CN109776815A - A method of recycling lignin from solvent pulping bleaching waste liquor - Google Patents
A method of recycling lignin from solvent pulping bleaching waste liquor Download PDFInfo
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- CN109776815A CN109776815A CN201910236385.4A CN201910236385A CN109776815A CN 109776815 A CN109776815 A CN 109776815A CN 201910236385 A CN201910236385 A CN 201910236385A CN 109776815 A CN109776815 A CN 109776815A
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Abstract
The method that the present invention relates to a kind of to recycle lignin from solvent pulping bleaching waste liquor, the method are as follows: the pH of the bleaching waste liquor of the isolated fiber of solvent method processing plant fiber material is adjusted to 1-6, then stirring is reacted under conditions of heating pressurization, obtain mixed serum, to slurries energization accelerated sedimentation, solid phase precipitation and separating liquid are obtained after separation of solid and liquid；In organic solvent by the dissolution of obtained solid phase precipitation, it is then centrifuged for separating, after gained supernatant is removed solvent, obtains lignin after the recovery.The present invention passes through the adjustment to technique, the good lignin of purity is high, activity has been recovered to from bleaching waste liquor, the rate of recovery of lignin is greater than 95%, the lignin purity of recycling is 98% or more, the COD of waste liquid is reduced simultaneously, the organic loading of discharge is reduced, production process is more environmentally friendly, is suitable for large-scale promotion.
Description
Technical field
The invention belongs to plant fiber material process fields, and in particular to one kind is recycled from solvent pulping bleaching waste liquor
The method of lignin.
Background technique
Plant fiber processing technique includes physical method, physical-chemical method, chemical method, bioanalysis etc., inferior separating effect, group
Get that rate is low, wherein conventional acid, alkaline process the high requirements on the equipment, seriously polluted；And bioanalysis is at high cost, the period is long.
The solvent method processing technique to grow up in recent years can carry out better component separation.Solvent method is exactly adopted
It substitutes inorganic drug with organic solvent to handle plant fiber material, under certain condition, organic solvent can be with degrading plant
Lignin in raw material achievees the purpose that lignin, cellulose, hemicellulose efficiently separate.
Solvent method processing technique belongs to the new processing method of pollution-free low energy consumption, and comprehensive benefit is more excellent, has obtained at present
Fairly large application is arrived.But meanwhile it is generally higher by the fiber magma Kappa number that solvent method is handled, i.e., in fiber
Lignin residual is more, could need to effectively be removed lignin by bleaching.Thus remain major part in its bleaching waste liquor
Lignin, bleaching waste liquor organic loading is higher.After the fiber that conventional method obtains is bleached, wooden disposition in bleaching waste liquor
Can be poor, content is few, and it is at high cost if extracting, therefore necessity of typically no recycling.And the fibre prepared by solvent method
After dimension is bleached, the lignin properties in bleaching waste liquor are different from traditional industrial lignin, and activity is more preferable, excellent using more having
Gesture, but extraction is also more difficult, does not there is relevant research yet at present.
Summary of the invention
Lignin is recycled from solvent pulping bleaching waste liquor in order to solve the above technical problems, the present invention provides a kind of
It is good to be recovered to purity is high, activity from the bleaching waste liquor that solvent method handles the isolated fiber of plant fiber material for method
Lignin, while reducing the COD of waste liquid, have a good application prospect.
In order to achieve the above objectives, the invention adopts the following technical scheme:
The method that the present invention provides a kind of from solvent pulping bleaching waste liquor recycles lignin, the method includes with
Lower step:
(1) pH of bleaching waste liquor is adjusted to 1-6, then stirring is reacted under conditions of heating pressurization, is mixed
It closes slurries and solid phase precipitation and separating liquid is obtained after separation of solid and liquid to slurries energization accelerated sedimentation；The bleaching waste liquor is solvent method
Handle the bleaching waste liquor of the isolated fiber of plant fiber material；
(2) the solid phase precipitation dissolution obtained step (1) in organic solvent, is then centrifuged for separating, by gained supernatant
After removing solvent, lignin after the recovery is obtained.
