CN110258158A - A kind of method of high-speed water jet preparation sisal hemp nano-cellulose - Google Patents
A kind of method of high-speed water jet preparation sisal hemp nano-cellulose Download PDFInfo
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- CN110258158A CN110258158A CN201910541325.3A CN201910541325A CN110258158A CN 110258158 A CN110258158 A CN 110258158A CN 201910541325 A CN201910541325 A CN 201910541325A CN 110258158 A CN110258158 A CN 110258158A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
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Abstract
The present invention provides a kind of methods of high-speed water jet preparation sisal hemp nano-cellulose, comprising: sisal hemp pretreatment;Prepare chloro fourth ethylmethylimidazolium ion solution;Sisal cellulose is added into chloro fourth ethylmethylimidazolium ion solution, uniform stirring, it is completely spare after clarification;It refines to obtain homogeneous phase solution by high-speed water jet;Boiling water will be added in homogeneous phase solution, obtain suspension after stirring;Suspension is placed in centrifuge separation, abandons supernatant, deionized water is added and washes away remaining chloro fourth ethylmethylimidazolium ion solution, obtains regenerated cellulose;Regenerated cellulose is lyophilized, nano-cellulose is obtained.The present invention is dissolved sisal cellulose using solion, there is no destruction to sisal fiber, then it is refined by high-speed water jet and carries out fiber nanosizing, not only shorten process time, and fiber diameter is uniform, it can satisfy nanoscale requirement, preparation method is simple, can be realized the purpose of nano-cellulose continuous production.
Description
Technical field
The invention belongs to cellulose processing technique field, in particular to a kind of high-speed water jet prepares sisal hemp nano-cellulose
Method.
Background technique
Plant fiber is mainly made of lumber fibre, grass fiber, three kinds of bast fiber.Sisal hemp is to belong to bast fiber one
Class has many advantages, such as that production period is short, investment is less, harvest time is long.The sisal hemp planting scale of China and export volume sustainable growth.Mesh
The plantation of preceding country sisal hemp is concentrated mainly on the ground such as Guangdong, Guangxi, Hainan, and according to statistics, China's sisal hemp cultivated area is about 1.5 ten thousand
Hectare, can produce 3.7 ten thousand tons of fiber per year.As world today's dosage maximum, a kind of hard fibre widest in area, sisal fiber tool
There is tough and hard wear resistant, high resilience, quality is hard and soft, it is not easy to go mouldy, brittle failure, hardening, corrosion-resistant, antistatic, the characteristics such as pulling force is big, because
This sisal fiber has a wide range of applications in fields such as fishery, industrial and mineral, navigation, transport and oil fields.
Nano-cellulose is the minimal physical structural unit of super-micro-fine fibres of the diameter less than 100nm and cellulose.With
Non-nanofiber element is compared, and nano-cellulose not only has the property of general fibre element, also there is many good characteristics.It is such as huge
Specific surface area, high-purity, high-crystallinity, high intensity, high-hydrophilic, high Young's modulus, hyperfine structure, good thixotropy
With polymolecularity etc., it is made to have huge answer in fields such as building, papermaking, cosmetics, food, automobile, electronic product, medicine
Use prospect.
The method for preparing nano-cellulose has very much, mainly including physical method, chemical method and 3 kinds of bioanalysis.Wherein, physics
Material is mainly directly ground to Nano grade by the effect of power using such as ball mill, pulverizer mechanical equipment by method, but
These are haveed the shortcomings that a lot using the method for physical mechanical equipment, not only have very violent destruction to fiber, but also drop
Solution is serious, will have a direct impact on the physical property and intensity of nano-cellulose fiber, in addition, this physical method time is long, energy consumption
Greatly, the particle size range obtained is very big, and only a small number of can reach Nano grade, in addition, the prior art there are also some uses about
The device of liquid refining, this device mainly use microjet high pressure homogenizer, and microjet high pressure homogenizer mainly passes through height
Shear action is pressed to reach refinement purpose, high-pressure homogeneous machine equipment is expensive, easily blocks, higher cost;In addition, existing chemical method
Different degrees of environmental pollution can all be caused with bioanalysis, do not have practicability, for this purpose, be badly in need of research and develop one kind can obtain it is high-quality
The method for measuring sisal hemp nano-cellulose.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides one kind can obtain of uniform size receive
Rice cellulose, and preparation method is simple, the method for easily operated high-speed water jet preparation sisal hemp nano-cellulose.
