CN109518507A - The method of lignin and the preparation method of lignin particle in a kind of hydrotropes removal sawdust - Google Patents
The method of lignin and the preparation method of lignin particle in a kind of hydrotropes removal sawdust Download PDFInfo
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- CN109518507A CN109518507A CN201811167333.8A CN201811167333A CN109518507A CN 109518507 A CN109518507 A CN 109518507A CN 201811167333 A CN201811167333 A CN 201811167333A CN 109518507 A CN109518507 A CN 109518507A
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- lignin
- sawdust
- hydrotropes
- sodium
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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Abstract
The invention discloses the methods of lignin in a kind of hydrotropes removal sawdust, comprising the following steps: (1) wood chip is ground into sawdust of the size less than 20 mesh in grinder；(2) ground sawdust is added in hydrotropes solution, is reacted in constant temperature oscillation box；The hydrotropes are one kind of isopropyl toluene sodium sulfonate, sodium butylbenzene sulfonate, ethyl phenenyl azochlorosulfonate acid sodium, acid dimethyl sodium, toluenesulfonic acid sodium salt, isooctane base sodium sulfonate, benzene sulfonic acid sodium salt, butyl sulfonic acid sodium；(3) after reaction, solid and liquid are separated using the mode of vacuum filtration.The present invention can efficiently remove lignin in sawdust under lower temperature, normal pressure, reuse after can recycling, and have the function that reduce energy consumption.Lignin particle of the invention has the advantages that raw material is cheap and easy to get, easy to use, has good practical application value, the preparation method simple process of lignin particle of the invention, easy to operate, product subsequent processing is simple, is easy to realization of industrialization.
Description
Technical field
The present invention relates to pulping and paper-making field, in particular in a kind of hydrotropes removal sawdust the method for lignin and
The preparation method of lignin particle.
Background technique
Lignin is one of the main component of tracheid's wall, and lignin is as a kind of filling and adhesive in wood
Matter bonds and is reinforced between cellulose fibre that can make in a manner of physically or chemically in wood cell wall, increases timber
Mechanical strength and the ability for resisting microbial attack.
Lignin is a kind of aromatic Organic Ingredients, have it is nontoxic, inexpensive, easily by the peculiar property of biological decomposition.Wood
The purified modification of quality can be used as feed, miberal powder binder, Oilfield Chemicals, asphalt emulsifier, active carbon, cement diminishing
Agent, metal passivation auxiliary agent, chemical grouting material etc..Although the industrial applications of lignin Related product have been achieved for flourishing
Development, but since industrial lignin annual output is huge, annual only about 1% industrial lignin is converted into valuable work at present
Industry product.Therefore, it opens up the new way that lignin utilizes and is increasingly becoming the hot spot studied both at home and abroad.Since lignin product has
Have abundant from a wealth of sources, active group, non-toxic resistant, it is renewable and degradable many advantages, such as, therefore with boundless
Application space.If can be raw material with lignin, the preparation of lignin micro-and nano-particles be realized, this will provide a kind of lignin-base
The new way of product higher value application.
Pulp and paper industry energy conservation, is lowered consumption, reduces carbon emission, passes through biorefinery as energy-intensive industries
Technology makes enterprises in pulp and paper industry transition and upgrade to become the emphasis of Future Projects science and technology.Existing delignification technology, such as alkaline process and
Sulfite pulping technique requires to operate at high temperature, and using pressurizing vessel, and chemical recovery is expensive.And some
In method using organic solvent removal lignin, the removal rate of lignin is relatively low, such as milled wood lignin preparation process, ground wood
50% of the yield rate of lignin less than full lignin, and the yield of ethyl alcohol lignin is only equivalent to the 8%- of Klason lignin
10%.It would therefore be desirable to develop quick delignification under low-temperature atmosphere-pressure, and simplify the method for chemical recovery, to be papermaking
And biorefinery industry provides renewable and biodegradable lignocellulosic, and then to realize that pulping energy consumption reduces by 50%
Target, if can be reduced the 50% of present pulping energy consumption, this will be the energy-efficient important breakthrough of pulp and paper industry.