According to the present invention, the pH of waste liquid is 1-6 during carrying out processing recycling lignin to bleaching waste liquor, such as can
To be the specific point value between 1,2,3,4,5 or 6 and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is not
Exclusive list again.
PH is one of the key factor for influencing lignin recovery rate, and when pH is excessively high, (> 6) is difficult to realize to lignin
It extracts and recycles.When pH is too low (< 1), although can be realized the recycling to lignin, obtained waste liquid after being separated by solid-liquid separation
Middle hydrogen ion concentration is excessively high, and direct emission can adversely affect environment, therefore should strongly avoid in actual production.
According to the present invention, the temperature of step (1) described reaction is 120-200 DEG C, such as can be 120 DEG C, 130 DEG C, 140
DEG C, 150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C, 190 DEG C or the specific point value between 200 DEG C and above-mentioned numerical value, as space is limited and
For concise consideration, the present invention no longer exclusive list.
According to the present invention, the pressure of step (1) described reaction be 1.5-3MPa, such as can be 1.5MPa, 1.8MPa,
Specific point value between 2MPa, 2.3MPa, 2.5MPa, 2.8MPa or 3MPa and above-mentioned numerical value, as space is limited and for simplicity
The considerations of, the present invention no longer exclusive list.
The control of temperature and pressure is of great significance for the extraction and recycling of lignin, when temperature and pressure deficiency
When, the rate of recovery of lignin will appear apparent decline.When temperature and pressure is excessively high, increases energy consumption and equipment is wanted
It asks, does not utilize control cost, while the lignin purity generated can reduce, performance has different degrees of decline.
In addition, the present invention during the reaction deposits the slurries energization obtained after heating compressive reaction, using can
The various factors couplings such as electrochemical reaction, mass transfer, air bearing of the solube metallic under extra electric field accelerate the sedimentation speed of lignin molecule
Rate can further increase the precipitation rate of recovery of lignin.
According to the present invention, the revolving speed of step (1) described stirring is 60-800r/min, such as can be 60r/min, 100r/
Min, 200r/min, 300r/min, 400r/min, 500r/min, 600r/min, 700r/min or 800r/min and above-mentioned
Specific point value between numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the time of step (1) described stirring be 0.2-3h, such as can be 0.2h, 0.5h, 0.8h, 1h,
Specific point value between 1.3h, 1.5h, 1.8h, 2h, 2.3h, 2.5h, 2.8h or 3h and above-mentioned numerical value as space is limited and goes out
In concise consideration, the present invention no longer exclusive list.
According to the present invention, step (1) concrete operations to slurries energization accelerated sedimentation are as follows: be added into mixed serum
Working electrode and metal salt solution, then in 10-90A/m2Current density under settle 10-60min.
Illustratively, during the above-mentioned energization accelerated sedimentation, working electrode can be aluminium or iron electrode, and metal salt is molten
Liquid can be sodium chloride solution, but it is non-be only limitted to this, conventional working electrode and metal salt solution are suitable for the present invention.
According to the present invention, the concentration of metal salt is 0.5-3g/L in the mixed serum, such as can be 0.5g/L, 1g/
L, the specific point value between 1.5g/L, 2g/L, 2.5g/L or 3g/L and above-mentioned numerical value is examined as space is limited and for concise
Consider, the present invention no longer exclusive list.
According to the present invention, the mode of step (1) described separation of solid and liquid is film filtering, and the film can be molecular cut off
200 or more filter membrane, filter plant are unlimited.
The present invention is separated by the mixed slurry that film filtering obtains step (1), in addition to will go back other than lignin retention
Other macromolecular substances can be retained, later use organic solvent, which carries out dissolution, can remove impurity, purifying lignin.
