CN107641993A - The preparation method of microfine cellulose - Google Patents
The preparation method of microfine cellulose Download PDFInfo
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- CN107641993A CN107641993A CN201710985300.3A CN201710985300A CN107641993A CN 107641993 A CN107641993 A CN 107641993A CN 201710985300 A CN201710985300 A CN 201710985300A CN 107641993 A CN107641993 A CN 107641993A
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Abstract
The present invention relates to a kind of preparation method of microfine cellulose, comprise the following steps：Cellulosic material is prepared into cellulose films or cellulose coiled material by copy paper technique；The cellulose films or cellulose coiled material are handled with radiosensitizer；Cellulose films or the cellulose coiled material after radiosensitizer is handled is handled in radiation environment with radioactive ray；Cellulose films or the cellulose coiled material after radioactive ray process is subjected to air-flow smashing, obtains microfine cellulose.The present invention is combined by copy paper technique, RADIATION PROCESSING technique and gas flow crushing process, and using pristine fibre element slurry as raw material, it is high in micro-nano rank, the microfine cellulose that draw ratio is 5 120, production efficiency to obtain size compared with low energy consumption.
Description
Technical field
The present invention relates to cellulosic material, more particularly to a kind of preparation method of microfine cellulose.
Background technology
Cellulose is that nature contains most abundant natural polymer, has good chemical stability, biocompatibility
And degradability.The methods of by mechanical lapping, chemical acidolysis and biological enzymolysis, microfine cellulose can be prepared.Microfine cellulose
Material is by as green additive, for application studies such as high polymer material (rubber, plastics, fiber) enhancing, lightweights.
The conventional method for preparing microfine cellulose needs to carry out in the liquid phase at present, the too high outstanding problem of energy consumption, prepares
Cheng Keneng is polluted.Such as when high-pressure homogeneous processing or microjet processing preparation microfine cellulose, the quality hundred of raw material slurry
Divide than being usually no more than 10%, fabrication cycles, which are more than 5 times, can just obtain effective product.In addition, raw materials size also needs accurately to control,
Otherwise easily equipment is caused to block.Though extra-fine grinding processing can avoid disadvantages described above to a certain extent, abrasive wear is held very much
Easily it is contaminated product.Chemical acidolysis and biological enzymolysis technique prepare microfine cellulose and then need to use chemical-biological preparation,
Later separation purifying technique complex operation.
The content of the invention
Based on the deficiency of above-mentioned preparation method, the system of the controllable microfine cellulose of a kind of low energy consumption of present invention offer, size
Preparation Method.
A kind of preparation method of microfine cellulose, comprises the following steps：
Cellulosic material is prepared into cellulose films or cellulose coiled material by copy paper technique；
Cellulose films or the cellulose coiled material after being handled with radiosensitizer；
Cellulose films or the cellulose coiled material after radiosensitizer is handled is used into radiation in radiation environment
Line is handled；
Cellulose films or the cellulose coiled material after radioactive ray process is subjected to air-flow smashing, obtains superfine fibre
Element.
In one of the embodiments, the cellulosic material is bleaching needle-point leaf pulp or bleached hardwood pulp or purified cotton
The dregs of rice are starched.
In one of the embodiments, the technological parameter of the copy paper technique is：Cellulose films or the cellulose volume
The drying temperature of material is not higher than 85 DEG C.Now, the water capacity of cellulose films or the cellulose coiled material is 7-12%.
In one of the embodiments, the grammes per square metre of cellulose films or the cellulose coiled material obtained by copy paper technique
For 30-80g/m2。
In one of the embodiments, the radiosensitizer is strong oxidizer, the strong oxidizer be hydrogen peroxide or
Sodium peroxydisulfate.Radiosensitizer produces strong oxidative free radical by high-energy ray irradiation decomposable asymmetric choice net.Radiosensitizer dosage is fibre
Tie up the 2%-15% of plain material quality.
In one of the embodiments, described when handling the cellulose films or coiled material with radiosensitizer, technique is
Spraying or dipping.
In one of the embodiments, the radioactive ray are gamma-rays or electron beam, and radiographic source is60Co or137Cs, it is described
The dose of radiation of radioactive ray is 20-300KGy.The radiation environment is air, vacuum or inert gas, preferable radiation environment
For vacuum or inert gas.
