CN105131129A - Preparation method for nanocellulose - Google Patents
Preparation method for nanocellulose Download PDFInfo
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Abstract
The invention provides a preparation method for nanocellulose, and belongs to the field of biological nanometer materials. According to the preparation method, the problems that in an existing method, foreign ions cannot be thoroughly removed, the steps are complicated, and the energy consumption is high are solved. The method comprises the steps that firstly, nanocellulose suspension liquid is prepared; secondly, alkaline anion-exchange resin is placed in an ion exchange device, and activity treatment is performed on the alkaline anion-exchange resin; the obtained nanocellulose suspension liquid is poured from an upper opening of the ion exchange device, flows through the alkaline anion-exchange resin processed through activity treatment and flows out from a lower outlet of the ion exchange device, and first treatment liquid is obtained; the ion exchange device is washed with deionized water, and second treatment liquid is obtained; the obtained first treatment liquid and the obtained second treatment liquid are centrifugalized, nanocellulose precipitation is obtained, and after freeze drying is performed, the nanocellulose is obtained. The preparation method is simple and short in time, the cost is saved, foreign ions are not introduced, and the size and property of the nanocellulose are not changed.
Description
Technical field
The invention belongs to biomass nano Material Field, be specifically related to a kind of preparation method of nano-cellulose.
Technical background
As a kind of novel nano meter biomaterial, nano-cellulose is subject to the extensive concern of all circles day by day.Nano-cellulose is defined as at least one dimension size and reaches 1 ~ 100nm, and can disperse the cellulose crystals forming stable suspension in water.Common nano-cellulose is mainly divided into the nano-cellulose of plant origin and the nano-cellulose of non-plant origin.Mineral acid hydrolysis Mierocrystalline cellulose is the important channel obtaining nano-cellulose.Cellulosic pars amorpha can remove by mineral acid hydrolysis, while reduction Microcrystalline Cellulose size, obtains the nano-cellulose of high-crystallinity.Mineral acid used in nano-cellulose preparation process has sulfuric acid, hydrochloric acid, phosphoric acid etc.Wherein sulfuric acid is the most conventional, also have people by sulfuric acid and hydrochloric acid with certain proportion with the use of.Nineteen forty-seven Nickerson and Habrle, at document IndEngChemRes, is raw material with timber in 39 (11) (1947), pp.1507 – 1512, adopts the method for hydrochloric acid and sulfuric acid mixed hydrolysis, prepares nano-cellulose soliquid.Bondeson etc. at document Cellulose, 2006, describe one acid hydrolysis Picea excelsa wood pulp in 13 (2): 171-180, prepare the method for stable nano-cellulose suspension.Gray at Biomacromolecules, 2005,6 (2): 1048-1054 and the document such as Cellulose, 2006,938:26-32 in describe the method that the raw materials such as sulfuric acid solution cotton, wood pulp obtain the nano-cellulose of different qualities in detail.
But the mineral acid solution reported at present prepares the method for nano-cellulose, dispels the process of residual acid in nano-cellulose suspension, there is different problems, and the existence of residual acid can produce material impact to the performance of the nano-cellulose of preparation.Sulfonic existence in such as nano-cellulose, can reduce the thermostability of nano-cellulose.Usual method is washed the low-temperature centrifugation that the nano-cellulose suspension prepared carries out repeatedly.Nanjing Forestry University is in the patent of CN103172886A at application publication number, and provide the detailed step of this method: the suspension after acidolysis, thin up makes hydrolysis reaction stop.Centrifugal remove portion acid solution, distilled water wash, centrifugal several repeatedly, cellulose suspension is filled in dialysis tubing and dialyses, and reaches neutral, to remove remaining acid solution to pH value.The centrifugal rotational speed that this processing mode needs is very high, and workload is large, and length consuming time, energy consumption is high.Guangzhou Inst of Chemistry, Chinese Academy of Sciences is in the patent of CN1141321C at Authorization Notice No., and provide one lower concentration highly basic (such as sodium hydroxide) antacid method, the method is easy to operate, and cost is low.But this method can not remove the acid ion in nano-cellulose, and introduce new foreign ion (such as sodium ion).The nano-cellulose I simultaneously causing acidolysis to obtain changes nano-cellulose II into.Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences is in the patent of CN104448007A at application publication number, providing a kind of formic acid replaces mineral acid to prepare the method for nano-cellulose, and this method solves the removal of inorganic liquid acid and reclaims the problem of difficulty.But this method needs underpressure distillation, and energy consumption is high, and cost is high.
