CN107201685B - The pilot production line and its technique of Cellulose nanocrystal are extracted from biomass resource - Google Patents
The pilot production line and its technique of Cellulose nanocrystal are extracted from biomass resource Download PDFInfo
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- CN107201685B CN107201685B CN201710348427.4A CN201710348427A CN107201685B CN 107201685 B CN107201685 B CN 107201685B CN 201710348427 A CN201710348427 A CN 201710348427A CN 107201685 B CN107201685 B CN 107201685B
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- reaction kettle
- storage tank
- acidolysis
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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
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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Abstract
The invention discloses a kind of from biomass resource extracts the pilot production line and its technique of Cellulose nanocrystal.Including purification system, acidolysis system and after-treatment system;The purification system includes the alkali storage tank being sequentially connected, alkali leaching reaction kettle, vacuum filtration machine, purified product storage tank;The acidolysis system includes the sulfuric acid storage tank being sequentially connected, acidolysis reaction kettle;The after-treatment system successively includes tube centrifuge, washing kettle, ultrasonic dispersers, product storage tank.Different raw material, different method for hydrolysis be present invention can be suitably applied to the different demands of reactor.Cellulose nanocrystal pilot production line design of the present invention is succinct effective, and test effect is good, rationally distributed, has good market prospects and application value.
Description
Technical field
The pilot production line of extraction Cellulose nanocrystal and its production from biomass resource that present invention relates particularly to a kind of
Technique.
Background technique
One research is realized into industrialized production from the achievement in laboratory, is a huge and complicated process.This is not only
It is only indiscriminately imitating and expanding for the pure raw material that will be used in laboratory, step, equipment etc..It is put used by common laboratory
The step of big mode is amplifying method step by step, the method mainly has: the optimization of the type selecting, process conditions of equipment, the increase of reaction vessel.
Lectotype selection is the reactor for selecting different structure and pattern, is studied same reaction process.The type selecting of equipment is determined
Later it is necessary to the Optimization Work of the progress process conditions in optional test equipment, at this moment main task is to each technique
The investigation of condition, and it is screened out from it optimum process condition.The increase emphasis point of reaction vessel is the size to reaction vessel
Their influences to materials conversion rate and reaction selectivity are mainly investigated in the selection of size.Enlarged experiment production is small
The industrialized research approach of simulation that experiment carries out after achieving the desired results in order to realize industrialization.Scale up test will be according to work
Industryization degree to be achieved determines its scale, and solve on the basis of laboratory research to be likely encountered in industry
All the problem of being likely to occur.
Pilot plant test is to reduce conversion risk in order to make scientific achievement comply with market and industrialized requirement, improve conversion ratio,
And the batch carried out amplifies trial production.The purpose of this process is to verify, improve, and improves laboratory result or theoretical result,
Various uncertain factors are eliminated, the related technique of product, equipment the relevant technologies reliability data, parameter and intermediate products matter are obtained
Controllable test stone is measured, is allowed to match with other the relevant technologies, is actually consistent with production, it is consistent with social demand,
To make new technology comply in production, new product is successfully introduced to the market.Pilot plant test is that scientific and technological achievement is converted to productivity
Necessary links, the success or failure of achievement industrialization depend primarily on the success or failure of pilot scale, and therefore, pilot plant test is critically important.But pilot scale
Test does not obtain enough attention in China, and " pilot scale blank " phenomenon is than more serious.And for safety and manufacturing requirements
A pilot plant test line should be more established for relatively high civil explosive industry, this has the development of civil explosive industry and safe mass production
Extremely important function and significance.
