CN1709913A - Method for preparing nano microcrystal fiber powder capable of dispersing in non hydrosolvent and use thereof - Google Patents
Method for preparing nano microcrystal fiber powder capable of dispersing in non hydrosolvent and use thereof Download PDFInfo
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- CN1709913A CN1709913A CN 200510035599 CN200510035599A CN1709913A CN 1709913 A CN1709913 A CN 1709913A CN 200510035599 CN200510035599 CN 200510035599 CN 200510035599 A CN200510035599 A CN 200510035599A CN 1709913 A CN1709913 A CN 1709913A
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Abstract
This invention has disclosed a method of preparation and application to a kind of nano-microcrystalline cellulose powder which can disperse in non-aqueous solvent. Separate nano-microcrystalline whose particle diameter is between 30 to 50nm averagely, add hydrophilicity low-molecule surface active agent, surfactant, then heat drying. Put stated powder by 1:5-20 proportion into dimethyl formamide, dimethyl acetamide or dimethyl pyrrolidone, adopt the supersound oscillation to separate, can make nano-microcrystalline reach the separation of the size of nanometer.
Description
Technical field
The present invention relates to a kind of can in non-aqueous solvent, the preparation method and the dispersion in non-aqueous solvents such as dimethyl formamide, N,N-DIMETHYLACETAMIDE or dimethyl pyrrolidone thereof of dispersive nano micro crystal cellulose powder the application.
Background technology
Mierocrystalline cellulose is widespread in nature, and is a kind of inexhaustible, nexhaustible recyclability resource.In world oil, coal and natural gas source exhausted day by day today, use the Mierocrystalline cellulose of environmental protection, wide material sources to become the focus of whole world research as industrial chemicals and intermediate.
The range of molecular weight distributions of natural cellulose is wide, does not wait the degree of crystallinity height to millions of from hundreds of thousands of.Nano micro crystal cellulose is made fine cellulose existence form, CN1334272A; CN1369508A discloses the manufacture method of relevant nano micro crystal cellulose.
The nano micro crystal cellulose surfactivity is high and chemical property is active, is with a wide range of applications, and can be used as the packing material and the raw material in fields such as food, medicine, chemical industry.
There is the hydroxyl of more much amounts in the nano micro crystal cellulose surface, under drying regime, form the intensive hydrogen bond between particle surface, cause the reunion that can not be split between the nano micro crystal cellulose particle that adopts after the general method heat drying dewaters, and reunite in case formation adopts physical method to be difficult to carry out redispersion.
The nano micro crystal cellulose wetting ability is extremely strong, easily be dispersed in the water medium, and to be dispersed in the water also is its best way of storing at present that this has limited its range of application to a certain extent.
Reported in the United States Patent (USP) 3539365 that adding carboxymethyl cellulose by blend usually overcomes the reunion that takes place because of surperficial hydrogen bond action between the microfine cellulose crystallite.Owing to can't guarantee that in the blend process carboxymethyl cellulose is uniformly distributed between the microfine cellulose crystallite, cause still local the existence to be reunited.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method that can in non-aqueous solvent, make nano-scale rank dispersive nano micro crystal cellulose powder.
Another object of the present invention is to propose the dispersion of prepared nano micro crystal cellulose powder in non-aqueous solvents such as dimethyl formamide, N,N-DIMETHYLACETAMIDE or dimethyl pyrrolidone to use.
Preparation can be made nano-scale rank dispersive nano micro crystal cellulose powder in non-aqueous solvent method is: the nano micro crystal cellulose of particle diameter between 30～50nm is dispersed in the water, in this nano micro crystal cellulose aqueous dispersion, add the wetting ability low-molecular-weight surfactant, its weight part accounts for 0.1～3% of nano micro crystal cellulose net weight, heat drying is with the water in the system of removing then, promptly make the basis that contains low-molecular-weight surfactant can be in non-aqueous solvent dispersive nano micro crystal cellulose powder.
Described wetting ability low-molecular-weight surfactant can adopt any in PEG200, PEG400, PEG600, PEG800, PEG1000, PEG2000, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, Span series of surfactants, the OP series of surfactants or their mixture.
