CN107201685A - 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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- CN107201685A CN107201685A CN201710348427.4A CN201710348427A CN107201685A CN 107201685 A CN107201685 A CN 107201685A CN 201710348427 A CN201710348427 A CN 201710348427A CN 107201685 A CN107201685 A CN 107201685A
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- alkali
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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
Abstract
The invention discloses a kind of pilot production line and its technique that Cellulose nanocrystal is extracted from biomass resource.Including purification system, acidolysis system and after-treatment system；The purification system includes alkali storage tank, alkali leaching reactor, vacuum filtration machine, the purified product storage tank being sequentially connected；The acidolysis system includes sulfuric acid storage tank, the acidolysis reaction kettle being sequentially connected；The after-treatment system includes tube centrifuge, washing kettle, ultrasonic dispersers, product storage tank successively.It present invention can be suitably applied to the different demands of different raw material, different method for hydrolysis to reactor.Cellulose nanocrystal pilot production line design of the present invention is succinct effective, and test effect is good, rationally distributed, with good market prospects and application value.
Description
Technical field
Present invention relates particularly to a kind of pilot production line that Cellulose nanocrystal is extracted from biomass resource and its production
Technique.
Background technology
Achievement by a research from laboratory realizes industrialized production, is a huge and complicated process.This is not only
Only it is pure indiscriminately imitating the raw material used in laboratory, step, equipment etc. and expand.What common laboratory was used puts
The step of big mode is amplifying method step by step, the method mainly has：Optimization, the increase of reaction vessel of the type selecting, process conditions of equipment.
Lectotype selection is the reactor from different structure and pattern, and same reaction process is studied.Type selecting to 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 therefrom filter out optimum process condition.The increase emphasis point of reaction vessel is the size to reaction vessel
The selection of size, mainly investigates their influences to materials conversion rate and reaction selectivity.Enlarged experiment production is small
Experiment is industrialized and the industrialized research approach of simulation of progress after producing a desired effect in order to realize.Scale up test will be according to work
Industryization wants degree to which to determine its scale, and solves what is be likely encountered in industry on the basis of laboratory research
It is all the problem of be likely to occur.
Pilot plant test is that reduction conversion risk improves conversion ratio in order that scientific achievement complies with market and industrialized requirement,
And the batch amplification trial production carried out.The purpose of this process is to verify, improved, and improves laboratory result or theoretical result,
Various uncertain factors are eliminated, the relevant technique of product, equipment correlation technique reliability data, parameter and intermediate products matter is obtained
The controllable test stone of amount, is allowed to match with other correlation techniques, is consistent with produce reality, consistent with social demand,
So that new technology is complied with 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
Experiment 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 more be set up for high civil explosive industry by comparing, and this big production of development and safety to civil explosive industry has
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 of native cellulose is extracted from, is that one kind has height
Crystallinity and rigid bar-shaped biomass nano particle, because of its unique rod-like nano pattern, have high-crystallinity, high resiliency mould concurrently
Amount, high specific strength, wide material sources, preparation technology are relatively easy, biodegradable, biocompatibility is good and the spy such as renewable
Property, it is widely used in the reinforcer of high-performance composite materials.On the other hand, the Cellulose nanocrystal tool with Rod-like shape
There is special liquid crystal nematic, can be widely applied to various functions material, such as optics controllable material, bio-medical material, receive
Rice coating, the antibacterial packaging material of barrier etc..It is reported that Japanese papermaking association develops utilize Cellulose nanocrystal to be used for table recently
Finishing coat, the paper cup product with barrier properties for gases.Cellulose nanocrystal is with its numerous advantage, in material, chemistry, the energy
Etc. huge application potential is shown in various fields, in order to further expand its commercial Application, serialization large-scale production just shows
Obtain particularly important.At present, preparation of the Cellulose nanocrystal in the lab scale of laboratory has reached its maturity, and how to realize industrial metaplasia
Production then has no report.Therefore, a continuous pilot scale line of production technology is set up, realizes and 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
Ask.
The content of the invention
It is an object of the invention to provide it is a kind of from biomass resource extract Cellulose nanocrystal pilot production line and
Its technique.
It is as follows using technical scheme to reach above-mentioned purpose：
From biomass resource extract Cellulose nanocrystal pilot production line, including purification system, acidolysis system and after
Processing system；
The purification system includes alkali storage tank, alkali leaching reactor, vacuum filtration machine, the purified product storage tank being sequentially connected；
The acidolysis system includes sulfuric acid storage tank, the acidolysis reaction kettle being sequentially connected；
The after-treatment system includes tube centrifuge, washing kettle, ultrasonic dispersers, product storage tank successively；
The alkali storage tank soaks reactor by the first pipeline and alkali and is connected, and the alkali leaching reactor is by the second pipeline and very
Empty suction filtration machine 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 the 3rd 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 passes through the 3rd transmission
Band is connected with washing kettle, the washing kettle by the 5th pipeline and tube centrifuge formation circulation loop be connected, 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.
