CN107460759A - A kind of method for quickly purifying of nano-cellulose suspension - Google Patents
A kind of method for quickly purifying of nano-cellulose suspension Download PDFInfo
- Publication number
- CN107460759A CN107460759A CN201710709661.5A CN201710709661A CN107460759A CN 107460759 A CN107460759 A CN 107460759A CN 201710709661 A CN201710709661 A CN 201710709661A CN 107460759 A CN107460759 A CN 107460759A
- Authority
- CN
- China
- Prior art keywords
- nano
- cellulose suspension
- cellulose
- ammonium
- carbonate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229920002678 cellulose Polymers 0.000 title claims abstract description 66
- 239000001913 cellulose Substances 0.000 title claims abstract description 66
- 239000000725 suspension Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 41
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 21
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 21
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005119 centrifugation Methods 0.000 claims abstract description 13
- 150000002500 ions Chemical class 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 238000007710 freezing Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 3
- 238000002242 deionisation method Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000000502 dialysis Methods 0.000 abstract description 6
- 239000003643 water by type Substances 0.000 abstract description 4
- 239000013081 microcrystal Substances 0.000 abstract description 2
- 239000000084 colloidal system Substances 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- PRKQVKDSMLBJBJ-UHFFFAOYSA-N ammonium carbonate Chemical class N.N.OC(O)=O PRKQVKDSMLBJBJ-UHFFFAOYSA-N 0.000 description 1
- 235000011162 ammonium carbonates Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of method for quickly purifying of nano-cellulose suspension.This method adds ammonium hydrogen carbonate or ammonium carbonate in nano-cellulose suspension precipitates nano-cellulose, removes the former foreign ion in nano-cellulose after repeatedly centrifuging.Ammonium hydrogen carbonate or ammonium carbonate are decomposed into gas with the method for heating again to escape, obtain pure nano-cellulose suspension.The present invention adds ammonium hydrogen carbonate or ammonium carbonate in nano-cellulose suspension, destroys the stable colloid state of nano-cellulose suspension, nano-cellulose precipitation is separated with the former foreign ion in supernatant by centrifugation.The ammonium hydrogen carbonate or ammonium carbonate being newly introduced into can be decomposed into gas effusion by simple heating means from fibrous suspension, obtain the nano-cellulose suspension of high-purity.This purification process can also replace sour water solution to prepare the dialysis procedure during nano micro crystal cellulose, not only saved a large amount of high purity waters of dialysis procedure needs, also saved the dialysis of 37 days and take.
Description
Technical field
The invention belongs to natural macromolecular material field, and in particular to a kind of fast purifying side of nano-cellulose suspension
Method.
Background technology
Due to the microsize of nano-cellulose, therefore the ion adulterated in nano-cellulose can not be by filtering or centrifuging
Method remove.Now, the general method using dialysis removes the foreign ion in nano-cellulose suspension, and this method both needed
Substantial amounts of high purity water is wanted, but it is very time-consuming.For example, traditional sour water solution prepares nano-cellulose process, it is necessary to after to sour water solution
The long-time that is carried out 3-7 days with a large amount of high purity waters of slurry dialyse, to remove the ion remained in fibre stuff after sour water solution.Both
It is time-consuming, the waste of a large amount of high purity waters is caused again.
The content of the invention
For overcome the deficiencies in the prior art, the invention provides a kind of fast purifying side of nano-cellulose suspension
Method, i.e., ammonium hydrogen carbonate or ammonium carbonate are added in nano-cellulose suspension, destroy the stable glue of nano-cellulose suspension
Body state, it can be isolated and purified with simple centrifugal method.The ammonium hydrogen carbonate or ammonium carbonate of introducing can be boiled using heating
The method of boiling itself is decomposed into gas effusion, and the nano-cellulose suspension of high-purity is made.
The present invention is achieved through the following technical solutions.
A kind of method for quickly purifying of nano-cellulose suspension, comprises the following steps：
（1）Ammonium hydrogen carbonate or ammonium carbonate are added in cellulose suspension, is well mixed, obtains mixed liquor；
（2）With high speed freezing centrifuge centrifugation step（1）Gained mixed liquor, the Cellulose precipitates for taking centrifugation to obtain, uses deionization
Centrifuged after repeatedly addition ammonium hydrogen carbonate or ammonium carbonate are well mixed after water dilution, centrifugation is repeated several times, up to former foreign ion is gone
Except clean；
（3）It will centrifuge for the last time after obtained precipitation dilutes with deionized water, heating is boiled, and makes ammonium hydrogen carbonate or ammonium carbonate complete
It is complete to be decomposed into gas effusion, then the nano-cellulose suspension of high-purity can be made.
Preferably, step（1）The cellulose suspension is nano-cellulose suspension or can not pass through the commonly side of centrifugation
The cellulose suspension of method precipitation separation.