In sum, existing removal mineral acid solution prepares the method for residual acid in nano-cellulose process, main existence thoroughly cannot remove many, consuming time many, the problems such as energy consumption is high of foreign ion, step, so be badly in need of a kind of method that process preparing nano-cellulose to mineral acid solution is optimized.
Summary of the invention
The object of the invention is thoroughly to remove foreign ion, complex steps and the high problem of energy consumption to solve existing method, and a kind of preparation method of nano-cellulose is provided.
The invention provides a kind of preparation method of nano-cellulose, the method comprises:
Step one: prepare nano-cellulose suspension;
Step 2: basic anion exchange resin is put into ion exchange unit, carries out activity process to basic anion exchange resin;
Step 3: nano-cellulose suspension step one obtained is from ion exchange unit impouring suitable for reading, and the basic anion exchange resin of nano-cellulose suspension flow after activity process, exports and flow out, obtain treatment solution I below ion exchange unit;
Step 4: use deionized water rinsing ion exchange unit, obtains treatment solution II;
Step 5: the treatment solution II that the treatment solution I step 3 obtained and step 4 obtain carries out centrifugal, obtains nano-cellulose precipitation, after lyophilize, obtains nano-cellulose.
Preferably, described step one is prepared after cellulosic material mineral acid is carried out acidolysis by nano-cellulose suspension and is obtained.
Preferably, described cellulosic material is selected from the one in Microcrystalline Cellulose, cotton, timber, bamboo wood, stalk, absorbent cotton, wood pulp, straw pulp, bamboo pulp, xylon or bamboo fibers etc.
Preferably, described mineral acid is selected from one or more in sulfuric acid, hydrochloric acid or nitric acid.
Preferably, described basic anion ion exchange resin is strongly basic anion exchange resin and weak base anion-exchange resin.
Preferably, described ion exchange unit is separating funnel.
Preferably, the consumption of the basic anion exchange resin after described activity process is the basic anion exchange resin after every milliliter of nano-cellulose suspension uses the process of 1-10g activity.
Preferably, described carries out activity process to basic anion exchange resin, and concrete steps are:
Step 1: soaked in deionized water by basic anion exchange resin, stirs 3-60 minute, is then filled in ion exchange unit;
Step 2: poured into by sodium chloride solution in ion exchange unit, makes basic anion exchange resin be immersed in sodium chloride solution, soaks after 10-30 hour, releases liquid, then uses deionized water rinsing basic anion exchange resin 2-4 time;
Step 3: poured into by hydrochloric acid soln in ion exchange unit, makes basic anion exchange resin be immersed in hydrochloric acid soln, leaves standstill after 1-4 hour, releases liquid, then with deionized water rinsing to neutral;
Step 4: poured into by sodium hydroxide solution in ion exchange unit, makes basic anion exchange and is immersed in sodium hydroxide solution, leave standstill after 1-4 hour, release liquid, then uses deionized water, rinses to neutral;
Step 5: repeating step 3 and step 4,2-4 time, namely obtains activated basic anionite-exchange resin.
Beneficial effect of the present invention
The invention provides a kind of preparation method of nano-cellulose, the method is the method utilizing basic anion exchange resin to dispel acid hydrolyzation to prepare nano-cellulose residual acid, and the method makes full use of activated basic anionite-exchange resin to SO in liquid
4 2-, Cl
-, NO
3 -isoionic absorption, and go out OH at dissociation in water
-, realize dispelling of residual acid in nano-cellulose suspension prepared by acid hydrolyzation, and basic anion exchange resin can reuse process nano-cellulose suspension.Compare with prior art, the inventive method adopts simple deacidite removing mineral acid solution to prepare the method for residual acid in nano-cellulose suspension process, step is simple, decrease the time of preparing nano-cellulose, reduce energy consumption simultaneously, provide cost savings, and do not introduce foreign ion, also do not change size and the character of nano-cellulose.
Accompanying drawing explanation
Fig. 1 is the TEM picture of nano-cellulose prepared by the nano-cellulose prepared of the embodiment of the present invention 1 and traditional method.
Fig. 2 is the infrared spectrum of nano-cellulose prepared by the nano-cellulose prepared of the embodiment of the present invention 1 and traditional method.
