CN109679134A - A kind of starch blending cellulose aerogels and its preparation and application - Google Patents
A kind of starch blending cellulose aerogels and its preparation and application Download PDFInfo
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- CN109679134A CN109679134A CN201811633979.0A CN201811633979A CN109679134A CN 109679134 A CN109679134 A CN 109679134A CN 201811633979 A CN201811633979 A CN 201811633979A CN 109679134 A CN109679134 A CN 109679134A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/12—Amylose; Amylopectin; Degradation products thereof
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Abstract
The present invention provides a kind of starch blending cellulose aerogels and its preparation and application.Cellulose aerogels are modified using starch, starch blending cellulose aerogels are made with high-pressure homogeneous blending and vacuum freeze drying in auxiliary.The present invention utilizes the strongly hydrophilic of starch, copolyreaction is realized with cellulose whiskers after miniaturization and aging process, improve the performance of cellulose base aeroge, make full use of cheap raw material, simplify preparation process flow, provides source abundant to improve composite material combination property.Starch blending cellulose aerogels of the invention have many advantages, such as that density is small, porosity is high, cubical contraction is small, oil absorbency is good and Dynamic Viscoelastic performance is good compared with general fibre element base aeroge.
Description
Technical field
The present invention relates to cellulose base aeroges, and in particular to a kind of starch blending cellulose aerogels and its preparation and answers
With.
Background technique
The method of commonly used processing water pollution has physical treatment, chemical treatment and biological treatment at present, wherein with object
The absorption managed in processing method is the most simple and easy, therefore the most commonly used.Natural material adsorbent has wheat straw, rice hull ash, resin etc.,
But it is not used largely due to its adsorptivity difference and reusable property poor the disadvantages of.SiO2Aeroge, graphene oxide airsetting
The inorganic aerogels such as glue have many advantages, such as high-absorbility, high porosity, bigger serface, but it can not degrade, it is possible to cause
Secondary pollution, and it is at high cost the disadvantages of, significantly limitation application range.Therefore, prepare a kind of novel, green, high-absorbility, can quilt
The recyclable materials of environment degradable have important economic benefit and environmental benefit extremely urgent, and cellulose base aeroge is one
The effective alternative materials of kind.
Cellulose aerogels not only inherit the high porosity and large surface of prior-generation aeroge as aeroge of new generation
Product, and overcome the not biodegradable problem of inorganic aerogels raw cellulose.People are to cellulose base airsetting in recent years
The research of glue is increasingly deep, and researcher wishes by being processed to realize that it is functional and improves to cellulose base aeroge
The disadvantage of oil-water separativeness difference and poor mechanical property etc..Scientist attempts by by cellulose and MnFe2O4, SiO2, chitosan
Equal other materials mixing carrys out the oil absorptive function of reinforcing fiber element aeroge and improves its mechanical property, but because of its material expensive or system
Application is limited for complex process.The present invention prepares aeroge using starch blending cellulose, can make full use of cheap raw material,
Simplify preparation process flow, while oil absorptive function creep resistance and the Dynamic Viscoelastic spy of cellulose base aeroge can be significantly increased
Property, it is domestic at present there is not yet addition starch improves the research of cellulose base aeroge performance.
Summary of the invention
The object of the present invention is to provide a kind of starch blending cellulose aerogels and its preparation and application, to improve composite wood
The comprehensive performance of material.
Starch blending cellulose aerogels provided by the present invention are raw material by microcrystalline cellulose, amylomaize
It is made.
Starch blending cellulose aerogels provided by the present invention, are as follows: cellulose aerogels are modified using starch,
Auxiliary is with starch blending cellulose aerogels made from high-pressure homogeneous blending and vacuum freeze drying.
Starch blending cellulose aerogels provided by the present invention are prepared by a method comprising the following steps to obtain:
1) blend solution of microcrystalline cellulose, amylomaize and water is prepared；
2) above-mentioned blend solution is subjected to high-pressure homogeneous processing, obtains homogenizing fluid；
3) it will be taken out after the freezing of above-mentioned homogenizing fluid, thaw and stir, sodium hydroxide and urea is added, obtain wet gel；
4) wet gel is successively replaced using hydrochloric acid, water, obtains white hydrogel；
5) above-mentioned white hydrogel is subjected to vacuum freeze drying processing, obtains aeroge.
In above method step 1), the microcrystalline cellulose and amylomaize pass through at ultramicro grinding before blending
Reason, to reduce its partial size and destroy its crystalline texture；
The ultramicro grinding carries out in planetary ball mill；
The planetary ball mill uses stainless steel grinding jar；
The zirconia ball that the medium that the planetary ball mill uses is 6~10mm for diameter, the medium and the crystallite are fine
Tieing up plain, amylomaize mass ratio can be 2~10:1 and 2~6:1 respectively, and filling rate can be 25~75%.
The ultramicro grinding time can be 1~8h；
The granularity of the microcrystalline cellulose and amylomaize after the ultramicro grinding can be respectively 10~30 μ
M and 5~15 μm.
The blended liquid needs to handle by high speed shear before high-pressure homogeneous processing, shearing rotating speed can for 6000~
10000r/min, time can be 5~15min, concretely shear 10min under 8000r/min revolving speed；
The pressure of the high-pressure homogeneous processing can be 40~80MPa,
The high-pressure homogeneous processing cycle carries out repeatedly, and concretely 2~5 times；
Concretely circulation carries out 3 times under 60MPa pressure.
