CN106750384B - A kind of method of amino silane modified nano-cellulose aerogel - Google Patents
A kind of method of amino silane modified nano-cellulose aerogel Download PDFInfo
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Abstract
The present invention is a kind of method of amino silane modified nano-cellulose aerogel, comprising: 1) nano-cellulose suspension is made to become translucent colloid；2) nano-cellulose colloid is extruded into spherical or corynebacterium hydrogel；3) molding nanofiber hydrogel is made to become alcogel；4) nano-cellulose aerogel is made；5) gaseous state organic amine is adsorbed on nano-cellulose aerogel surface；6) vacuum recycles remaining organic amine catalyst；7) gaseous state amino silane is chemically reacted with nano-cellulose aerogel；8) vacuum recycles unreacted amino silane；9) nano-cellulose aerogel of corresponding Aminosilylation is made.Advantage: 1) solvent recovery, separation process encountered in liquid phase modifying process, the technique for simplifying aminated modification are eliminated；2) nano-cellulose aerogel prototype micro three-dimensional net structure is kept, modified grafting density and uniformity are improved；3) process is simple high-efficient at low cost.
Description
Technical field
The present invention relates to a kind of methods of amino silane modified nano-cellulose aerogel, and it is compound to belong to wood fibre
Field of material technology.
Background technique
Nano-cellulose is that spatially size is in the cellulose substances of Nano grade (1-100nm) to one or more dimensions,
It is a kind of natural polymer.The features such as reproducibility of its concrete fiber element, bio-compatibility be good, biodegradable, meanwhile, it
Also have the characteristics that biggish specific surface area, superior mechanical property and optical characteristics.Aeroge is a kind of with high-permeability
The material of three-dimensional net structure has the spies such as high porosity, higher specific surface area, extremely low density, the low capacity of heat transmission
Point.Currently, aeroge biological medicine carrier, photoelectric sensor, catalysis technique, adsorption technology, in terms of all have it is latent
Application.Nano-cellulose aerogel, which is nano-cellulose, is formed by gel by physically or chemically effect, it has simultaneously
There is the characteristic of nano-cellulose, aeroge, therefore, nano-cellulose aerogel has very extensive potential application foreground.
Currently, people are more and more interested to carry out nano-cellulose aerogel in order to be able to satisfy the application of every field
Functional modification carries out functional amido, the nanofiber of functional amido to nano-cellulose in particular by amino containing silane
Plain aeroge can be used for stationary phase, carbon dioxide gas and the metal ion adsorbent of all kinds of chromatographies, fixed biological enzyme molecule and
Antibody prepares semiconductor device and chemical sensor etc..
It is close that the functional amido method of nano-cellulose aerogel can severely impact the orientation of amino containing silane molecule, surface
The thickness of degree, amino containing silane molecule " coating ", will affect the hydroxyl type of action of amino silane molecules Yu nano-cellulose surface,
Finally affect the characteristic of aminated nano-cellulose aerogel.
It is mainly carried out in liquid phase (including water phase, organic phase) currently, nano-cellulose aerogel functional amido is modified,
When functional modification, amino containing silane molecule is difficult to control in nano-cellulose surface point distribution, after modified, nano-cellulose table
The thickness offset of the amino containing silane molecule " coating " in face is serious；Meanwhile the auto polymerization phenomenon between amino containing silane is serious, from
It is poly- to will lead to part potential close or blocking in nano-cellulose aerogel, porosity, the specific surface area of Primordial Qi gel are reduced,
Moreover, grafting density is low, generally only 3-6mmolN/g.In addition, when liquid phase is modified, there are solvent recovery, separating technology are complicated,
For this reason, it may be necessary to develop a kind of new process, the above problem encountered in liquid phase modifying process is overcome.
Summary of the invention
Proposed by the present invention is a kind of method of amino silane modified nano-cellulose aerogel, in the method, first
It is then activated using amino silane with by organic amine using the hydroxyl on anhydrous low molecule organic amine activation nano-cellulose surface
The hydroxyl on nano-cellulose surface chemically reacted, above-mentioned activation and chemical reaction process between gas-solid phase into
Row.The purpose of the present invention is intended to improve amino silane molecules and is uniformly distributed on nano-cellulose surface；It eliminates between amino containing silane
Autohemagglutination, retain nano-cellulose aerogel prototype micro three-dimensional net structure；Improve amino containing silane and cellulose surface
The efficiency of hydroxyl reaction, improves grafting density, is grafted uniformity.