According to the present invention, step (1) separating liquid obtained after the separation of solid and liquid is discharged after being adsorbed using active carbon,
It can be re-used after the active carbon heating；In addition, waste liquid can be further decreased by being adsorbed using active carbon to separating liquid
Organic loading and COD, make up to discharge standard.
According to the present invention, the concrete operations of step (2) described dissolution are as follows: the solid phase precipitation that obtains step (1) and organic
It is stirred after solvent mixing, supersonic oscillations after the completion of stirring, until lignin is completely dissolved.
According to the present invention, step (2) organic solvent is acetone, Isosorbide-5-Nitrae-dioxane, dimethylformamide or pyridine
In any one, preferably acetone.
According to the present invention, the solvent in the supernatant is removed in step (2) in the way of film evaporation and concentration, then will
The solution spray drying obtained after concentration, obtains lignin after the recovery.
The method of the present invention that lignin is recycled from bleaching waste liquor includes following step as a preferred technical solution,
It is rapid:
(1) pH of bleaching waste liquor is adjusted to 1-6, then with 60-800r/ under conditions of 120-200 DEG C, 1.5-3MPa
Mixed serum is obtained after the revolving speed stirring 0.2-3h of min, working electrode and metal salt solution, control are then added into mixed serum
The concentration of metal salt is 0.5-3g/L in slurrying liquid, in 10-90A/m2Current density under settle 10-60min, after film filtering
To solid phase precipitation and separating liquid, discharged after obtained separating liquid is adsorbed using active carbon, it can after the active carbon heating
It re-uses；The bleaching waste liquor is the bleaching waste liquor that solvent method handles the isolated fiber of plant fiber material；
(2) it is stirred after mixing solid phase precipitation and organic solvent that step (1) obtains, ultrasonic wave shakes after the completion of stirring
It swings, until lignin is completely dissolved, is then centrifuged for separating, the solvent in gained supernatant is removed in the way of film evaporation and concentration,
Then the solution obtained after concentration is spray-dried, obtains lignin after the recovery.
Compared with prior art, the present invention at least has the advantages that
For the present invention by the adjustment to technique, the bleaching of the fiber isolated from solvent method processing plant fiber material is useless
The good lignin of purity is high, activity is recovered in liquid, the rate of recovery of lignin is greater than 95%, and the lignin purity of recycling exists
98% or more.After lignin obtains recycling, the COD of waste liquid can reduce, reduce the organic loading of discharge, production process more ring
It protects, has a good application prospect.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) bleaching waste liquor of the isolated fiber of plant fiber material is handled using acetic acid as organic solvent as raw material,
The pH of waste liquid is adjusted to 3,200 DEG C are then heated under the pressure of 1.5MPa, 1h is stirred with the revolving speed of 200r/min
After obtain mixed serum, aluminium electrode and NaCl solution are added into mixed serum, the concentration for controlling NaCl is 2g/L, in 90A/m2
Current density under settle 10min, film filtering then is carried out to gained slurries, isolated solid phase precipitation and filtrate utilize work
Property charcoal will obtained filtrate absorption after discharge, active carbon heating after can re-use；
(2) it is stirred by solid phase precipitation that step (1) obtains and after thering is acetone to mix, supersonic oscillations after the completion of stirring
For a period of time, it until lignin is completely dissolved, is then centrifuged for separating, be removed in the way of film evaporation and concentration in gained supernatant
The solution obtained after concentration is spray-dried by solvent, obtains the lignin that purity is 98.7%.
After testing, the rate of recovery of lignin is 96.3% in the present embodiment.
