 of weight 1.5% stirs 25min, obtains Al
2O
3Aqeous suspension with SMA-g-MPEO750.
Embodiment 8:
Add 2.5g SMA in the reaction flask of 250mL, the 9.3g molecular weight is that (2/1, V/V) mixed solvent stirs and makes its dissolving, adds 0.76g DMAP, 25 ℃ of reaction 48h down for 750 MPEO and 106ml methylene dichloride/tetrahydrofuran (THF); Be added in the ether, separate out throw out, filter, be drying to obtain SMA-g-MPEO750.
With Al
2O
3With water by weight mark be that 60% and 40% ratio cooperates, stir into uniform suspension, with the pH value to 9.3 that the NaOH solution of 0.01mol/L is regulated suspension, adding accounts for Al
2O
3The SMA-g-MPEO750 of weight 0.6% stirs 35min, obtains Al
2O
3Aqeous suspension with SMA-g-MPEO750.
Claims (4)
1, the aqeous suspension of a kind of aluminium sesquioxide and polystyrene-maleic anhydride grafting methoxypolyglycol polymer, this suspension is made up of following material by weight percentage: aluminium sesquioxide is 40～70%, water is 30～60%, the mass percent sum of aluminium sesquioxide and water is 100%, and polystyrene-maleic anhydride grafting methoxypolyglycol polymer is 0.1～2.0% of an aluminium sesquioxide weight.
2, the aqeous suspension of aluminium sesquioxide according to claim 1 and polystyrene-maleic anhydride grafting methoxypolyglycol polymer, it is characterized in that described polystyrene-maleic anhydride grafting methoxypolyglycol polymer is is catalyzer with 4-(dimethylamino) pyridine, polystyrene-maleic anhydride and methoxy poly (ethylene glycol) carry out esterification and obtain.
3, the aqeous suspension preparation method of described aluminium sesquioxide of claim 1 and polystyrene-maleic anhydride grafting methoxypolyglycol polymer is characterized in that this method may further comprise the steps:
(1) aluminium sesquioxide and water are cooperated by weight, stir into uniform suspension;
(2) regulate pH value to 9～10 of above-mentioned suspension with the NaOH solution of 0.005～0.03mol/L;
(3) add polystyrene-maleic anhydride grafting methoxypolyglycol polymer, stir 10～60min.
4, the aqeous suspension preparation method of aluminium sesquioxide according to claim 3 and polystyrene-maleic anhydride grafting methoxypolyglycol polymer, it is characterized in that wherein the preparation method of the polystyrene-maleic anhydride grafting methoxypolyglycol polymer described in the step (3) is: with polystyrene-maleic anhydride and methoxy poly (ethylene glycol) stirring and dissolving in solvent, add 4-(dimethylamino) pyridine, carry out esterification; Reaction product is added in the ether, separates out throw out; Filter drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100250755A CN100545217C (en) | 2007-07-11 | 2007-07-11 | Aqeous suspension of aluminium sesquioxide and polystyrene-maleic anhydride grafting methoxypolyglycol polymer and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100250755A CN100545217C (en) | 2007-07-11 | 2007-07-11 | Aqeous suspension of aluminium sesquioxide and polystyrene-maleic anhydride grafting methoxypolyglycol polymer and preparation method thereof |
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|---|---|
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| CN100545217C true CN100545217C (en) | 2009-09-30 |
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| CN104693663A (en) * | 2015-02-13 | 2015-06-10 | 江苏苏博特新材料股份有限公司 | Aluminum oxide/pectinate polyether block polyacrylic acid copolymer suspension system and preparation method thereof |
| CN112442183A (en) * | 2019-09-05 | 2021-03-05 | 财团法人工业技术研究院 | Aqueous polymer, dispersion and aqueous coating material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6123875A (en) * | 1998-07-24 | 2000-09-26 | Korea Research Institute Of Chemical Technology | Process for producing a rubber elastic copolymer, an ion-conducting thin membrane composition containing the copolymer, an ion-conducting thin membrane and a process for producing the same, and a solid electrochemical material containing the membrane |
| CN1712381A (en) * | 2004-06-21 | 2005-12-28 | 中国科学院广州化学研究所 | Polyether graft poly-carboxylic acid concrete water reducer preparation |
| CN1887712A (en) * | 2006-07-18 | 2007-01-03 | 中国铝业股份有限公司 | Prepn process of stable alpha-alumina suspension liquid |
-
2007
- 2007-07-11 CN CNB2007100250755A patent/CN100545217C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6123875A (en) * | 1998-07-24 | 2000-09-26 | Korea Research Institute Of Chemical Technology | Process for producing a rubber elastic copolymer, an ion-conducting thin membrane composition containing the copolymer, an ion-conducting thin membrane and a process for producing the same, and a solid electrochemical material containing the membrane |
| CN1712381A (en) * | 2004-06-21 | 2005-12-28 | 中国科学院广州化学研究所 | Polyether graft poly-carboxylic acid concrete water reducer preparation |
| CN1887712A (en) * | 2006-07-18 | 2007-01-03 | 中国铝业股份有限公司 | Prepn process of stable alpha-alumina suspension liquid |
Non-Patent Citations (4)
| Title |
|---|
| 4-Dialkylaminopyridines as Highly Active Acylation Catalysts. Gerhard Hofle, Wolfgang Steglich, and Helmut Vorbruggen.Angewandte Chemie International Edition in English. 1978 |
| 4-Dialkylaminopyridines as Highly Active Acylation Catalysts. Gerhard Hofle,Wolfgang Steglich,and Helmut Vorbruggen.Angewandte Chemie International Edition in English. 1978 * |
| lMicrospheresFormed byComplexCoacervationofPartiallyMPEG-GraftedPoly(styrene-alt-maleicanhydride)withPDADMAC andCross-Linking withPolyamines. Xiangchun Yin and Harald D.H. StoverHydrogel.Macromolecules,Vol.36 No.23. 2003 |
| lMicrospheresFormed byComplexCoacervationofPartiallyMPEG-GraftedPoly(styrene-alt-maleicanhydride)withPDADMAC andCross-Linking withPolyamines. Xiangchun Yin and Harald D.H. StoverHydrogel.Macromolecules,Vol.36 No.23. 2003 * |
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