Mixture quality, the distilled water of the mixture of microcrystalline cellulose and amylomaize and sodium hydroxide and urea
Ratio successively can be 2~4:16~19:81, concretely 4:19:81；
The mass ratio of sodium hydroxide and urea can in the mixture of the sodium hydroxide and urea are as follows: 4~7:12 specifically may be used
For 7:12；
The amylomaize accounts for the 5% of the quality of the mixture of the microcrystalline cellulose and amylomaize
~25%.
The mass ratio of the amylomaize and microcrystalline cellulose can are as follows: 1:3~19, concretely 1:3-9,1:4-
9,3:17-27,1:3,1:4,3:17,1:9,1:19.
In above method step 3), the temperature of the freezing can be -10~-30 DEG C, and the time can be 15~30min, specifically
It can are as follows: 15min is freezed under conditions of -20 DEG C.
It further include that the wet gel is placed in in -20 DEG C of refrigerators the operation freezed for 24 hours before being replaced.
In above method step 4), the hydrochloric acid can be the hydrochloric acid of volumetric concentration 1%~6% (concretely 5%).
The operation replaced using hydrochloric acid are as follows: the wet gel is washed using hydrochloric acid, it is described wash into
Row is multiple, concretely 3~5 times, preferably 5 times；
The mass ratio of wet gel and hydrochloric acid can be 1:1；
The operation replaced using water are as follows: wash the gel after hydrochloric acid is replaced using distilled water, institute
It states washing and carries out repeatedly concretely 3~5 times, preferably 5 times.
The pH value range of the white hydrogel is 6.5~7.5.
In above method step 5), the operation of the vacuum freeze drying processing are as follows: the white hydrogel is poured into training
It supports and carries out vacuum freeze drying processing in ware, wherein amount of the white hydrogel in culture dish are as follows: diameter is the training of 9cm
It supports and shifts hydrogel described in 90~95mL in ware.
The condition of the vacuum freeze drying are as follows:
Temperature can be -60~-30 DEG C, concretely -30 DEG C；
Vacuum degree can be 10~15Pa, concretely 12Pa；
Drying time can be 40~60h, concretely 48h.
The starch blending cellulose aerogels that the above method is prepared also belong to protection scope of the present invention.
Above-mentioned starch blending cellulose aerogels also belong to this as application of the adsorbent material in absorbing organic solvent, oil
The protection scope of invention.
Above-mentioned starch blending cellulose aerogels apply also for sewage treatment, organic solvent, oil in absorption effluent etc..
It is described oil concretely: pump oil, linseed oil.
Starch blending cellulose aerogels prepared by the present invention have certain oil absorption, such as in pump oil and linseed oil
Middle immersion reaches oil suction saturation for 24 hours, and absorption multiplying power is respectively 8.86~10.63 (g/g) and 9.13~11.44 (g/g).Oil suction
Starch blending cellulose aerogels afterwards oil can be discharged to achieve the purpose that reuse by way of being centrifuged or squeezing.
The test for carrying out dynamic characteristics to starch blending cellulose aerogels prepared by the present invention shows that starch can be shown
Write the creep resistance and Dynamic viscoelasticity of fiber reinforced for improving cellulose base aeroge.Have very for the exploitation of cellulose base aeroge
Good application prospect.
Aeroge of the present invention has totally biodegradable characteristic using degradable substances such as starch and celluloses.Pass through
Addition starch can not only improve the performance of the aeroge, can also reduce preparation cost.With good economic value and ring
It supports value value, be worth further investigation and promote.
The invention has the following beneficial effects:
1. preparing aeroge by starch and cellulose blending, the aeroge of high porosity high-specific surface area low-density is obtained
It can be applied to sewage treatment link.
2. there is tridimensional network by the starch blending cellulose aerogels that vacuum freeze drying obtains, suction can be used as
Attached dose, organic solvent, oil etc. are absorbed extensively, and can achieve the purpose that recycling by simple physics mode.
3. economic cost can be lowered by adding starch in cellulose aerogels, popularization and use tool to the aeroge
There is social economic value.
4. starch blending cellulose aerogels have oleophilic drainage characteristic, organic solvent, the oil etc. in water can be effectively absorbed,
It is pollution-free to water body, therefore there is great application potential.
The present invention utilizes the strongly hydrophilic of starch, realizes that copolymerization is anti-with cellulose whiskers after miniaturization and aging process
It answers, improves the performance of cellulose base aeroge, makes full use of cheap raw material, simplify preparation process flow, to improve composite material
Comprehensive performance provides source abundant.
Starch blending cellulose aerogels of the invention are compared with general fibre element base aeroge, the small, hole with density
The advantages that rate is high, cubical contraction is small, oil absorbency is good and Dynamic Viscoelastic performance is good.Currently, domestic there is not yet addition starch
Improve the report of cellulose base aeroge.
Detailed description of the invention
Fig. 1 is creep-recovery curve of the starch blending cellulose of 1-5 of embodiment of the present invention preparation.
Fig. 2 is the storage modulus (A) of the different content starch blending cellulose of 1-5 of embodiment of the present invention preparation, loss mould
(B) and tan δ (C) are measured with frequency variation curve.