Summary of the invention
In order to overcome the disadvantages mentioned above and deficiency of the prior art, the purpose of the present invention is to provide a kind of hydrotropes to go
Except the method for lignin in sawdust, lignin in sawdust can be efficiently removed under lower temperature, normal pressure, repeated after can recycling
It uses, has haved the function that reduce energy consumption.
Another object of the present invention is to provide a kind of preparation methods of lignin particle, and preparation method is simple, realizes
The higher value application of lignin.
The purpose of the present invention is achieved through the following technical solutions:
A kind of method that hydrotropes remove lignin in sawdust, comprising the following steps:
(1) wood chip is ground into sawdust of the size less than 20 mesh in grinder；
(2) ground sawdust, solid-to-liquid ratio 1:10-20, in constant temperature oscillation box are added in hydrotropes solution
It is reacted, controls -90 DEG C of temperature 50 C, time 10-60min；
The hydrotropes are isopropyl toluene sodium sulfonate, sodium butylbenzene sulfonate, ethyl phenenyl azochlorosulfonate acid sodium, dimethyl benzene sulphur
One kind of sour sodium, toluenesulfonic acid sodium salt, isooctane base sodium sulfonate, benzene sulfonic acid sodium salt, butyl sulfonic acid sodium；
(3) after reaction, solid and liquid are separated using the mode of vacuum filtration.
The hydrotropes aqueous solution of the hydrotropes concentration of polymer solution 40%-60%.
The wood chip is the one or more of many paper grade (stock) wood types such as Eucalyptus, Korean pine wood, poplar.
A kind of preparation method of lignin particle, comprising the following steps:
It is 5-10 DEG C that temperature, which is added, in the liquid that the method for lignin obtains in hydrotropes removal sawdust
Cold water carries out the regeneration of lignin；Gained lignin particle is centrifuged, the lignin particle distillation collected
After water is centrifuged washed several times with water, it is freeze-dried.
The rate of the centrifuge separation is 5000-10000r.
The time with distilled water centrifugation washing is 5-20min.Compared with prior art, the present invention has the following advantages that
With the utility model has the advantages that
Lignin minimizing technology of the invention, simple process, best removal rate accelerate lignin from plant up to 82.1%
Removing speed in fiber reduces the lignin residual in paper making pulp, effectively reduces the energy consumption, avoid the mistake of chemicals
It uses more and resource consumption, recovery utilization rate height is at low cost.
Lignin particle of the invention has the advantages that raw material is cheap and easy to get, easy to use, has good practical application
Value, the preparation method simple process of lignin particle of the invention, easy to operate, product subsequent processing is simple, is easy to industry
Change and realizes.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, embodiments of the present invention are not limited thereto.
Embodiment 1
(1) common Eucalyptus wood chip is selected, wood chip is ground into sawdust of the size less than 20 mesh in grinder, configures matter
Measure the isopropyl toluene sulfonic acid sodium water solution of concentration 40%-60%.
(2) 50ml hydrotropes solution is added in the flask of 150ml, the ground sawdust of 5g is then added,
It is reacted in constant temperature oscillation box, controls 80 DEG C of temperature, time 30min.
(3) after reaction, solid and liquid are separated using the mode of vacuum filtration, 5-10 DEG C is added in a liquid
The regeneration of cold water progress lignin.Gained lignin particle is centrifuged, the lignin particle being collected by centrifugation is used
It after distilling water washing for several times, is freeze-dried, lignin particle is obtained after the completion of dry.
| Solution concentration (%) | 40 | 45 | 50 | 55 | 60 |
| Lignin removing rate (%) | 32.5 | 40.9 | 50.7 | 66.2 | 82.1 |
For contrast effect, common digestion process is selected, conditions of cooking: 30% (Na of alkali charge2O meter), liquor ratio 1:5 (g/
ML), heating-up time 1.5h, soaking time 3.5h, 170 DEG C of boiling temperature, the recovery rate of lignin, will be obtained by boiling up to 93.6%
Black liquor is filtered with 200 mesh screen cloths, is heated to 60 DEG C, slowly enters the H of 10wt.% while stirring2SO4Solution makes pH value 2.0.
