CN109161032A - A kind of extracting method of lignin - Google Patents
A kind of extracting method of lignin Download PDFInfo
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- CN109161032A CN109161032A CN201810954964.8A CN201810954964A CN109161032A CN 109161032 A CN109161032 A CN 109161032A CN 201810954964 A CN201810954964 A CN 201810954964A CN 109161032 A CN109161032 A CN 109161032A
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- lignin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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Abstract
The invention discloses a kind of extracting methods of lignin, and its step are as follows: the plant tissue of crushing is heat-treated by the separation of lignin with inorganic acid, is filtered, is dried；The extraction of lignin, the sample alkaline matter for processing that will be dried in above-mentioned steps, filtering retain filtrate；The purification of lignin: being added suitable nonionic surfactant in the resulting filtrate of above-mentioned steps, and heating stirring filters to get lignin solid is arrived.Lignin solid obtained by the method for the invention has many advantages, such as that purity is high, water content is low, soluble impurity is few, and eliminates the process of evaporation water, and extraction time and the cost of lignin is greatly saved.
Description
Technical field
The present invention relates to materials and chemical technology field, and in particular to a kind of extracting method of lignin.
Background technique
It is well known that petroleum is the blood of modern industry, while petroleum is also a kind of non-renewable resource.Find one kind
The new resource instead of petroleum is extremely urgent.Phenolic resin, needed for phenol be mainly derived from petroleum.In order to reduce
The production cost of phenolic resin is badly in need of the new reproducible raw material of one kind to substitute petroleum.Lignin is as a kind of reproducible
Natural Polyphenols high molecular polymer, there are a large amount of aldehyde radical and hydroxyls in structure, so can close with phenol and formaldehyde
At the dosage for reducing phenol and formaldehyde when phenolic resin.But current acidity extraction lignin process is complicated, dispersion degree is poor, together
When its activity it is not high, influence the popularization in novolak resin material of lignin.
Chinese patent CN107033367A discloses a kind of lignin extraction and modified method, and very good solution is wooden
The dispersion of element, simplifies the process of extraction.But the lignin water-retention value obtained in this way is higher, and contains centainly
Water-solubility impurity.
Summary of the invention
The present invention is to solve the above problem in the prior art, a kind of extracting method of lignin of proposition.
The extracting method of lignin provided by the invention leads in last extraction process and a certain amount of nonionic table is added
Face activating agent, to achieve the purpose that different material and lignin separation.The lignin extracted, the wood obtained with commonsense method
Quality is compared, and water-retention value is lower, and impurity is also less.
To achieve the above object, the invention adopts the following technical scheme:
The present invention provides a kind of extracting methods of lignin, comprising the following steps:
(1) separation of lignin: the plant tissue of crushing is heat-treated with inorganic acid, is filtered, is dried, spare；
(2) extraction of lignin: the sample alkaline matter for processing that will be dried in step (1), filtering retain filtrate；
(3) purification of lignin: being added suitable nonionic surfactant in step (2) resulting filtrate, heating
Stirring filters the lignin solid to get high-purity.
Further, in step (1), the plant tissue that every 100g is crushed, the inorganic acid dosage is 5g-40g.
Further, in step (1), the inorganic acid is selected from least one of sulfuric acid, hydrochloric acid.
Further, in step (1), controlled at 140-180 DEG C when the heat treatment.
Further, in step (1), the drying temperature is 90-100 DEG C, drying time 2-5h.
Further, in step (2), the plant tissue that every 100g is crushed, the alkaline matter dosage is 0.5L-1L.
Further, in step (2), the alkaline matter is the NaOH solution of 2mol/L.
Further, in step (3), the plant tissue that every 100g is crushed, the dosage of the nonionic surfactant is
0.1g-0.5g。
Further, in step (3), the nonionic surfactant is selected from -10 (OP- of polyoxethylene octylphenyl phenol ether
10), at least one of nonylphenol polyoxyethylene ether -10 (NP-10), fatty alcohol polyoxyethylene ether (AEO-9).
