CN106824235B - A kind of poplar slab dissolving pulp prepares the acid catalyst of ultra-fine microcrystalline cellulose and prepares the method for ultra-fine microcrystalline cellulose - Google Patents
A kind of poplar slab dissolving pulp prepares the acid catalyst of ultra-fine microcrystalline cellulose and prepares the method for ultra-fine microcrystalline cellulose Download PDFInfo
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- 235000019813 microcrystalline cellulose Nutrition 0.000 title claims abstract description 66
- 229920000168 Microcrystalline cellulose Polymers 0.000 title claims abstract description 63
- 229920000875 Dissolving pulp Polymers 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 40
- 241000219000 Populus Species 0.000 title claims abstract description 37
- 239000008108 microcrystalline cellulose Substances 0.000 title claims abstract description 33
- 229940016286 microcrystalline cellulose Drugs 0.000 title claims abstract description 33
- 239000003377 acid catalyst Substances 0.000 title claims abstract description 26
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000007171 acid catalysis Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000007670 refining Methods 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims 1
- 239000008107 starch Substances 0.000 claims 1
- 235000019698 starch Nutrition 0.000 claims 1
- 239000002956 ash Substances 0.000 abstract description 26
- 235000002918 Fraxinus excelsior Nutrition 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 2
- 235000010980 cellulose Nutrition 0.000 description 10
- 229920002678 cellulose Polymers 0.000 description 10
- 239000001913 cellulose Substances 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 150000002972 pentoses Chemical class 0.000 description 4
- 241000609240 Ambelania acida Species 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 description 2
- 239000010905 bagasse Substances 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000000630 fibrocyte Anatomy 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229940124531 pharmaceutical excipient Drugs 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- -1 stability Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to microcrystalline cellulose technical field, in particular to a kind of poplar slab dissolving pulp prepares the acid catalyst of ultra-fine microcrystalline cellulose, HCl, H3BO3、H2SO4、H3PO4Mass ratio with ammonium persulfate is 1:1:1:1:0.01.The method for preparing ultra-fine microcrystalline cellulose using poplar slab dissolving pulp: the PFI defibrination pretreatment of poplar slab dissolving pulp；Acid catalysis；Filtration washing.For the size controlling of the ultra-fine microcrystalline cellulose obtained using the method for the present invention at 15 microns hereinafter, even can control at 5 microns, content of ashes is low, has boundless application prospect；Method of the invention is environmentally protective, at low cost, pollution is low, yield is high, and raw material poplar slab dissolving pulp is easy to get, and has very much the market competitiveness.
Description
Technical field
The present invention relates to microcrystalline cellulose technical field, in particular to a kind of poplar slab dissolving pulp prepares superfine microcrystal fibre
Tie up the acid catalyst of element, the method for further relating to prepare ultra-fine microcrystalline cellulose.
Background technique
Cellulose is natural macromolecular material most abundant in nature and with biodegradability.Cellulosic molecule is
The system staggeredly combined by the orderly crystal region of nematic and amorphous region, by intramolecular and intermolecular hydrogen bond and Van der Waals force
Maintain the supramolecular structure and fibrilliform morphology of self assembly.The world today face resource rapidly deplete, the situation of environmental degradation
Under, focus on developing reproducible cellulose resource with own strategic significance.But cellulose is as a kind of natural polymer chemical combination
Object limits its scope of application in performance and physical aspect, if micro Nano material can be prepared into, so that it may certain
The performance for optimizing it in degree makes this renewable resource of cellulose have more extensive application range.
Microcrystalline cellulose (micro-crystalline cellulose, MCC) is the fiber of purifying, part depolymerization
Element, mainly by cellulose (content is generally 96-98%), hemicellulose (content is generally 2-4%) and inorganic matter, (content is about
0.05%, such as ash content) composition.For granular size generally between 20-80um, levelling off degree of polymerization does not have fiber between 15-375
Property and it is more liquid, stability, chemical inertness and physiological inertia are higher.MCC has been widely used in each industry neck
Domain, on pharmaceutical excipient especially in medical industry, as adhesive, disintegrating agent, diluent and lubricant；Also it can be used as
The efficient additive of foods and cosmetics improves their performance.Ultra-fine microcrystalline cellulose (ultra-fine micro-
Crystalline cellulose) it is good microcrystalline cellulose, granular size is generally less than 10um, and purposes is extensively in MCC.