Specific technical solution of the present invention is as follows:
The present invention provides a kind of methods of high-speed water jet preparation sisal hemp nano-cellulose, and the method includes following steps
It is rapid:
S1, sisal hemp is pre-processed, and prepares sisal cellulose;
S2, chloro fourth ethylmethylimidazolium ion solution is prepared;
S3, the sisal cellulose prepared in step S1 is added to the chloro fourth ethyl first prepared into step S2
Mixed solution is obtained in base imidazol ion solution, the mixed solution is placed in uniform magnetic agitation in microwave abstracting synthesizer,
It is spare after the complete clear of the mixed solution by stirring;
S4, the mixed solution spare in step S3 is refined by high-speed water jet, is obtained for cycle refinement 1-2 time equal
Phase solution;
S5, boiling water will be added in super-voltage micro jet treated the homogeneous phase solution, and with being vigorously stirred, after stirring
Obtain the suspension that regeneration has the sisal cellulose;
S6, the suspension after stirring in step S5 is placed in high speed freezing centrifuge, and is in the range of speeds
It is centrifuged repeatedly separation under the conditions of 6000-10000r/min, controls centrifugation 10-15min every time, abandons supernatant, deionization is added
Water concussion, washes away the remaining chloro fourth ethylmethylimidazolium ion solution, repeats 3-5 times, obtains regenerated cellulose;
S7, the regenerated cellulose obtained in step S6 is placed in freeze drier 24-36h is lyophilized, be averaged
Nano-cellulose of the partial size in 60-80nm.
Further, in step S1, sisal hemp is pre-processed, and prepare sisal cellulose, specifically includes the following steps:
S101, will shred after the sisal hemp be placed in concentration be 1-3% nitric acid in, and temperature be 100-120 DEG C in
Handle 3-5h;
S102, using the sisal hemp of distilled water repeated flushing step S101, until eluent is in neutrality;
S103, by treated in the step S102 sisal hemp using the sodium hydroxide that concentration is 1-3% at 100-110 DEG C
Processing 2-4h obtains the sisal cellulose.
Further, in step S2, chloro fourth ethylmethylimidazolium ion solution is prepared, following methods are specifically included:
S201, N- methylimidazole and chloro-normal butane are blended in flask in the ratio of 5:8;
S202, by the flask as heating reflux reaction 24-36h in 110-120 DEG C of oil bath pan;
S203, the product after reaction is placed in Rotary Evaporators remove unreacted chloro-normal butane after to get to institute
State chloro fourth ethylmethylimidazolium ion solution.
Further, in step S3, the concentration for the sisal cellulose being added in the mixed solution is 3-5wt%.
Further, in step S3, the microwave power of the microwave abstracting synthesizer is 400-800W, solution temperature model
Enclose is 110-160 DEG C.
Preferably, in step S4, the pressure limit of the high-speed water jet is 5-25kpsi.
Preferably, the volume ratio of the boiling water and the homogeneous phase solution that are added in step S5 is 5:1-10:1.
Preferably, the boiling water is the distilled water boiled.
The invention has the benefit that the present invention uses chloro fourth ethylmethylimidazolium ion solution by sisal fiber first
Element dissolution, does not have destruction to sisal fiber, then carries out fiber nanosizing by the refinement of high-speed water jet equipment, not only contracts
Short process time, and fibre dimensions are uniform, uniform particle sizes, can satisfy nanoscale requirement, in process of production not only energy consumption
It is small, it is at low cost, and not will cause the waste of sisal hemp raw material, and preparation method is simple, and it is easy to operate, it can be realized nano-cellulose company
The purpose that continuous metaplasia produces.
Detailed description of the invention
Fig. 1 is the flow chart for the method that high-speed water jet described in embodiment 1 prepares sisal hemp nano-cellulose;
Fig. 2 is the particle size distribution figure for the nano-cellulose that the microjet method of the prior art in experiment one obtains;
Fig. 3 is the particle size distribution figure for the nano-cellulose that the method that embodiment 3 provides obtains;
Fig. 4 is the transmission electron microscope picture for the nano-cellulose that the microjet method of the prior art in experiment one obtains;
Fig. 5 is the transmission electron microscope picture for the nano-cellulose that the method that embodiment 3 provides obtains.
Specific embodiment
Below with reference to following embodiment, invention is further described in detail.
Embodiment 1
As shown in Figure 1, the embodiment of the present invention 1 provides a kind of method of high-speed water jet preparation sisal hemp nano-cellulose,
Method the following steps are included:
S1, sisal hemp pre-processed first, and prepares sisal cellulose, preprocessing process, which is kept in mind, to make sisal cellulose
At destruction.
S2, chloro fourth ethylmethylimidazolium ion solution is secondly prepared, the solution of preparation is to dissolve cellulose.