Fig. 3 is the storage modulus (A) and loss mould of the different content starch blending cellulose of 1-5 of embodiment of the present invention preparation
Amount (B) varies with temperature curve.
Specific embodiment
The present invention will be described below by way of specific embodiments, but the present invention is not limited thereto.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material etc., are commercially available unless otherwise specified.
Amylomaize as used in the following examples is purchased from: Shanghai food raw material firm, trade name Gao Zhi
Chain cornstarch.
Microcrystalline cellulose as used in the following examples is purchased from: Sigma-Aldrich company, trade name
microcrystalline。
A method of using starch blending cellulose aerogels, cellulose aerogels are modified using starch, it is auxiliary
It helps and starch blending cellulose aerogels is made with high-pressure homogeneous blending and vacuum freeze drying.
The specific preparation methods of starch blending cellulose aerogels the following steps are included:
Specific embodiment 1: a kind of preparation method and performance characterization of starch blending cellulose aerogels
One, the preparation of starch blending cellulose aerogels
1, starch blending cellulose wet gel system
(1) blend solution of microcrystalline cellulose, amylomaize and water is prepared
It accurately weighs 4g (being accurate to 0.0001g) microcrystalline cellulose and amylomaize is added in beaker, crystallite is fine
The mass ratio of dimension element and amylomaize is 19:1.It measures 81mL distilled water and microcrystalline cellulose and high straight-chain maize shallow lake is added
In the mixture of powder, the suspension of 0.049g/mL is formed.Not add amylomaize sample as blank control.It will
Suspension high speed shear 10min under conditions of 8000r/min.
(2) high-pressure homogeneous processing
By the microcrystalline cellulose of shearing refinement and starch mixed solution, high-pressure homogeneous acquisition three times is equal under conditions of 60MPa
Even white emulsion.
(3) wet gel is formed
The emulsion obtained after will be high-pressure homogeneous takes out defrosting after freezing 15min under conditions of -20 DEG C, accurately weighs 7g
(being accurate to 0.0001g) sodium hydroxide and 12g (being accurate to 0.0001g) urea are added in the emulsion of low temperature, with 400r/min
Revolving speed stir to emulsion transparent wet gel state be presented.Wet gel is placed in -20 DEG C of refrigerators and is freezed for 24 hours.
(4) wet gel is neutralized
Wet gel after taking out freezing, is vigorously stirred 30min at room temperature.The wet gel 5%HCl that will be obtained
(wet gel and HCl mass ratio wash 5 times for 1:1), then are washed with distilled water 5 times, change once every 6h, until pH is in
Property, it is to be advisable between 6.5~7.5 with pH meter registration.
2, prepared by starch blending cellulose aerogels
Obtained wet gel is transferred in the culture dish that diameter is 9cm, is placed in freeze-drying in vacuum freeze drier
48h.Wherein the condenser temperature of vacuum freeze drying is -30 DEG C, pressure 12Pa.
Two, the measurement of oil absorption
Oil absorbency test is carried out to above-mentioned starch blending cellulose aerogels.It is carried out using linseed oil and pumping fluid
Absorption test, utilizes its oil absorbency of gravimetric detemination.Aeroge is cut into and is similar to 1 × 1 × 1 (cm3) square, claim
12h dipped in oil, which reaches, after weight weighs after adsorption saturation state is moved back to 1min on rack and calculates absorption multiplying power.Calculate absorption
Multiplying power formula (1) is as follows:
Wherein W is the quality of aeroge after absorption, W0For aeroge original quality, C is absorption multiplying power.
In triplicate, results are averaged for every group of test.Starch blending cellulose aerogels are to linseed in the present embodiment
The absorption multiplying power of oil and pumping fluid is respectively (9.05 ± 0.27) g/g (mean+SD) and (9.13 ± 0.24) g/g
(mean+SD).
Three, creep performance test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), creep-recovery test is carried out.Aeroge is cut into 1cm3Cube.Test setting pretightning force (0.01N), 30
DEG C balance 2min, apply the stress of 0.0001MPa and maintain 10min, cancel stress, make sample restore 10min.Pass through omnipotent point
Software is analysed, the creep-recovery curve for obtaining sample is as shown in Figure 1.
Creep curve is described using Burgers model.Burgers model is calculated as shown in formula (2).
ε (t) represents the creep strain of aeroge sample；σ0Represent on-load pressure, 0.0001MPa；EMAnd ηMRespectively represent wheat
The viscosity of the elasticity modulus of Ke Siwei spring and Maxwell's damping；EKAnd ηKRespectively represent Kelvin's spring elasticity modulus and
The viscosity of Kelvin's damping, wherein τ=ηK/EK, lag time needed for the deformation for generation 63.2%；T is the time of load.
Test is respectively provided with to be repeated three times, and results are averaged.
Four, frequency scanning test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), test is performed a scan.Aeroge is cut into 1cm3Cube.Temperature setting is 30 DEG C.Frequency range is
0.1Hz~50Hz, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ', loss modulus G " and loss are obtained
Factor t an δ with frequency change curve.
Five, temperature scanning is tested
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), temperature scanning test is carried out.Aeroge is cut into 1cm3Cube.Set of frequency is 1Hz.Temperature range is
30-100 DEG C, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ' and loss modulus G " are obtained with temperature
Change curve.