Technical solution of the invention: a kind of method of amino silane modified nano-cellulose aerogel, including it is as follows
Step:
(1) nano-cellulose suspension is made to become translucent colloid；
(2) nano-cellulose colloid is extruded into spherical or corynebacterium hydrogel；
(3) molding nanofiber hydrogel is made to become alcogel；
(4) nano-cellulose aerogel is made；
(5) gaseous state organic amine is adsorbed on nano-cellulose aerogel surface；
(6) vacuum recycles remaining organic amine catalyst；
(7) gaseous state amino silane is chemically reacted with nano-cellulose aerogel；
(8) vacuum recycles unreacted amino silane；
(9) nano-cellulose aerogel of Aminosilylation is made.
Advantages of the present invention:
1) be conducive to amino containing silane molecule to be uniformly distributed on nano-cellulose surface；Be conducive to eliminate between amino containing silane
Autohemagglutination, can not only efficiently functionalized nano-fiber element aeroge, and holding nano-cellulose aerogel prototype micro three-dimensional
Network structure, to improve modified grafting density, uniformity；
2) appropriate catalyst is used, the hydroxyl on nano-cellulose surface is activated, to improve amino containing silane and cellulose table
The efficiency of the hydroxyl reaction in face, improves grafting density, is grafted uniformity；
3) the invention belongs to gas-solid phase chemical modification process, eliminate solvent recovery encountered in liquid phase modifying process,
Separation process, the technique for enormously simplifying the aminated modification of nano-cellulose；
4) relative to initial hydrogel, which is made amino silane nano-cellulose spherical aerogel diameter shrinking percentage 1-
3%；Radially, axially shrinking percentage is respectively 1-3%, 1-4% to rodlike aeroge, BET surface area 600-800m2/g, and average pore size is
15-25nm, average Kong Rongwei 1.1-1.6 cm3/g, organic amine grafting density are 7-10mmolN/g, gained aeroge it is cross-section
In (20,000 times) SEM image of face and longitudal section, without the cohesive body of amino silane autohemagglutination formation.
Specific embodiment
A kind of method of amino silane modified nano-cellulose aerogel, includes the following steps:
(1) the nano-cellulose powder for weighing 4.0-8.0g, is distributed in the deionized water of 200-400ml at room temperature, matches
Mass percent processed is 2-4% nano-cellulose suspension；In the case where power is 200-500w, it is ultrasonically treated suspension 2-5min,
The suspension is set to become translucent colloid；
(2) nano-cellulose colloid is extruded into spherical or bar-shaped hydrogel with the automatic moulding device of outlet diameter 1-4mm
In the CaCl2 solution of 0.02-1.0M, solid-to-liquid ratio 1-10(V/V), 8-12h is stood at room temperature；
(3) filtering removal CaCl2 solution, obtains molding nanofiber hydrogel, mass concentration 50,80 is respectively adopted
T-butanol solution with 100% carries out solvent displacement to molded nanofiber hydrogel, and time swap is respectively 2-4h,
4-6 h, 5-8h make molding nanofiber hydrogel become alcogel；
(4) it is 35-50 °C in temperature, under the conditions of pressure is 10-30MPa, nano-cellulose alcogel is carried out overcritical
Carbon dioxide abstraction 1-3h removes the remaining tert-butyl alcohol in gel, molding nano-cellulose aerogel is made；
(5) the molding nano-cellulose aerogel of 3-6g is laid on the porous plate in double-layer vacuum reaction kettle, is added
Lid sealing, starts vacuum system, the pressure in reaction kettle is made to be down to 10-40kPa；
(6) it is calculated by every gram of nano-cellulose aerogel addition 0.3-1.0mol, 0.9- is added in aforesaid reaction vessel
The anhydrous positive structure organic amine of the C3-C5 of 6mol.In the case where temperature is 25-30 °C, absolute pressure is 10-40kPa, reaction kettle is kept the temperature
30-50min, then, vacuum recycle remaining organic amine catalyst；
(7) 20-40mL is added by every gram of nano-cellulose aerogel, the N- (β-ammonia of 60-240ml is added in reaction kettle
Ethyl)-γ-aminopropyltriethoxy one methoxy silane or N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane or N-
(β-aminoethyl)-γ-aminopropyltriethoxy trimethoxy silane；Controlling absolute pressure inside reaction kettle is 80-100Pa；
(8) temperature of reaction kettle is increased to 110-130 DEG C, starts timing, carry out 10-16h wait react, later, vacuum is returned
Unreacted amino silane is received, is finished to amino silane recycling, takes out the molding nano-cellulose aerogel of Aminosilylation；
It (9) is 35-50 DEG C in temperature, under the conditions of pressure is 10-50MPa, to the molding nano-cellulose of Aminosilylation
Aeroge carries out supercritical carbon dioxide extracting, and time 1-3h removes residual amino silane, and the molding of Aminosilylation is made
Nano-cellulose aerogel；
A) relative to initial hydrogel, spherical aerogel diameter shrinking percentage 1-3%；Rodlike aeroge radially, axially shrinking percentage
Respectively 1-3%, 1-4%；
B) BET surface area 600-800m2/g；
C) average pore size is 15-25nm；
D) average Kong Rongwei 1.1-1.6 cm3/g；
E) organic amine grafting density is 7-10mmolN/g；
F) in the cross section of gained aeroge and (20,000 times) SEM image of longitudal section, without amino silane from combinate form
At cohesive body.