The raw material for preparing MCC at present mainly has purified cotton, wood pulp, bagasse and other plant fiber materials, is taken
Technique mainly includes the techniques such as acid-catalyzed hydrolysis, ion liquid dissolving and enzyme hydrolysis, then through washing, separation, dry MCC powder
End.
The at high cost of MCC is prepared with purified cotton, and prepares MCC with wood pulp, bagasse and other plant fiber materials, also
It need to be brightened and be reduced ash treatment.The sour dosage that MCC is prepared using acid-catalyzed hydrolysis technique is big, temperature is high；Ionic liquid
At high cost, recycling it is difficult；The enzyme hydrolysis time is long, MCC yield is low.Therefore, a kind of low cost, low pollution, high yield pulp1 are found
The method for preparing microcrystalline cellulose is the important channel for developing and using new functional fiber element.
The one kind of poplar slab as wood machining residues, the dissolving pulp price prepared with it is low, and its alpha-cellulose
Content is high, and hemi-cellulose content is low, degree of polymerization 450-700, and whiteness is high, and content of ashes is low (less than 0.05%), is particularly suitable for preparing micro-
Crystalline cellulose.
Summary of the invention
In order to solve above to prepare that microcrystalline cellulose is at high cost, big, the sour dosage of pollution is big, yield is low asks in the prior art
Topic, this application provides the acid catalyst used when a kind of poplar slab dissolving pulp prepares ultra-fine microcrystalline cellulose, Ke Yijin
Cellulose in one step depolymerization dissolving pulp destroys the amorphous domain in cellulose.
The present invention also provides the method for preparing ultra-fine microcrystalline cellulose using poplar slab dissolving pulp, the method costs
It is low, pollution is small, sour dosage is small, yield is high.
What the present invention was obtained through the following steps:
A kind of poplar slab dissolving pulp prepares the acid catalyst of ultra-fine microcrystalline cellulose, HCl, H3BO3、H2SO4、H3PO4With
The mass ratio of ammonium persulfate is 1:1:1:1:0.01.
A method of ultra-fine microcrystalline cellulose is prepared using poplar slab dissolving pulp, comprising the following steps:
(1) the PFI defibrination pretreatment of poplar slab dissolving pulp；
(2) acid catalysis: acid catalyst is the 10-50% of poplar slab dissolving pulp oven dry stock quality；
(3) filtration washing.
The method, acid catalyst is the 30-50% of poplar slab dissolving pulp oven dry stock quality in preferred steps (2).
The method, the PFI defibrination pretreatment operation of poplar slab dissolving pulp is as follows in preferred steps (1): control PFI
Refining pressure be 3.33 ± 0.1N/mm, 1460 ± 30rpm of axle rotational speed, refining concentration 10 ± 0.2%, 25 ± 1 DEG C of slurry temperature,
The defibrination time is 2-60 min.
The method, acid catalyst concentration is 10-50% in preferred steps (2), and the slurry of poplar slab dissolving pulp is dense to be
3.0-5.0%, temperature are 70-90 DEG C, mixing speed 200-300rpm, time 30-120min.
The method in preferred steps (3), carries out the microcrystalline cellulose obtained after step (2) acid catalysis true
Sky filtering, obtains microcrystalline cellulose filter cake, then is washed with deionized water to the conductivity of cleaning solution lower than 200uS/cm, after washing
Microcrystalline cellulose filter cake is placed in 65 ± 1 DEG C of baking ovens and is dried.
The average grain diameter of the method, the ultra-fine microcrystalline cellulose preferably obtained is less than 15um, and ash content is less than 0.050%.
Poplar slab dissolving pulp is pre-processed by means of PFI fiberizer first, makes dissolving pulp fibrocyte pars intramuralis and outside
Fibrillating is carried out, the degree of polymerization of poplar slab dissolving pulp is reduced, then dissolving pulp carries out acid catalysis processing, benefit by treated
With the cellulose in the further depolymerization dissolving pulp of ingredient in acid catalyst, the amorphous domain in cellulose is destroyed, is surpassed
Subtle crystalline cellulose.