Specific embodiment 2: a kind of preparation method and performance characterization of starch blending cellulose aerogels
One, the preparation of starch blending cellulose aerogels
1, starch blending cellulose wet gel system
(1) blend solution of microcrystalline cellulose, amylomaize and water is prepared
It accurately weighs 4g (being accurate to 0.0001g) microcrystalline cellulose and amylomaize is added in beaker, crystallite is fine
The mass ratio of dimension element and amylomaize is 9:1.It measures 81mL distilled water and microcrystalline cellulose and high straight-chain maize shallow lake is added
In the mixture of powder, the suspension of 0.049g/mL is formed.Not add amylomaize sample as blank control.It will
Suspension high speed shear 10min under conditions of 8000r/min.
(2) high-pressure homogeneous processing
By the microcrystalline cellulose of shearing refinement and starch mixed solution, high-pressure homogeneous acquisition three times is equal under conditions of 60MPa
Even white emulsion.
(3) wet gel is formed
The emulsion obtained after will be high-pressure homogeneous takes out defrosting after freezing 15min under conditions of -20 DEG C, accurately weighs 7g
(being accurate to 0.0001g) sodium hydroxide and 12g (being accurate to 0.0001g) urea are added in the emulsion of low temperature, with 400r/min
Revolving speed stir to emulsion transparent wet gel state be presented.Wet gel is placed in -20 DEG C of refrigerators and is freezed for 24 hours.
(4) wet gel is neutralized
Wet gel after taking out freezing, is vigorously stirred 30min at room temperature.The wet gel 5%HCl that will be obtained
(wet gel and HCl mass ratio wash 5 times for 1:1), then are washed with distilled water 5 times, change once every 6h, until pH is in
Property, it is to be advisable between 6.5~7.5 with pH meter registration.
2, prepared by starch blending cellulose aerogels
Obtained wet gel is transferred in the culture dish that diameter is 9cm, is placed in freeze-drying in vacuum freeze drier
48h. wherein vacuum freeze drying condenser temperature be -30 DEG C, pressure 12Pa.
Two, the measurement of oil absorption
Oil absorbency test is carried out to above-mentioned starch blending cellulose aerogels.It is carried out using linseed oil and pumping fluid
Absorption test, utilizes its oil absorbency of gravimetric detemination.Aeroge is cut into and is similar to 1 × 1 × 1 (cm3) square, claim
12h dipped in oil, which reaches, after weight weighs after adsorption saturation state is moved back to 1min on rack and calculates absorption multiplying power.Calculate absorption
Multiplying power formula (1) is as follows:
Wherein W is the quality of aeroge after absorption, W0For aeroge original quality, C is absorption multiplying power.
In triplicate, results are averaged for every group of test.Starch blending cellulose aerogels are to linseed in the present embodiment
The absorption multiplying power of oil and pumping fluid is respectively (9.24 ± 0.42) g/g (mean+SD) and (10.00 ± 0.64) g/g
(mean+SD).
Three, creep performance test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), creep-recovery test is carried out.Aeroge is cut into 1cm3Cube.Test setting pretightning force (0.01N), 30
DEG C balance 2min, apply the stress of 0.0001MPa and maintain 10min, cancel stress, make sample restore 10min.Pass through omnipotent point
Software is analysed, the creep-recovery curve for obtaining sample is as shown in Figure 1.
Creep curve is described using Burgers model.Burgers model is calculated as shown in formula (2).
ε (t) represents the creep strain of aeroge sample；σ0Represent on-load pressure, 0.0001MPa；EMAnd ηMRespectively represent wheat
The viscosity of the elasticity modulus of Ke Siwei spring and Maxwell's damping；EKAnd ηKRespectively represent Kelvin's spring elasticity modulus and
The viscosity of Kelvin's damping, wherein τ=ηK/EK, lag time needed for the deformation for generation 63.2%；T is the time of load.
Test is respectively provided with to be repeated three times, and results are averaged.
Four, frequency scanning test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), test is performed a scan.Aeroge is cut into 1cm3Cube.Temperature setting is 30 DEG C.Frequency range is
0.1Hz~50Hz, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ', loss modulus G " and loss are obtained
Factor t an δ with frequency change curve.
Five, temperature scanning is tested
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), temperature scanning test is carried out.Aeroge is cut into 1cm3Cube.Set of frequency is 1Hz.Temperature range is
30-100 DEG C, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ' and loss modulus G " are obtained with temperature
Change curve.
Specific embodiment 3: a kind of preparation method and performance characterization of starch blending cellulose aerogels
One, the preparation of starch blending cellulose aerogels
1, starch blending cellulose wet gel system
(1) blend solution of microcrystalline cellulose, amylomaize and water is prepared
It accurately weighs 4g (being accurate to 0.0001g) microcrystalline cellulose and amylomaize is added in beaker, crystallite is fine
The mass ratio of dimension element and amylomaize is 17:3.It measures 81mL distilled water and microcrystalline cellulose and high straight-chain maize shallow lake is added
In the mixture of powder, the suspension of 0.049g/mL is formed.Not add amylomaize sample as blank control.It will
Suspension high speed shear 10min under conditions of 8000r/min.
(2) high-pressure homogeneous processing
By the microcrystalline cellulose of shearing refinement and starch mixed solution, high-pressure homogeneous acquisition three times is equal under conditions of 60MPa
Even white emulsion.