Cellulose films after copy paper PROCESS FOR TREATMENT or coiled material are subjected to radiation process processing, improve the soft of cellulosic material
Adhesion between toughness and reduction cellulosic molecule.High-energy ray processing technology is highly controllable, can accurately control and ensure product
Performance.Cellulose is more beneficial for follow-up ultramicro grinding after ray is processed in mechanical property.
In one of the embodiments, the technological parameter of the air-flow crushing is：Airflow humidity is 15%-70%.By
Cellulose films or coiled material after irradiation have certain toughness, in this humidity range, can obtain satisfactory ultra-fine fibre
Tie up cellulosic material.
In one of the embodiments, the technological parameter of the air-flow crushing is：The operating pressure of airslide disintegrating mill is 500
KPas -1200 kPas.The microfine cellulose of controllable specification can be made by the time and grading device for adjusting air-flow crushing.
Product is prepared under dry state, is not required to handle using traditional acidolysis or chemical reagent, technical process does not produce " three wastes ", is also not required to
Want hygrometric state crushing or mechanical deep cooling crush (liquid nitrogen need to be added).So as to save a large amount of energy consumptions, production at utmost ensure that
Security, the feature of environmental protection and economical.
Compared with existing scheme, the invention has the advantages that：
The preparation method of above-mentioned microfine cellulose, prepared by copy paper technique, RADIATION PROCESSING technique and gas flow crushing process
Obtained microfine cellulose has the characteristic that specific surface area is big, surface topography and draw ratio are controllable.Copy paper technique is by pristine fibre
Plain slurry is prepared into sheet material or coiled material, rather than pristine fibre element slurry is directly irradiated, and avoids radiating uneven, guarantee
The stability of radiation process.The grammes per square metre and drying temperature of sheet material and coiled material are controlled, is advantageous to gas flow crushing process
Pulverization process, gas flow crushing process of the present invention carries out under dry state, to obtain size in micro-nano rank, length compared with low energy consumption
For 10 μm -800 μm；A diameter of 0.5 μm -50 μm；Draw ratio is 5-120 microfine cellulose, and production efficiency is high, and size is controllable.
The microfine cellulose that the application is obtained using specific preparation method has excellent mechanical property, can extensive use
In functional composite material, adsorption and separation material and biologic medical base material.
Embodiment
The preparation method of the microfine cellulose of the present invention is described in further detail below in conjunction with specific embodiment.
The raw material sources of the present invention are commercially available.
Embodiment 1
The present embodiment provides a kind of preparation method of microfine cellulose, comprises the following steps：
20kg bleaching needle-point leaf pulps are taken, 30g/m is prepared by semi-automatic paper machine2Cellulose films.Wherein, cellulose
The drying temperature of sheet material is 85 DEG C, water capacity 7-12%.Bleaching needle-point leaf pulp fibre length is 2mm-4mm, a diameter of 25 μm-
50μm；
By the sodium peroxydisulfate solution spraying of mass concentration 5% on above-mentioned cellulose films；
The above-mentioned cellulose films sprayed are placed in60Under Co gamma-rays, irradiation dose 60kGy；
Cellulose films by irradiation are subjected to fine processing on airslide disintegrating mill.Airflow humidity controls
20%, stream pressure is 1200 kPas, and it is 450 μm -500 μm that fibre length, which is made, a diameter of 1 μm -5 μm of microfine cellulose into
Product.
Embodiment 2
The present embodiment provides a kind of preparation method of microfine cellulose, comprises the following steps：
20kg bleached hardwood pulps are taken, 60g/m is prepared by semi-automatic paper machine2Cellulose films.Wherein, cellulose
The drying temperature of sheet material is 50 DEG C, water capacity 7-12%.The bleaching wealthy wood pulp cellulose length of pin is 0.8mm-1.5mm, a diameter of 5
μm-10μm；
By the sodium peroxydisulfate solution spraying of mass concentration 2% on above-mentioned cellulose films；
The above-mentioned cellulose films sprayed are placed in60Under Co gamma-rays, irradiation dose 20kGy；
Cellulose films by irradiation are subjected to fine processing on airslide disintegrating mill.Airflow humidity controls
20%, stream pressure is 600 kPas, and it is 100 μm -300 μm that fibre length, which is made, a diameter of 0.8 μm -1.5 μm of superfine fibre
Plain finished product.