Embodiment
Below in conjunction with specific embodiments technical scheme of the present invention is described in further detail.Object is to make those skilled in the art have understanding and cognition clearly to the application.Following specific embodiment should not be understood or be interpreted as the restriction to the application's claims request protection domain in any degree.
The invention provides a kind of preparation method of nano-cellulose, the method comprises:
Step one: prepare nano-cellulose suspension;
Step 2: basic anion exchange resin is put into ion exchange unit, carries out activity process to basic anion exchange resin;
Step 3: nano-cellulose suspension step one obtained is from ion exchange unit impouring suitable for reading, and the basic anion exchange resin of nano-cellulose suspension flow after activity process, exports and flow out, obtain treatment solution I below ion exchange unit;
Step 4: use deionized water rinsing ion exchange unit, obtains treatment solution II;
Step 5: the treatment solution II that the treatment solution I step 3 obtained and step 4 obtain carries out centrifugal, obtains nano-cellulose precipitation, after lyophilize, obtains nano-cellulose.
According to the present invention, obtain after cellulosic material mineral acid is carried out acidolysis by the described method preparing nano-cellulose suspension, concrete steps are preferably: cellulosic material is put into inorganic acid solution, at 45-60 DEG C, reacts 3-6 hour, after reaction terminates, by solution in deionized water, prevent it from continuing hydrolysis, remove supernatant liquor after leaving standstill, add deionized water, repeat to leave standstill process 3-5 time except supernatant liquor, after finally adding deionized water, obtain nano-cellulose suspension; Described cellulosic material is preferably selected from the one in Microcrystalline Cellulose, cotton, linters, timber, bamboo wood, stalk, absorbent cotton, wood pulp, straw pulp, bamboo pulp, xylon or bamboo fibers etc., and described mineral acid is preferably selected from one or more in sulfuric acid, hydrochloric acid or nitric acid.
According to the present invention, basic anion exchange resin is put into ion exchange unit, activity process is carried out to basic anion exchange resin; Described does not have particular requirement to ion exchange unit, available any container with coutroi velocity device, preferred commercial separating funnel; Described basic anion ion exchange resin preferably includes strongly basic anion exchange resin or weak base anion-exchange resin, is not particularly limited, and can be any model bought.Be more preferably strong base #201 (resin processing plant of Nankai University), strong base 717, strong base 201*7 (Shanghai Resin Factory), AmerliteXE-98, AmerliteIRA-400, Dowex1, Dowex2, LewatitMII, weak base 330 (Shanghai Resin Factory), weak base #301 (resin processing plant of Nankai University), AmerliteIR-4B, Dowex3, PermutitW or WofatitM, most preferably be strong base #201 (resin processing plant of Nankai University), strong base 717, strong base 201*7 (Shanghai Resin Factory), AmerliteXE-98, AmerliteIRA-400, Dowex1, Dowex2, LewatitMII.
Described carries out activity process to basic anion exchange resin, and concrete steps are:
Step 1, soaked in deionized water the basic anion exchange resin that weighs, make it fully expand, after mechanical stirring 3-60 minute, the impurity that removing suspends and resin in small, broken bits, be filled in the basic anion exchange resin cleaned in ion exchange unit;
Step 2, sodium chloride solution is poured in ion exchange unit, make basic anion exchange resin be immersed in sodium chloride solution, soak after 10-30 hour, release liquid, then use deionized water rinsing basic anion exchange resin 2-4 time; The mass concentration of described sodium chloride solution is preferably 2%-10%;
Step 3, hydrochloric acid soln is poured in ion exchange unit, basic anion exchange resin is made to be immersed in hydrochloric acid soln, leave standstill after 1-4 hour, release liquid, in switch, rinse the basic anion exchange resin of above-mentioned process to neutral with deionized water, the massfraction of described hydrochloric acid soln is preferably 2%-5% again;
Step 4, sodium hydroxide solution are poured in ion exchange unit, basic anion exchange resin is made to be immersed in sodium hydroxide solution, leave standstill after 1-4 hour, release liquid, then in switch, rinse the basic anion exchange resin of above-mentioned process to neutral with deionized water, the massfraction of described sodium hydroxide is preferably 2%-5%;
Step 5, repeating step 3 and step 4,2-4 time, namely obtain activated basic anionite-exchange resin.