Preferably, step（1）The dosage of the ammonium hydrogen carbonate or ammonium carbonate is the 0.5%-3% of cellulose suspension quality.
Preferably, step（2）The rotating speed of the high speed freezing centrifuge is 4000-12000rpm.
Preferably, step（2）In time for centrifuging every time be 5-30min.
Preferably, step（2）The number of the repeated centrifugation is 4-6 times.
Preferably, step（3）It is 20- that the ammonium hydrogen carbonate or ammonium carbonate decompose heating boiling time used completely
120min。
Preferably, step（3）In the electrical conductivity of nano-cellulose suspension after purification be less than 800us/cm.
Preferably, a kind of method for quickly purifying of nano-cellulose suspension, specifically includes following steps：
Nano-cellulose suspension quality 0.5%-3% ammonium hydrogen carbonate or ammonium carbonate is added in nano-cellulose suspension, is mixed
After closing uniformly, 5-30min is centrifuged under 4000-12000rpm with high speed freezing centrifuge.The Cellulose precipitates that centrifugation obtains are taken,
Repeat to centrifuge after adding ammonium hydrogen carbonate or ammonium carbonate mixing mixing after being diluted with deionized water.The centrifugal process is repeated several times, directly
Removed to former foreign ion clean.It will centrifuge for the last time after obtained precipitation dilutes with deionized water, 20- is boiled in heating
The 120min times, ammonium hydrogen carbonate or ammonium carbonate is set to be completely decomposed into gas effusion, then the nano-cellulose that high-purity can be made hangs
Supernatant liquid.
Compared with prior art, the present invention has advantages below and beneficial effect：
In the inventive method, the foreign ion in nano-cellulose suspension can be removed by simple and quick centrifugal method.Compared with
The dialysis process generally used now, had both saved a large amount of high purity waters, and had saved the dialysis of 3-7 days again and take, and had very strong
Economic value and practical value.
Embodiment
The specific implementation to the present invention is further described with reference to embodiments, but embodiments of the present invention are unlimited
In this.
Embodiment 1
100g by plant fiber material through the concentrated sulfuric acid hydrolyze and use in alkali and after fibrous suspension（Concentration is 5wt%, conductance
Rate is 50ms/cm）In, add 1.75g ammonium hydrogen carbonate and be well mixed.Centrifuged with high speed freezing centrifuge under 4000rpm
10min, repeats the centrifugal process 6 times.Deionized water 100ml is added in obtained Cellulose precipitates, boils 20min（Period
Water is continuously replenished, maintains 100ml liquid levels）, you can obtain the cellulose suspension of high-purity.
The electrical conductivity of high purity cellulose suspension made from the present embodiment is 600us/cm, illustrates that nano-cellulose suspends
Foreign ion in liquid can quickly and easily be removed by the purification process of the present invention.
Embodiment 2
In the nano micro crystal cellulose suspension that 100g concentration is 2 wt% NaCl containing 3g（Electrical conductivity is 55ms/cm）In, add
3g ammonium hydrogen carbonate is well mixed.10min is centrifuged under 12000rpm with high speed freezing centrifuge, repeats the centrifugal process 5 times.
Deionized water 300ml is added in obtained Cellulose precipitates, boils 120min（Water is continuously replenished in period, maintains 300ml liquid
Position）, you can obtain the cellulose suspension of high-purity.
The electrical conductivity of high purity cellulose suspension made from the present embodiment is 150us/cm, illustrates that nano-cellulose suspends
Foreign ion in liquid can quickly and easily be removed by the purification process of the present invention.
Embodiment 3
Obtained nano-cellulose suspension is aoxidized in the TEMPO that 100g concentration is 1 wt% NaCl containing 1g（Electrical conductivity is 20ms/
cm）In, add 0.5g ammonium carbonates and be well mixed.10min is centrifuged under 8000rpm with high speed freezing centrifuge, repeats the centrifugation
Process 4 times.Deionized water 200ml is added in obtained Cellulose precipitates, boils 70min（Water is continuously replenished in period, maintains
200ml liquid levels）, you can obtain the cellulose suspension of high-purity.
The electrical conductivity of high purity cellulose suspension made from the present embodiment is 80.5us/cm, illustrates that nano-cellulose hangs
Foreign ion in supernatant liquid can quickly and easily be removed by the purification process of the present invention.
Claims (8)
1. a kind of method for quickly purifying of nano-cellulose suspension, it is characterised in that comprise the following steps：
（1）Ammonium hydrogen carbonate or ammonium carbonate are added in cellulose suspension, is well mixed, obtains mixed liquor；
（2）With high speed freezing centrifuge centrifugation step（1）Gained mixed liquor, the Cellulose precipitates for taking centrifugation to obtain, uses deionization
Centrifuged after repeatedly addition ammonium hydrogen carbonate or ammonium carbonate are well mixed after water dilution, centrifugation is repeated several times, up to former foreign ion is gone
Except clean；
（3）It will centrifuge for the last time after obtained precipitation dilutes with deionized water, heating is boiled, and makes ammonium hydrogen carbonate or ammonium carbonate complete
It is complete to be decomposed into gas effusion, then the nano-cellulose suspension of high-purity can be made.