By such scheme, first pipeline is provided with the first safety valve and first flowmeter, and second pipeline is set
There is the first discharge valve, the vacuum filtration machine liquid outlet is provided with the first pH detection means.
By such scheme, the 3rd pipeline is provided with the second safety valve and second flowmeter.
By such scheme, the four, the 5th pipeline is respectively arranged with the second discharge valve, the 3rd safety valve, the described 6th
Pipeline is provided with the 3rd discharge valve and the 2nd pH detection means.
By such scheme, the acidolysis reaction kettle also possesses the heating system heated for sour water solution.
By such scheme, the acidolysis reaction kettle is jacket reactor.
By such 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 that Cellulose nanocrystal is extracted 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 standby；
2) water in step 1, sodium hydroxide are injected into alkali storage tank, stirring is configured to the alkali lye of certain mass concentration；By 1
The sodium hydroxide of middle cotton linter and above-mentioned certain mass fraction adds alkali by charging aperture and soaks reactor, opens alkali leaching reactor and stirs
Mix motor to be stirred, alkali leaching 10-20h；
3) alkali leaching reactor discharge valve is opened, the product after alkali immersion in step 2 is passed through vacuum filtration machine, suction filtration, is washed
Wash to close to neutrality and produce purified product；
4) water in step 1, the concentrated sulfuric acid are injected into sulfuric acid storage tank, stirring is configured to the sulfuric acid solution of certain mass concentration；
Purified product in step 3 and the above-mentioned sulfuric acid solution prepared are added into acidolysis reaction kettle unlatching stirring by charging aperture and added
Heat, acidolysis reaction 40min~60min at 40~50 DEG C adds frozen water terminating reaction；
5) acidolysis reaction kettle discharge valve is opened, the product after acidolysis in step 4 is centrifuged through tube centrifuge, lower floor is consolidated
Body precipitation is passed through washing reaction kettle, washs 15~20min, and the product after washing is returned into the tubular type by circulation loop centrifuges
Machine is centrifuged；After repeated washing, centrifugation three times, centrifugation lower floor solid product adds a small amount of water dilution, and detection pH value is close to after neutral
It is passed through ultrasonic dispersers and is uniformly dispersed and produces products C NC suspension；
6) freeze-drying of CNC suspension is produced into 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, it is possible to achieve
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.
It present invention can be suitably applied to the different demands of different raw material, different method for hydrolysis to reactor.
Cellulose nanocrystal pilot production line design of the present invention is succinct effective, and test effect is good, rationally distributed, with good
Good market prospects and application value.
Brief description of the drawings
Fig. 1 is Cellulose nanocrystal pilot production line process chart of the present invention；
Fig. 2 is Cellulose nanocrystal pilot production line schematic device of the present invention；
Fig. 3 is extraction Cellulose nanocrystal TEM figures in embodiment 1；
Fig. 4 is extraction Cellulose nanocrystal XRD in embodiment 1；
Fig. 5 is extraction Cellulose nanocrystal TEM figures in embodiment 2；
Fig. 6 is extraction Cellulose nanocrystal XRD in embodiment 2；
Wherein：1st, alkali storage tank；2nd, stirring motor is purified；3rd, the first agitating shaft；4th, alkali leaching reactor；5th, the first discharge valve；
6th, the first safety valve；7th, first flowmeter；8th, it is filtered by vacuum machine；9th, the first pH detection means；10th, purified product storage tank；11st, sulphur
Acid storage tank；12nd, acidolysis kettle stirring motor；13rd, the first stop valve；14th, the second stop valve；15th, the second safety valve；16th, second
Gauge；17th, the second agitating shaft；18th, acidolysis reaction kettle；19th, the second discharge valve；20th, the 2nd pH detection means；21st, tubular type is centrifuged
Machine；22nd, washing kettle stirring motor；23rd, the 3rd agitating shaft；24th, washing kettle；25th, the 3rd safety valve；26th, the 3rd discharge valve；27、
Ultrasonic dispersers；28th, product reservoir.
Embodiment
Following examples further explain technical scheme, but not as limiting the scope of the invention.
The present invention extracts the pilot production line of Cellulose nanocrystal referring to the drawings shown in 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 alkali storage tank 1, alkali leaching reactor 4, vacuum filtration machine 8, the purified product storage tank 10 being sequentially connected；
The alkali storage tank 1 soaks reactor 4 by the first pipeline and alkali and is connected, and the alkali leaching reactor 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 reactor 4 is provided with
Purify the agitating shaft 3 of stirring motor 2 and first.First pipeline is provided with the first safety valve 6 and first flowmeter 7, 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 means 9.