According to the present invention, by the nano-cellulose suspension that obtains slowly from ion exchange unit impouring suitable for reading, the basic anion exchange resin of nano-cellulose suspension flow after activity process, below ion exchange unit, outlet is flowed out, and obtains treatment solution I; The consumption of activated basic anionite-exchange resin is the deacidite that every milliliter of nano-cellulose suspension uses 1-10g drying.
According to the present invention, use deionized water rinsing ion exchange unit, to clean out wherein residual nano-cellulose, obtain treatment solution II;
According to the present invention, the treatment solution I obtained and treatment solution II are carried out centrifugal, water unnecessary in removing treatment solution, obtain nano-cellulose precipitation, after lyophilize, obtain nano-cellulose.
According to the present invention, described activated basic anionite-exchange resin can carry out processing rear recycling, and continue process nano-cellulose suspension, the concrete steps of process are:
1, pour in ion exchange unit with the sodium chloride solution that mass concentration is 2%-10%, make activated basic anionite-exchange resin be immersed in sodium chloride solution, soak after 10-30 hour, release liquid, then use deionized water rinsing exchange resin 2-4 time;
2, be that 2%-5% sodium hydroxide solution is poured in ion exchange unit by massfraction, exchange resin is made to be immersed in sodium hydroxide solution, leave standstill after 1-4 hour, release liquid, then with deionized water, the deacidite of above-mentioned process is rinsed to neutral in switch, be reusable deacidite.
Below in conjunction with embodiment, the present invention will be further described in detail.
Embodiment 1
(1) micrometer fibers element 1g being of a size of 20 microns is added in the 10ml sulphuric acid soln prepared, and wherein the massfraction of sulfuric acid is 64%, and stirred suspension is also heated to 45 DEG C, reacts 3 hours; After reaction terminates, solution is poured in the deionized water of 50ml, prevent it from continuing hydrolysis, supernatant liquor is removed after leaving standstill, 60 milliliters of nano-cellulose suspension are obtained after adding deionized water, repeat to leave standstill process 3-5 time except supernatant liquor, after finally adding deionized water, obtain 60 milliliters of nano-cellulose suspension;
(2) 600g strongly basic anion exchange resin 717 is put into the separating funnel of 1000ml, activity process is carried out to strongly basic anion exchange resin 717;
(3) by pending nano-cellulose suspension lentamente from the separating funnel impouring suitable for reading that active strongly basic anion exchange resin 717 is housed, nano-cellulose suspension flow is after active strongly basic anion exchange resin 717, export outflow from below, obtain treatment solution I;
(4) continue to use the active strongly basic anion exchange resin 717 of the deionized water rinsing of 20% of nano-cellulose suspension vol, to clean out wherein residual nano-cellulose, obtain treatment solution II;
(5) treatment solution I and treatment solution II are carried out centrifugal, water unnecessary in removing treatment solution, obtain nano-cellulose precipitation, after lyophilize, obtain white powder, be nano-cellulose.
Nano-cellulose embodiment 1 obtained and the nano-cellulose adopting traditional method to prepare characterize, described traditional method obtains nano-cellulose suspension by sulphuric acid hydrolysis micrometer fibers element, the experiment condition specifically prepared in the experiment condition of nano-cellulose suspension and embodiment 1 is completely the same, then suspension is centrifugal, dialysis successively, lyophilize obtain nano-cellulose.
The evidence that the nano-cellulose deacidification effect that the embodiment of the present invention 1 obtains is consistent with the deacidification effect of traditional method is that the pH value of the dispersion liquid after the nano-cellulose prepared by measuring above-mentioned two kinds of methods dissolves in water carries out.The concrete implementation step measuring nano-cellulose dispersion liquid pH value is as follows:
(1) nano-cellulose prepared by the nano-cellulose prepared by the embodiment of the present invention 1 by 0.01g respectively and traditional method is placed in 40ml water, after stirring ultrasonic 15 minutes, obtains nano-cellulose dispersion liquid.
(2) use PH tester to measure the pH value of nano-cellulose dispersion liquid prepared by above-mentioned (1) respectively, test result is in table one.
