CN102911374A - Preparation method for 2.0 generation of polyamidoamine PAMAM dendrimer - Google Patents
Preparation method for 2.0 generation of polyamidoamine PAMAM dendrimer Download PDFInfo
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- CN102911374A CN102911374A CN201210446763XA CN201210446763A CN102911374A CN 102911374 A CN102911374 A CN 102911374A CN 201210446763X A CN201210446763X A CN 201210446763XA CN 201210446763 A CN201210446763 A CN 201210446763A CN 102911374 A CN102911374 A CN 102911374A
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Abstract
The invention provides a preparation method for 2.0 generation of polyamidoamine (PAMAM) dendrimer, and belongs to the technical field of polymer materials. The method adopts a 'one-pot method' to synthesize PAMAM dendrimer, which greatly reduces synthetic procedures, lowers preparation cost, greatly reduces raw material and solvent consumption, and reduces separating frequency and dendrimer synthesize cost. The method can accelerate the realization of large-scale application of the PAMAM dendrimer in related industrial fields.
Description
Technical field
The invention belongs to field of polymer material preparing technology, particularly a kind of 2.0 generation polyamide-amine dendrimer the preparation method.
Background technology
Polyamide-amine dendrimer is the macromolecular material that a class has dissaving structure, structurally is different from traditional branched polymer, and its size, shape are controlled, and there is cavity inside, and the surface has abundant functional group etc.The proposition of dendrimer is the thing of nearly two more than ten years, is one of focus of at present research.Dendrimer all is comprised of three distinct portions usually: first part is the active centre, is the start-up portion of dendrimer; Second section is positioned at the middle part of dendrimer by the internal layer that a plurality of repetition branching units form; Third part is to have the skin that enriches surface functional group, is the end part of dendrimer, and these three parts influence each other and consisted of an independently molecular system.Dendrimer distributes and has monodispersity, and has the constructional feature of the uniquenesses such as topology, makes it demonstrate wide potential application foreground in various fields such as mould material, nano composite material, biological medicine carrier, catalyzer.
At present, the synthetic method of polyamide-amine dendrimer mainly contains the method for dispersing, convergence method and disperses the convergence combined techniques, but no matter adopts any synthetic method all to need the reaction of multistep and needs underpressure distillation repeatedly to separate.For example need underpressure distillation twice in synthetic 1.0 generations during polyamide-amine dendrimer; In synthetic 2.0 generations, need during polyamide-amine dendrimer underpressure distillation four times just passable; Need 2n underpressure distillation when synthesizing n for polyamide-amine dendrimer, so just caused its synthesis step loaded down with trivial details, preparation cost is very high, has limited its application in industry.Find through literature search, have no report about the research of adopting " one kettle way " preparation polyamide-amine dendrimer at present.
Summary of the invention
The object of the present invention is to provide a kind of 2.0 generation polyamide-amine dendrimer the preparation method.Adopt " one kettle way " synthesizing polyamides amine dendrimer, can reduce synthetic step like this, reduce the cost of preparation.Can reduce greatly starting material and solvent usage quantity like this, reduce the number of times that separates, reduce the synthetic cost of dendrimer, can accelerate to realize the large-scale application of polyamide-amine dendrimer in the related industries field.
Provided by the present invention a kind of 2.0 generation polyamide-amine dendrimer preparation method's concrete steps as follows:
(1) add successively quadrol and anhydrous methanol in the reactor, under agitation condition, slowly drip methyl acrylate, under 20-30 ℃ temperature of reaction, reaction 6-12h, obtain 0.5 generation polyamide-amine dendrimer, the molfraction of described quadrol, anhydrous methanol and methyl acrylate is respectively 1,10,4;
(2) obtain dripping in the 0.5 generation polyamide-amine dendrimer quadrol in described step (1) and carry out amidate action, add simultaneously anhydrous methanol, under 20-30 ℃ temperature of reaction, the reaction 12-24h obtain 1.0 generation polyamide-amine dendrimer absolute methanol solution, the molfraction of described quadrol and anhydrous methanol is respectively 4,2;
(3) under agitation condition, to step (2) obtain 1.0 generation polyamide-amine dendrimer absolute methanol solution in slowly drip methyl acrylate, the molfraction of described methyl acrylate is 8, under 20-30 ℃ temperature of reaction, the reaction 6-12h, obtain 1.5 generation polyamide-amine dendrimer;
(4) dripping molfraction in the 1.5 generation polyamide-amine dendrimers that step (3) obtains is that 8 quadrol carries out amidate action, add simultaneously molfraction and be 4 anhydrous methanol, under 20-30 ℃ temperature of reaction, the reaction 12-24h obtain 2.0 generation polyamide-amine dendrimer absolute methanol solution, then underpressure distillation remove anhydrous methanol obtain 2.0 generation polyamide-amine dendrimer.