Acidolysis system includes sulfuric acid storage tank 11, the acidolysis reaction kettle 18 being sequentially connected；The sulfuric acid storage tank passes through the 3rd 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；3rd pipe
Road is provided with the second safety valve 15 and second flowmeter 16.Set respectively on the cold and hot logistics water inlet pipe of acidolysis reaction kettle chuck
There are the first stop valve 13 and the second stop valve 14.The acidolysis reaction kettle is additionally provided with the stirring of acidolysis kettle stirring motor 12 and second
Axle 17.
After-treatment system includes tube centrifuge 21, washing kettle 24, ultrasonic dispersers 27, product storage tank 28 successively；It is described
Acidolysis reaction kettle is connected by the 4th pipeline with tube centrifuge, and the tube centrifuge passes through the 3rd conveyer belt and washing kettle phase
Even, the washing kettle is connected by the 5th pipeline with tube centrifuge formation circulation loop, 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, the 3rd safety valve 25, and the 6th pipeline is provided with the 3rd discharge valve 26 and the 2nd pH
Detection means 20.The washing kettle stirring is additionally provided with the agitating shaft 23 of washing kettle stirring motor 22 and the 3rd.
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, give over to standby；
(2) water in (1), sodium hydroxide are injected into alkali storage tank, stirring is configured to the alkali lye of 2% mass concentration；Close the
One discharge valve, weigh respectively 1 part of cotton linter and sodium hydroxide solution in above-mentioned (1), 20 parts, pass through charging aperture and add alkali leaching reaction
Kettle, opens alkali leaching stirring motor and is stirred, while stirring, alkali leaching 12h；
(3) the first discharge valve is opened, the product in (2) after alkali immersion is passed through vacuum filtration machine, suction filtration, is washed to approaching
Neutrality produces purified product；
(4) water in (1), sulfuric acid are injected into sulfuric acid storage tank, stirring is configured to the sulfuric acid solution of 65% mass concentration；Point
Also known as take 1 part of purified product and sulfuric acid solution in above-mentioned (3), 20 parts, acidolysis reaction kettle added by charging aperture open acidolysis and stir
Motor is mixed to be stirred, and toward the heating medium that certain temperature is passed through in reacting kettle jacketing, 45 DEG C of acidolysis reaction 45min are added
A large amount of frozen water terminating reactions.
(5) the second discharge valve is opened, by the product after acidolysis in (4) through centrifuge；It is anti-that washing is passed through from charging aperture
Kettle is answered, 15~20min is washed, the 3rd discharge valve is opened, the product after washing is passed through centrifuge；Repeated centrifugation, washing
After three times, centrifuge lower floor's solid product and add a small amount of water dilution, it is scattered equal that detection pH value is passed through ultrasonic dispersers close to after neutrality
It is even to produce products C NC suspension.
(6) suspension freeze-drying in (5) is produced into sulphuric acid hydrolysis CNC powder.
Sulfuric acid waste produced by above-mentioned experiment is added after sodium carbonate neutralization, is evaporated using multi-effect evaporator as solid
Waste sodium sulphate crude product.
It was found from accompanying drawing 3 and 4, the present embodiment production line and production technology are extracted obtained cellulose from cotton linter and received
Meter Jing has Rod-like shape, and draw ratio is 10~30, and with 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, give over to standby；
(2) water in (1), potassium hydroxide are injected into alkali storage tank, stirring is configured to the alkali lye of 5% mass concentration；Weigh
1 part of ascidian powder in (1) is stated, 30 parts of potassium hydroxide solution adds alkali by charging aperture and soaks reactor, opens alkali leaching stirring motor
It is stirred, while stirring, alkali leaching 40h；
(3) the first outlet valve is opened, the product after alkali immersion in (2) is passed through vacuum filtration machine, suction filtration, washing to neutrality
And it is configured to 300 parts of suspension；5 parts of glacial acetic acid and 10 parts of liquor natrii hypochloritises are added, are bleached in triplicate to suspension
For white, add the multiple suction filtration of distilled water, washing and obtain purified product to close to neutrality.
(4) water in (1), sulfuric acid are injected into sulfuric acid storage tank, stirring is configured to the sulfuric acid solution of 55% mass concentration；Point
4 parts of purified product in above-mentioned (3) is also known as taken, 300 parts of sulfuric acid solution adds acidolysis reaction kettle by charging aperture and opens acidolysis stirring
Motor is stirred, and toward the heating medium that certain temperature is passed through in reacting kettle jacketing, acidolysis reaction 120min at 50 DEG C is added
A large amount of frozen water terminating reactions.
