CN107033367A - A kind of lignin extraction and modified method - Google Patents
A kind of lignin extraction and modified method Download PDFInfo
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- CN107033367A CN107033367A CN201611093408.3A CN201611093408A CN107033367A CN 107033367 A CN107033367 A CN 107033367A CN 201611093408 A CN201611093408 A CN 201611093408A CN 107033367 A CN107033367 A CN 107033367A
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- Prior art keywords
- lignin
- solid
- heating
- naoh
- modified method
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Classifications
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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
Abstract
The present invention relates to a kind of lignin extraction and modified method, step is as follows：(1) plant tissue smashed, suction filtration drying are first heat-treated with sulfuric acid；(2) use filtrate after NaOH alkali cleanings, suction filtration standby again；(3) heating removes the water constituent in filtrate, obtains alkali lignin solid；(4) lignin solid, NaOH solids, phenol and water are mixed, heat modification reaction.The present invention utilizes agricultural wastes, obtains polymolecularity, the lignin of high activity, reduces its destruction burnt to environment.
Description
Technical field
The present invention relates to material and chemical technology field, more particularly to a kind of lignin extraction and modified method.
Background technology
The world today, oil persistently skyrockets as non-renewable resources, price, causes being produced into for phenolic resin adhesive
This also more and more higher, and the phenol of one of important source material as phenolic resin adhesive, its price remain high for a long time.In order to
The production cost of phenolic resin adhesive is reduced, other more cheap raw materials are found instantly rather hot to replace phenol to become
The research topic of door.And continuing to develop with society, environmental protection is that this more must be used more required by social each side
Natural polymer replaces phenol and formaldehyde to turn into a kind of trend.
There is substantial amounts of aldehyde radical and hydroxyl in its structure as a kind of natural polyphenol family macromolecule polymer in lignin, therefore
The consumption of phenol and formaldehyde is reduced when this can be with phenol and formaldehyde novolak resin.But current acidity extraction lignin
Process is complicated, decentralization is poor, while its activity is not high, influences the popularization in novolak resin material of lignin.
The content of the invention
The present invention is a kind of method provided by the present invention to provide lignin extraction and modified method, reaches institute
The higher purpose of the lignin good dispersion of extraction, activity.
Technical scheme is as follows：
(1) plant tissue of crushing is taken, 5% sulfuric acid solution is added, immersion a period of time, then filters, drying filter residue is treated
With；
(2) the stand-by sample of drying in step (1) is dissolved in concentration 2mol/L NaOH solution, agitating and heating, then
Filtering, collects filtrate；
(3) filtrate in step (2) is subjected to heating evaporation, alkali lignin solid is obtained after going water removal；
(4) the alkali lignin solid in step (3), phenol, NaOH solids and deionized water are mixed, agitating and heating one
The section time, obtain activating lignin liquor.
Further, the crush plant tissue and the mass ratio of 5% sulfuric acid solution in step (1) are 10:1~1:1, heating
Temperature is 40~90 DEG C, and the time is 1~24h.
Further, the mass ratio of lignin solid and phenol is 1 in step (4):1~50:1, NaOH solid with it is wooden
The mass ratio of plain solid is 1:100~100:100, heating-up temperature is 40~90 DEG C, and the time is 1~24h.
The present invention has following superiority：
(1) lignin that alkali solution technique is extracted improves the decentralization of molecule；
(2) reaction of phenol and lignin improves the activity of lignin.
Embodiment
The present invention is described in further details with specific embodiment below, but the present invention is not only limited in detail below in fact
Example is applied, but illustrated embodiment is not necessarily referring to the lignin liquor of optimal applicable elements.
Embodiment one
(1) plant tissue after 90g crushing is taken to be placed in 30g 5% sulfuric acid, 70 DEG C of heating stirring 3h.Then filter, wash
Wash, be put into baking oven and dry 24h；
(2) solid after drying is placed in 1L 2mol/L NaOH solution, then 80 DEG C of heating stirring 10h filter,
Collect filtrate；
(3) alkali lignin solid is obtained after the filtrate in step (2) being heated into 100 DEG C of evaporation water constituents, 24h；
(4) 100g alkali lignins solid, 2g phenol, 1g NaOH solids and 20g deionized waters are blended, are warming up to 50 DEG C,
Heating stirring 3h.Produce modified lignin resin.