Embodiment 2
(1) bleaching waste liquor of the isolated fiber of plant fiber material is handled using methanol as organic solvent as raw material,
The pH of waste liquid is adjusted to 1,120 DEG C are then heated under the pressure of 3MPa, 0.2h is stirred with the revolving speed of 800r/min
After obtain mixed serum, aluminium electrode and NaCl solution are added into mixed serum, the concentration for controlling NaCl is 3g/L, in 60A/m2
Current density under settle 30min, film filtering then is carried out to gained slurries, isolated solid phase precipitation and filtrate utilize work
Property charcoal will obtained filtrate absorption after discharge, active carbon heating after can re-use；
(2) it is stirred by solid phase precipitation that step (1) obtains and after thering is Isosorbide-5-Nitrae-dioxane to mix, it is super after the completion of stirring
Sonication for a period of time, until lignin is completely dissolved, is then centrifuged for separating, and is removed on gained in the way of film evaporation and concentration
The solution obtained after concentration is spray-dried by the solvent in clear liquid, obtains the lignin that purity is 98.2%.
After testing, the rate of recovery of lignin is 95.9% in the present embodiment.
Embodiment 3
(1) bleaching waste liquor that the isolated fiber of plant fiber material is handled using butanediol as organic solvent is original
Material, is adjusted to 5 for the pH of waste liquid, 150 DEG C is then heated under the pressure of 2.2MPa, is stirred with the revolving speed of 60r/min
Mixed serum is obtained after 3h, aluminium electrode and NaCl solution are added into mixed serum, and the concentration for controlling NaCl is 1g/L, in 10A/
m2Current density under settle 60min, film filtering then is carried out to gained slurries, isolated solid phase precipitation and filtrate utilize
Active carbon discharges after adsorbing obtained filtrate, can re-use after active carbon heating；
(2) it is stirred by solid phase precipitation that step (1) obtains and after thering is acetone to mix, supersonic oscillations after the completion of stirring
For a period of time, it until lignin is completely dissolved, is then centrifuged for separating, be removed in the way of film evaporation and concentration in gained supernatant
The solution obtained after concentration is spray-dried by solvent, obtains the lignin that purity is 99.0%.
After testing, the rate of recovery of lignin is 96.7% in the present embodiment.
Embodiment 4
(1) bleaching waste liquor of the isolated fiber of plant fiber material is handled using ethyl alcohol as organic solvent as raw material,
The pH of waste liquid is adjusted to 4.2,180 DEG C are then heated under the pressure of 2MPa, is stirred with the revolving speed of 100r/min
Mixed serum is obtained after 2.5h, and aluminium electrode and NaCl solution are added into mixed serum, the concentration for controlling NaCl is 0.5g/L,
80A/m2Current density under settle 25min, film filtering then carried out to gained slurries, isolated solid phase precipitation and filtrate,
It will be discharged after the absorption of obtained filtrate using active carbon, can be re-used after active carbon heating；
(2) it is stirred by solid phase precipitation that step (1) obtains and after thering is dimethylformamide to mix, it is super after the completion of stirring
Sonication for a period of time, until lignin is completely dissolved, is then centrifuged for separating, and is removed on gained in the way of film evaporation and concentration
The solution obtained after concentration is spray-dried by the solvent in clear liquid, obtains the lignin that purity is 98.5%.
After testing, the rate of recovery of lignin is 95.4% in the present embodiment.
Embodiment 5
(1) bleaching waste liquor that the isolated fiber of plant fiber material is handled using ethylenediamine as organic solvent is original
Material, is adjusted to 6 for the pH of waste liquid, 180 DEG C is then heated under the pressure of 1.8MPa, is stirred with the revolving speed of 150r/min
Mixed serum is obtained after 2h, and aluminium electrode and NaCl solution are added into mixed serum, the concentration for controlling NaCl is 1.5g/L,
50A/m2Current density under settle 50min, film filtering then carried out to gained slurries, isolated solid phase precipitation and filtrate,
It will be discharged after the absorption of obtained filtrate using active carbon, can be re-used after active carbon heating；
(2) it is stirred by solid phase precipitation that step (1) obtains and after thering is pyridine to mix, supersonic oscillations after the completion of stirring
For a period of time, it until lignin is completely dissolved, is then centrifuged for separating, be removed in the way of film evaporation and concentration in gained supernatant
The solution obtained after concentration is spray-dried by solvent, obtains the lignin that purity is 98.8%.