(3) wet gel is formed
The emulsion obtained after will be high-pressure homogeneous takes out defrosting after freezing 15min under conditions of -20 DEG C, accurately weighs 7g
(being accurate to 0.0001g) sodium hydroxide and 12g (being accurate to 0.0001g) urea are added in the emulsion of low temperature, with 400r/min
Revolving speed stir to emulsion transparent wet gel state be presented.Wet gel is placed in -20 DEG C of refrigerators and is freezed for 24 hours.
(4) wet gel is neutralized
Wet gel after taking out freezing, is vigorously stirred 30min at room temperature.The wet gel 5%HCl that will be obtained
(wet gel and HCl mass ratio wash 5 times for 1:1), then are washed with distilled water 5 times, change once every 6h, until pH is in
Property, it is to be advisable between 6.5~7.5 with pH meter registration.
2, prepared by starch blending cellulose aerogels
Obtained wet gel is transferred in the culture dish that diameter is 9cm, is placed in freeze-drying in vacuum freeze drier
48h. wherein vacuum freeze drying condenser temperature be -30 DEG C, pressure 12Pa.
Two, the measurement of oil absorption
Oil absorbency test is carried out to above-mentioned starch blending cellulose aerogels.It is carried out using linseed oil and pumping fluid
Absorption test, utilizes its oil absorbency of gravimetric detemination.Aeroge is cut into and is similar to 1 × 1 × 1 (cm3) square, claim
12h dipped in oil, which reaches, after weight weighs after adsorption saturation state is moved back to 1min on rack and calculates absorption multiplying power.Calculate absorption
Multiplying power formula (1) is as follows:
Wherein W is the quality of aeroge after absorption, W0For aeroge original quality, C is absorption multiplying power.
In triplicate, results are averaged for every group of test.Starch blending cellulose aerogels are to linseed in the present embodiment
The absorption multiplying power of oil and pumping fluid is respectively (10.63 ± 0.43) g/g (mean+SD) and (11.44 ± 0.36) g/
G (mean+SD).
Three, creep performance test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), creep-recovery test is carried out.Aeroge is cut into 1cm3Cube.Test setting pretightning force (0.01N), 30
DEG C balance 2min, apply the stress of 0.0001MPa and maintain 10min, cancel stress, make sample restore 10min.Pass through omnipotent point
Software is analysed, the creep-recovery curve for obtaining sample is as shown in Figure 1.
Creep curve is described using Burgers model.Burgers model is calculated as shown in formula (2).
ε (t) represents the creep strain of aeroge sample；σ0Represent on-load pressure, 0.0001MPa；EMAnd ηMRespectively represent wheat
The viscosity of the elasticity modulus of Ke Siwei spring and Maxwell's damping；EKAnd ηKRespectively represent Kelvin's spring elasticity modulus and
The viscosity of Kelvin's damping, wherein τ=ηK/EK, lag time needed for the deformation for generation 63.2%；T is the time of load.
Test is respectively provided with to be repeated three times, and results are averaged.
Four, frequency scanning test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), test is performed a scan.Aeroge is cut into 1cm3Cube.Temperature setting is 30 DEG C.Frequency range is
0.1Hz~50Hz, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ', loss modulus G " and loss are obtained
Factor t an δ with frequency change curve.
Five, temperature scanning is tested
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), temperature scanning test is carried out.Aeroge is cut into 1cm3Cube.Set of frequency is 1Hz.Temperature range is
30-100 DEG C, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ' and loss modulus G " are obtained with temperature
Change curve.
Specific embodiment 4: a kind of preparation method and performance characterization of starch blending cellulose aerogels
One, the preparation of starch blending cellulose aerogels
1, starch blending cellulose wet gel system
(1) blend solution of microcrystalline cellulose, amylomaize and water is prepared
It accurately weighs 4g (being accurate to 0.0001g) microcrystalline cellulose and amylomaize is added in beaker, crystallite is fine
The mass ratio of dimension element and amylomaize is 4:1.It measures 81mL distilled water and microcrystalline cellulose and high straight-chain maize shallow lake is added
In the mixture of powder, the suspension of 0.049g/mL is formed.Not add amylomaize sample as blank control.It will
Suspension high speed shear 10min under conditions of 8000r/min.
(2) high-pressure homogeneous processing
By the microcrystalline cellulose of shearing refinement and starch mixed solution, high-pressure homogeneous acquisition three times is equal under conditions of 60MPa
Even white emulsion.
(3) wet gel is formed
The emulsion obtained after will be high-pressure homogeneous takes out defrosting after freezing 15min under conditions of -20 DEG C, accurately weighs 7g
(being accurate to 0.0001g) sodium hydroxide and 12g (being accurate to 0.0001g) urea are added in the emulsion of low temperature, with 400r/min
Revolving speed stir to emulsion transparent wet gel state be presented.Wet gel is placed in -20 DEG C of refrigerators and is freezed for 24 hours.
(4) wet gel is neutralized
Wet gel after taking out freezing, is vigorously stirred 30min at room temperature.The wet gel 5%HCl that will be obtained
(wet gel and HCl mass ratio wash 5 times for 1:1), then are washed with distilled water 5 times, change once every 6h, until pH is in
Property, it is to be advisable between 6.5~7.5 with pH meter registration.