Embodiment 3
The present embodiment provides a kind of preparation method of microfine cellulose, comprises the following steps：
Take 10kg to refine cotton dregs slurry, 30g/m is prepared by semi-automatic paper machine2Cellulose coiled material.Wherein, cellulose tablet
The drying temperature of material is 85 DEG C, water capacity 7-12%.Refined cotton dregs pulp fibres length is 8mm-12mm, a diameter of 15 μm of -30 μ
m；
Above-mentioned cellulose coiled material is immersed in the sodium peroxydisulfate solution of mass concentration 20%, liquid is taken off and dries；
Impregnated above-mentioned cellulose coiled material is placed in60Under Co gamma-rays, irradiation dose 150kGy；
Cellulose coiled material by irradiation is subjected to fine processing on airslide disintegrating mill.Airflow humidity controls
15%, stream pressure is 1200 kPas, and it is 500 μm -800 μm that fibre length, which is made, a diameter of 2 μm -4 μm of microfine cellulose into
Product.
Comparative example 1
This comparative example provides a kind of preparation method of microfine cellulose, comprises the following steps：
20kg bleaching needle-point leaf pulps are taken, after adding the sodium peroxydisulfate solution of mass concentration 5%, are placed in60Under Co gamma-rays, spoke
It is 60kGy according to dosage；Wherein, bleaching needle-point leaf pulp fibre length is 2mm-4mm, a diameter of 25 μm -50 μm；
Cellulose by irradiation is subjected to fine processing on airslide disintegrating mill.Airflow humidity control is 20%, gas
Flowing pressure is 1200 kPas, and it is 2mm-3mm that fibre length, which is made, a diameter of 25 μm -45 μm of microfine cellulose finished product.
Comparative example 2
This comparative example provides a kind of preparation method of microfine cellulose, comprises the following steps：
20kg bleaching needle-point leaf pulps are taken, 30g/m is prepared by semi-automatic paper machine2Cellulose films.Wherein, cellulose
The drying temperature of sheet material is 90 DEG C.Bleaching needle-point leaf pulp fibre length is 2mm-4mm, a diameter of 25 μm -50 μm；
By the sodium peroxydisulfate solution spraying of mass concentration 5% on above-mentioned cellulose films；
The above-mentioned cellulose films sprayed are placed in60Under Co gamma-rays, irradiation dose 60kGy；
Cellulose films by irradiation are subjected to fine processing on airslide disintegrating mill.Airflow humidity controls
20%, stream pressure is 1200 kPas, and it is 800 μm -950 μm that fibre length, which is made, a diameter of 20 μm -50 μm of microfine cellulose
Finished product.
Comparative example 3
This comparative example provides a kind of preparation method of microfine cellulose, comprises the following steps：
20kg bleaching needle-point leaf pulps are taken, 100g/m is prepared by semi-automatic paper machine2Cellulose films.Wherein, fiber
The drying temperature of cellulose sheet is 85 DEG C, water capacity 7-12%.Bleaching needle-point leaf pulp fibre length is 2mm-4mm, a diameter of 25 μ
m-50μm；
By the sodium peroxydisulfate solution spraying of mass concentration 5% on above-mentioned cellulose films；
The above-mentioned cellulose films sprayed are placed in60Under Co gamma-rays, irradiation dose 60kGy；
Cellulose films by irradiation are subjected to fine processing on airslide disintegrating mill.Airflow humidity controls
20%, stream pressure is 1200 kPas, and it is 1mm-1.5mm that fibre length, which is made, a diameter of 25 μm -50 μm of microfine cellulose into
Product.
The present invention is combined by copy paper technique, RADIATION PROCESSING technique and gas flow crushing process, with pristine fibre element slurry
For raw material, the microfine cellulose being prepared.
In comparative example 1, copy paper technique is not carried out, after causing air-flow crushing, cellulose fine processing effect unobvious.
In comparative example 2, drying temperature is too high in copy paper technique, and after air-flow crushing, fiber is straight after the processing of cellulose fine
Footpath changes unobvious.
In comparative example 3, grammes per square metre is excessive in copy paper technique, and air-flow crushing cellulose is not up to ultra-fine effect.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. a kind of preparation method of microfine cellulose, it is characterised in that comprise the following steps：
Cellulosic material is prepared into cellulose films or cellulose coiled material by copy paper technique；
The cellulose films or cellulose coiled material are handled with radiosensitizer；
Cellulose films or the cellulose coiled material after radiosensitizer is handled is entered in radiation environment with radioactive ray
Row processing；
Cellulose films or the cellulose coiled material after radioactive ray process is subjected to air-flow smashing, obtains microfine cellulose.