In described preparation method, the temperature of system heat drying is controlled at 105～120 ℃ of scopes.
The prepared nano micro crystal cellulose powder that contains low-molecular-weight surfactant of the present invention can be used in the dispersion in dimethyl formamide, N,N-DIMETHYLACETAMIDE or the dimethyl pyrrolidone, method is that described powder is joined in dimethyl formamide, N,N-DIMETHYLACETAMIDE or the dimethyl pyrrolidone with 1: 5～20 ratio, adopt sonic oscillation to disperse 0.5～2h, and make nano micro crystal cellulose reach the dispersion of nano-scale therein.
The present invention adopts and add an amount of wetting ability low-molecular-weight surfactant in the nano micro crystal cellulose aqueous dispersion, after stirring, physical mechanical is isolated and the dual consonance effect of chemical bond affine (as hydrogen bond), remove water in the system at the above proper temperature scope of the boiling point of water inner drying, tensio-active agent progressively replaces water molecules and is penetrated between the nano micro crystal cellulose particle in removal process, reach the effect that stops reunion, thereby make the nano micro crystal cellulose powder that contains low-molecular-weight surfactant.Through evidence, this nano micro crystal cellulose powder can reach other dispersion of nano-scale level in non-aqueous solvents such as dimethyl formamide, N,N-DIMETHYLACETAMIDE or dimethyl pyrrolidone, can expand the nano micro crystal cellulose range of application greatly.
Embodiment
Embodiment one
Add the 1.2% tensio-active agent OP-10 that weight part accounts for the nano micro crystal cellulose net weight in the nano micro crystal cellulose aqueous dispersion, fully mix, be heated to 110 ℃ of dry 6h and dewater, promptly make of the present invention can be in non-aqueous solvent dispersive nano micro crystal cellulose powder.Products therefrom joins in the dimethyl formamide with 1: 5 ratio, and the back that stirs adopts sonic oscillation to disperse 2h.Detecting the Microcrystalline Cellulose that shows through above processing by electron microscope is dispersed in the dimethyl formamide with the nano level size particles.Detect grain diameter in the nano level scope through transmission electron microscope.
Embodiment two
Add the 1.5% tensio-active agent Span-80 that weight part accounts for the nano micro crystal cellulose net weight in the nano micro crystal cellulose aqueous dispersion, fully mix, be heated to 105 ℃ of dry 4h and dewater, promptly make of the present invention can be in non-aqueous solvent dispersive nano micro crystal cellulose powder.Products therefrom joins in the dimethyl formamide with 1: 10 ratio, and the back that stirs adopts sonic oscillation to disperse 1.5h.The electron microscope result shows that Microcrystalline Cellulose is dispersed in the dimethyl formamide with the nano level size particles.Detect grain diameter in the nano level scope through transmission electron microscope.
Embodiment three
Add 1% Surfactant PEG 1000 that weight part accounts for the nano micro crystal cellulose net weight in the nano micro crystal cellulose aqueous dispersion, fully mix, be heated to 115 ℃ of dry 2h and dewater, promptly make of the present invention can be in non-aqueous solvent dispersive nano micro crystal cellulose powder.Products therefrom joins in the N,N-DIMETHYLACETAMIDE with 1: 15 ratio, and the back that stirs adopts sonic oscillation to disperse 1h.Show that by the electron microscope detection Microcrystalline Cellulose is dispersed in the N,N-DIMETHYLACETAMIDE with the nano level size particles.Detect grain diameter in the nano level scope through transmission electron microscope.
Embodiment four
Add 1.5% Surfactant PEG 500 and the 1.5% tensio-active agent Span-80 that weight part accounts for the nano micro crystal cellulose net weight in the nano micro crystal cellulose aqueous dispersion, fully mix, be heated to 120 ℃ of dry 2h and dewater, promptly make of the present invention can be in non-aqueous solvent dispersive nano micro crystal cellulose powder.Products therefrom joins in the dimethyl pyrrolidone with 1: 20 ratio, and the back that stirs adopts sonic oscillation to disperse 0.5h.The electron microscope detected result shows that Microcrystalline Cellulose is dispersed in the dimethyl pyrrolidone with the nano level size particles.Detect grain diameter in the nano level scope through transmission electron microscope.