A kind of 2. method for quickly purifying of nano-cellulose suspension according to claim 1, it is characterised in that step
（1）The cellulose suspension is nano-cellulose suspension or can not hanged by the cellulose that common precipitated by centrifugation separates
Supernatant liquid.
A kind of 3. method for quickly purifying of nano-cellulose suspension according to claim 1, it is characterised in that step
（1）The dosage of the ammonium hydrogen carbonate or ammonium carbonate is the 0.5%-3% of cellulose suspension quality.
A kind of 4. method for quickly purifying of nano-cellulose suspension according to claim 1, it is characterised in that step
（2）The rotating speed of the high speed freezing centrifuge is 4000-12000rpm.
A kind of 5. method for quickly purifying of nano-cellulose suspension according to claim 1, it is characterised in that step
（2）In time for centrifuging every time be 5-30min.
A kind of 6. method for quickly purifying of nano-cellulose suspension according to claim 1, it is characterised in that step
（2）The number of the repeated centrifugation is 4-6 times.
A kind of 7. method for quickly purifying of nano-cellulose suspension according to claim 1, it is characterised in that step
（3）It is 20-120min that the ammonium hydrogen carbonate or ammonium carbonate decompose heating boiling time used completely.
A kind of 8. method for quickly purifying of nano-cellulose suspension according to claim 1, it is characterised in that step
（3）In the electrical conductivity of nano-cellulose suspension after purification be less than 800us/cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710709661.5A CN107460759B (en) | 2017-08-18 | 2017-08-18 | Rapid purification method of nano-cellulose suspension |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710709661.5A CN107460759B (en) | 2017-08-18 | 2017-08-18 | Rapid purification method of nano-cellulose suspension |
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| Publication Number | Publication Date |
|---|---|
| CN107460759A true CN107460759A (en) | 2017-12-12 |
| CN107460759B CN107460759B (en) | 2020-12-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710709661.5A Expired - Fee Related CN107460759B (en) | 2017-08-18 | 2017-08-18 | Rapid purification method of nano-cellulose suspension |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165094A (en) * | 2017-12-15 | 2018-06-15 | 华南理工大学 | A kind of nano-cellulose base pen core aqueous ink and preparation method thereof |
| CN109457524A (en) * | 2018-12-29 | 2019-03-12 | 珠海市东辰制药有限公司 | The purification process and purifier apparatus of nano micro crystal cellulose |
| JP2019038970A (en) * | 2017-08-29 | 2019-03-14 | 東亞合成株式会社 | Method for producing cellulose nanofiber powder |
| CN109609036A (en) * | 2018-12-06 | 2019-04-12 | 武汉科丝力纤维制造有限公司 | A kind of environment-friendly modified foamed ceramics adhesive and its preparation process |
| CN110656526A (en) * | 2019-10-08 | 2020-01-07 | 齐鲁工业大学 | Method for preparing nano-cellulose from fiber slurry |
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Cited By (8)
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|---|---|---|---|---|
| JP2019038970A (en) * | 2017-08-29 | 2019-03-14 | 東亞合成株式会社 | Method for producing cellulose nanofiber powder |
| CN108165094A (en) * | 2017-12-15 | 2018-06-15 | 华南理工大学 | A kind of nano-cellulose base pen core aqueous ink and preparation method thereof |
| CN108165094B (en) * | 2017-12-15 | 2021-07-16 | 华南理工大学 | Nano cellulose-based pen core water-based ink and preparation method thereof |
| CN109609036A (en) * | 2018-12-06 | 2019-04-12 | 武汉科丝力纤维制造有限公司 | A kind of environment-friendly modified foamed ceramics adhesive and its preparation process |
| CN109457524A (en) * | 2018-12-29 | 2019-03-12 | 珠海市东辰制药有限公司 | The purification process and purifier apparatus of nano micro crystal cellulose |
| CN109457524B (en) * | 2018-12-29 | 2023-10-20 | 珠海市东辰制药有限公司 | Purification method and purification equipment of nano microcrystalline cellulose |
| CN110656526A (en) * | 2019-10-08 | 2020-01-07 | 齐鲁工业大学 | Method for preparing nano-cellulose from fiber slurry |
| CN110656526B (en) * | 2019-10-08 | 2021-10-01 | 齐鲁工业大学 | Method for preparing nano-cellulose from fiber slurry |
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| CN107460759B (en) | 2020-12-22 |
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