Cellulose is that most wide boiomacromolecule is distributed on the earth, is widely present in the various biomass resources of nature,
Such as various plants, animal and bacteria cellulose.The Cellulose nanocrystal for extracting from native cellulose is a kind of with height
The rodlike biomass nano particle of crystallinity and rigidity has both high-crystallinity, high resiliency mould because of its unique rod-like nano pattern
Amount, high specific strength, from a wealth of sources, preparation process is relatively easy, biodegradable, biocompatibility is good and the spies such as renewable
Property, it is widely used in the reinforcing filler of high-performance composite materials.On the other hand, the Cellulose nanocrystal with Rod-like shape has
There is special liquid crystal nematic, can be widely applied to various functional materials, such as the controllable material of optics, bio-medical material, receives
Rice coating, the antibacterial packaging material of barrier etc..It is reported that Japanese papermaking association is developed recently using Cellulose nanocrystal for table
Finishing coat, the paper cup product with barrier properties for gases.Cellulose nanocrystal is with its numerous advantage, in material, chemistry, the energy
Etc. show huge application potential in various fields, in order to further expand its industrial application, serialization large-scale production is just shown
It obtains particularly important.Currently, preparation of the Cellulose nanocrystal in the lab scale of laboratory has reached its maturity, and how to realize industrial metaplasia
Production then has not been reported.Therefore, a continuous pilot scale line of production technology is established, realization is extracted from various native cellulose resources
Cellulose nanocrystal and put into batch production large-scale production be develop new material, improve abandoned biomass resource utilization must
It asks.
Summary of the invention
The purpose of the present invention is to provide a kind of from biomass resource extract Cellulose nanocrystal pilot production line and
Its technique.
In order to achieve the above objectives, as follows using technical solution:
From biomass resource extract Cellulose nanocrystal pilot production line, including purification system, acidolysis system and after
Processing system;
The purification system includes the alkali storage tank being sequentially connected, alkali leaching reaction kettle, vacuum filtration machine, purified product storage tank;
The acidolysis system includes the sulfuric acid storage tank being sequentially connected, acidolysis reaction kettle;
The after-treatment system successively includes tube centrifuge, washing kettle, ultrasonic dispersers, product storage tank;
The alkali storage tank passes through the first pipeline and is connected with alkali leaching reaction kettle, and the alkali leaching reaction kettle is by the second pipeline and very
Empty pump filter is connected, and the vacuum filtration machine is connected by the first conveyer belt with purified product storage tank;
The sulfuric acid storage tank is connected by third pipeline with acidolysis reaction kettle, and the purified product storage tank passes through the second transmission
Band is connected with acidolysis reaction kettle;
The acidolysis reaction kettle is connected by the 4th pipeline with tube centrifuge, and the tube centrifuge is transmitted by third
Band is connected with washing kettle, and the washing kettle is connected by the 5th pipeline and tube centrifuge formation circulation loop, the tubular type from
Scheming is connected by the 6th pipeline with ultrasonic dispersers, and the ultrasonic dispersers are connected by the 7th pipeline with product storage tank.
According to the above scheme, first pipeline is provided with the first safety valve and first flowmeter, the second pipeline setting
There is the first discharge valve, the vacuum filtration machine liquid outlet is provided with the first pH detection device.
According to the above scheme, the third pipeline is provided with the second safety valve and second flowmeter.
According to the above scheme, the four, the 5th pipeline is respectively arranged with the second discharge valve, third safety valve, and the described 6th
Pipeline is provided with third discharge valve and the 2nd pH detection device.
According to the above scheme, the acidolysis reaction kettle also possesses the heating system for the heating of sour water solution.
According to the above scheme, the acidolysis reaction kettle is jacket reactor.
According to the above scheme, the pilot production line is arranged on moveable platform.
