CN102584059A - Preparation method of rapid dispersion powder for nano-crystalline cellulose - Google Patents
Preparation method of rapid dispersion powder for nano-crystalline cellulose Download PDFInfo
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Abstract
The invention provides a preparation method of rapid dispersion powder for nano-crystalline cellulose, relates to a preparation method of the rapid dispersion powder for the nano-crystalline cellulose, and aims to solve the technical problem of poor rapid dispersibility of the nano-crystalline cellulose prepared by adopting the conventional inorganic acid hydrolysis method. The preparation method comprises the steps that I, the nano-crystalline cellulose is prepared; II, the nano-crystalline cellulose is emulsified; III, 1,4-dioxane is added to aqueous dispersion liquid of the emulsified nano-crystalline cellulose to obtain mixed dispersion liquid, and the mixed dispersion liquid is frozen to obtain frozen gel; and IV, after the frozen gel is dried, the rapid dispersion powder for the nano-crystalline cellulose is obtained. The rapid dispersion powder for the nano-crystalline cellulose, which is provided by the invention, can be rapidly dispersed into deionized water, anhydrous alcohol, dimethylformamide, dimethylacetamide or acetic acid, the preparation method is simple and easy to operate and the preparation cost is low. The rapid dispersion powder for the nano-crystalline cellulose, which is prepared by adopting the preparation method, can serve as a nano strengthening agent to be applied to the industrial fields of building materials, and the like.
Description
Technical field
The present invention relates to the preparation method of nano-cellulose powder.
Background technology
Nano-cellulose is a kind of novel macromolecular material, has particular structure and good performance, can be used as nanometer strengthener and is applied to industrial fields such as material of construction.But existing nano-cellulose bad dispersibility with the preparation of mineral acid hydrolysis method; As when this nano-cellulose is added to the water; Only have the nano-cellulose about 1% can well be dispersed in the water, the preparation dispersion effect is suspension-s preferably, after the add-on of nano-cellulose increases again; Nano-cellulose can deposit, and has limited the range of application of nano-cellulose.
Summary of the invention
The present invention is the technical problem that will solve the nano-cellulose fast dispersibility difference of existing mineral acid hydrolysis method preparation, and provides a kind of nano-cellulose to disperse the preparation method of powder fast.
A kind of nano-cellulose of the present invention disperses the preparation method of powder fast, carries out according to the following steps:
One, the preparation of nano-cellulose: add the ratio that 100mL quality percentage composition is 50% sulphuric acid soln in 1g～3g Microcrystalline Cellulose; It is in 50% the sulphuric acid soln that Microcrystalline Cellulose is joined the quality percentage composition; Be acidolysis reaction 2.0h under 50 ℃ the condition in temperature, obtain nano-cellulose suspension-s, after the spinning; Solid formation is extremely neutral with deionized water wash, obtain nano-cellulose;
Two, the emulsification of nano-cellulose: the quality percentage composition by nano-cellulose is 1.0%, will in the nano-cellulose that step 1 obtains, add deionized water, obtains the nano-cellulose aqueous dispersions; Be that 5%～30% polyoxyethylene glycol of nano-cellulose quality joins in the nano-cellulose aqueous dispersions with quality again; In temperature is that 30 ℃～80 ℃, stirring velocity are heated and stirred 5min～30min under the condition of 100r/min～800r/min, obtains emulsification nano-cellulose aqueous dispersions;
Three, freezing gelation: by 1; The volume ratio of the emulsification nano-cellulose aqueous dispersions of 4-dioxane and step 2 preparation is 1: 5～20 ratio, and low whipping speed is under the condition of 100r/min～800r/min, with 1; The 4-dioxane splashes in the emulsification nano-cellulose aqueous dispersions of step 2 preparation with the speed of 60/min～180 droplet/min; After dropwising, continue again to stir 5min～30min, obtain mixed dispersion liquid; It is that-10 ℃～-20 ℃ refrigeration chamber cools off 2.0h～12.0h that mixed dispersion liquid is put into freezing temp, obtains freezing gel;
Four, lyophilize: with the freezing gel that step 3 obtains, be that 20Pa, cold hydrazine temperature are lyophilize 12.0h～20.0h in-50 ℃ the freeze drier, obtain nano-cellulose and disperse powder fast in vacuum tightness.
The molecular weight of the polyoxyethylene glycol described in the step 2 is 2000,4000,6000,8000,10000 or 20000.