Result shows, and nano-cellulose dispersion liquid pH value prepared by two kinds of methods is close, and difference is 0.02.Consider the test error of instrument, can reach a conclusion, the nano-cellulose dispersion liquid prepared of the inventive method and the conventional centrifugal nano-cellulose dispersion liquid acid content prepared of dialysing is consistent, namely prepare in nano-cellulose process, the inventive method except residual acid effect with traditional through centrifugal, the effect of removing the acid remained of dialyse is consistent.And the crystal habit of nano-cellulose and size are not affected.Fig. 1 is the TEM picture of nano-cellulose prepared by the nano-cellulose prepared of the embodiment of the present invention 1 and traditional method.As we know from the figure, nano-cellulose consistent size prepared by two kinds of different treatment methods, length is 100-200 nanometer, and diameter is for being less than 100 nanometers, and the nano-cellulose that above-mentioned two kinds of different treatment methods obtain is all bar-shaped.
The evidence that the structure of above-mentioned two kinds of nano-celluloses is consistent uses Fourier transform infrared (FT-IR) to carry out.Fig. 2 is the infrared spectrum of nano-cellulose prepared by the nano-cellulose prepared of the embodiment of the present invention 1 and traditional method, Fig. 2 can find out, each peak of the nano-cellulose that the inventive method process obtains and the nano-cellulose obtained by centrifugal, dialysis treatment in position and the intensity at peak be identical.
Using plasma emission spectrometer (ICP) proves that the embodiment of the present invention 1 method and traditional method, sodium hydroxide neutralization method are prepared nano-cellulose and compared and do not introduce new impurity.Wherein, in sodium hydroxide with the method preparing nano-cellulose be, nano-cellulose suspension is obtained by sulphuric acid hydrolysis micrometer fibers element, the experiment condition specifically prepared in the experiment condition of nano-cellulose suspension and embodiment 1 is completely the same, again with in sodium hydroxide solution instillation nano-cellulose suspension, to nano-cellulose suspension PH=7, after centrifugal, obtain nano-cellulose through lyophilize.
(1) getting 0.01g is respectively placed in 40ml water by the nano-cellulose that embodiment 1 method, traditional method and sodium hydroxide neutralization method prepare, and after stirring, ultrasonic 15 minutes, after leaving standstill, gets 15ml supernatant liquor;
(2) respectively ultimate analysis is carried out to the supernatant liquor that three kinds of methods obtain by ICP.Test result is in table 1.
As known from Table 1, use the method for sodium hydroxide neutralization to prepare nano-cellulose, introduce impurity-sodium element.And in nano-cellulose prepared by the inventive method and the nano-cellulose that logical traditional method obtains, do not introduce impurity element.
Table 1
| Sulphur | Carbon | Other | PH | |
| The nano-cellulose that embodiment 1 obtains | Have | Have | Nothing | 6.78 |
| The nano-cellulose that traditional method obtains | Have | Have | Nothing | 6.76 |
| The nanofiber that sodium hydroxide neutralizing treatment obtains | Have | Have | Sodium | - |
Embodiment 2
(1) micrometer fibers element 1g being of a size of 50 microns is added in the 18ml sulphuric acid soln prepared, and wherein the massfraction of sulfuric acid is 64%, and stirred suspension is also heated to 45 DEG C, reacts 3 hours; After reaction terminates, solution is poured in the deionized water of 90ml, prevent it from continuing hydrolysis, supernatant liquor is removed after leaving standstill, 108 milliliters of nano-cellulose suspension are obtained after adding deionized water, repeat to leave standstill process 3-5 time except supernatant liquor, after finally adding deionized water, obtain 108ml nano-cellulose suspension;
(2) by the separating funnel that 108g strongly basic anion exchange resin #201 puts into, activity process is carried out to basic anion exchange resin;
(3) by pending nano-cellulose suspension lentamente from the separating funnel impouring suitable for reading that active strongly basic anion exchange resin #201 is housed, nano-cellulose suspension flow is after active strongly basic anion exchange resin #201, export outflow from below, obtain treatment solution I;
(4) continue to use the active strongly basic anion exchange resin #201 of the deionized water rinsing of 20% of nano-cellulose suspension vol, to clean out wherein residual nano-cellulose, obtain treatment solution II;
(5) treatment solution I and treatment solution II are carried out centrifugal, water unnecessary in removing treatment solution, obtain nano-cellulose precipitation, after lyophilize, obtain white powder, be nano-cellulose.