2, prepared by starch blending cellulose aerogels
Obtained wet gel is transferred in the culture dish that diameter is 9cm, is placed in freeze-drying in vacuum freeze drier
48h.Wherein the condenser temperature of vacuum freeze drying is -30 DEG C, pressure 12Pa.
Two, the measurement of oil absorption
Oil absorbency test is carried out to above-mentioned starch blending cellulose aerogels.It is carried out using linseed oil and pumping fluid
Absorption test, utilizes its oil absorbency of gravimetric detemination.Aeroge is cut into and is similar to 1 × 1 × 1 (cm3) square, claim
12h dipped in oil, which reaches, after weight weighs after adsorption saturation state is moved back to 1min on rack and calculates absorption multiplying power.Calculate absorption
Multiplying power formula (1) is as follows:
Wherein W is the quality of aeroge after absorption, W0For aeroge original quality, C is absorption multiplying power.
In triplicate, results are averaged for every group of test.Starch blending cellulose aerogels are to linseed in the present embodiment
The absorption multiplying power of oil and pumping fluid is respectively (9.94 ± 0.45) g/g (mean+SD) and (10.55 ± 0.54) g/g
(mean+SD).
Three, creep performance test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), creep-recovery test is carried out.Aeroge is cut into 1cm3Cube.Test setting pretightning force (0.01N), 30
DEG C balance 2min, apply the stress of 0.0001MPa and maintain 10min, cancel stress, make sample restore 10min.Pass through omnipotent point
Software is analysed, the creep-recovery curve for obtaining sample is as shown in Figure 1.
Creep curve is described using Burgers model.Burgers model is calculated as shown in formula (2).
ε (t) represents the creep strain of aeroge sample；σ0Represent on-load pressure, 0.0001MPa；EMAnd ηMRespectively represent wheat
The viscosity of the elasticity modulus of Ke Siwei spring and Maxwell's damping；EKAnd ηKRespectively represent Kelvin's spring elasticity modulus and
The viscosity of Kelvin's damping, wherein τ=ηK/EK, lag time needed for the deformation for generation 63.2%；T is the time of load.
Test is respectively provided with to be repeated three times, and results are averaged.
Four, frequency scanning test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), test is performed a scan.Aeroge is cut into 1cm3Cube.Temperature setting is 30 DEG C.Frequency range is
0.1Hz~50Hz, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ', loss modulus G " and loss are obtained
Factor t an δ with frequency change curve.
Five, temperature scanning is tested
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), temperature scanning test is carried out.Aeroge is cut into 1cm3Cube.Set of frequency is 1Hz.Temperature range is
30-100 DEG C, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ' and loss modulus G " are obtained with temperature
Change curve.
Specific embodiment 5: a kind of preparation method and performance characterization of starch blending cellulose aerogels
One, the preparation of starch blending cellulose aerogels
1, starch blending cellulose wet gel system
(1) blend solution of microcrystalline cellulose, amylomaize and water is prepared
It accurately weighs 4g (being accurate to 0.0001g) microcrystalline cellulose and amylomaize is added in beaker, crystallite is fine
The mass ratio of dimension element and amylomaize is 3:1.It measures 81mL distilled water and microcrystalline cellulose and high straight-chain maize shallow lake is added
In the mixture of powder, the suspension of 0.049g/mL is formed.Not add amylomaize sample as blank control.It will
Suspension high speed shear 10min under conditions of 8000r/min.
(2) high-pressure homogeneous processing
By the microcrystalline cellulose of shearing refinement and starch mixed solution, high-pressure homogeneous acquisition three times is equal under conditions of 60MPa
Even white emulsion.
(3) wet gel is formed
The emulsion obtained after will be high-pressure homogeneous takes out defrosting after freezing 15min under conditions of -20 DEG C, accurately weighs 7g
(being accurate to 0.0001g) sodium hydroxide and 12g (being accurate to 0.0001g) urea are added in the emulsion of low temperature, with 400r/min
Revolving speed stir to emulsion transparent wet gel state be presented.Wet gel is placed in -20 DEG C of refrigerators and is freezed for 24 hours.
(4) wet gel is neutralized
Wet gel after taking out freezing, is vigorously stirred 30min at room temperature.The wet gel 5%HCl that will be obtained
(wet gel and HCl mass ratio wash 5 times for 1:1), then are washed with distilled water 5 times, change once every 6h, until pH is in
Property, it is to be advisable between 6.5~7.5 with pH meter registration.
2, prepared by starch blending cellulose aerogels
Obtained wet gel is transferred in the culture dish that diameter is 9cm, is placed in freeze-drying in vacuum freeze drier
48h. wherein vacuum freeze drying condenser temperature be -30 DEG C, pressure 12Pa.
Two, the measurement of oil absorption
Oil absorbency test is carried out to above-mentioned starch blending cellulose aerogels.It is carried out using linseed oil and pumping fluid
Absorption test, utilizes its oil absorbency of gravimetric detemination.Aeroge is cut into and is similar to 1 × 1 × 1 (cm3) square, claim
12h dipped in oil, which reaches, after weight weighs after adsorption saturation state is moved back to 1min on rack and calculates absorption multiplying power.Calculate absorption
Multiplying power formula (1) is as follows:
Wherein W is the quality of aeroge after absorption, W0For aeroge original quality, C is absorption multiplying power.
