CN106046393B - A kind of bamboo liquefied method - Google Patents
A kind of bamboo liquefied method Download PDFInfo
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- CN106046393B CN106046393B CN201610556933.8A CN201610556933A CN106046393B CN 106046393 B CN106046393 B CN 106046393B CN 201610556933 A CN201610556933 A CN 201610556933A CN 106046393 B CN106046393 B CN 106046393B
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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
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
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Abstract
The present invention provides a kind of bamboo liquefied methods, include the following steps: that (1) pre-processes: by bamboo wood crushed material using hot water in 80-90 DEG C after digestion 8-10 hours, filtering, again using ethyl acetate-isopropanol mixed solvent in 70-85 DEG C extracting 12-24 hours, it filters, pretreated bamboo wood powder is obtained after filtration cakes torrefaction；(2) it liquefies: by bamboo wood powder, phenol and catalyst BF pretreated obtained by part steps (1)3It is added in reaction vessel, is stirred to react in 100-120 DEG C 4-6 hours, remaining pretreated bamboo wood powder is during which added portionwise, filters while hot after reaction, filtrate is bamboo liquefied substance.The present invention is first preprocessed by bamboo wood crushed material, utmostly removes the impurity for being wherein not involved in Liquefaction Products in Phenol and formaldehyde condensation reaction, reduces liquefied substance and prepares impurity content in phenolic resin product, improves phenol product assay in liquefied substance.
Description
Technical field
The invention belongs to bamboo processing processing technology fields, and in particular to a kind of bamboo liquefied method.
Background technique
Bamboo be the important component of the forest reserves be known as the second forest title China be located in the world's bamboo distribution in
Heart bamboo grove area ranks first in the world, and is mainly distributed on southern 17 provinces, various with the further rise of bamboo processing industry
Bamboo wood defective material is also stepped up.Therefore, it is significant to develop the huge regenerated resources progress deep processing of this energy storage.
Bamboo wood is a kind of perennial natural plants trunk, and chemical component is more complicated.Research shows that: cellulose, half fiber
Dimension element, lignin be the main component to form bamboo culm wall, directly participation bamboo wood material formation, three's total amount 90% with
On, wherein content of cellulose accounts for 40%~60%, and bamboo wood also contains grease, sugar other than containing cellulose, hemicellulose, lignin
Class and protein-based equal substances.In addition, also containing a small amount of ash content and extract.
Bamboo liquefied is one of the effective ways of bamboo wood comprehensive utilization, and bamboo liquefied refers to the presence in certain organic matters
Under, convert bamboo wood to the thermochemical process of liquid, and then bamboo wood defective material can be changed into the high macromolecule material of application value
Material.It is one of the effective means of bamboo wood trans-utilization using bamboo wood and its waste-material-preparing bamboo liquefied substance phenolic resin.It is right at present
Thermosetting phenolic resin, especially based Wood Adhesives, phenolic foam material are focused primarily upon in bamboo wood and its waste modified resin
Deng.
Chinese patent CN102504275A generates bamboo liquefied product using phenol and polyethylene glycol collective effect, and uses
Acid as catalyst, synthesis under normal pressure 30-90min, reaction temperature are 110-170 DEG C.It can be obtained using the liquifying method that the patent provides
Higher liquefied fraction, but use made from the method in liquefied substance containing grease, carbohydrate and the impurity such as protein-based, three
Content is up to 10%, these impurity are present in the adhesive and phenolic foam products of the subsequent preparation of bamboo liquefied substance, and in product
From its internal precipitation in use process, the performance of product is greatly reduced.Therefore, a kind of bamboo liquefied of low impurity content is developed
Object preparation method becomes urgent problem to be solved.
Summary of the invention
The present invention provides a kind of bamboo liquefied methods, include the following steps:
(1) it pre-processes: by bamboo wood crushed material using hot water in 80-90 DEG C after digestion 8-10 hour, filtering, then using second
Acetoacetic ester-isopropanol mixed solvent in 70-85 DEG C extracting 12-24 hours, filtering, after filtration cakes torrefaction pretreated bamboo wood
Powder.In addition to containing main component cellulose, hemicellulose, lignin in bamboo wood, also containing grease, carbohydrate and protein-based etc.
Impurity, these impurity are simultaneously not involved in the liquefaction reaction and subsequent and formaldehyde condensation reaction of phenol, but in the form of impurity
It is present in the phenolic resin product of bamboo liquefied substance, and constantly moves to surface from inside in product use process, influences
The performance and stability of product.80-90 DEG C of hot water digestion bamboo wood crushed material is first used, convenient for the removing of bamboo fiber, so that miscellaneous
Matter separate out, then extracted using mixed solvent ethyl acetate-isopropanol, impurity is further dissolved in the mixed solvent, from
And impurity is utmostly removed, improve liquefied substance purity.
(2) it liquefies: by bamboo wood powder, phenol and catalyst BF pretreated obtained by part steps (1)3Reaction is added
It in container, is stirred to react in 100-120 DEG C 4-6 hours, remaining pretreated bamboo wood powder is during which added portionwise, reaction terminates
It filters while hot afterwards, filtrate is bamboo liquefied substance.
Preferably, the mass ratio of bamboo wood crushed material described in step (1) and hot water is 1:10-20.
Preferably, the dosage of mixed solvent described in step (1) is 15-20 times of bamboo wood crushed material quality.
Preferably, the mass ratio of the in the mixed solvent ethyl acetate and isopropanol is 1:1.5-2, using the proportion
MIXED SOLVENT EXTRACTION effect is best.