It is at nano-cellulose surface adsorption polyoxyethylene glycol that nano-cellulose of the present invention disperses powder fast, thereby forms the coated with polyethylene glycol layer on the nano-cellulose surface, adds 1; The 4-dioxane is avoided occurring breaking away from the nano-cellulose surface because of freezing stage polyoxyethylene glycol solubleness falls sharply, and obtains nano-cellulose/polyoxyethylene glycol/1; 4-dioxane/water mixes freezing gel; Dewater with 1 through lyophilize, the 4-dioxane obtains wrapping up the fluffy solid of nano-cellulose of one deck polyoxyethylene glycol again; Polyoxyethylene glycol can make prepared nano-cellulose solid disperse to form aaerosol solution fast.
Nano-cellulose of the present invention disperses powder can be scattered in fast in deionized water, absolute ethyl alcohol, N (DMF), N,N-DIMETHYLACETAMIDE or the acetate fast.Dispersing method is: disperseing the volume ratio of powder and solvent fast in nano-cellulose is that 1: 20～100 ratio disperses powder to join in the solvent nano-cellulose fast; Stir 1min～10min with 100r/min～1000r/min speed, accomplish the dispersion that nano-cellulose disperses powder fast.After nano-cellulose wherein of the present invention disperses powder to add in the solvent fast, stirring under the 2min situation, dispersion effect is best fast in deionized water, and the mass content that can be dispersed in the nano-cellulose in the water can reach 5%; Relatively poor in the DMF organic solvent, solid content can reach about 0.2%.
The present invention prepares nano-cellulose and disperses the method for powder simple, easy to operate fast under the prerequisite that does not change the Mierocrystalline cellulose self character, preparation cost is low.Microcrystalline Cellulose in the inventive method can derive from wood pulp, straw pulp, bamboo pulp and agricultural stalk etc.
The nano-cellulose of the present invention's preparation disperses powder in different solvents, can reach nano level dispersion fast fast, can be used as nanometer strengthener and is applied to industrial fields such as material of construction.
Description of drawings
Fig. 1 is the transmission electron microscope figure that tests the nano-cellulose that obtains once step 1;
Fig. 2 is a particle size distribution figure of testing the nano-cellulose that obtains once step 1;
Fig. 3 disperses the environmental scanning electron microscope figure of powder fast for the nano-cellulose of test one preparation;
Fig. 4 obtains the Fourier transform infrared spectroscopy figure that nano-cellulose disperses powder fast for the nano-cellulose of polyoxyethylene glycol, step 1 preparation in the test one with through step 4; Wherein a is that molecular weight is the Fourier transform infrared spectroscopy of 4000 polyoxyethylene glycol, and b is the Fourier transform infrared spectroscopy that nano-cellulose disperses powder fast, and c is the Fourier transform infrared spectroscopy of the nano-cellulose of step 1 preparation;
Fig. 5 is for being the particle size distribution figure of the oyster white nano-cellulose aaerosol solution of solvent with water in the test one;
Fig. 6 is for being the particle size distribution figure of the oyster white nano-cellulose aaerosol solution of solvent with N (DMF) in the test one.
Embodiment
Embodiment one: a kind of nano-cellulose of this embodiment disperses the preparation method of powder fast, carries out according to the following steps:
One, the preparation of nano-cellulose: add the ratio that 100mL quality percentage composition is 50% sulphuric acid soln in 1g～3g Microcrystalline Cellulose; It is in 50% the sulphuric acid soln that Microcrystalline Cellulose is joined the quality percentage composition; Be acidolysis reaction 2.0h under 50 ℃ the condition in temperature, obtain nano-cellulose suspension-s, after the spinning; Solid formation is extremely neutral with deionized water wash, obtain nano-cellulose;
Two, the emulsification of nano-cellulose: the quality percentage composition by nano-cellulose is 1.0%, will in the nano-cellulose that step 1 obtains, add deionized water, obtains the nano-cellulose aqueous dispersions; Be that 5%～30% polyoxyethylene glycol of nano-cellulose quality joins in the nano-cellulose aqueous dispersions with quality again; In temperature is that 30 ℃～80 ℃, stirring velocity are heated and stirred 5min～30min under the condition of 100r/min～800r/min, obtains emulsification nano-cellulose aqueous dispersions;
Three, freezing gelation: by 1; The volume ratio of the emulsification nano-cellulose aqueous dispersions of 4-dioxane and step 2 preparation is 1: 5～20 ratio, and low whipping speed is under the condition of 100r/min～800r/min, with 1; The 4-dioxane splashes in the emulsification nano-cellulose aqueous dispersions of step 2 preparation with the speed of 60/min～180 droplet/min; After dropwising, continue again to stir 5min～30min, obtain mixed dispersion liquid; It is that-10 ℃～-20 ℃ refrigeration chamber cools off 2.0h～12.0h that mixed dispersion liquid is put into freezing temp, obtains freezing gel;
Four, lyophilize: with the freezing gel that step 3 obtains, be that 20Pa, cold hydrazine temperature are lyophilize 12.0h～20.0h in-50 ℃ the freeze drier, obtain nano-cellulose and disperse powder fast in vacuum tightness.