The beneficial effects of the present invention are:
(1) size controlling of the ultra-fine microcrystalline cellulose obtained using the method for the present invention is at 15 microns or less, it might even be possible to
At 5 microns, content of ashes is low for control, has boundless application prospect；
(2) method of the invention is environmentally protective, at low cost, pollution is low, sour dosage is small, yield is high, and raw material poplar slab
Dissolving pulp is easy to get, and has very much the market competitiveness.
Detailed description of the invention
Fig. 1 is the grain size distribution for the MCC that embodiment 1 is prepared,
Fig. 2 is the grain size distribution for the MCC that embodiment 3 is prepared,
Fig. 3 is the grain size distribution for the MCC that embodiment 4 is prepared,
Fig. 4 is the grain size distribution for the MCC that comparative example 1 is prepared.
Specific embodiment
Invention is further explained combined with specific embodiments below:
Embodiment 1:
(1) take poplar slab dissolving pulp (alpha-cellulose content 93%, poly-pentose 3.7%, the degree of polymerization 488, whiteness 83%ISO,
Content of ashes 0.04%) over dry 5g, control PFI defibrination pretreating process are as follows: refining pressure is 3.33 ± 0.1N/mm, axle rotational speed
1460 ± 30rpm, refining concentration 10%, 25 ± 1 DEG C of slurry temperature, the defibrination time is 20 min；
(2) acid catalysis technique is controlled are as follows: the dense slurry of dissolving pulp is 4%, and acid catalyst is poplar slab dissolving pulp oven dry stock matter
The 30% of amount, temperature are 80 DEG C, mixing speed 250rpm, time 60min, acid catalyst HCl, H3BO3、H2SO4、
H3PO4It is mixed to get with ammonium persulfate according to mass ratio 1:1:1:1:0.01；
(3) filtration washing technique are as follows: vacuum filter is carried out to the MCC obtained after acid catalysis, obtains MCC filter cake, then spend
Ion is washed to the conductivity of cleaning solution lower than 200uS/cm, and the MCC filter cake after washing, which is placed in 65 ± 1 DEG C of baking ovens, to be dried
It is dry.
Partial size, ash content and yield measurement are carried out to the MCC of acquisition, partial size is as shown in Figure 1, average grain diameter is 1.985um, ash
It is divided into 0.030%, yield 87.5%.
Embodiment 2:
(1) take poplar slab dissolving pulp (alpha-cellulose content 93%, poly-pentose 3.7%, the degree of polymerization 488, whiteness 83%ISO,
Content of ashes 0.04%) over dry 5g, control PFI defibrination pretreating process are as follows: refining pressure is 3.33 ± 0.1N/mm, axle rotational speed
1460 ± 30rpm, refining concentration 10%, 25 ± 1 DEG C of slurry temperature, the defibrination time is 2 min；
(2) acid catalysis technique is controlled are as follows: the dense slurry of dissolving pulp is 4%, and acid catalyst is poplar slab dissolving pulp oven dry stock matter
The 10% of amount, temperature are 80 DEG C, mixing speed 250rpm, time 60min, acid catalyst HCl, H3BO3、H2SO4、
H3PO4It is mixed to get with ammonium persulfate according to mass ratio 1:1:1:1:0.01；
(3) filtration washing technique are as follows: vacuum filter is carried out to the MCC obtained after acid catalysis, obtains MCC filter cake, then spend
Ion is washed to the conductivity of cleaning solution lower than 200uS/cm, and the MCC filter cake after washing, which is placed in 65 ± 1 DEG C of baking ovens, to be dried
It is dry.
Partial size, ash content and yield measurement are carried out to the MCC of acquisition, because partial size is more than 10 um, no particle diameter distribution image is put down
Equal partial size is 12.200um, ash content 0.035%, yield 88.9%.