In triplicate, results are averaged for every group of test.Starch blending cellulose aerogels are to linseed in the present embodiment
The absorption multiplying power of oil and pumping fluid is respectively (8.86 ± 0.28) g/g (mean+SD) and (9.47 ± 0.46) g/g
(mean+SD).
Three, creep performance test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), creep-recovery test is carried out.Aeroge is cut into 1cm3Cube.Test setting pretightning force (0.01N), 30
DEG C balance 2min, apply the stress of 0.0001MPa and maintain 10min, cancel stress, make sample restore 10min.Pass through omnipotent point
Software is analysed, the creep-recovery curve for obtaining sample is as shown in Figure 1.
Creep curve is described using Burgers model.Burgers model is calculated as shown in formula (2).
ε (t) represents the creep strain of aeroge sample；σ0Represent on-load pressure, 0.0001MPa；EMAnd ηMRespectively represent wheat
The viscosity of the elasticity modulus of Ke Siwei spring and Maxwell's damping；EKAnd ηKRespectively represent Kelvin's spring elasticity modulus and
The viscosity of Kelvin's damping, wherein τ=ηK/EK, lag time needed for the deformation for generation 63.2%；T is the time of load.
Test is respectively provided with to be repeated three times, and results are averaged.
Four, frequency scanning test
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), test is performed a scan.Aeroge is cut into 1cm3Cube.Temperature setting is 30 DEG C.Frequency range is
0.1Hz~50Hz, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ', loss modulus G " and loss are obtained
Factor t an δ with frequency change curve.
Five, temperature scanning is tested
By aeroge sample be placed in Dynamic Mechanical Analyzer (DMA, Q800, TA Instruments, New Castle, DE,
USA on), temperature scanning test is carried out.Aeroge is cut into 1cm3Cube.Set of frequency is 1Hz.Temperature range is
30-100 DEG C, controlled strain 0.15%.By omnipotent analysis software, storage modulus G ' and loss modulus G " are obtained with temperature
Change curve.
The oil absorbency analysis of the starch blending cellulose aerogels of embodiment 1-5 preparation
The absorption multiplying power of 1 starch blending cellulose aerogels of table
Note: numerical value is the mean+SD of 3 measurements in table.WithLSD method carries out Multiple range test, and same column indicates difference
Lowercase indicates that group difference is significant (p < 0.05).
As shown in Table 1, gained aeroge is 7.97~10.63 to the absorptivity range of pumping fluid, the absorption of linseed oil
Rate range is 8.98~11.44.Compared with being not added with starch aeroge, the adsorption rate of the aeroge after adding starch is significantly mentioned
It is high.When content of starch is 15%, aeroge reaches maximum to the absorptivity of pump oil and linseed oil.
Creep performance analysis (the S of the starch blending cellulose aerogels of embodiment 1-5 preparation0CA,S5CA,S10CA,
S15CA,S20CA,S25CA respectively represents 0%, 5%, 10%, 15%, 20% and 25% content of starch):
Fig. 1 and table 2 be respectively in starch blending cellulose aerogels creep performance test creep-recovery curve and
Burgers model parameter.
The strain curve of sample aeroge has typical creeping characteristic as can be seen from Figure 1, and passage at any time is presented
Similar trend out.Deformation of creep curve can be divided into three phases: first stage is that aeroge strain is fast in a short time
Speed increases；Second stage is delayed deformation and strain being slowly increased at any time of aeroge；Last stage is removal external force
Strain Restoration stage afterwards.It plays initial strain to steeply rise, then slowly rise again.In Restoration stage, the reverse be true.Starch
When content is no more than 20%, creep strain curve is significantly lower than S0CA illustrates that starch is distributed well in cellulose base aeroge,
The addition of starch enhances its creep-resistant property.S10The creep strain of CA is minimum, illustrates that the creep resistance of aeroge at this time is maximum.
When starch additive amount is more than 20%, creep strain curve is apparently higher than other aeroges.This may be due to excessive starch
Caused by cannot being evenly distributed in cellulose base aeroge.
Four parameter value (E obtained in the Burgers modelM,EK, τ and ηM) and coefficient of determination R2As shown in table 2.It can be with
Find out, the coefficient of determination (R of each parameter2) it is all larger than 0.989, illustrate that 4 yuan of Burgers models can preferably characterize aeroge
Creep behaviour.EMIt is a kind of transient creep deformation, can be recovered immediately when removing external force.Numerical value is bigger, and the elasticity of material is got over
It is good.The E from table it can also be seen that when content of starch increases to 15% from 0MValue increases, and content of starch is 20% to 25%
Between when EMValue reduces, and illustrates that excessive starch can destroy the viscosity of cellulose base aeroge.When content of starch reaches 15%, gas
Gel elastomer is best.EKIt represents delayed elasticity modulus and τ is lag time needed for the deformation of generation 63.2%, be worth bigger, material
Expect more viscous.When content of starch reaches 15%, EKIt is relatively high with the value of τ.ηMRepresent the viscosity of Maxwell's damping.S15CA reaches
To maximum ηMValue is 1.777 ± 0.359MPas-1, it means that S15CA has least reversible deformation quantity and better viscoelastic
Property.However once it is added beyond 15% content of starch, ηMValue significantly reduce, even lower than S0CA.By upper table analysis it is found that
High amylose starches, which is added, can be improved the viscoplasticity and croop property of cellulose base aeroge.The starch that content of starch is 15% is total
Combined filament element aeroge has best viscoplasticity.When additive amount is lower than this value, the machine of starch blending cellulose aerogels
Tool performance obtains different degrees of raising.