The nano-cellulose of this embodiment preparation disperses powder can be scattered in fast in deionized water, absolute ethyl alcohol, N (DMF), N,N-DIMETHYLACETAMIDE or the acetate fast.Dispersing method is: disperseing the volume ratio of powder and solvent fast in nano-cellulose is that 1: 20～100 ratio disperses powder to join in the solvent nano-cellulose fast; Stir 1min～10min with 100r/min～1000r/min speed, accomplish the dispersion that nano-cellulose disperses powder fast.After nano-cellulose wherein of the present invention disperses powder to add in the solvent fast, stirring under the 2min situation, dispersion effect is best fast in deionized water, and the mass content that can be dispersed in the nano-cellulose in the water can reach 5%; Relatively poor in the DMF organic solvent, solid content can reach 0.2%.This embodiment prepares nano-cellulose and disperses the method for powder simple, easy to operate fast under the prerequisite that does not change the Mierocrystalline cellulose self character, preparation cost is low.
Embodiment two: this embodiment and embodiment one are different is that the quality of polyoxyethylene glycol in the step 2 is 10%～25% of a nano-cellulose quality.Other is identical with embodiment one.
Embodiment three: this embodiment and embodiment one are different is that the quality of polyoxyethylene glycol in the step 2 is 20% of a nano-cellulose quality.Other is identical with embodiment one.
Embodiment four: this embodiment is different with one of embodiment one to three is in the step 31, and the volume ratio of the emulsification nano-cellulose aqueous dispersions of 4-dioxane and step 2 preparation is 1: 10～18, stirring velocity is 200r/min～700r/min.Other is identical with one of embodiment one to three.
Embodiment five: this embodiment is different with one of embodiment one to three is in the step 31, and the volume ratio of the emulsification nano-cellulose aqueous dispersions of 4-dioxane and step 2 preparation is that 1: 15, stirring velocity are 400r/min.Other is identical with one of embodiment one to three.
Embodiment six: what this embodiment was different with one of embodiment one to five is to dropwise continued in the step 3 to stir 10min～25min.Other is identical with one of embodiment one to five.
Embodiment seven: what this embodiment was different with one of embodiment one to six is to dropwise continued to stir 20min.Other is identical with one of embodiment one to six.
Embodiment eight: this embodiment is different with one of embodiment one to seven is that freezing temp is that-12 ℃～-18 ℃, cooling time are 4h～10h in the step 3.Other is identical with one of embodiment one to seven.
Embodiment nine: what this embodiment was different with one of embodiment one to eight is that sublimation drying is 15h～18h in the step 4.Other is identical with one of embodiment one to eight.
Embodiment ten: this embodiment is different with one of embodiment one to nine is that the molecular weight of the polyoxyethylene glycol described in the step 2 is 2000～20000; Other is identical with one of embodiment one to nine.
Demonstrate,prove beneficial effect of the present invention with following test test:
Test one: a kind of nano-cellulose of this test one disperses the preparation method of powder fast, carries out according to the following steps:
One, the preparation of nano-cellulose: it is in 50% the sulphuric acid soln that the 2g Microcrystalline Cellulose is joined 100mL quality percentage composition; In temperature acidolysis reaction 2.0h under 50 ℃ the condition; Obtain nano-cellulose suspension-s; After the spinning, solid formation is extremely neutral with deionized water wash, obtain nano-cellulose;
Two, the emulsification of nano-cellulose: the quality percentage composition by nano-cellulose is 1.0%, will in the nano-cellulose that step 1 obtains, add deionized water, obtains the nano-cellulose aqueous dispersions; Being that 4000 polyoxyethylene glycol joins in the nano-cellulose aqueous dispersions with the 0.2g molecular weight again, is that 50 ℃, stirring velocity are heated and stirred 20min under the condition of 500r/min in temperature, obtains emulsification nano-cellulose aqueous dispersions;
Three, freezing gelation: by 1, the volume ratio of the emulsification nano-cellulose aqueous dispersions of 4-dioxane and step 2 preparation is 1: 15 a ratio, and low whipping speed is under the condition of 500r/min; With 1; The 4-dioxane splashes in the emulsification nano-cellulose aqueous dispersions of step 2 preparation with the speed of 100/min, dropwises continued and stirs 20min, obtains mixed dispersion liquid; Mixed dispersion liquid is put into freezing temp cool off 10h, obtain freezing gel for-15 ℃ refrigeration chamber;
Four, lyophilize: with the freezing gel that step 3 obtains, be that 20Pa, cold hydrazine temperature are lyophilize 12h in-50 ℃ the freeze drier, obtain nano-cellulose and disperse powder fast in vacuum tightness.