Embodiment 3:
(1) take poplar slab dissolving pulp (alpha-cellulose content 93%, poly-pentose 3.7%, the degree of polymerization 488, whiteness 83%ISO,
Content of ashes 0.04%) over dry 5g, control PFI defibrination pretreating process are as follows: refining pressure is 3.33 ± 0.1N/mm, axle rotational speed
1460 ± 30rpm, refining concentration 10%, 25 ± 1 DEG C of slurry temperature, the defibrination time is 2 min；
(2) acid catalysis technique is controlled are as follows: the dense slurry of dissolving pulp is 4%, and acid catalyst is poplar slab dissolving pulp oven dry stock matter
The 50% of amount, temperature are 80 DEG C, mixing speed 250rpm, time 60min, acid catalyst HCl, H3BO3、H2SO4、
H3PO4It is mixed to get with ammonium persulfate according to mass ratio 1:1:1:1:0.01；
(3) filtration washing technique are as follows: vacuum filter is carried out to the MCC obtained after acid catalysis, obtains MCC filter cake, then spend
Ion is washed to the conductivity of cleaning solution lower than 200uS/cm, and the MCC filter cake after washing, which is placed in 65 ± 1 DEG C of baking ovens, to be dried
It is dry.
Partial size, ash content and yield measurement are carried out to the MCC of acquisition, partial size is as shown in Fig. 2, average grain diameter is 2.120um, ash
It is divided into 0.040%, yield 80.3%.
Embodiment 4:
(1) take poplar slab dissolving pulp (alpha-cellulose content 93%, poly-pentose 3.7%, the degree of polymerization 488, whiteness 83%ISO,
Content of ashes 0.04%) over dry 5g, control PFI defibrination pretreating process are as follows: refining pressure is 3.33 ± 0.1N/mm, axle rotational speed
1460 ± 30rpm, refining concentration 10%, 25 ± 1 DEG C of slurry temperature, the defibrination time is 60 min；
(2) acid catalysis technique is controlled are as follows: the dense slurry of dissolving pulp is 4%, and acid catalyst is poplar slab dissolving pulp oven dry stock matter
The 50% of amount, temperature are 80 DEG C, mixing speed 250rpm, time 60min, acid catalyst HCl, H3BO3、H2SO4、
H3PO4It is mixed to get with ammonium persulfate according to mass ratio 1:1:1:1:0.01；
(3) filtration washing technique are as follows: vacuum filter is carried out to the MCC obtained after acid catalysis, obtains MCC filter cake, then spend
Ion is washed to the conductivity of cleaning solution lower than 200uS/cm, and the MCC filter cake after washing, which is placed in 65 ± 1 DEG C of baking ovens, to be dried
It is dry.
Partial size, ash content and yield measurement are carried out to the MCC of acquisition, partial size is as shown in figure 3, average grain diameter is 2.218um, ash
It is divided into 0.043%, yield 72.4%.
Comparative example 1:
It is compared with embodiment 4, omits the PFI defibrination pretreatment in step (1), the acid catalyst in step (2) is poplar
The 200% of slab dissolving pulp oven dry stock quality, remaining is identical with embodiment 4, carries out partial size, ash content and yield to the MCC of acquisition and surveys
Amount, average grain diameter are 2.702 um, see that Fig. 4 ash content is 0.043%, yield 40.30%.
Comparative example 2
Compared with embodiment 4, acid catalyst is HCl, H in step (2)3BO3、H2SO4、H3PO4According to mass ratio 1:1:1:1
It is mixed to get, remaining is identical with embodiment 4, carries out partial size, ash content and yield to the MCC of acquisition and measures, average grain diameter is
2.815 um, ash content 0.064%, yield 61.32%.
Comparative example 3
Compared with embodiment 4, acid catalyst is HCl, H in step (2)3BO3、H2SO4、H3PO4With ammonium persulfate according to matter
For amount than 2:1:2:1:0.01, remaining is identical with embodiment 4, carries out partial size, ash content and yield to the MCC of acquisition and measures, average grain
Diameter is 2.876 um, ash content 0.056%, yield 58.75%.
Comparative example 4
Compared with embodiment 4, acid catalyst is HCl, H in step (2)2SO4、H3PO4With ammonium persulfate according to mass ratio 1:
1:1:0.01, remaining is identical with embodiment 4, carries out partial size, ash content and yield to the MCC of acquisition and measures, average grain diameter is
2.922 um, ash content 0.059%, yield 63.20%.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the limit of embodiment
System, other any changes made without departing from the spirit and principles of the present invention, modification, combination, substitution, simplification should be
Equivalence replacement mode, is included within the scope of the present invention.
Claims (8)
1. the acid catalyst that a kind of poplar slab dissolving pulp prepares ultra-fine microcrystalline cellulose, it is characterised in that HCl, H3BO3、H2SO4、
H3PO4Mass ratio with ammonium persulfate is 1:1:1:1:0.01.