Embodiment
(1) 1.5g nano-cellulose is weighed, is distributed in 50g deionized water, under the conditions of power is 300W, ultrasound
3min.Then outlet diameter is that nano-cellulose colloid is extruded into spherical shape by the automatic moulding device of 3mm, is placed in the CaCl2 of 0.2M
In solution, solid-to-liquid ratio 5(V/V), 10h is stood at room temperature；Filtering removal CaCl2 solution, obtains molding nano-cellulose water
Gel.The t-butanol solution that mass concentration 50,80 and 100% is respectively adopted is molten to molded nanofiber hydrogel progress
Agent displacement, time swap is respectively 3,5,6h, and molding nanofiber hydrogel is made to become alcogel；It is 45 ° in temperature
C under the conditions of pressure is 15 MPa, carries out 2 h of supercritical carbon dioxide extracting to nano-cellulose alcogel, removes in gel
The remaining tert-butyl alcohol obtains molding nano-cellulose aerogel.3g nano-cellulose aerogel spheric granules is weighed, is laid in
It on porous plate in vacuum reaction kettle, seals, the absolute pressure controlled in reaction kettle is 20kPa, is added in a kettle
The anhydrous n-propylamine of 1.5mol；Under 25 °C, after reaction kettle is kept the temperature 40min, vacuum recycles remaining propylamine.By the N- of 90mL
(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane is added in reaction kettle；Absolute pressure keeps 85Pa inside reaction kettle
When, reaction kettle is put into rapidly in the oil bath that temperature is 120 °C, when reactor temperature is raised to 120 °C, starts timing, instead
It should carry out 14 h.Later, vacuum recycles unreacted amino silane, finishes to amino silane recycling, takes out Aminosilylation
Nano-cellulose aerogel.It is 45 °C in temperature, under the conditions of pressure is 150 MPa, to the nano-cellulose gas of Aminosilylation
Gel carries out 1.5 h of supercritical carbon dioxide extracting, removes residual amino silane, obtains the nano-cellulose ball of Aminosilylation
Shape aeroge；Its shrinking percentage is 2.1%(relative to raw water gel), 660 m2/g of BET surface area, average pore size is 20 nm, is put down
Equal hole holds 1.3cm3/g；Organic amine grafting density is 9mmolN/g.(20, the 000 times) SEM image in the cross section of the aeroge
In, without the cohesive body of amino silane autohemagglutination formation；
(2) 1.5g nano-cellulose is weighed, is distributed in 50g deionized water, under the conditions of power is 300W, ultrasound
3min.Then outlet diameter is that nano-cellulose colloid is extruded into corynebacterium hydrogel by the automatic moulding device of 4mm, is placed in 0.2M
CaCl2 solution in, solid-to-liquid ratio 5(V/V), stand 10h at room temperature；Filtering removal CaCl2 solution, obtains molding Nanowire
Tie up hydrogel.The t-butanol solution of mass concentration 50,80 and 100% is respectively adopted to molded nanofiber hydrogel
Solvent displacement is carried out, time swap is respectively 3,5,6h, and molding nanofiber hydrogel is made to become alcogel；In temperature
It is 45 °C, under the conditions of pressure is 15 MPa, 2 h of supercritical carbon dioxide extracting is carried out to nano-cellulose alcogel, removing is solidifying
The remaining tert-butyl alcohol in glue, obtains molding nano-cellulose aerogel.The rodlike aeroge of 3g nano-cellulose is weighed, is tiled
On the porous plate in vacuum reaction kettle, seal, control reaction kettle in absolute pressure be 20kPa, in a kettle plus
Enter the anhydrous n-propylamine of 1.5mol；Under 25 °C, after reaction kettle is kept the temperature 40min, vacuum recycles remaining propylamine.By 90mL's
N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane is added in reaction kettle；Absolute pressure keeps 85Pa inside reaction kettle
When, reaction kettle is put into rapidly in the oil bath that temperature is 120 °C, when reactor temperature is raised to 120 °C, starts timing, instead