It is including following using the production technology of the above-mentioned pilot production line for extracting Cellulose nanocrystal from biomass resource
Step:
1) according to the extracting method of certain existing Cellulose nanocrystal, by weight, cotton linter, hydroxide are weighed respectively
Sodium, the concentrated sulfuric acid, water give over to spare;
2) water, the sodium hydroxide in step 1 are injected into alkali storage tank, stirring is configured to the lye of certain mass concentration;By 1
The sodium hydroxide of middle cotton linter and above-mentioned certain mass score is added alkali by feed inlet and soaks reaction kettle, opens alkali leaching reaction kettle and stirs
It mixes motor to be stirred, alkali soaks 10-20h;
3) it opens alkali and soaks reaction kettle discharge valve, the product after alkali in step 2 is impregnated is passed through vacuum filtration machine, filters, washes
It washs to close neutral up to purified product;
4) water, the concentrated sulfuric acid in step 1 are injected into sulfuric acid storage tank, stirring is configured to the sulfuric acid solution of certain mass concentration;
By in step 3 purified product and above-mentioned prepared sulfuric acid solution by feed inlet be added acidolysis reaction kettle open stirring and add
Heat, acidolysis reaction 40min~60min at 40~50 DEG C are added ice water and terminate reaction;
5) acidolysis reaction kettle discharge valve is opened, the product after acidolysis in step 4 is centrifuged through tube centrifuge, lower layer is consolidated
Body precipitating is passed through washing reaction kettle, washs 15~20min, and the product after washing is returned to the tubular type by circulation loop and is centrifuged
Machine centrifugation;After repeated washing, centrifugation three times, it is centrifuged lower layer's solid product and a small amount of water dilution is added, detection pH value is close to after neutrality
Ultrasonic dispersers are passed through to be uniformly dispersed up to products C NC suspension;
6) CNC suspension is freeze-dried up to CNC powder.
The beneficial effects of the present invention are:
Cellulose nanocrystal pilot production line of the present invention uses jacket reactor, by changing heat transferring medium, may be implemented
Effective switching between heating process and cooling procedure, is simplified pilot production line.
Cellulose nanocrystal pilot production line of the present invention is mounted on moveable platform, is moved easily, can be in difference
Simulated experiment is carried out under scene condition.
Different raw material, different method for hydrolysis be present invention can be suitably applied to the different demands of reactor.
Cellulose nanocrystal pilot production line design of the present invention is succinct effective, and test effect is good, rationally distributed, has good
Good market prospects and application value.
Detailed description of the invention
Fig. 1 is Cellulose nanocrystal pilot production line process flow chart of the present invention;
Fig. 2 is Cellulose nanocrystal pilot production line schematic device of the present invention;
Fig. 3 is that Cellulose nanocrystal TEM figure is extracted in embodiment 1;
Fig. 4 is that Cellulose nanocrystal XRD diagram is extracted in embodiment 1;
Fig. 5 is that Cellulose nanocrystal TEM figure is extracted in embodiment 2;
Fig. 6 is that Cellulose nanocrystal XRD diagram is extracted in embodiment 2;
Wherein: 1, alkali storage tank;2, stirring motor is purified;3, the first agitating shaft;4, alkali soaks reaction kettle;5, the first discharge valve;
6, the first safety valve;7, first flowmeter;8, machine is filtered by vacuum;9, the first pH detection device;10, purified product storage tank;11, sulphur
Acid storage tank;12, acidolysis kettle stirring motor;13, the first shut-off valve;14, the second shut-off valve;15, the second safety valve;16, second
Meter;17, the second agitating shaft;18, acidolysis reaction kettle;19, the second discharge valve;20, the 2nd pH detection device;21, tubular type is centrifuged
Machine;22, washing kettle stirring motor;23, third agitating shaft;24, washing kettle;25, third safety valve;26, third discharge valve;27,
Ultrasonic dispersers;28, product storage tank.
Specific embodiment
Following embodiment further illustrates technical solution of the present invention, but not as limiting the scope of the invention.
The present invention extracts the pilot production line of Cellulose nanocrystal referring to shown in attached drawing 2 from biomass resource.