This transmission electron microscope figure that tests the nano-cellulose that obtains once step 1 is as shown in Figure 1, and as can beappreciated from fig. 1 step 1 prepares nano-cellulose and is bar-shaped, is woven into netted.
This particle size distribution figure of testing the nano-cellulose that obtains once step 1 is as shown in Figure 2, and as can beappreciated from fig. 2 inhomogeneous through the nano-cellulose size-grade distribution that step 1 obtains, median size is 144.6nm;
The nano-cellulose of this test one preparation disperses the environmental scanning electron microscope figure of powder as shown in Figure 3 fast, and as can beappreciated from fig. 3, the nano-cellulose of this test one preparation disperses powder to be particulate state fast.
With the nano-cellulose of polyoxyethylene glycol, step 1 preparation with obtain nano-cellulose through step 4 and disperse powder to carry out the Fourier transform infrared spectroscopy test fast; The nano-cellulose of the polyoxyethylene glycol that obtains, step 1 preparation and obtain nano-cellulose through step 4 and disperse the Fourier transform infrared spectroscopy figure of powder as shown in Figure 4 fast; Wherein a is that molecular weight is the Fourier transform infrared spectroscopy of 4000 polyoxyethylene glycol; B is the Fourier transform infrared spectroscopy that nano-cellulose disperses powder fast, and c is the Fourier transform infrared spectroscopy of the nano-cellulose of step 1 preparation; As can beappreciated from fig. 4 the result shows that nano-cellulose disperses powder still to have cellulosic basic chemical structure fast.
The nano-cellulose of this test one preparation disperses the dispersivity test of powder in water fast:
Disperseing the volume ratio of powder and water fast in the nano-cellulose of this test one preparation is 1: 50 ratio; Disperse powder to be added to the water fast the nano-cellulose of this test one preparation; Stir 2min with 500r/min speed and disperse, obtain oyster white nano-cellulose dispersion soln.
The particle size distribution figure of the oyster white nano-cellulose dispersion soln that obtains is as shown in Figure 5; As can beappreciated from fig. 5; Nano-cellulose even particle size distribution, median size are 203.7nm, so the nano-cellulose of this test one preparation disperses powder to have good dispersiveness fast.
Dispersion effect is best fast in deionized water, and the mass content of nano-cellulose is 5%, because jitter time is merely 2min, explains that the nano-cellulose of this test one preparation disperses powder to disperse soon fast.
The nano-cellulose of this test one preparation disperses the dispersivity test of powder in DMF fast:
Disperseing the volume ratio of powder and DMF fast in the nano-cellulose of this test one preparation is 1: 50 ratio; Disperse powder to join among the DMF fast the nano-cellulose of this test one preparation; Stir 2min with 500r/min speed and disperse, obtain oyster white nano-cellulose aaerosol solution.
The particle size distribution figure of the oyster white nano-cellulose aaerosol solution that obtains is as shown in Figure 6; As can beappreciated from fig. 6, show that its size-grade distribution is inhomogeneous, median size is 273.3nm; After the nano-cellulose of this test one preparation disperses powder to add among the DMF fast; Dispersion in the DMF organic solvent disperses in than deionized water relatively poor, and solid content is 0.2%, and the nano-cellulose of this a test preparation disperses powder generally dispersed in DMF fast.