Embodiment 3
(1) will cleaning and dried 10g linters is added in the 85ml sulphuric acid soln prepared, wherein the volume fraction of sulfuric acid is 30%, and stirred suspension is also heated to 60 DEG C, reacts 6 hours; After reaction terminates, solution is poured in the deionized water of 425ml, prevent it from continuing hydrolysis, supernatant liquor is removed after leaving standstill, 510 milliliters of nano-cellulose suspension are obtained after adding deionized water, repeat to leave standstill process 3-5 time except supernatant liquor, after finally adding deionized water, obtain the nano-cellulose suspension of 510ml;
(2) 2500g strongly basic anion exchange resin 717 is put into separating funnel, activity process is carried out to basic anion exchange resin;
(3) by pending nano-cellulose suspension lentamente from the separating funnel impouring suitable for reading that active strongly basic anion exchange resin 717 is housed, nano-cellulose suspension flow is after active strongly basic anion exchange resin 717, export outflow from below, obtain treatment solution I;
(4) continue to use the active strongly basic anion exchange resin 717 of the deionized water rinsing of 20% of nano-cellulose suspension vol, to clean out wherein residual nano-cellulose, obtain treatment solution II;
(5) treatment solution I and treatment solution II are carried out centrifugal, water unnecessary in removing treatment solution, obtain nano-cellulose precipitation, after lyophilize, obtain white powder, be nano-cellulose.
Embodiment 4
(1) 2g bamboo pulp added in the 100ml sulphuric acid soln prepared, wherein the massfraction of sulfuric acid is 46%, and stirred suspension is also heated to 45 DEG C, reacts 4 hours; After reaction terminates, solution is poured in 500ml deionized water, prevent it from continuing hydrolysis, supernatant liquor is removed after leaving standstill, 600 milliliters of nano-cellulose suspension are obtained after adding deionized water, repeat to leave standstill process 3-5 time except supernatant liquor, after finally adding deionized water, obtain 600ml nano-cellulose suspension;
(2) 1800g strongly basic anion exchange resin 717 is put into separating funnel, activity process is carried out to basic anion exchange resin;
(3) by pending nano-cellulose suspension lentamente from the separating funnel impouring suitable for reading that active strongly basic anion exchange resin 717 is housed, nano-cellulose suspension flow is after active strongly basic anion exchange resin 717, export outflow from below, obtain treatment solution I;
(4) continue to use the active strongly basic anion exchange resin 717 of the deionized water rinsing of 20% of nano-cellulose suspension vol, to clean out wherein residual nano-cellulose, obtain treatment solution II;
(5) treatment solution I and treatment solution II are carried out centrifugal, water unnecessary in removing treatment solution, obtain nano-cellulose precipitation, after lyophilize, obtain white powder, be nano-cellulose.
Claims (8)
1. a preparation method for nano-cellulose, is characterized in that, the method comprises:
Step one: prepare nano-cellulose suspension;
Step 2: basic anion exchange resin is put into ion exchange unit, carries out activity process to basic anion exchange resin;
Step 3: nano-cellulose suspension step one obtained is from ion exchange unit impouring suitable for reading, and the basic anion exchange resin of nano-cellulose suspension flow after activity process, exports and flow out, obtain treatment solution I below ion exchange unit;
Step 4: use deionized water rinsing ion exchange unit, obtains treatment solution II;
Step 5: the treatment solution II that the treatment solution I step 3 obtained and step 4 obtain carries out centrifugal, obtains nano-cellulose precipitation, after lyophilize, obtains nano-cellulose.
2. the preparation method of a kind of nano-cellulose according to claim 1, is characterized in that, described step one is prepared after cellulosic material mineral acid is carried out acidolysis by nano-cellulose suspension and obtained.
3. the preparation method of a kind of nano-cellulose according to claim 2, it is characterized in that, described cellulosic material is selected from the one in Microcrystalline Cellulose, cotton, linters, timber, bamboo wood, stalk, absorbent cotton, wood pulp, straw pulp, bamboo pulp, xylon or bamboo fibers.
4. the preparation method of a kind of nano-cellulose according to claim 2, is characterized in that, described mineral acid is selected from one or more in sulfuric acid, hydrochloric acid or nitric acid.
5. the preparation method of a kind of nano-cellulose according to claim 1, is characterized in that, described basic anion ion exchange resin is strongly basic anion exchange resin and weak base anion-exchange resin.
6. the preparation method of a kind of nano-cellulose according to claim 1, is characterized in that, described ion exchange unit is separating funnel.