The pelleted by centrifugation separating treatment for having a large amount of Precipitation by 5000r/min is deposited in can be observed at this time.However under this condition
The random pattern of obtained lignin deposit, can not be prepared lignin microballoon.
Embodiment 2
(1) common boiling wood chip is selected, wood chip is ground into sawdust of the size less than 20 mesh in grinder, configures matter
Measure the isopropyl toluene sulfonic acid sodium water solution of concentration 60%.
(2) 50ml hydrotropes solution is added in the flask of 150ml, the ground sawdust of 5g is then added,
It is reacted in constant temperature oscillation box, controls -90 DEG C of temperature 50 C, time 30min.
(3) after reaction, solid and liquid are separated using the mode of vacuum filtration, 5-10 DEG C is added in a liquid
The regeneration of cold water progress lignin.Gained lignin particle is centrifuged, the lignin particle being collected by centrifugation is used
It after distilling water washing for several times, is freeze-dried, lignin particle is obtained after the completion of dry.
| Temperature (DEG C) | 50 | 60 | 70 | 80 | 90 |
| Lignin removing rate (%) | 51.7 | 61.3 | 72.5 | 82.1 | 85.6 |
Embodiment 3
(1) common boiling wood chip is selected, wood chip is ground into sawdust of the size less than 20 mesh in grinder, configures matter
Measure the isopropyl toluene sulfonic acid sodium water solution of concentration 60%.
(2) 50ml hydrotropes solution is added in the flask of 150ml, the ground sawdust of 5g is then added,
It is reacted in constant temperature oscillation box, controls 80 DEG C of temperature, time 10-60min.
(3) after reaction, solid and liquid are separated using the mode of vacuum filtration, 5-10 DEG C is added in a liquid
The regeneration of cold water progress lignin.Gained lignin particle is centrifuged, the lignin particle being collected by centrifugation is used
It after distilling water washing for several times, is freeze-dried, lignin particle is obtained after the completion of dry.
| Reaction time (min) | 10 | 20 | 30 | 40 | 50 | 60 |
| Lignin removing rate (%) | 47.1 | 64.5 | 82.1 | 86.6 | 88.5 | 90.1 |
Embodiment 4
(1) common boiling wood chip is selected, wood chip is ground into sawdust of the size less than 20 mesh in grinder, is matched respectively
Set the isopropyl toluene sodium sulfonate (A), sodium butylbenzene sulfonate (B), ethyl phenenyl azochlorosulfonate acid sodium (C), dimethylbenzene sulphur of mass concentration 60%
Sour sodium (D), toluenesulfonic acid sodium salt (E), isooctane base sodium sulfonate (F), benzene sulfonic acid sodium salt (G), butyl sulfonic acid sodium (H) aqueous solution.
(2) 50ml hydrotropes solution is added in the flask of 150ml, the ground sawdust of 5g is then added,
It is reacted in constant temperature oscillation box, controls 80 DEG C of temperature, time 30min.
(3) after reaction, solid and liquid are separated using the mode of vacuum filtration, 5-10 DEG C is added in a liquid
The regeneration of cold water progress lignin.Gained lignin particle is centrifuged, the lignin particle being collected by centrifugation is used
It after distilling water washing for several times, is freeze-dried, lignin particle is obtained after the completion of dry.
| Hydrotropes type | A | B | C | D | E | F | G | H |
| Lignin removing rate (%) | 82.1 | 79.5 | 75.3 | 72.1 | 69.5 | 66.2 | 63.1 | 60.5 |
Embodiment 5
(1) common boiling wood chip is selected, wood chip is ground into sawdust of the size less than 20 mesh in grinder, configures matter
Measure the isopropyl toluene sulfonic acid sodium water solution of concentration 40%-60% (C).
(2) 50ml hydrotropes solution is added in the flask of 150ml, the ground sawdust of 5g is then added,
It is reacted, is controlled -90 DEG C of temperature 50 C (T) in constant temperature oscillation box, the time is 10-60min (t).