It should carry out 14 h.Later, vacuum recycles unreacted amino silane, finishes to amino silane recycling, takes out Aminosilylation
Nano-cellulose aerogel.It is 45 °C in temperature, under the conditions of pressure is 15 MPa, to the nano-cellulose gas of Aminosilylation
Gel carries out 1.5 h of supercritical carbon dioxide extracting, removes residual amino silane, obtains the nano-cellulose stick of Aminosilylation
Shape aeroge；Radially, axially shrinking percentage is respectively 1.8% and 2.3%(relative to initial hydrogel for it), 690 m2/ of BET surface area
G, average pore size are 20 nm, and average hole holds 1.2cm3/g；Organic amine grafting density be 9.2mmolN/g, the aeroge it is cross-section
In (20,000 times) SEM image of face and longitudal section, without the cohesive body of amino silane autohemagglutination formation.
Claims (6)
1. a kind of method of amino silane modified nano-cellulose aerogel, it is characterized in that this method comprises the following steps:
(1) nano-cellulose suspension is made to become translucent colloid；
(2) nano-cellulose colloid is extruded into spherical or corynebacterium hydrogel；
(3) molding nanofiber hydrogel is made to become alcogel；
(4) nano-cellulose aerogel is made；
(5) gaseous state organic amine is adsorbed on nano-cellulose aerogel surface；
(6) vacuum recycles remaining organic amine catalyst；
(7) gaseous state amino silane is chemically reacted with nano-cellulose aerogel；
(8) vacuum recycles unreacted amino silane；
(9) nano-cellulose aerogel of Aminosilylation is made；
The step (1) makes nano-cellulose suspension become translucent colloid: weighing powdered nano-cellulose, divides at room temperature
It is scattered in deionized water, preparation mass percent is 2-4% nano-cellulose suspension；In the case where power is 200-500w, at ultrasound
Suspension 2-5min is managed, the suspension is made to become translucent colloid；
Nano-cellulose colloid is extruded into spherical or bar-shaped hydrogel by the step (2): with outlet diameter 1-4mm it is automatic at
Nano-cellulose colloid is extruded into spherical shape with type device or length is the bar-shaped hydrogel of 5-15mm in the CaCl of 0.02-1.0M2It is molten
In liquid, solid-to-liquid ratio is 1-10 V/V, stands 8-12h at room temperature；
Step (5) the gaseous state organic amine is adsorbed on nano-cellulose aerogel surface: by molding nano-cellulose gas
Gel is laid on the porous plate in double-layer vacuum reaction kettle, is sealed, and is started vacuum system, is made the absolute pressure in reaction kettle
It is down to 10-40kPa by force, calculates, is added in aforesaid reaction vessel suitable by every gram of nano-cellulose aerogel addition 0.3-1.0mol
The anhydrous positive structure organic amine of the C3-C5 of amount protects reaction kettle in the case where temperature is 25-30 DEG C, reaction kettle absolute pressure is 10-40kPa
Warm 30-50min；
Step (7) the gaseous state amino silane is chemically reacted with nano-cellulose aerogel；By every gram of nano-cellulose gas
Gel adds 20-40mL, and one methoxy silane of N- (β-aminoethyl)-γ-aminopropyltriethoxy or N- (β-ammonia are added in reaction kettle
Ethyl)-γ-aminopropyltriethoxy dimethoxysilane or N- (β-aminoethyl)-γ-aminopropyltriethoxy trimethoxy silane；Control
Absolute pressure is 80-100Pa inside reaction kettle, and temperature of reaction kettle is increased to 110-130 DEG C, starts timing, and reaction carries out 10-
16h。
The nano-cellulose aerogel of Aminosilylation is made in the step (9): it is 35-50 DEG C in temperature, pressure 10-
Under the conditions of 50MPa, supercritical carbon dioxide extracting carried out to the nano-cellulose aerogel of Aminosilylation, time 1-3h,
Remaining amino silane is removed, the nano-cellulose aerogel of corresponding Aminosilylation is obtained.