(5) the second outlet valve is opened, by the product after acidolysis in (4) through centrifuge；It is anti-that washing is passed through from charging aperture
Kettle is answered, 15~20min is washed, the 3rd outlet valve is opened, the product after washing is passed through centrifuge；Repeated centrifugation, washing
After three times, centrifuge lower floor's solid product and add a small amount of water dilution, it is scattered equal that detection pH value is passed through ultrasonic dispersers close to after neutrality
It is even to produce product ascidian CNC suspension.
(6) suspension freeze-drying in (5) is produced into ascidian Cellulose nanocrystal powder.
Sulfuric acid waste produced by above-mentioned experiment is added after sodium carbonate neutralization, is evaporated using multi-effect evaporator as solid
Waste sodium sulphate crude product.
It was found from accompanying drawing 5 and 6, the present embodiment production line and production technology extract obtained cellulose nanometer from ascidian
Crystalline substance has Rod-like shape, and draw ratio is 60~70, and with high-crystallinity.
Claims (8)
1. the pilot production line of Cellulose nanocrystal is extracted from biomass resource, including purification system, acidolysis system and rear place
Reason system；It is characterized in that：
The purification system includes alkali storage tank, alkali leaching reactor, vacuum filtration machine, the purified product storage tank being sequentially connected；
The acidolysis system includes sulfuric acid storage tank, the acidolysis reaction kettle being sequentially connected；
The after-treatment system includes tube centrifuge, washing kettle, ultrasonic dispersers, product storage tank successively；
The alkali storage tank soaks reactor by the first pipeline and alkali and is connected, and the alkali leaching reactor 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 the 3rd pipeline with acidolysis reaction kettle, the purified product storage tank by the second conveyer belt with
Acidolysis reaction kettle is connected；
The acidolysis reaction kettle is connected by the 4th pipeline with tube centrifuge, the tube centrifuge by the 3rd conveyer belt with
Washing kettle is connected, and the washing kettle is connected by the 5th pipeline with tube centrifuge formation circulation loop, 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 claimed in claim 1, it is characterised in that institute
State the first pipeline and be 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 means.
3. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as claimed in claim 1, it is characterised in that institute
State the 3rd pipeline and be provided with the second safety valve and second flowmeter.
4. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as claimed in claim 1, it is characterised in that institute
State the four, the 5th pipelines and be respectively arranged with the second discharge valve, the 3rd safety valve, the 6th pipeline be provided with the 3rd discharge valve and
2nd pH detection means.
5. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as claimed in claim 1, it is characterised in that institute
State acidolysis reaction kettle and also possess the heating system heated for sour water solution.
6. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as claimed in claim 1, it is characterised in that institute
Acidolysis reaction kettle is stated for jacket reactor.
7. the pilot production line of Cellulose nanocrystal is extracted from biomass resource as claimed 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 comprise the following steps：
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 standby；
2) water in step 1, sodium hydroxide are injected into alkali storage tank, stirring is configured to the alkali lye of certain mass concentration；By cotton in 1
The sodium hydroxide of short flannel and above-mentioned certain mass fraction adds alkali by charging aperture and soaks reactor, opens alkali leaching reactor stirring electricity
Machine is stirred, alkali leaching 10-20h；
3) alkali leaching reactor discharge valve is opened, the product after alkali immersion in step 2 vacuum filtration machine is passed through, suction filtration, washing are extremely
Purified product is produced close to neutrality；
4) water in step 1, the concentrated sulfuric acid are injected into sulfuric acid storage tank, stirring is configured to the sulfuric acid solution of certain mass concentration；Will step
Purified product and the above-mentioned sulfuric acid solution prepared in rapid 3 add acidolysis reaction kettle by charging aperture and open stirring and heating,
Acidolysis reaction 40min~60min at 40~50 DEG C, adds frozen water terminating reaction；
5) acidolysis reaction kettle discharge valve is opened, the product after acidolysis in step 4 is centrifuged through tube centrifuge, lower floor's solid is sunk
Shallow lake is passed through washing reaction kettle, washs 15~20min, by the product after washing by circulation loop return the tube centrifuge from
The heart；After repeated washing, centrifugation three times, centrifugation lower floor solid product adds a small amount of water dilution, and detection pH value is close to being passed through after neutral
Ultrasonic dispersers, which are uniformly dispersed, produces products C NC suspension；
6) freeze-drying of CNC suspension is produced into CNC powder.
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| CN111760533A (en) * | 2020-07-08 | 2020-10-13 | 刘帆 | Ultrasonic micro-airflow biomass production line system |
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