Claims (4)
1, a kind of can be in non-aqueous solvent the method for making of dispersive nano micro crystal cellulose powder, it is characterized in that the nano micro crystal cellulose of particle diameter between 30～50nm is dispersed in the water, in this nano micro crystal cellulose aqueous dispersion, add the wetting ability low-molecular-weight surfactant, its weight part accounts for 0.1～3% of nano micro crystal cellulose net weight, heat drying is with the water in the system of removing then, promptly make originally can be in non-aqueous solvent dispersive nano micro crystal cellulose powder.
2, the method for making of nano micro crystal cellulose powder according to claim 1 is characterized in that described wetting ability low-molecular-weight surfactant is any in PEG200, PEG400, PEG600, PEG800, PEG1000, PEG2000, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, Span series of surfactants, the OP series of surfactants or their mixture.
3, the method for making of nano micro crystal cellulose powder according to claim 1 is characterized in that the temperature to the system heat drying is 105～120 ℃.
4, the dispersion of the prepared powder of claim 1 in dimethyl formamide, N,N-DIMETHYLACETAMIDE or dimethyl pyrrolidone used, method is that described powder is joined in dimethyl formamide, N,N-DIMETHYLACETAMIDE or the dimethyl pyrrolidone with 1: 5～20 ratio, the employing sonic oscillation disperses, and makes nano micro crystal cellulose reach the dispersion of nano-scale therein.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100355993A CN100340576C (en) | 2005-06-30 | 2005-06-30 | Method for preparing nano microcrystal fiber powder capable of dispersing in non hydrosolvent and use thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100355993A CN100340576C (en) | 2005-06-30 | 2005-06-30 | Method for preparing nano microcrystal fiber powder capable of dispersing in non hydrosolvent and use thereof |
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| CN1709913A true CN1709913A (en) | 2005-12-21 |
| CN100340576C CN100340576C (en) | 2007-10-03 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007096180A2 (en) * | 2006-02-23 | 2007-08-30 | J. Rettenmaier & Söhne GmbH & Co. KG | Base paper and production thereof |
| CN106854287A (en) * | 2016-12-20 | 2017-06-16 | 华南理工大学 | A kind of method for disperseing nanocrystalline cellulose powder in an aqueous medium |
| CN109081988A (en) * | 2018-07-13 | 2018-12-25 | 东北林业大学 | A method of polyolefin-based composite material is prepared using surfactant-dispersed micro-nano cellulose |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1171904C (en) * | 2000-07-18 | 2004-10-20 | 中国科学院广州化学研究所 | Nm-class microcrystal cellulose and its preparing process |
| CN1314462A (en) * | 2001-04-13 | 2001-09-26 | 白金花 | Nanometer washing powder and preparing method |
| CN1302997C (en) * | 2003-11-14 | 2007-03-07 | 中山大学 | Nanometer titanium dioxide powder dispersion method |
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2005
- 2005-06-30 CN CNB2005100355993A patent/CN100340576C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007096180A2 (en) * | 2006-02-23 | 2007-08-30 | J. Rettenmaier & Söhne GmbH & Co. KG | Base paper and production thereof |
| WO2007096180A3 (en) * | 2006-02-23 | 2008-01-03 | Rettenmaier & Soehne Gmbh & Co | Base paper and production thereof |
| CN106854287A (en) * | 2016-12-20 | 2017-06-16 | 华南理工大学 | A kind of method for disperseing nanocrystalline cellulose powder in an aqueous medium |
| CN106854287B (en) * | 2016-12-20 | 2019-07-16 | 华南理工大学 | A method of dispersing nanocrystalline cellulose powder in an aqueous medium |
| CN109081988A (en) * | 2018-07-13 | 2018-12-25 | 东北林业大学 | A method of polyolefin-based composite material is prepared using surfactant-dispersed micro-nano cellulose |
| CN109081988B (en) * | 2018-07-13 | 2020-08-14 | 东北林业大学 | Method for preparing polyolefin-based composite material by dispersing micro-nano cellulose through surfactant |
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| CN100340576C (en) | 2007-10-03 |
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Granted publication date: 20071003 Termination date: 20120630 |