S3, the sisal cellulose prepared in step S1 is added the chloro fourth ethylmethylimidazolium that is prepared into step S2 from
Mixed solution is obtained in sub- solution, mixed solution is placed in uniform magnetic agitation in microwave abstracting synthesizer, to by stirring
It is spare after the complete clear of mixed solution;The present invention uses chloro fourth ethylmethylimidazolium ion solution by sisal fiber first
After element dissolution, this processing does not have destruction to sisal fiber, overcomes in the prior art using directly crushing or object
Reason equipment the methods of is milled, and has very violent destruction to fiber, is effectively reduced the economic cost of sisal fiber production, is kept away
The waste of sisal hemp raw material is exempted from.
S4, mixed solution spare in step S3 is refined by high-speed water jet, is mixed for cycle refinement 1-2 times
Liquid;Microjet method mainly by the differential pressure gradients of high pressure homogenizer, cavitation effect, shearing-crushing and hits broken effect
It combines to achieve the purpose that refinement;High-speed water jet is different from microjet, can obtain nano-cellulose of uniform size, and
And yield is higher, will not damage cellulose morning.
S5, boiling water will be added in super-voltage micro jet treated homogeneous phase solution, and with being vigorously stirred, is obtained after stirring
Regeneration has the suspension of sisal cellulose, and boiling water is simultaneously adjoint to be vigorously stirred and cellulose can be made to be precipitated.
S6, the suspension after stirring in step S5 is placed in high speed freezing centrifuge, and is 6000r/ in the range of speeds
It is centrifuged repeatedly separation under the conditions of min, controls centrifugation 10min every time, the effect of centrifugal treating mainly can be by liquid and fiber
Element separation, abandons supernatant, and deionized water concussion is added, washes away remaining chloro fourth ethylmethylimidazolium ion solution, repeats 3
It is secondary, obtain regenerated cellulose.
S7, regenerated cellulose obtained in step S6 is placed in freeze drier 24-36h is lyophilized, obtain average grain diameter
In the nano-cellulose of 60nm.
The preparation method of sisal hemp nano-cellulose provided by the invention is using chloro fourth ethylmethylimidazolium ion first
Solution dissolves sisal hemp, obtains liquid homogeneous phase solution, is then not only shortened its nanosizing using high-speed water jet thinning apparatus
Process time, and scale is uniform, can satisfy nanoscale production requirement, preparation method is simple, and it is easy to operate, it can be realized and receive
The purpose of rice cellulose continuous production, it is practical.
Embodiment 2
As shown in Figure 1, the embodiment of the present invention 2 provides a kind of method of high-speed water jet preparation sisal hemp nano-cellulose,
Method the following steps are included:
S1, sisal hemp is pre-processed, and prepares sisal cellulose, specific method includes:
S101, the sisal hemp after shredding is placed in the nitric acid that concentration is 2%, and is to handle 4h in 110 DEG C in temperature;
S102, using the sisal hemp of distilled water repeated flushing step S101, until eluent is in neutrality;S103, it will be handled in step S102
Sisal hemp afterwards obtains sisal cellulose in 105 DEG C of processing 3h using the sodium hydroxide that concentration is 2%.
S2, chloro fourth ethylmethylimidazolium ion solution is prepared, specific method includes:
S201, N- methylimidazole and chloro-normal butane are blended in flask in the ratio of 5:8;S202, by flask as
Heating reflux reaction 30h in 115 DEG C of oil bath pan;S203, it the product after reaction is placed in Rotary Evaporators removes unreacted
Chloro-normal butane after to get arrive chloro fourth ethylmethylimidazolium ion solution.
S3, the sisal cellulose prepared in step S1 is added the chloro fourth ethylmethylimidazolium that is prepared into step S2 from
Mixed solution is obtained in sub- solution, mixed solution is placed in uniform magnetic agitation in microwave abstracting synthesizer, to by stirring
It is spare after the complete clear of mixed solution;
S4, mixed solution spare in step S3 is refined by high-speed water jet, is mixed for cycle refinement 1-2 times
Liquid;
S5, boiling water will be added in super-voltage micro jet treated homogeneous phase solution, and with being vigorously stirred, is obtained after stirring
Regeneration has the suspension of sisal cellulose;
S6, the suspension after stirring in step S5 is placed in high speed freezing centrifuge, and is 8000r/ in the range of speeds
It is centrifuged repeatedly separation under the conditions of min, controls centrifugation 13min every time, abandons supernatant, deionized water concussion is added, washes away residual
Chloro fourth ethylmethylimidazolium ion solution, be repeated 4 times, obtain regenerated cellulose.