The inventive method preparation is simple, and the inventive method is compared with prior synthesizing method, owing to used less quadrol and reduced the separation number of times in building-up process in the amidation stage, has saved raw material, has reduced disengaging time and energy consumption.
Embodiment
Embodiment 1: at first 0.01 mole quadrol and 0.1 mole anhydrous methanol added in the there-necked flask of 250ml successively, under agitation condition, slowly drips 0.04 mole methyl acrylate, and under 30 ℃ temperature of reaction, reaction 6h; And then directly to drip mol ratio be that 0.04 mole quadrol carries out amidate action, adds simultaneously mol ratio and be 0.02 mole anhydrous methanol, and under 20 ℃ temperature of reaction, reaction 24h obtains the absolute methanol solution of 1.0 generation PAMAM.Under agitation condition, slowly drip 0.08 mole methyl acrylate, under 20 ℃ temperature of reaction, reaction 12h; And then the quadrol that drips 0.08 mole carries out amidate action, adds simultaneously 0.04 mole anhydrous methanol, under 20 ℃ temperature of reaction, and reaction 20h, anhydrous methanol is removed in last underpressure distillation, obtains the polyamide-amine dendrimer in 2.0 generations.
Embodiment 2: at first 0.01 mole quadrol and 0.1 mole anhydrous methanol added in the there-necked flask of 250ml successively, under agitation condition, slowly drips 0.04 mole methyl acrylate, and under 25 ℃ temperature of reaction, reaction 10h; And then directly to drip mol ratio be that 0.04 mole quadrol carries out amidate action, adds simultaneously mol ratio and be 0.02 mole anhydrous methanol, and under 25 ℃ temperature of reaction, reaction 18h obtains the absolute methanol solution of 1.0 generation PAMAM.Under agitation condition, slowly drip 0.08 mole methyl acrylate, under 20 ℃ temperature of reaction, reaction 12h; And then the quadrol that drips 0.08 mole carries out amidate action, adds simultaneously 0.04 mole anhydrous methanol, under 20 ℃ temperature of reaction, and reaction 24h, anhydrous methanol is removed in last underpressure distillation, obtains the polyamide-amine dendrimer in 2.0 generations.
Embodiment 3: at first 0.01 mole quadrol and 0.1 mole anhydrous methanol added in the there-necked flask of 250ml successively, under agitation condition, slowly drips 0.04 mole methyl acrylate, and under 20 ℃ temperature of reaction, reaction 12h; And then directly to drip mol ratio be that 0.04 mole quadrol carries out amidate action, adds simultaneously mol ratio and be 0.02 mole anhydrous methanol, and under 20 ℃ temperature of reaction, reaction 24h obtains the absolute methanol solution of 1.0 generation PAMAM.Under agitation condition, slowly drip 0.08 mole methyl acrylate, under 20 ℃ temperature of reaction, reaction 12h; And then the quadrol that drips 0.08 mole carries out amidate action, adds simultaneously 0.04 mole anhydrous methanol, under 30 ℃ temperature of reaction, and reaction 12h, anhydrous methanol is removed in last underpressure distillation, obtains the polyamide-amine dendrimer in 2.0 generations.