Preferably, the mass ratio of the pretreated bamboo wood powder, phenol and catalyst is 1:2-3:0.05-
0.12。
The invention has the benefit that
The present invention is first preprocessed by bamboo wood crushed material, utmostly removes and is wherein not involved in Liquefaction Products in Phenol and formaldehyde condensation
The impurity of reaction reduces liquefied substance and prepares impurity content in phenolic resin product, improves phenol product assay in liquefied substance.
Specific embodiment
In order to which technical solution of the present invention and advantage is more clearly understood, with reference to embodiments to the present invention carry out into
One step is described in detail.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit this hair
It is bright.
Embodiment 1
(1) pre-process: 10g bamboo wood crushed material and 100g deionized water are placed in there-necked flask, in 90 DEG C digestion 8 hours
Afterwards, it filters, then 150g mass ratio is used to extract 24 hours for the mixed solvent of the ethyl acetate-isopropanol of 1:1.5 in 70 DEG C,
It filters, the pretreated bamboo wood powder of 9.2g is obtained after filtration cakes torrefaction；
(2) it liquefies: by bamboo wood powder, 18g phenol and 0.9g catalyst BF pretreated obtained by 3g step (1)3It is added
It in there-necked flask, is stirred to react in 100 DEG C 6 hours, the pretreated bamboo wood powder of remaining 6g, reaction knot is during which added in three batches
It is filtered while hot after beam, filtrate is bamboo liquefied substance.
Embodiment 2
(1) pre-process: 10g bamboo wood crushed material and 150g deionized water are placed in there-necked flask, in 80 DEG C digestion 10 hours
Afterwards, it filters, then 180g mass ratio is used to extract 20 hours for the mixed solvent of the ethyl acetate-isopropanol of 1:1.8 in 80 DEG C,
It filters, the pretreated bamboo wood powder of 9.0g is obtained after filtration cakes torrefaction；
(2) it liquefies: by bamboo wood powder, 22.5g phenol and 0.45g catalyst BF pretreated obtained by 3g step (1)3
It is added in there-necked flask, is stirred to react in 110 DEG C 5 hours, the pretreated bamboo wood powder of remaining 6g is during which added in three batches, instead
It is filtered while hot after answering, filtrate is bamboo liquefied substance.
Embodiment 3
(1) pre-process: 10g bamboo wood crushed material and 200g deionized water are placed in there-necked flask, in 85 DEG C digestion 9 hours
Afterwards, it filters, then 270g mass ratio is used to extract 12 hours for the mixed solvent of the ethyl acetate-isopropanol of 1:2 in 85 DEG C, mistake
It filters, the pretreated bamboo wood powder of 9.0g is obtained after filtration cakes torrefaction；
(2) it liquefies: by bamboo wood powder, 27g phenol and 1.08g catalyst BF pretreated obtained by 3g step (1)3Add
Enter in there-necked flask, be stirred to react in 120 DEG C 4 hours, the pretreated bamboo wood powder of remaining 6g is during which added in three batches, reacts
After filter while hot, filtrate is bamboo liquefied substance.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (1)
1. a kind of bamboo liquefied method, which is characterized in that the bamboo liquefied method includes the following steps:
(1) it pre-processes: by bamboo wood crushed material using hot water in 80-90 DEG C after digestion 8-10 hour, filtering, then using acetic acid second
Ester-isopropanol mixed solvent in 70-85 DEG C extracting 12-24 hours, filtering, after filtration cakes torrefaction pretreated bamboo wood powder
End；
(2) it liquefies: reaction vessel is added in bamboo wood powder pretreated obtained by part steps (1), phenol and catalyst BF3
In, it is stirred to react in 100-120 DEG C 4-6 hours, remaining pretreated bamboo wood powder is during which added portionwise, takes advantage of after reaction
Heat filtering, filtrate are bamboo liquefied substance;The mass ratio of bamboo wood crushed material described in step (1) and hot water is 1:10-20;Step
Suddenly the dosage of mixed solvent described in (1) is 15-20 times of bamboo wood crushed material quality;The in the mixed solvent ethyl acetate with
The mass ratio of isopropanol is 1:1.5-2;The mass ratio of the pretreated bamboo wood powder, phenol and catalyst is 1:2-3:
0.05-0.12。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610556933.8A CN106046393B (en) | 2016-07-15 | 2016-07-15 | A kind of bamboo liquefied method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610556933.8A CN106046393B (en) | 2016-07-15 | 2016-07-15 | A kind of bamboo liquefied method |
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| Publication Number | Publication Date |
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| CN106046393A CN106046393A (en) | 2016-10-26 |
| CN106046393B true CN106046393B (en) | 2019-03-05 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619547B (en) * | 2009-07-27 | 2012-04-04 | 黄山学院 | Method of high-value comprehensive utilization of bamboo remainders |
| CN101885825B (en) * | 2010-07-21 | 2012-03-28 | 华南理工大学 | Plant fiber-based polyol, preparation method thereof and use thereof |
| CN102633886A (en) * | 2011-02-11 | 2012-08-15 | 李翠花 | Method for preparing plant-based polyether polyol by straw liquefaction |
| CN103554400A (en) * | 2013-10-14 | 2014-02-05 | 中国林业科学研究院林产化学工业研究所 | Liquefaction method of lignin for preparing thermoplastic phenolic resin |
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Effective date of registration: 20191106 Address after: Anji County, Zhejiang province 313300 Huzhou City Dipu Street martyr Tower Village Patentee after: Zhejiang Kun Hong new materials Co., Ltd. Address before: Anji County, Zhejiang province 314422 Huzhou City Dipu Town Tower Village Industrial Zone ' Patentee before: ANJI WEILONG WPC ENVIRONMENTAL PROTECTION MATERIALS CO., LTD. |