2. the method for a kind of amino silane modified nano-cellulose aerogel according to claim 1, it is characterized in that described
Step (3) makes molding nanofiber hydrogel become alcogel: filtering removal CaCl2Solution obtains molding Nanowire
Tie up hydrogel；Then, the t-butanol solution of mass concentration 50,80 and 100% is respectively adopted to molded nano-cellulose water
Gel carries out solvent displacement, and time swap is respectively 2-4h, 4-6 h, 5-8h, becomes molding nanofiber hydrogel
Alcogel.
3. the method for a kind of amino silane modified nano-cellulose aerogel according to claim 2, it is characterized in that described
Nano-cellulose aerogel is made in step (4): being 35-50 DEG C in temperature, under the conditions of pressure is 10-30MPa, to molding nanometer
Cellulose alcogel carries out supercritical carbon dioxide extracting 1-3h, removes the remaining tert-butyl alcohol in gel, and nanofiber is made
Plain aeroge.
4. the method for a kind of amino silane modified nano-cellulose aerogel according to claim 1, it is characterized in that described
Step (6) vacuum recycles remaining organic amine catalyst: after adsorption process, in 25-30 DEG C of temperature, reaction kettle absolute pressure
For under 30-70kPa, vacuum recycles remaining organic amine catalyst.
5. the method for a kind of amino silane modified nano-cellulose aerogel according to claim 1, it is characterized in that described
Step (8) vacuum recycles unreacted amino silane: reaction terminates, and is 110-130 DEG C in temperature, absolute pressure 80-140Pa
Under the conditions of, vacuum recycles unreacted amino silane, finishes to amino silane recycling, takes out the nano-cellulose of Aminosilylation
Aeroge.
6. the method for a kind of amino silane modified nano-cellulose aerogel according to claim 1, it is characterized in that described
The nano-cellulose aerogel of corresponding Aminosilylation is made in step (9): amino silane nanofiber is made in the process
Plain spherical aerogel diameter shrinking percentage 1-3%；Radially, axially shrinking percentage is respectively 1-3%, 1-4%, the surface BET to rodlike aeroge
Product 600-800m2/ g, average pore size 15-25nm, average Kong Rongwei 1.1-1.6 cm3/ g, organic amine grafting density are 7-
10mmolN/g in the cross section of gained aeroge and 20000 times of SEM images of longitudal section, is formed without amino silane autohemagglutination
Cohesive body.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880410A (en) * | 2010-07-21 | 2010-11-10 | 武汉大学 | High-strength transparent cellulose material and preparation method thereof |
| CN103265010A (en) * | 2013-05-27 | 2013-08-28 | 东华大学 | Three-dimensional carbon fiber based aerogel material and preparation method thereof |
| CN103288416A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Modified three-dimensional fiber-based aerogel material and preparation method thereof |
| CN106009031A (en) * | 2016-07-15 | 2016-10-12 | 东北林业大学 | Method for improving mechanical strength of cellulose aerogel |
-
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- 2016-12-29 CN CN201611241789.5A patent/CN106750384B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880410A (en) * | 2010-07-21 | 2010-11-10 | 武汉大学 | High-strength transparent cellulose material and preparation method thereof |
| CN103265010A (en) * | 2013-05-27 | 2013-08-28 | 东华大学 | Three-dimensional carbon fiber based aerogel material and preparation method thereof |
| CN103288416A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Modified three-dimensional fiber-based aerogel material and preparation method thereof |
| CN106009031A (en) * | 2016-07-15 | 2016-10-12 | 东北林业大学 | Method for improving mechanical strength of cellulose aerogel |
Non-Patent Citations (1)
| Title |
|---|
| "纤维素气凝胶及其疏水改性研究进展";刘昕昕等;《广东化工》;20160531;第43卷(第5期);第97-100页 |
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