Burgers model parameter in 2 starch blending cellulose aerogels creep performance test of table
Note: numerical value is the mean+SD of 3 measurements in table.WithLSD method carries out Multiple range test, and same column indicates difference
Lowercase indicates that group difference is significant (p < 0.05).
The frequency scanning of the starch blending cellulose aerogels of embodiment 1-5 preparation analyzes (S0CA,S5CA,S10CA,
S15CA,S20CA,S25CA respectively represents 0%, 5%, 10%, 15%, 20% and 25% content of starch):
Fig. 2 is that storage modulus (A), loss modulus (B) and the tan δ (C) of different content starch blending cellulose become with frequency
Change curve.
It can be observed from fig. 2 that storage modulus G ', loss modulus G " and fissipation factor tan δ increase with the increase of frequency
Add.In entire frequency range, G ' value is much larger than G " value, illustrates the elastic property of the material better than adhering performance.Work as addition
10% starch, G ', G " and tan δ have reached maximum value, this shows that adding appropriate amount of starch can be improved cellulose base airsetting
The mechanical property of glue.In entire frequency range, when content of starch value is respectively 20% and 25%, G ' and G " are minimum, and starch adds
Add and excessively will lead to electrostatic agglomeration, excessive starch is unevenly distributed in aeroge, influences the friendship of starch and microcrystalline cellulose
Connection.
The temperature scanning of the starch blending cellulose aerogels of embodiment 1-5 preparation analyzes (S0CA,S5CA,S10CA,
S15CA,S20CA,S25CA respectively represents 0%, 5%, 10%, 15%, 20% and 25% content of starch):
Fig. 3 is that the storage modulus (A) of different content starch blending cellulose and loss modulus (B) vary with temperature curve.
From figure 3, it can be seen that as the temperature rises, G ' value reduces after formerly increasing.May be due to aeroge compared with
Porosity is higher under low temperature, and aeroge is caused to be dehydrated, and storage modulu increases.Aeroge starts to adsorb the water in air after heating
Point, become soft, storage modulu reduces.When content of starch is respectively 10% and 15%, storage modulu is greater than not starch-containing
Aeroge, illustrate to be added suitable starch into material with better stiffness characteristics.When content of starch is 20% and 25%,
Storage modulus is minimum, illustrates that aeroge rigidity is minimum at this time.
Claims (10)
1. a kind of starch blending cellulose aerogels are made of microcrystalline cellulose, amylomaize of raw material.
2. the method for preparing starch blending cellulose aerogels described in claim 1, comprising: 1) prepare microcrystalline cellulose, height
The blend solution of straight chain corn starch and water；
2) above-mentioned blend solution is subjected to high-pressure homogeneous processing, obtains homogenizing fluid；
3) it will be taken out after the freezing of above-mentioned homogenizing fluid, thaw and stir, sodium hydroxide and urea is added, obtain wet gel；
4) wet gel is successively replaced using hydrochloric acid, water, obtains white hydrogel；
5) above-mentioned white hydrogel is subjected to vacuum freeze drying processing, obtains aeroge.
3. according to the method described in claim 1, it is characterized by: in step 1), the microcrystalline cellulose and high straight-chain maize
Starch passes through ultramicro crushing treatment before blending；
The granularity of the microcrystalline cellulose and amylomaize after the ultramicro grinding is respectively 10~30 μm and 5~
15μm。
4. method according to claim 1 or 2, it is characterised in that: the blended liquid is high-pressure homogeneous preceding by cutting at a high speed
Processing is cut, the revolving speed of the shearing is 6000~10000r/min, and the time is 5~15min；
The high-pressure homogeneous pressure is 40~80MPa,
The high-pressure homogeneous circulation carries out multiple.
5. method according to any of claims 1-4, it is characterised in that: microcrystalline cellulose and amylomaize
Mixture and sodium hydroxide and the mixture quality of urea and the ratio of distilled water be followed successively by 2~4:16~19:81；
The mass ratio of sodium hydroxide and urea in the mixture of the sodium hydroxide and urea are as follows: 4~7:12；
The amylomaize account for the quality of the mixture of the microcrystalline cellulose and amylomaize 5%~
25%；
The mass ratio of the amylomaize and microcrystalline cellulose are as follows: 1:3~19.
6. method according to any one of claims 1-5, it is characterised in that: in step 3), the temperature of the freezing is-
10~-30 DEG C, the time is 15~30min.
7. method according to claim 1 to 6, it is characterised in that: in step 5), the vacuum freeze drying
Condition are as follows:
Temperature is -60~-30 DEG C；
Vacuum degree is 10~15Pa；
Drying time is 40~60h.
8. the starch blending cellulose aerogels that any one of claim 2-7 the method is prepared.
9. starch blending cellulose aerogels described in claim 1 or 8 are as adsorbent material in absorbing organic solvent, oil
Using.
10. application of the starch blending cellulose aerogels in sewage treatment described in claim 1 or 8.
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