(3) after reaction, solid and liquid are separated using the mode of vacuum filtration, certain temperature is added in a liquid
The regeneration of cold water progress lignin.Gained lignin particle is centrifuged, the lignin particle being collected by centrifugation is used
It after distilling water washing for several times, is freeze-dried, lignin particle is obtained after the completion of dry.Following table is several to go compared with high lignin
Except the partial size contrast table for the lignin particle that rate obtains.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. a kind of method of lignin in hydrotropes removal sawdust, which comprises the following steps:
(1) wood chip is ground into sawdust of the size less than 20 mesh in grinder；
(2) ground sawdust is added in hydrotropes solution, solid-to-liquid ratio 1:10-20 is carried out in constant temperature oscillation box
Reaction controls -90 DEG C of temperature 50 C, time 10-60min；
The hydrotropes are isopropyl toluene sodium sulfonate, sodium butylbenzene sulfonate, ethyl phenenyl azochlorosulfonate acid sodium, acid dimethyl
One kind of sodium, toluenesulfonic acid sodium salt, isooctane base sodium sulfonate, benzene sulfonic acid sodium salt, butyl sulfonic acid sodium；
(3) after reaction, solid and liquid are separated using the mode of vacuum filtration.
2. the method for lignin in hydrotropes removal sawdust according to claim 1, which is characterized in that described water-soluble
The hydrotropes aqueous solution of cosolvent solution mass concentration 40%-60%.
3. the method for lignin in hydrotropes removal sawdust according to claim 1, which is characterized in that the wood chip
For the one or more of many paper grade (stock) wood types such as Eucalyptus, Korean pine wood, poplar.
4. a kind of preparation method of lignin particle, which comprises the following steps:
It is added in the liquid that the method for lignin obtains in any one of claims 1 to 3 hydrotropes removal sawdust
The cold water that temperature is 5-10 DEG C, carries out the regeneration of lignin；Gained lignin particle is centrifuged, the wood collected
After quality particle is centrifuged washed several times with water with distilled water, it is freeze-dried.
5. the preparation method of lignin particle according to claim 4, which is characterized in that the rate of the centrifuge separation is
5000-10000r。
6. the preparation method of lignin particle according to claim 4, which is characterized in that described be centrifuged with distilled water is washed
Time be 5-20min.
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| CN201811167333.8A CN109518507A (en) | 2018-10-08 | 2018-10-08 | The method of lignin and the preparation method of lignin particle in a kind of hydrotropes removal sawdust |
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| CN201811167333.8A CN109518507A (en) | 2018-10-08 | 2018-10-08 | The method of lignin and the preparation method of lignin particle in a kind of hydrotropes removal sawdust |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111979817A (en) * | 2020-07-20 | 2020-11-24 | 云南云景林纸股份有限公司 | Method for removing lignin from plant fiber |
Citations (3)
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|---|---|---|---|---|
| CN102464802A (en) * | 2010-11-19 | 2012-05-23 | 北京林业大学 | Preparation method of lignin |
| CN104389216A (en) * | 2014-10-21 | 2015-03-04 | 国际竹藤中心 | Method for separating lignin and holocellulose from wood fiber raw materials and application thereof |
| CN106087513A (en) * | 2016-08-04 | 2016-11-09 | 北京林业大学 | A kind of fractionation method of sulfate-reducing conditions |
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2018
- 2018-10-08 CN CN201811167333.8A patent/CN109518507A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| CN102464802A (en) * | 2010-11-19 | 2012-05-23 | 北京林业大学 | Preparation method of lignin |
| CN104389216A (en) * | 2014-10-21 | 2015-03-04 | 国际竹藤中心 | Method for separating lignin and holocellulose from wood fiber raw materials and application thereof |
| CN106087513A (en) * | 2016-08-04 | 2016-11-09 | 北京林业大学 | A kind of fractionation method of sulfate-reducing conditions |
Non-Patent Citations (2)
| Title |
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| KORPINEN,R.等: "Lignin extraction from wood biomass by a hydrotropic solution", 《O’PAPEL》 * |
| LIHENG CHEN等: "Rapid and near-complete dissolution of wood lignin at≤80℃ by a recyclable acid hydrotrope", 《SCIENCE ADVANCES》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111979817A (en) * | 2020-07-20 | 2020-11-24 | 云南云景林纸股份有限公司 | Method for removing lignin from plant fiber |
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Application publication date: 20190326 |