S7, regenerated cellulose obtained in step S6 is placed in freeze drier 30h is lyophilized, obtained average grain diameter and exist
The nano-cellulose of 70nm.
Above-described embodiment is on the basis of embodiment 1, it is further provided how to be pre-processed to obtain fiber to sisal hemp
Element, while providing and how preparing chloro fourth ethylmethylimidazolium ion solution, mainly prevent sisal hemp from existing sisal hemp pretreatment
It is damaged in treatment process, plays the protective effect to sisal hemp, saved sisal hemp raw material, reduce production cost.
Embodiment 3
As shown in Figure 1, the embodiment of the present invention 3 provides a kind of method of high-speed water jet preparation sisal hemp nano-cellulose,
Method the following steps are included:
S1, sisal hemp is pre-processed, and prepares sisal cellulose, specific method includes: first to be existed with the nitric acid that concentration is 3%
120 DEG C of processing sisal hemp 5h, then with distilled water repeated flushing until eluent is in neutrality, then using concentration is 3% hydroxide
Sodium is in 110 DEG C of processing 4h.
S2, prepare chloro fourth ethylmethylimidazolium ion solution, specific method include: by N- methylimidazole and chloro just
Butane is blended in flask in the ratio of 5:8, then the heating reflux reaction 36h in 110-120 DEG C of oil bath pan, then will be anti-
Product after answering is placed in Rotary Evaporators remove unreacted chloro-normal butane after to get to chloro fourth ethylmethylimidazolium from
Sub- solution.
S3, the sisal cellulose prepared in step S1 is added the chloro fourth ethylmethylimidazolium that is prepared into step S2 from
Mixed solution is obtained in sub- solution, the concentration for the sisal cellulose being added in mixed solution is 5wt%, mixed solution is placed in micro-
Wave extracts uniform magnetic agitation in synthesizer, and the microwave power of microwave abstracting synthesizer is 800W, and solution temperature range is 160
DEG C, it is spare after the complete clear of the mixed solution by stirring;
S4, mixed solution spare in step S3 is refined by high-speed water jet, the pressure model of high-speed water jet equipment
It encloses for 25kpsi, obtains homogeneous phase solution cycle refinement 2 times, high-speed water jet equipment is by Britain Constant Systems
The TS 1.1kw type high pressure cell cracker of Limited's purchase.
S5, boiling water will be added in super-voltage micro jet treated homogeneous phase solution, boiling water is the distilled water boiled, addition
The volume ratio of boiling water and homogeneous phase solution is 5:1-10:1, and with being vigorously stirred, and regeneration is obtained after stirring sisal cellulose
Suspension,;
S6, the suspension after stirring in step S5 is placed in high speed freezing centrifuge, and is 10000r/ in the range of speeds
It is centrifuged repeatedly separation under the conditions of min, controls centrifugation 15min every time, abandons supernatant, deionized water concussion is added, washes away residual
Chloro fourth ethylmethylimidazolium ion solution, be repeated 5 times, obtain regenerated cellulose.
S7, regenerated cellulose obtained in step S6 is placed in freeze drier 36h is lyophilized, obtained average grain diameter and exist
The nano-cellulose of 80nm.
Experiment one: granularmetric analysis experiment
The sisal hemp of equivalent weight will be weighed as basic material, the microjet side of difference selection example 3 and the prior art
Method prepares nano-cellulose, and the finished product of preparation is carried out size distribution intensive analysis, and analysis result is as shown in Figures 2 and 3, figure
The particle size distribution figure of 2 nano-celluloses obtained for the microjet method of the prior art, Fig. 3 are the method system that embodiment 3 provides
The particle size distribution figure of standby nano-cellulose, it can be seen from the figure that there is single normal distribution peak in two figures, but such as
Shown in Fig. 3, the nano-cellulose uniform particle sizes that embodiment 3 provides, opposite Fig. 2, nano-cellulose is closer spherical, three dimension scale
It is not much different, is more able to satisfy nanoscale requirement, therefore the nano-cellulose obtained using the method that the embodiment of the present invention 3 provides is more
It is able to satisfy the market demand, obtains nano-grade cellulosic more evenly.
Furthermore obtained nano-cellulose is weighed, forms ratio with basic material, nanometer is obtained by embodiment 3
The yield rate of cellulose is higher, and waste raw material are less, and practicability is stronger.