From biomass resource extract Cellulose nanocrystal pilot production line, including purification system, acidolysis system and after
Processing system;
Purification system includes the alkali storage tank 1 being sequentially connected, alkali leaching reaction kettle 4, vacuum filtration machine 8, purified product storage tank 10;
The alkali storage tank 1 soaks reaction kettle 4 with alkali by the first pipeline and is connected, and the alkali leaching reaction kettle 4 is taken out by the second pipeline and vacuum
Filter connected 8, the vacuum filtration machine 8 is connected by the first conveyer belt with purified product storage tank 10;Alkali leaching reaction kettle 4 is provided with
Purify stirring motor 2 and the first agitating shaft 3.First pipeline is provided with the first safety valve 6 and first flowmeter 7, and described
Two pipelines are provided with the first discharge valve 5, and the vacuum filtration machine liquid outlet is provided with the first pH detection device 9.
Acidolysis system includes the sulfuric acid storage tank 11 being sequentially connected, acidolysis reaction kettle 18;The sulfuric acid storage tank passes through third pipe
Road is connected with acidolysis reaction kettle, and the purified product storage tank is connected by the second conveyer belt with acidolysis reaction kettle;The third pipe
Road is provided with the second safety valve 15 and second flowmeter 16.It is respectively set on the cold and hot logistics water inlet pipe of acidolysis reaction kettle collet
There are the first shut-off valve 13 and the second shut-off valve 14.The acidolysis reaction kettle is additionally provided with acidolysis kettle stirring motor 12 and the second stirring
Axis 17.
After-treatment system successively includes tube centrifuge 21, washing kettle 24, ultrasonic dispersers 27, product storage tank 28;It is described
Acidolysis reaction kettle is connected by the 4th pipeline with tube centrifuge, and the tube centrifuge passes through third conveyer belt and washing kettle phase
Even, the washing kettle forms circulation loop with tube centrifuge by the 5th pipeline and is connected, and the tube centrifuge passes through the 6th
Pipeline is connected with ultrasonic dispersers, and the ultrasonic dispersers are connected by the 7th pipeline with product storage tank.Four, the 5th pipe
Road is respectively arranged with the second discharge valve 19, third safety valve 25, and the 6th pipeline is provided with third discharge valve 26 and the 2nd pH
Detection device 20.The washing kettle stirring is additionally provided with washing kettle stirring motor 22 and third agitating shaft 23.
It is as follows using above-mentioned pilot production line sulfuric acid solution Cellulose nanocrystal technique:
Embodiment 1
(1) according to the extracting method of certain existing Cellulose nanocrystal, by weight, cotton linter, hydrogen-oxygen are weighed respectively
Change sodium, the concentrated sulfuric acid, water, gives over to spare;
(2) water, the sodium hydroxide in (1) are injected into alkali storage tank, stirring is configured to the lye of 2% mass concentration;Close the
One discharge valve weighs cotton linter and 1 part of sodium hydroxide solution, 20 parts in above-mentioned (1) respectively, and alkali leaching reaction is added by feed inlet
Kettle is opened alkali leaching stirring motor and is stirred, and while agitating, alkali soaks 12h;
(3) the first discharge valve is opened, the product after alkali in (2) is impregnated is passed through vacuum filtration machine, filters, washs to close
Neutral purified product to obtain the final product;
(4) water, the sulfuric acid in (1) are injected into sulfuric acid storage tank, stirring is configured to the sulfuric acid solution of 65% mass concentration;Point
Purified product and 1 part of sulfuric acid solution, 20 parts in above-mentioned (3) also known as are taken, the unlatching acidolysis of acidolysis reaction kettle is added by feed inlet and is stirred
It mixes motor to be stirred, and is passed through the heat medium of certain temperature into reacting kettle jacketing, 45 DEG C of acidolysis reaction 45min are added
A large amount of ice water terminate reaction.