Claims (1)
- One kind 2.0 generation polyamide-amine dendrimer the preparation method, it is characterized in that these preparation method's concrete steps are as follows:(1) add successively quadrol and anhydrous methanol in the reactor, under agitation condition, slowly drip methyl acrylate, under 20-30 ℃ temperature of reaction, reaction 6-12h, obtain 0.5 generation polyamide-amine dendrimer, the molfraction of described quadrol, anhydrous methanol and methyl acrylate is respectively 1,10,4;(2) obtain dripping in the 0.5 generation polyamide-amine dendrimer quadrol in described step (1) and carry out amidate action, add simultaneously anhydrous methanol, under 20-30 ℃ temperature of reaction, the reaction 12-24h obtain 1.0 generation polyamide-amine dendrimer absolute methanol solution, the molfraction of described quadrol and anhydrous methanol is respectively 4,2;(3) under agitation condition, to step (2) obtain 1.0 generation polyamide-amine dendrimer absolute methanol solution in slowly drip methyl acrylate, the molfraction of described methyl acrylate is 8, under 20-30 ℃ temperature of reaction, the reaction 6-12h, obtain 1.5 generation polyamide-amine dendrimer;(4) dripping molfraction in the 1.5 generation polyamide-amine dendrimers that step (3) obtains is that 8 quadrol carries out amidate action, add simultaneously molfraction and be 4 anhydrous methanol, under 20-30 ℃ temperature of reaction, the reaction 12-24h obtain 2.0 generation polyamide-amine dendrimer absolute methanol solution, then underpressure distillation remove anhydrous methanol obtain 2.0 generation polyamide-amine dendrimer.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232363A (en) * | 2013-04-18 | 2013-08-07 | 西安理工大学 | Method for continuously preparing poly(amido-amine) |
| CN104479141A (en) * | 2014-11-28 | 2015-04-01 | 安徽工业大学 | Method for preparing extracting agent containing high-density amino groups and ether functional groups |
| CN105482573A (en) * | 2015-12-28 | 2016-04-13 | 杭州名匠建筑装饰工程有限公司 | Super self-cleaning organic building external wall coating and preparation method thereof |
| CN108126677A (en) * | 2017-12-28 | 2018-06-08 | 安徽工业大学 | A kind of preparation method of carbon composite for Acid Dye Wastewater processing |
| CN109181659A (en) * | 2018-09-10 | 2019-01-11 | 长江大学 | End group is the dendrimer intercalator and preparation method thereof of quaternary ammonium group |
| CN109287624A (en) * | 2018-10-08 | 2019-02-01 | 威海晨源分子新材料有限公司 | A kind of application of dendritic interphase in pesticide |
| CN110144377A (en) * | 2019-07-15 | 2019-08-20 | 鲁东大学 | A kind of preparation method of shellfish high F value oligopeptide |
| CN112430333A (en) * | 2020-11-30 | 2021-03-02 | 长江大学 | Demulsifier, carbon nano tube/hyperbranched polymer and preparation method and application thereof |
-
2012
- 2012-11-11 CN CN201210446763XA patent/CN102911374A/en active Pending
Non-Patent Citations (1)
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| 章昌华等: "一种聚酰胺胺-苯甲醛树状大分子的合成及其荧光性能", 《精细化工》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232363A (en) * | 2013-04-18 | 2013-08-07 | 西安理工大学 | Method for continuously preparing poly(amido-amine) |
| CN103232363B (en) * | 2013-04-18 | 2016-01-20 | 西安理工大学 | The continuous production method of polyamide-amide |
| CN104479141A (en) * | 2014-11-28 | 2015-04-01 | 安徽工业大学 | Method for preparing extracting agent containing high-density amino groups and ether functional groups |
| CN105482573A (en) * | 2015-12-28 | 2016-04-13 | 杭州名匠建筑装饰工程有限公司 | Super self-cleaning organic building external wall coating and preparation method thereof |
| CN108126677A (en) * | 2017-12-28 | 2018-06-08 | 安徽工业大学 | A kind of preparation method of carbon composite for Acid Dye Wastewater processing |
| CN109181659A (en) * | 2018-09-10 | 2019-01-11 | 长江大学 | End group is the dendrimer intercalator and preparation method thereof of quaternary ammonium group |
| CN109287624A (en) * | 2018-10-08 | 2019-02-01 | 威海晨源分子新材料有限公司 | A kind of application of dendritic interphase in pesticide |
| CN110144377A (en) * | 2019-07-15 | 2019-08-20 | 鲁东大学 | A kind of preparation method of shellfish high F value oligopeptide |
| CN112430333A (en) * | 2020-11-30 | 2021-03-02 | 长江大学 | Demulsifier, carbon nano tube/hyperbranched polymer and preparation method and application thereof |
| CN112430333B (en) * | 2020-11-30 | 2022-08-30 | 长江大学 | Demulsifier, carbon nano tube/hyperbranched polymer and preparation method and application thereof |
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Application publication date: 20130206 |