Claims (10)
1. a nano-cellulose disperses the preparation method of powder fast, it is characterized in that nano-cellulose disperses the preparation method of powder to carry out according to the following steps fast:
One, the preparation of nano-cellulose: add the ratio that 100mL quality percentage composition is 50% sulphuric acid soln in 1g～3g Microcrystalline Cellulose; It is in 50% the sulphuric acid soln that Microcrystalline Cellulose is joined the quality percentage composition; Be acidolysis reaction 2.0h under 50 ℃ the condition in temperature, obtain nano-cellulose suspension-s, after the spinning; Solid formation is extremely neutral with deionized water wash, obtain nano-cellulose;
Two, the emulsification of nano-cellulose: the quality percentage composition by nano-cellulose is 1.0%, will in the nano-cellulose that step 1 obtains, add deionized water, obtains the nano-cellulose aqueous dispersions; Be that 5%～30% polyoxyethylene glycol of nano-cellulose quality joins in the nano-cellulose aqueous dispersions with quality again; In temperature is that 30 ℃～80 ℃, stirring velocity are heated and stirred 5min～30min under the condition of 100r/min～800r/min, obtains emulsification nano-cellulose aqueous dispersions;
Three, freezing gelation: by 1; The volume ratio of the emulsification nano-cellulose aqueous dispersions of 4-dioxane and step 2 preparation is 1: 5～20 ratio, and low whipping speed is under the condition of 100r/min～800r/min, with 1; The 4-dioxane splashes in the emulsification nano-cellulose aqueous dispersions of step 2 preparation with the speed of 60/min～180 droplet/min; After dropwising, continue again to stir 5min～30min, obtain mixed dispersion liquid; It is that-10 ℃～-20 ℃ refrigeration chamber cools off 2.0h～12.0h that mixed dispersion liquid is put into freezing temp, obtains freezing gel;
Four, lyophilize: with the freezing gel that step 3 obtains, be that 20Pa, cold hydrazine temperature are lyophilize 12.0h～20.0h in-50 ℃ the freeze drier, obtain nano-cellulose and disperse powder fast in vacuum tightness.
2. a kind of nano-cellulose according to claim 1 disperses the preparation method of powder fast, and the quality that it is characterized in that polyoxyethylene glycol in the step 2 is 10%～25% of a nano-cellulose quality.
3. a kind of nano-cellulose according to claim 1 disperses the preparation method of powder fast, and the quality that it is characterized in that polyoxyethylene glycol in the step 2 is 20% of a nano-cellulose quality.
4. the preparation method who disperses powder according to claim 1,2 or 3 described a kind of nano-celluloses fast; It is characterized in that in the step 31, the volume ratio of the emulsification nano-cellulose aqueous dispersions of 4-dioxane and step 2 preparation is 1: 10～18, stirring velocity is 200r/min～700r/min.
5. the preparation method who disperses powder according to claim 1,2 or 3 described a kind of nano-celluloses fast; It is characterized in that in the step 31, the volume ratio of the emulsification nano-cellulose aqueous dispersions of 4-dioxane and step 2 preparation is that 1: 15, stirring velocity are 400r/min.
6. the preparation method who disperses powder according to claim 1,2 or 3 described a kind of nano-celluloses fast is characterized in that dropwising in the step 3 continued and stirs 10min～25min.
7. the preparation method who disperses powder according to claim 1,2 or 3 described a kind of nano-celluloses fast is characterized in that dropwising in the step 3 continued and stirs 20min.
8. the preparation method who disperses powder according to claim 1,2 or 3 described a kind of nano-celluloses fast is characterized in that in the step 3 that freezing temp is that-12 ℃～-18 ℃, cooling time are 4h～10h.
9. claim 1,2 or 3 described a kind of nano-celluloses disperse the preparation method of powder fast, it is characterized in that sublimation drying is 15h～18h in the step 4.
10. claim 1,2 or 3 described a kind of nano-celluloses disperse the preparation method of powder fast, and the molecular weight that it is characterized in that the polyoxyethylene glycol described in the step 2 is 2000～20000.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103275336A (en) * | 2013-06-19 | 2013-09-04 | 天津科技大学 | Preparation method for cellulose crystal susceptible to re-dispersion after drying |
| CN107460759A (en) * | 2017-08-18 | 2017-12-12 | 华南理工大学 | A kind of method for quickly purifying of nano-cellulose suspension |
| CN117362457A (en) * | 2023-10-17 | 2024-01-09 | 江苏蜀扬春新材料科技有限公司 | Green efficient preparation method of nanocellulose |
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| CN101874043A (en) * | 2007-11-26 | 2010-10-27 | 国立大学法人东京大学 | Cellulose nanofiber and process for production thereof, and cellulose nanofiber dispersion |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103275336A (en) * | 2013-06-19 | 2013-09-04 | 天津科技大学 | Preparation method for cellulose crystal susceptible to re-dispersion after drying |
| CN103275336B (en) * | 2013-06-19 | 2015-06-10 | 天津科技大学 | Preparation method for cellulose crystal susceptible to re-dispersion after drying |
| CN107460759A (en) * | 2017-08-18 | 2017-12-12 | 华南理工大学 | A kind of method for quickly purifying of nano-cellulose suspension |
| CN107460759B (en) * | 2017-08-18 | 2020-12-22 | 华南理工大学 | Rapid purification method of nano-cellulose suspension |
| CN117362457A (en) * | 2023-10-17 | 2024-01-09 | 江苏蜀扬春新材料科技有限公司 | Green efficient preparation method of nanocellulose |
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Application publication date: 20120718 |