The main functional group of lignin has methoxyl group, phenolic hydroxyl group, alcoholic extract hydroxyl group, carbonyl and carboxyl etc., and lignin knot
Most of phenolic hydroxyl group in structure is all connected in the form of ehter bond with other structures.Moreover, containing a large amount of benzene ring structure.Institute
With lignin has good hydrophobic oleophilic oil.The present invention is found surprisingly that in experiment, is added during extracting lignin
Enter certain nonionic emulsifier, lignin can be wrapped up wherein, be allowed to completely cut off completely with water phase and come.May be because,
Lignin is wrapped in the inside by the lipophilic group of surfactant, forms a stable protective layer.Because of this status of lignin
Son amount is larger, can not form nanoscale droplet, and the lignin for being emulsified agent package is made to be easier to precipitate instead.
Moreover, because the reason of emulsifier, some water-soluble substances adulterated in lignin are ostracised in water phase,
It cannot be introduced into the lignin wrapped up inside emulsifier, so that the lignin extracted is purer.
The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that
The extracting method of lignin provided by the invention leads in last extraction process and a certain amount of nonionic table is added
Face activating agent, to achieve the purpose that different material and lignin separation；The lignin extracted, the wood obtained with commonsense method
Quality is compared, and water-retention value is lower, and clarity is high, and impurity is also less；And the process of evaporation water is eliminated, so greatly save
The extraction time of lignin and cost.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
Embodiment 1
The smashed plant tissue of 100g is taken to be placed in 50% hydrochloric acid of 80g, 150 DEG C are stirred 8 hours, and then plus water is by salt
Acid is diluted to 5%, flows back 2 hours at 150 DEG C.Then it is filtered, washed, is put into baking oven in 92 DEG C of drying 2h.After drying
Solid is placed in the NaOH solution of the 2mol/L of 1L, is added 0.2g polyoxethylene octylphenyl phenol ether -10 (OP-10), is stirred at 70 DEG C
It mixes 2 hours, filters, lignin solid can be obtained.
Embodiment 2
The smashed plant tissue of 100g is taken to be placed in 25% sulfuric acid of 40g, 180 DEG C of heating stirring 5h.Then it filters, wash
It washs, is put into baking oven in 100 DEG C of drying 2.5h；Solid after drying is placed in the NaOH solution of the 2mol/L of 0.5L, adds 0.5
Gram fatty alcohol polyoxyethylene ether (AEO-9) stirs 5 hours under room temperature, lignin solid is obtained after suction filtration；
Embodiment 3
The smashed plant tissue of 100g is taken to be placed in 5% sulfuric acid of 100g, 140 DEG C of heating stirring 6h.Then it filters, wash
It washs, is put into baking oven in 95 DEG C of drying 3h；Solid after drying is placed in the NaOH solution of the 2mol/L of 1L, is added 0.3 gram
Nonylphenol polyoxyethylene ether -10 (NP-10) stirs 3 hours at 50 DEG C, lignin solid can be obtained after suction filtration.
Comparative example:
According to the method that patent CN107033367A is provided, the lignin solid of extraction.