2. the preparation method of microfine cellulose according to claim 1, it is characterised in that the cellulosic material is bleaching pin
Leaf wood pulp or bleached hardwood pulp or refined cotton dregs slurry.
3. the preparation method of microfine cellulose according to claim 1, it is characterised in that the technological parameter of the copy paper technique
For：The drying temperature of cellulose films or the cellulose coiled material is not higher than 85 DEG C.
4. the preparation method of microfine cellulose according to claim 3, it is characterised in that obtained by copy paper technique described
The grammes per square metre of cellulose films or cellulose coiled material is 30-80g/m2。
5. the preparation method of microfine cellulose according to claim 1, it is characterised in that the radiosensitizer is Strong oxdiative
Agent, the strong oxidizer are hydrogen peroxide or sodium peroxydisulfate.
6. the preparation method of microfine cellulose according to claim 1, it is characterised in that described to handle institute with radiosensitizer
When stating cellulose films or cellulose coiled material, technique is spraying or dipping.
7. the preparation method of microfine cellulose according to claim 6, it is characterised in that the radioactive ray are gamma-rays or electricity
Beamlet, radiographic source are60Co or137Cs, the dose of radiation of the radioactive ray is 20-300KGy.
8. according to the preparation method of any one of the claim 1-7 microfine celluloses, it is characterised in that the air-flow crushing
Technological parameter is：Airflow humidity is 15%-70%.
9. according to the preparation method of any one of the claim 1-7 microfine celluloses, it is characterised in that the air-flow crushing
Technological parameter is：The operating pressure of airslide disintegrating mill is 500-1200 kPas.
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| CN201710985300.3A CN107641993B (en) | 2017-10-20 | 2017-10-20 | Preparation method of superfine cellulose |
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| CN201710985300.3A CN107641993B (en) | 2017-10-20 | 2017-10-20 | Preparation method of superfine cellulose |
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| CN107641993A true CN107641993A (en) | 2018-01-30 |
| CN107641993B CN107641993B (en) | 2020-01-14 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642945A (en) * | 2018-05-22 | 2018-10-12 | 天马（安徽）国药科技股份有限公司 | A kind of preparation method of superfine notoginseng powder cellulose |
| CN110240253A (en) * | 2019-07-23 | 2019-09-17 | 大连民族大学 | A method of utilizing remaining alkali Heat Treatment purified cotton black liquor |
| CN116253925A (en) * | 2023-03-21 | 2023-06-13 | 西南科技大学 | Gradient irradiation modification method for cotton waste |
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| CN101481424A (en) * | 2009-02-06 | 2009-07-15 | 北京大学 | Ultra-fine microcrystalline cellulose and preparation thereof |
| CN102727393A (en) * | 2012-07-10 | 2012-10-17 | 中国国旅贸易有限责任公司 | Ultra-fine microcrystalline cellulose talcum powder and preparation method of ultra-fine microcrystalline cellulose talcum powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101481424A (en) * | 2009-02-06 | 2009-07-15 | 北京大学 | Ultra-fine microcrystalline cellulose and preparation thereof |
| CN102727393A (en) * | 2012-07-10 | 2012-10-17 | 中国国旅贸易有限责任公司 | Ultra-fine microcrystalline cellulose talcum powder and preparation method of ultra-fine microcrystalline cellulose talcum powder |
Non-Patent Citations (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642945A (en) * | 2018-05-22 | 2018-10-12 | 天马（安徽）国药科技股份有限公司 | A kind of preparation method of superfine notoginseng powder cellulose |
| CN110240253A (en) * | 2019-07-23 | 2019-09-17 | 大连民族大学 | A method of utilizing remaining alkali Heat Treatment purified cotton black liquor |
| CN110240253B (en) * | 2019-07-23 | 2021-11-02 | 大连民族大学 | Method for treating refined cotton black liquor by using residual alkali waste heat |
| CN116253925A (en) * | 2023-03-21 | 2023-06-13 | 西南科技大学 | Gradient irradiation modification method for cotton waste |
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| CN107641993B (en) | 2020-01-14 |
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