CN106010396B - A kind of preparation method of bamboo liquefied substance base adhesive - Google Patents
A kind of preparation method of bamboo liquefied substance base adhesive Download PDFInfo
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- CN106010396B CN106010396B CN201610556931.9A CN201610556931A CN106010396B CN 106010396 B CN106010396 B CN 106010396B CN 201610556931 A CN201610556931 A CN 201610556931A CN 106010396 B CN106010396 B CN 106010396B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The present invention provides a kind of preparation method of bamboo liquefied substance base adhesive, the specific steps are：Will bamboo liquefied substance be added reaction vessel in, use NaOH adjust its PH be 89, addition 37% formalin, after 80 95 DEG C are reacted 46 hours, it is cooled to 30 40 DEG C and is added surfactants and montmorillonite, after 20 40min of insulated and stirred, obtain bamboo liquefied substance base adhesive.Used bamboo liquefied substance is preprocessed and liquefaction is made, and impurity content is low, and phenol product assay is high, and obtained adhesive small molecular impurity content is low, improves the adhesive strength and weatherability of adhesive.
Description
Technical field
The invention belongs to technical field of adhesive preparation, and in particular to the preparation method of bamboo liquefied substance base adhesive.
Background technology
Bamboo is that the important component of the forest reserves is known as title China of the second forest and is located in the distribution of world bamboo
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 composition 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.
Fu abyss etc.（Performance [D] the Beijing Forestry University of bamboo liquefied resinification kinetics and its product,
2010）Resin adhesive is successfully prepared under the catalysis of alkali using bamboo product rejectable waste Liquefaction Products in Phenol object and formaldehyde, it should
Adhesive is similar to the conventional structure of adhesive.But contain remaining grease, carbohydrate and protein in bamboo wood in the adhesive
The impurity such as class leverage the bond properties of product from its internal migration to surface during adhesive use.
Invention content
The present invention provides a kind of preparation method of bamboo liquefied substance base adhesive, concrete operation method is：
Bamboo liquefied substance is added in reaction vessel, uses NaOH to adjust its PH as 8-9,37% formalin is added, in
After 80-95 DEG C of reaction 4-6 hour, it is cooled to 30-40 DEG C of addition surfactant and montmorillonite, after insulated and stirred 20-40min,
Obtain bamboo liquefied substance base adhesive；
Lignin, cellulose and hemicellulose decompose after bamboo liquefied, and are grafted with phenolic hydroxyl group ring, generate a series of phenolate
Product, then carry out with formaldehyde being condensed obtained adhesive is added surfactant and illiteracy with lamellar structure is de- after reaction
Soil so that adhesive polymer strand and montmorillonite are effectively compound, on the one hand can increase the mechanical performance of adhesive, another party
Face, remaining a small amount of non-phenolate impurity in products is embedded by montmorillonite layer in bamboo liquefied substance, is reduced its molecular migration, is improved glue
The bond properties and weather resistance of stick.
The preparation method of the bamboo liquefied substance includes the following steps：
(1) it pre-processes：By bamboo wood crushed material using hot water after 80-90 DEG C of digestion 8-10 hour, filtering, then using second
The mixed solvent of acetoacetic ester-isopropanol extracts 12-24 hours in 70-85 DEG C, filtering, and pretreated bamboo wood is obtained after filtration cakes torrefaction
Powder.In addition to containing main component cellulose, hemicellulose, lignin in bamboo wood, also contain 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 surface is moved to from inside during product use, influences
The performance and stability of product.80-90 DEG C of hot water digestion bamboo wood crushed material is first used, is convenient for the stripping 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 bamboo liquefied substance, 37% formalin, surfactant and the mass ratio of montmorillonite are 1：
1.2-1.6:0.03-0.05:0.1-0.3。
Preferably, the surfactant is sodium sulfate of polyethenoxy ether of fatty alcohol, dodecyl sodium sulfate or single ten
Dialkyl phosphate potassium.
Preferably, the mass ratio of bamboo wood crushed material and hot water described in step (1) 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 proportioning
MIXED SOLVENT EXTRACTION best results.
Preferably, the mass ratio of the pretreated bamboo wood powder, phenol and catalyst is 1:2-3:0.05-
0.12。
Beneficial effects of the present invention are：
1, 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 contracting
The impurity for closing reaction, improves phenol product assay in liquefied substance.