2. a kind of method for preparing ultra-fine microcrystalline cellulose using poplar slab dissolving pulp, it is characterised in that the following steps are included:
(1) the PFI defibrination pretreatment of poplar slab dissolving pulp；
(2) acid catalysis: the acid catalyst in claim 1 is the 10-50% of poplar slab dissolving pulp oven dry stock quality；
(3) filtration washing.
3. according to the method described in claim 2, it is characterized in that acid catalyst is poplar slab dissolving pulp over dry in step (2)
Starch the 30-50% of quality.
4. according to the method described in claim 2, it is characterized in that the PFI defibrination of poplar slab dissolving pulp is located in advance in step (1)
Reason operation it is as follows: control PFI refining pressure be 3.33 ± 0.1N/mm, 1460 ± 30rpm of axle rotational speed, refining concentration 10 ±
0.2%, 25 ± 1 DEG C of slurry temperature, the defibrination time is 2-60 min.
5. according to the method described in claim 2, it is characterized in that acid catalyst concentration is 10-50%, poplar plate in step (2)
The dense slurry of skin dissolving pulp is 3.0-5.0%, and temperature is 70-90 DEG C, mixing speed 200-300rpm, time 30-120min.
6. according to the method described in claim 2, it is characterized in that in step (3), to what is obtained after step (2) acid catalysis
Microcrystalline cellulose carries out vacuum filter, obtains microcrystalline cellulose filter cake, then be washed with deionized water to the conductivity of cleaning solution and be lower than
200uS/cm, the microcrystalline cellulose filter cake after washing are placed in 65 ± 1 DEG C of baking ovens and are dried.
7. the method according to any one of claim 2-6, it is characterised in that obtained ultra-fine microcrystalline cellulose is averaged
Partial size is less than 15um, and ash content is less than 0.050%.
8. according to the method described in claim 2, it is characterized in that the PFI defibrination of poplar slab dissolving pulp is located in advance in step (1)
The defibrination time is 2-20min in reason operation.
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| CN201710034469.0A CN106824235B (en) | 2017-01-18 | 2017-01-18 | A kind of poplar slab dissolving pulp prepares the acid catalyst of ultra-fine microcrystalline cellulose and prepares the method for ultra-fine microcrystalline cellulose |
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| CN201710034469.0A CN106824235B (en) | 2017-01-18 | 2017-01-18 | A kind of poplar slab dissolving pulp prepares the acid catalyst of ultra-fine microcrystalline cellulose and prepares the method for ultra-fine microcrystalline cellulose |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102912667A (en) * | 2012-10-17 | 2013-02-06 | 山东轻工业学院 | Method for producing dissolving pulp by using poplar slabs |
| CN102947345A (en) * | 2009-12-15 | 2013-02-27 | 加拿大国家研究委员会 | Cellulose nanocrystals from renewable biomass |
| CN104293858A (en) * | 2013-07-19 | 2015-01-21 | 天津科技大学 | Preparation method for nano-microcrystalline cellulose |
| CN105002768A (en) * | 2015-07-30 | 2015-10-28 | 齐鲁工业大学 | Removing method for lignin in poplar slab dissolving pulp prehydrolysis waste liquor |
| CN105884908A (en) * | 2016-06-17 | 2016-08-24 | 东华大学 | Preparation method of carboxylated cellulose nanoparticles |
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2017
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102947345A (en) * | 2009-12-15 | 2013-02-27 | 加拿大国家研究委员会 | Cellulose nanocrystals from renewable biomass |
| CN102912667A (en) * | 2012-10-17 | 2013-02-06 | 山东轻工业学院 | Method for producing dissolving pulp by using poplar slabs |
| CN104293858A (en) * | 2013-07-19 | 2015-01-21 | 天津科技大学 | Preparation method for nano-microcrystalline cellulose |
| CN105002768A (en) * | 2015-07-30 | 2015-10-28 | 齐鲁工业大学 | Removing method for lignin in poplar slab dissolving pulp prehydrolysis waste liquor |
| CN105884908A (en) * | 2016-06-17 | 2016-08-24 | 东华大学 | Preparation method of carboxylated cellulose nanoparticles |
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