Embodiment two
(1) plant tissue after 30g crushing is taken to be placed in 30g 5% sulfuric acid, 70 DEG C of heating stirring 1h.Then filter, wash
Wash, be put into baking oven and dry 24h；
(2) solid after drying is placed in 1L 2mol/L NaOH solution, then 80 DEG C of heating stirring 15h filter,
Collect filtrate；
(3) alkali lignin solid is obtained after the filtrate in step (2) being heated into 100 DEG C of evaporation water constituents, 24h；
(4) 100g alkali lignins solid, 2g phenol, 1g NaOH solids and 20g deionized waters are blended, are warming up to 50 DEG C,
Heating stirring 3h.Produce modified lignin resin.
Embodiment three
(1) plant tissue after 300g crushing is taken to be placed in 30g 5% sulfuric acid, 70 DEG C of heating stirring 14h.Then filter,
Washing, is put into baking oven and dries 24h；
(2) solid after drying is placed in 1L 2mol/L NaOH solution, then 80 DEG C of heating stirring 15h filter,
Collect filtrate；
(3) alkali lignin solid is obtained after the filtrate in step (2) being heated into 100 DEG C of evaporation water constituents, 24h；
(4) 100g alkali lignins solid, 2g phenol, 1g NaOH solids and 20g deionized waters are blended, are warming up to 50 DEG C,
Heating stirring 3h.Produce modified lignin resin.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For the personnel of the technical field of the invention, this is not being departed from
On the premise of inventive concept, many simple deduction or replace can be also made, protection scope of the present invention should be all considered as belonging to.
Claims (3)
1. a kind of lignin extraction and modified method, it is characterized in that, comprise the following steps：
(1) plant tissue of crushing is taken, 5% sulfuric acid solution is added, immersion a period of time, then filtering, drying filter residue are stand-by；
(2) the stand-by sample of drying in step (1) is dissolved in concentration 2mol/L NaOH solution, then agitating and heating filters,
Collect filtrate；
(3) filtrate in step (2) is subjected to heating evaporation, alkali lignin solid is obtained after going water removal；
(4) the alkali lignin solid in step (3), phenol, NaOH solids and deionized water are mixed, during one section of agitating and heating
Between, obtain activating lignin liquor.
2. lignin extraction according to claim 1 and modified method, it is characterised in that：Crushing in step (1) is planted
The mass ratio of thing tissue and 5% sulfuric acid solution is 10:1~1:1, heating-up temperature is 40~90 DEG C, and the time is 1~24h.
3. lignin extraction according to claim 1 and modified method, it is characterised in that：Lignin is consolidated in step (4)
The mass ratio of body and phenol is 1:1~50:The mass ratio of 1, NaOH solid and lignin solid is 1:100~100:100, heating
Temperature is 40~90 DEG C, and the time is 1~24h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611093408.3A CN107033367A (en) | 2016-12-02 | 2016-12-02 | A kind of lignin extraction and modified method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611093408.3A CN107033367A (en) | 2016-12-02 | 2016-12-02 | A kind of lignin extraction and modified method |
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| Publication Number | Publication Date |
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| CN107033367A true CN107033367A (en) | 2017-08-11 |
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| CN201611093408.3A Pending CN107033367A (en) | 2016-12-02 | 2016-12-02 | A kind of lignin extraction and modified method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161032A (en) * | 2018-08-21 | 2019-01-08 | 上海昶法新材料有限公司 | A kind of extracting method of lignin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892877A (en) * | 2015-06-09 | 2015-09-09 | 中国林业科学研究院林产化学工业研究所 | Phenolated lignin modified expandable resorcinol-phenol-formaldehyde resin and preparation method thereof |
-
2016
- 2016-12-02 CN CN201611093408.3A patent/CN107033367A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892877A (en) * | 2015-06-09 | 2015-09-09 | 中国林业科学研究院林产化学工业研究所 | Phenolated lignin modified expandable resorcinol-phenol-formaldehyde resin and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘纲勇等: ""麦草碱木素酚化改性及其制备 LPF 胶粘剂工艺研究"", 《高校化学工程学报》 * |
| 陈洪卓: ""木质素及其复合物在环氧树脂胶粘剂中的应用研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161032A (en) * | 2018-08-21 | 2019-01-08 | 上海昶法新材料有限公司 | A kind of extracting method of lignin |
| CN109161032B (en) * | 2018-08-21 | 2021-01-26 | 上海昶法新材料有限公司 | Method for extracting lignin |
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Application publication date: 20170811 |
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