2, adhesive is prepared using the bamboo liquefied substance of low impurity content of the present invention, product small molecular impurity contains
It measures low, improves the adhesive strength and weatherability of adhesive.
3, montmorillonite and surfactant are added in adhesive preparation process, is increasing the same of adhesive mechanical performance
When, it is further reduced non-phenolate impurity in products mobility, improves the adhesive strength and weatherability of adhesive.
Specific implementation mode
In order to make technical scheme of the present invention and advantage be more clearly understood, with reference to embodiments to the present invention into traveling
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) it pre-processes：10g bamboo woods crushed material and 100g deionized waters are placed in there-necked flask, in 90 DEG C of digestions 8 hours
Afterwards, it filters, then uses 150g mass ratioes for 1:The mixed solvent of 1.5 ethyl acetate-isopropanol extracts 24 hours 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 steps (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, obtains filtrate 14.2g, as bamboo liquefied substance；
(3) it polymerize：10g bamboo liquefied substances are added in there-necked flask, uses 20%NaOH- aqueous solutions to adjust its PH as 8, adds
Enter 37% formalins of 12g, after 80 DEG C are reacted 6 hours, is cooled to 30 DEG C of addition 4g sodium sulfate of polyethenoxy ether of fatty alcohol
With 2g montmorillonites, after insulated and stirred 30min, bamboo liquefied substance base adhesive is obtained, product viscosity is 900mPaS at 25 DEG C,
Hardening time is 40S, by product in laminated wood product, detection to be carried out according to IG/T 3026-1995 standards, bonding strength
For 2.52MPa.
Embodiment 2
(1) it pre-processes：10g bamboo woods crushed material and 150g deionized waters are placed in there-necked flask, in 80 DEG C of digestions 10 hours
Afterwards, it filters, then uses 180g mass ratioes for 1:The mixed solvent of 1.8 ethyl acetate-isopropanol extracts 20 hours 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 steps (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, obtains filtrate 18.3g, as bamboo liquefied substance.
(3) it polymerize：10g bamboo liquefied substances are added in there-necked flask, 20%NaOH- aqueous solutions is used to adjust its PH as 8.5,
37% formalins of 15g are added, after 90 DEG C are reacted 5 hours, is cooled to 35 DEG C and 3g dodecyl sodium sulfates and 1g illiteracies is added
De- soil after insulated and stirred 20min, obtains bamboo liquefied substance base adhesive, and product viscosity is 850mPaS at 25 DEG C, when solidification
Between be 55S, by product in laminated wood product, detection to be carried out according to IG/T 3026-1995 standards, bonding strength is
2.25MPa。
Embodiment 3
(1) it pre-processes：10g bamboo woods crushed material and 200g deionized waters are placed in there-necked flask, in 85 DEG C of digestions 9 hours
Afterwards, it filters, then uses 270g mass ratioes for 1:The mixed solvent of 2 ethyl acetate-isopropanol extracts 12 hours 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 steps (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, obtain filtrate 19.2g, as bamboo liquefied substance.
(3) it polymerize：10g bamboo liquefied substances are added in there-necked flask, uses 20%NaOH- aqueous solutions to adjust its PH as 9, adds
Enter 37% formalins of 16g, after 85 DEG C are reacted 4 hours, is cooled to 40 DEG C and 5g Monododecylphosphates potassium and 3g is added
Montmorillonite after insulated and stirred 40min, obtains bamboo liquefied substance base adhesive, and product viscosity is 1090mPaS, solidification at 25 DEG C
Time is 62S, by product in laminated wood product, detection foundation IG/T 3026-1995 standards to carry out, and bonding strength is
2.46MPa。
Comparative example 1
(1) it liquefies：By 3g bamboo woods powder, 18g phenol and 0.9g catalyst BF3It is added in there-necked flask, in 100 DEG C of stirrings
Reaction 6 hours, is during which added the pretreated bamboo wood powder of remaining 6g, filters while hot after reaction, obtain filtrate in three batches
13.8g, as bamboo liquefied substance；.
(2) it polymerize：10g bamboo liquefied substances are added in there-necked flask, uses 20%NaOH- aqueous solutions to adjust its PH as 9, adds
Enter 37% formalins of 16g, after 85 DEG C are reacted 4 hours, is cooled to 40 DEG C and 5g Monododecylphosphates potassium and 3g is added
Montmorillonite after insulated and stirred 40min, obtains bamboo liquefied substance base adhesive, and product viscosity is 820mPaS, solidification at 25 DEG C
Time is 78S, by product in laminated wood product, detection foundation IG/T 3026-1995 standards to carry out, and bonding strength is
1.53MPa。
Pass through comparative example 1 and comparative example 1, it can be deduced that：After pretreatment, obtained adhesive is glued for bamboo wood
Intensity higher.