After testing, the rate of recovery of lignin is 95.3% in the present embodiment.
Embodiment 6
(1) bleaching waste liquor that the isolated fiber of plant fiber material is handled using propylene glycol as organic solvent is original
Material, is adjusted to 4 for the pH of waste liquid, 140 DEG C is then heated under the pressure of 2MPa, is stirred with the revolving speed of 500r/min
Mixed serum is obtained after 0.5h, and iron electrode and NaCl solution are added into mixed serum, the concentration for controlling NaCl is 0.8g/L,
90A/m2Current density under settle 15min, film filtering then carried out to gained slurries, isolated solid phase precipitation and filtrate,
It will be discharged after the absorption of obtained filtrate using active carbon, can be re-used after active carbon heating；
(2) it is stirred by solid phase precipitation that step (1) obtains and after thering is acetone to mix, supersonic oscillations after the completion of stirring
For a period of time, it until lignin is completely dissolved, is then centrifuged for separating, be removed in the way of film evaporation and concentration in gained supernatant
The solution obtained after concentration is spray-dried by solvent, obtains the lignin that purity is 99.1%.
After testing, the rate of recovery of lignin is 96.1% in the present embodiment.
Comparative example 1
Compared with Example 3, other than step (1) is handled under normal pressure, other steps and condition and the complete phase of embodiment 1
Together.
After testing, the rate of recovery of lignin is 63.7% in this comparative example.
Comparative example 2
Compared with Example 3, other than step (1) is handled at normal temperature, other steps and condition and embodiment 1 are complete
It is exactly the same.
After testing, the rate of recovery of lignin is 58.2% in this comparative example.
Comparative example 3
Compared with Example 3, other than step (1) is handled at normal temperatures and pressures, other steps and condition and implementation
Example 1 is identical.
After testing, the rate of recovery of lignin is 41.5% in this comparative example.
Comparative example 4
Compared with Example 3, other than it 100 DEG C will be adjusted to the temperature of bleaching waste liquor processing in step (1), other steps
Rapid and condition is identical with embodiment 1.
After testing, the rate of recovery of lignin is 82.1% in this comparative example.
Comparative example 5
Compared with Example 3, other than it 1MPa will be adjusted to the pressure of bleaching waste liquor processing in step (1), other steps
Rapid and condition is identical with embodiment 1.
After testing, the rate of recovery of lignin is 76.7% in this comparative example.
Comparative example 6
Compared with Example 3, other than the pH in step (1) is adjusted to 8, other steps and condition and embodiment 1 are complete
At identical.
After testing, the rate of recovery of lignin is 15.3% in this comparative example.
Comparative example 7
Compared with Example 3, in addition to the mixed serum obtained in step (1) to heating compressive reaction directly carries out film filtering
It (is settled outside without being powered), other steps and condition are identical with embodiment 3.
After testing, the rate of recovery of lignin is 85.9% in this comparative example.