7. the preparation method of a kind of nano-cellulose according to claim 1, is characterized in that, the consumption of the basic anion exchange resin after active process is the basic anion exchange resin after every milliliter of nano-cellulose suspension uses the process of 1-10g activity.
8. the preparation method of a kind of nano-cellulose according to claim 1, is characterized in that, described carries out activity process to basic anion exchange resin, and concrete steps are:
Step 1: soaked in deionized water by basic anion exchange resin, stirs 3-60 minute, is then filled in ion exchange unit;
Step 2: poured into by sodium chloride solution in ion exchange unit, makes basic anion exchange resin be immersed in sodium chloride solution, soaks after 10-30 hour, releases liquid, then uses deionized water rinsing basic anion exchange resin 2-4 time;
Step 3: poured into by hydrochloric acid soln in ion exchange unit, makes basic anion exchange resin be immersed in hydrochloric acid soln, leaves standstill after 1-4 hour, releases liquid, then with deionized water rinsing to neutral;
Step 4: poured into by sodium hydroxide solution in ion exchange unit, makes basic anion exchange and is immersed in sodium hydroxide solution, leave standstill after 1-4 hour, release liquid, then uses deionized water, rinses to neutral;
Step 5: repeating step 3 and step 4,2-4 time, namely obtains activated basic anionite-exchange resin.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106106720A (en) * | 2016-06-27 | 2016-11-16 | 郭迎庆 | A kind of antibacterial degradable loofah fiber membrane preparation method |
| CN109970873A (en) * | 2019-04-03 | 2019-07-05 | 湖南九典宏阳制药有限公司 | A kind of preparation method of pharmaceutic adjuvant grade microcrystalline cellulose |
| CN110284352A (en) * | 2019-05-29 | 2019-09-27 | 浙江金昌特种纸股份有限公司 | A kind of bamboo wood nano-cellulose preparation method of super clean |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740341A (en) * | 2005-09-15 | 2006-03-01 | 陈秀恋 | Decolour and refining apparatus for ion exchange method of sugar cane juice |
| CN101709336A (en) * | 2009-12-21 | 2010-05-19 | 安徽丰原发酵技术工程研究有限公司 | Method for preparing high-concentration fructose syrup |
| CN101768221A (en) * | 2010-03-12 | 2010-07-07 | 福建农林大学 | Method for preparing nano-crystal cellulose II by using basic anion-exchange resin |
| CN101942102A (en) * | 2010-09-07 | 2011-01-12 | 东南大学 | Preparation method of powder nano cellulose |
| CN103172886A (en) * | 2013-03-14 | 2013-06-26 | 南京林业大学 | Method for quickly preparing colorful nanocrystalline cellulose film |
-
2015
- 2015-10-12 CN CN201510654764.7A patent/CN105131129B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740341A (en) * | 2005-09-15 | 2006-03-01 | 陈秀恋 | Decolour and refining apparatus for ion exchange method of sugar cane juice |
| CN101709336A (en) * | 2009-12-21 | 2010-05-19 | 安徽丰原发酵技术工程研究有限公司 | Method for preparing high-concentration fructose syrup |
| CN101768221A (en) * | 2010-03-12 | 2010-07-07 | 福建农林大学 | Method for preparing nano-crystal cellulose II by using basic anion-exchange resin |
| CN101942102A (en) * | 2010-09-07 | 2011-01-12 | 东南大学 | Preparation method of powder nano cellulose |
| CN103172886A (en) * | 2013-03-14 | 2013-06-26 | 南京林业大学 | Method for quickly preparing colorful nanocrystalline cellulose film |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106106720A (en) * | 2016-06-27 | 2016-11-16 | 郭迎庆 | A kind of antibacterial degradable loofah fiber membrane preparation method |
| CN109970873A (en) * | 2019-04-03 | 2019-07-05 | 湖南九典宏阳制药有限公司 | A kind of preparation method of pharmaceutic adjuvant grade microcrystalline cellulose |
| CN109970873B (en) * | 2019-04-03 | 2021-06-18 | 湖南九典宏阳制药有限公司 | Preparation method of pharmaceutical adjuvant grade microcrystalline cellulose |
| CN110284352A (en) * | 2019-05-29 | 2019-09-27 | 浙江金昌特种纸股份有限公司 | A kind of bamboo wood nano-cellulose preparation method of super clean |
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