Comparative example 2
(1) it pre-processes：10g bamboo woods crushed material and 100g deionized waters are placed in there-necked flask, in 90 DEG C of digestions 8 hours
Afterwards, it filters, then uses 150g mass ratioes for 1:The mixed solvent of 1.5 ethyl acetate-isopropanol extracts 24 hours 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 steps (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, obtains filtrate 14.2g, as bamboo liquefied substance；
(3) it polymerize：10g bamboo liquefied substances are added in there-necked flask, uses 20%NaOH- aqueous solutions to adjust its PH as 8, adds
Enter 37% formalins of 12g, after 80 DEG C of reactions 6 hours, is cooled to 30 DEG C and obtains bamboo liquefied substance base adhesive, at 25 DEG C
Product viscosity is 650mPaS, hardening time 110S, by product in laminated wood product, detection to be according to IG/T 3026-
1995 standards carry out, bonding strength 1.78MPa.
Pass through comparative example 1 and comparative example 2, it can be deduced that：Montmorillonite and the addition of surfactant are conducive to improve
Adhesive bonding strength shortens its hardening time.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, on the premise of not exceeding the technical scheme recorded in the claims also other variations and modifications.
Claims (6)
1. a kind of preparation method of bamboo liquefied substance base adhesive, which is characterized in that the preparation method is that：
Bamboo liquefied substance is added in reaction vessel, uses NaOH to adjust its p H as 8-9,37% formalin is added, in 80-
After 95 DEG C of reactions 4-6 hour, it is cooled to 30-40 DEG C of addition surfactant and montmorillonite, after insulated and stirred 20-40min, obtains
Bamboo liquefied substance base adhesive；
The preparation method of the bamboo liquefied substance includes the following steps：
(1) it pre-processes：By bamboo wood crushed material using hot water after 80-90 DEG C of digestion 8-10 hour, filtering, then using acetic acid second
The mixed solvent of ester-isopropanol extracts 12-24 hours in 70-85 DEG C, filtering, and pretreated bamboo wood powder is obtained after filtration cakes torrefaction
End；
(2) it liquefies：By bamboo wood powder, phenol and catalyst BF pretreated obtained by part steps (1)3Reaction vessel is added
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 matter of the bamboo liquefied substance, 37% formalin, surfactant and montmorillonite
Amount is than being 1：1.2-1.6:0.03-0.05:0.1-0.3.
2. the preparation method of bamboo liquefied substance base adhesive as described in claim 1, which is characterized in that the surface-active
Agent is sodium sulfate of polyethenoxy ether of fatty alcohol, dodecyl sodium sulfate or Monododecylphosphate potassium.
3. the preparation method of bamboo liquefied substance base adhesive as described in claim 1, which is characterized in that described in step (1)
The mass ratio of bamboo wood crushed material and hot water is 1：10-20.
4. the preparation method of bamboo liquefied substance base adhesive as described in claim 1, which is characterized in that described in step (1)
The dosage of mixed solvent is 15-20 times of bamboo wood crushed material quality.
5. the Preparation Method of bamboo liquefied substance base adhesive as claimed in claim 1 or 2, which is characterized in that the mixing is molten
The mass ratio of ethyl acetate and isopropanol is 1 in agent:1.5-2.
6. the preparation method of bamboo liquefied substance base adhesive as described in claim 1, which is characterized in that described pretreated
Bamboo wood powder, phenol and catalyst mass ratio be 1:2-3:0.05-0.12.
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| CN101885825A (en) * | 2010-07-21 | 2010-11-17 | 华南理工大学 | Plant fiber-based polyol, preparation method thereof and use thereof |
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| CN101885825A (en) * | 2010-07-21 | 2010-11-17 | 华南理工大学 | Plant fiber-based polyol, preparation method thereof and use thereof |
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| Title |
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| 竹材残料液化及其液化物胶粘剂的制备;傅深渊等;《林产工业》;20040518;第31卷(第3期);第35-38页 * |
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Effective date of registration: 20200320 Address after: Anji County, Zhejiang province 313000 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. |