(5) the second discharge valve is opened, the product after acidolysis in (4) is centrifuged through centrifuge;It is anti-that washing is passed through from feed inlet
Kettle is answered, 15~20min is washed, opens third discharge valve, the product after washing is passed through centrifuge centrifugation;Repeated centrifugation, washing
After three times, it is centrifuged lower layer's solid product and a small amount of water dilution is added, it is equal that detection pH value is passed through ultrasonic dispersers dispersion close to after neutrality
Even products C NC suspension to obtain the final product.
(6) suspension in (5) is freeze-dried up to sulphuric acid hydrolysis CNC powder.
After sodium carbonate neutralization is added in sulfuric acid waste caused by above-mentioned test, it is evaporated using multi-effect evaporator as solid
Waste sodium sulphate crude product.
From attached drawing 3 and 4 it is found that the cellulose that the present embodiment production line and production technology are extracted from cotton linter is received
Meter Jing has Rod-like shape, and draw ratio is 10~30, and has high-crystallinity.
Embodiment 2
(1) according to the extracting method of certain existing Cellulose nanocrystal, by weight, ascidian powder, hydrogen-oxygen are taken respectively
Change potassium, the concentrated sulfuric acid, water, gives over to spare;
(2) water, the potassium hydroxide in (1) are injected into alkali storage tank, stirring is configured to the lye of 5% mass concentration;It weighs
1 part of ascidian powder in (1) is stated, 30 parts of potassium hydroxide solution are added alkali by feed inlet and soak reaction kettle, open alkali and soak stirring motor
It is stirred, while agitating, alkali soaks 40h;
(3) the first outlet valve is opened, the product after alkali in (2) is impregnated is passed through vacuum filtration machine, filters, washs to neutrality
And it is configured to 300 parts of suspension;5 parts of glacial acetic acid and 10 parts of liquor natrii hypochloritis are added, are bleached in triplicate to suspension
For white, distilled water is added and repeatedly filters, wash to close to neutrality and obtain purified product.
(4) water, the sulfuric acid in (1) are injected into sulfuric acid storage tank, stirring is configured to the sulfuric acid solution of 55% mass concentration;Point
Purified product 4 part are also known as taken in above-mentioned (3), and 300 parts of sulfuric acid solution are added acidolysis reaction kettle by feed inlet and open acidolysis stirring
Motor is stirred, and the heat medium of certain temperature is passed through into reacting kettle jacketing, acidolysis reaction 120min at 50 DEG C, is added
A large amount of ice water terminate reaction.
(5) the second outlet valve is opened, the product after acidolysis in (4) is centrifuged through centrifuge;It is anti-that washing is passed through from feed inlet
Kettle is answered, 15~20min is washed, opens third outlet valve, the product after washing is passed through centrifuge centrifugation;Repeated centrifugation, washing
After three times, it is centrifuged lower layer's solid product and a small amount of water dilution is added, it is equal that detection pH value is passed through ultrasonic dispersers dispersion close to after neutrality
Even product ascidian CNC suspension to obtain the final product.
(6) suspension in (5) is freeze-dried up to ascidian Cellulose nanocrystal powder.
After sodium carbonate neutralization is added in sulfuric acid waste caused by above-mentioned test, it is evaporated using multi-effect evaporator as solid
Waste sodium sulphate crude product.
From attached Figures 5 and 6 it is found that the cellulose nanometer that the present embodiment production line and production technology are extracted from ascidian
Crystalline substance has Rod-like shape, and draw ratio is 60~70, and has high-crystallinity.