Experiment two: transmission electron microscope observing experiment
Two kinds of products obtained in experiment one are tested by transmission electron microscope observing respectively, obtain result such as Fig. 4 and Fig. 5 institute
Show, Fig. 4 is the transmission electron microscope picture for the nano-cellulose that the microjet of existing method obtains, and Fig. 5 is 3 high speed water jet of embodiment
The transmission electron microscope picture of obtained nano-cellulose, two width figures are compared and are learnt, the grain of the nano-cellulose under high-speed water jet processing
Diameter dimensional homogeneity is higher, while number of processes is also less compared to the nano-cellulose under the processing of existing microjet, operation letter
Single, energy consumption is few, it can be concluded that, can obtain that fibre dimensions are uniform, and uniform particle sizes can using method provided by the invention thus
Meet the nano-cellulose of nanoscale requirement.
The present invention is not limited to above-mentioned preferred forms, anyone can show that other are various under the inspiration of the present invention
The product of form, however, make any variation in its shape or structure, it is all that there is skill identical or similar to the present application
Art scheme, is within the scope of the present invention.
Claims (8)
1. a kind of method of high-speed water jet preparation sisal hemp nano-cellulose, which is characterized in that the described method comprises the following steps:
S1, sisal hemp is pre-processed, and prepares sisal cellulose;
S2, chloro fourth ethylmethylimidazolium ion solution is prepared;
S3, the sisal cellulose prepared in step S1 is added to the chloro fourth ethyl-methyl miaow prepared into step S2
Mixed solution is obtained in oxazolinium ion solution, the mixed solution is placed in uniform magnetic agitation in microwave abstracting synthesizer, wait pass through
Cross stirring the complete clear of the mixed solution after it is spare;
S4, the mixed solution spare in step S3 is refined by high-speed water jet, is mixed for cycle refinement 1-2 times
Liquid;
S5, boiling water will be added in super-voltage micro jet treated the homogeneous phase solution, and with being vigorously stirred, is obtained after stirring
Regeneration has the suspension of the sisal cellulose;
S6, the suspension after stirring in step S5 is placed in high speed freezing centrifuge, and is 6000- in the range of speeds
It is centrifuged repeatedly separation under the conditions of 10000r/min, controls centrifugation 10-15min every time, abandons supernatant, deionized water shake is added
It swings, washes away the remaining chloro fourth ethylmethylimidazolium ion solution, repeat 3-5 times, obtain regenerated cellulose;
S7, the regenerated cellulose obtained in step S6 is placed in freeze drier 24-36h is lyophilized, obtain average grain diameter
In the nano-cellulose of 60-80nm.
2. the method for high-speed water jet preparation sisal hemp nano-cellulose as described in claim 1, which is characterized in that step S1
In, sisal hemp is pre-processed, and prepare sisal cellulose, specifically includes the following steps:
S101, will shred after the sisal hemp be placed in concentration be 1-3% nitric acid in, and temperature be 100-120 DEG C in handle
3-5h;
S102, using the sisal hemp of distilled water repeated flushing step S101, until eluent is in neutrality;
S103, by treated in step S102, the sisal hemp uses the sodium hydroxide that concentration is 1-3% to handle at 100-110 DEG C
2-4h obtains the sisal cellulose.
3. the method for high-speed water jet preparation sisal hemp nano-cellulose as described in claim 1, which is characterized in that step S2
In, chloro fourth ethylmethylimidazolium ion solution is prepared, following methods are specifically included:
S201, N- methylimidazole and chloro-normal butane are blended in flask in the ratio of 5:8;
S202, by the flask as heating reflux reaction 24-36h in 110-120 DEG C of oil bath pan;
S203, the product after reaction is placed in Rotary Evaporators remove unreacted chloro-normal butane after to get to the chlorine
For fourth ethylmethylimidazolium ion solution.
4. the method for high-speed water jet preparation sisal hemp nano-cellulose as described in claim 1, which is characterized in that step S3
In, the concentration for the sisal cellulose being added in the mixed solution is 3-5wt%.
5. the method for high-speed water jet preparation sisal hemp nano-cellulose as described in claim 1, which is characterized in that step S3
In, the microwave power of the microwave abstracting synthesizer is 400-800W, and solution temperature range is 110-160 DEG C.
6. the method for high-speed water jet preparation sisal hemp nano-cellulose as described in claim 1, which is characterized in that step S4
In, the pressure limit of the high-speed water jet is 5-25kpsi.
7. the method for high-speed water jet preparation sisal hemp nano-cellulose as described in claim 1, which is characterized in that in step S5
The volume ratio of the boiling water and the homogeneous phase solution that are added is 5:1-10:1.
8. the method for high-speed water jet preparation sisal hemp nano-cellulose as claimed in claim 1 or 7, which is characterized in that described
Boiling water is the distilled water boiled.
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