Performance detection:
1) carrying out determination of moisture to lignin solid obtained by above-described embodiment 1-3 and comparative example (uses SFY-20T type quick
Moisture Meter measures), test result is as follows shown in table 1:
Table 1:
| Serial number | Moisture content (%) |
| Comparative example | 5% |
| Embodiment 1 | 0.9% |
| Embodiment 2 | 0.7% |
| Embodiment 3 | 0.7% |
2) dirt content test is carried out to lignin solid obtained by above-described embodiment 1-3 and comparative example and (passes through sample
Content of ashes indicates), test result is as follows shown in table 2:
Table 2:
| Serial number | Ash content (%) |
| Comparative example | 4% |
| Embodiment 1 | 0.10% |
| Embodiment 2 | 0.15% |
| Embodiment 3 | 0.09% |
3) effective content measurement is carried out (in conjunction with Klason to lignin solid obtained by above-described embodiment 1-3 and comparative example
Method and ultraviolet spectrophotometry detect), test result is as follows shown in table 3:
Table 3:
| Serial number | Effective content (%) |
| Comparative example | 90.7% |
| Embodiment 1 | 96.6% |
| Embodiment 2 | 96.2% |
| Embodiment 3 | 95.9% |
It can be seen that the content low 1% of moisture in lignin solid obtained by the present invention from result in table 1-3, and can
The impurity content of dissolubility is even more to be lower than 0.02%.On effective content, compared with comparative example, and reach 95% or more.This
The extracting method of invention overcomes original technical disadvantages to a certain extent, provides a kind of more preferably lignin extraction side
Method.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (9)
1. a kind of extracting method of lignin, which comprises the following steps:
(1) separation of lignin: the plant tissue of crushing is heat-treated with inorganic acid, is filtered, is dried, spare；
(2) extraction of lignin: the sample alkaline matter for processing that will be dried in step (1), filtering retain filtrate；
(3) purification of lignin: being added suitable nonionic surfactant in step (2) resulting filtrate, heating stirring,
Filter the lignin solid to get high-purity.
2. the extracting method of lignin according to claim 1, which is characterized in that in step (1), the plant of every 100g crushing
Object tissue, the inorganic acid dosage are 5g-40g.
3. the extracting method of lignin according to claim 1, which is characterized in that in step (1), the inorganic acid is selected from
At least one of sulfuric acid, hydrochloric acid.
4. the extracting method of lignin according to claim 1, which is characterized in that in step (1), the heat treatment time control
Temperature processed is 140-180 DEG C.
5. the extracting method of lignin according to claim 1, which is characterized in that in step (1), the drying temperature is
90-100 DEG C, drying time 2-5h.
6. the extracting method of lignin according to claim 1, which is characterized in that in step (2), the plant of every 100g crushing
Object tissue, the alkaline matter dosage are 0.5L-1L.
7. the extracting method of lignin according to claim 6, which is characterized in that in step (2), the neutral and alkali substance
For the NaOH solution of 2mol/L.
8. the extracting method of lignin according to claim 1, which is characterized in that in step (3), the plant of every 100g crushing
Object tissue, the dosage of the nonionic surfactant are 0.1g-0.5g.
9. the extracting method of lignin according to claim 8, which is characterized in that in step (3), the non-ionic surface
Activating agent is selected from polyoxethylene octylphenyl phenol ether -10 (OP-10), nonylphenol polyoxyethylene ether -10 (NP-10), fatty alcohol polyoxy
At least one of vinethene (AEO-9).
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| CN201810954964.8A CN109161032B (en) | 2018-08-21 | 2018-08-21 | Method for extracting lignin |
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| CN201810954964.8A CN109161032B (en) | 2018-08-21 | 2018-08-21 | Method for extracting lignin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818912A (en) * | 2019-10-23 | 2020-02-21 | 广东工业大学 | Method for rapidly preparing nanoscale lignin |
| CN115418003A (en) * | 2022-10-14 | 2022-12-02 | 安徽工业大学 | Method for recovering lignin precipitate in strengthening alkali pretreatment liquid |
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| CN110818912A (en) * | 2019-10-23 | 2020-02-21 | 广东工业大学 | Method for rapidly preparing nanoscale lignin |
| CN115418003A (en) * | 2022-10-14 | 2022-12-02 | 安徽工业大学 | Method for recovering lignin precipitate in strengthening alkali pretreatment liquid |
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| CN109161032B (en) | 2021-01-26 |
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Application publication date: 20190108 Assignee: JINING MINGSHENG NEW MATERIAL Co.,Ltd. Assignor: SHANGHAI CHANGFA NEW MATERIAL Co.,Ltd. Contract record no.: X2021310000048 Denomination of invention: A method for extracting lignin Granted publication date: 20210126 License type: Common License Record date: 20211215 |