Claims (8)
1. extracting the pilot production line of Cellulose nanocrystal from biomass resource, including purification system, acidolysis system and rear place
Reason system;It is characterized by:
The purification system includes the alkali storage tank being sequentially connected, alkali leaching reaction kettle, vacuum filtration machine, purified product storage tank;
The acidolysis system includes the sulfuric acid storage tank being sequentially connected, acidolysis reaction kettle;
The after-treatment system successively includes tube centrifuge, washing kettle, ultrasonic dispersers, product storage tank;
The alkali storage tank soaks reaction kettle with alkali by the first pipeline and is connected, and the alkali leaching reaction kettle is taken out by the second pipeline and vacuum
Filter is connected, and the vacuum filtration machine is connected by the first conveyer belt with purified product storage tank;
The sulfuric acid storage tank is connected by third pipeline with acidolysis reaction kettle, the purified product storage tank pass through the second conveyer belt and
Acidolysis reaction kettle is connected;
The acidolysis reaction kettle is connected by the 4th pipeline with tube centrifuge, the tube centrifuge pass through third conveyer belt and
Washing kettle is connected, and the washing kettle forms circulation loop with tube centrifuge by the 5th pipeline and is connected, the tube centrifuge
It is connected by the 6th pipeline with ultrasonic dispersers, the ultrasonic dispersers are connected by the 7th pipeline with product storage tank.
2. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as described in claim 1, it is characterised in that institute
It states the first pipeline and is provided with the first safety valve and first flowmeter, second pipeline is provided with the first discharge valve, the vacuum
Suction filtration machine liquid outlet is provided with the first pH detection device.
3. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as described in claim 1, it is characterised in that institute
It states third pipeline and is provided with the second safety valve and second flowmeter.
4. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as described in claim 1, it is characterised in that institute
State the four, the 5th pipelines and be respectively arranged with the second discharge valve, third safety valve, the 6th pipeline be provided with third discharge valve and
2nd pH detection device.
5. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as described in claim 1, it is characterised in that institute
It states acidolysis reaction kettle and also possesses the heating system heated for sour water solution.
6. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as described in claim 1, it is characterised in that institute
Stating acidolysis reaction kettle is jacket reactor.
7. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as described in claim 1, it is characterised in that institute
Pilot production line is stated to be arranged on moveable platform.
8. the production work of the pilot production line of Cellulose nanocrystal is extracted described in exploitation right any one of 1-6 from biomass resource
Skill, it is characterised in that the following steps are included:
1) according to the extracting method of certain existing Cellulose nanocrystal, by weight, weigh respectively cotton linter, sodium hydroxide,
The concentrated sulfuric acid, water give over to spare;
2) water, the sodium hydroxide in step 1) are injected into alkali storage tank, stirring is configured to the lye of certain mass concentration;By step
1) alkali leaching reaction kettle is added by feed inlet in the sodium hydroxide of cotton linter and above-mentioned certain mass score in, opens alkali and soaks reaction kettle
Stirring motor is stirred, and alkali soaks 10-20h;
3) it opens alkali and soaks reaction kettle discharge valve, the product after alkali in step 2) is impregnated is passed through vacuum filtration machine, filters, washs extremely
Close to neutral up to purified product;
4) water, the concentrated sulfuric acid in step 1) are injected into sulfuric acid storage tank, stirring is configured to the sulfuric acid solution of certain mass concentration;It will
Purified product and above-mentioned prepared sulfuric acid solution in step 3) are added acidolysis reaction kettle unlatching stirring by feed inlet and add
Heat, acidolysis reaction 40min~60min at 40~50 DEG C are added ice water and terminate reaction;
5) acidolysis reaction kettle discharge valve is opened, the product after acidolysis in step 4) is centrifuged through tube centrifuge, by lower layer's solid
Precipitating is passed through washing reaction kettle, washs 15~20min, the product after washing is returned to the tube centrifuge by circulation loop
Centrifugation;After repeated washing, centrifugation three times, it is centrifuged lower layer's solid product and a small amount of water dilution is added, detection pH value is led to close to after neutrality
Enter ultrasonic dispersers to be uniformly dispersed up to products C NC suspension;
6) CNC suspension is freeze-dried up to CNC powder.
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US7981337B2 (en) * | 2006-04-21 | 2011-07-19 | Wuhan University | Use of aqueous NaOH/thiourea solution in pilot-scale production of cellulose products |
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