It is wooden by embodiment 1-6 it is found that the present invention has been recovered to the good lignin of purity is high, activity from bleaching waste liquor
The rate of recovery of element is greater than 95%, and the lignin purity of recycling is 98% or more.By comparative example 1-3 it is found that when in room temperature and/or often
When pressure handles bleaching waste liquor, the rate of recovery of lignin sharply declines.By comparative example 4-5 it is found that when in treatment process
When temperature or hypotony, the rate of recovery of lignin compares embodiment 3 and more apparent decline occurs 80% or so.By
For comparative example 6 it is found that when pH is 7 in treatment process, the rate of recovery of lignin only has 15.3%, illustrates when pH is excessively high in waste liquid
Lignin hardly results in recycling.By comparative example 7 it is found that when without energization accelerated sedimentation, the rate of recovery of lignin is
85.9%, 10.3% is reduced compared with embodiment 3, illustrates the key factor for carrying out that accelerated sedimentation is raising lignin recovery rate that is powered
One of.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (10)
1. a kind of method for recycling lignin from solvent pulping bleaching waste liquor, which is characterized in that the method includes following
Step:
(1) pH of bleaching waste liquor is adjusted to 1-6, then stirring is reacted under conditions of heating pressurization, obtains mixing slurry
Liquid obtains solid phase precipitation and separating liquid after separation of solid and liquid to slurries energization accelerated sedimentation；The bleaching waste liquor is solvent method processing
The bleaching waste liquor of the isolated fiber of plant fiber material；
(2) the solid phase precipitation dissolution obtained step (1) in organic solvent, is then centrifuged for separating, gained supernatant removes molten
After agent, lignin after the recovery is obtained.
2. the method as described in claim 1, which is characterized in that the temperature of step (1) described reaction is 120-200 DEG C；
Preferably, the pressure of step (1) described reaction is 1.5-3MPa.
3. method according to claim 1 or 2, which is characterized in that the revolving speed of step (1) described stirring is 60-800r/min；
Preferably, the time of step (1) described stirring is 0.2-3h.
4. the method according to claim 1, which is characterized in that step (1) is described to slurries energization accelerated sedimentation
Concrete operations are as follows: working electrode and metal salt solution are added into mixed serum, then in 10-90A/m2Current density under
Settle 10-60min；
Preferably, the concentration of metal salt is 0.5-3g/L in the mixed serum.
5. method according to any of claims 1-4, which is characterized in that the mode of step (1) described separation of solid and liquid is film
Filtering.
6. the method according to claim 1 to 5, which is characterized in that obtained after the separation of solid and liquid point of step (1)
Chaotropic is discharged after being adsorbed using active carbon, is re-used after the active carbon heating.
7. as the method according to claim 1 to 6, which is characterized in that the concrete operations of step (2) described dissolution are as follows: will
It is stirred after solid phase precipitation and the organic solvent mixing that step (1) obtains, supersonic oscillations after the completion of stirring, until lignin is complete
Fully dissolved.
8. the method according to claim 1 to 7, which is characterized in that step (2) organic solvent is acetone, Isosorbide-5-Nitrae-
Any one in dioxane, dimethylformamide or pyridine, preferably acetone.
9. the method according to claim 1, which is characterized in that in step (2) in the way of film evaporation and concentration
The solvent in the supernatant is removed, then the solution obtained after concentration is spray-dried, obtains lignin after the recovery.
10. such as the described in any item methods of claim 1-9, which is characterized in that the described method comprises the following steps:
(1) pH of bleaching waste liquor is adjusted to 1-6, then with 60-800r/min under conditions of 120-200 DEG C, 1.5-3MPa
Revolving speed stirring 0.2-3h after obtain mixed serum, working electrode and metal salt solution, control are then added into mixed serum
The concentration of metal salt is 0.5-3g/L in slurries, in 10-90A/m2Current density under settle 10-60min, obtained after film filtering
Solid phase precipitation and separating liquid are discharged after being adsorbed obtained separating liquid using active carbon, can be weighed after the active carbon heating
It is new to utilize；The bleaching waste liquor is the bleaching waste liquor that solvent method handles the isolated fiber of plant fiber material；
(2) it is stirred after mixing solid phase precipitation and organic solvent that step (1) obtains, supersonic oscillations after the completion of stirring,
It is completely dissolved to lignin, is then centrifuged for separating, the solvent in gained supernatant is removed in the way of film evaporation and concentration, then
The solution obtained after concentration is spray-dried, lignin after the recovery is obtained.
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Application publication date: 20190521 |
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