CN110452635A - A kind of environment-friendly type tannin-chitosan-based adhesive - Google Patents
A kind of environment-friendly type tannin-chitosan-based adhesive Download PDFInfo
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- CN110452635A CN110452635A CN201910803059.7A CN201910803059A CN110452635A CN 110452635 A CN110452635 A CN 110452635A CN 201910803059 A CN201910803059 A CN 201910803059A CN 110452635 A CN110452635 A CN 110452635A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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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
- C09J105/00—Adhesives based on polysaccharides or on their derivatives, not provided for in groups C09J101/00 or C09J103/00
- C09J105/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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Abstract
The present invention relates to environment-friendly adhesive technical fields, and in particular to a kind of environment-friendly type tannin-chitosan-based adhesive, including following parts by weight component: 30-50 parts of condensed tannin, 15-35 parts of low viscosity chitosan, 1-5 parts of acid, 1-5 parts of curing agent, 500-700 parts of water；The present invention is using renewable native compound tannin and chitosan as raw material, prepare the chitosan-based adhesive of tannin-, the plywood production suitable for wood-based plate, obtained adhesive has good glue-joint strength and water resistance, and performance indicator meets the requirement of II class glued board specified in standard GB/T/T9846.3-2004.
Description
Technical field
The invention belongs to Wood-based Panel Production technical fields, and in particular to a kind of environment-friendly type tannin-chitosan-based adhesive.
Background technique
Since the middle of last century, using formaldehyde as three-aldehyde glue (i.e. the urea-formaldehyde resin adhesive, melamine-first of raw material
Urea formaldehyde adhesive, phenol-formaldehyde resin adhesive) it is had excellent performance with it, it is cheap, thus be able in timber industry field
It is widely used, but its product release formaldehyde in use, causes environmental and human health impacts to endanger, in addition with oil crisis
Rise, nonhazardous, the development of environmentally protective and renewable source biomass adhesive are paid close attention to by people.
Tannin based biomass adhesive has realized industrialized production in Europe, and now has no related industry report in China
It leads.A large amount of study on the modification work is improved the water resistance of tannin adhesive, such as isocyanates, hyperbranched branch by carrying out
Shape macromolecular and epoxy resin etc. are all used as modifying agent, and obtain it is gratifying as a result, but this kind of cross-linked modifier all
It is to use non-renewable resources based on petrochemical industry product base, it is difficult to meet green, the idea of development of regenerated resources.
Tannin (Tannins) is the compound in the fourth-largest source in plant after cellulose, hemicellulose, lignin.Root
According to the difference of structure, tannin is divided into Hydrolysable Tannins and condensed tannin.The research of tannin both at home and abroad is mainly with condensed tannin at present
Based on, yield accounts for the 90% of world's tannin total output.
Condensed tannin is a kind of natural polyphenol material by the monomer composition of flavonoids, is plant peel, polyphenol chemical combination in leaf
The main component of object, content account for the 3%-30% of bark, leaf.Often contain compact carbon aquation in its repeated monomer structure
Closing object A ring and B ring (as shown in chemical structure 1) and phenol has with similar chemical structure compared with high reaction activity.In timber work
Tannin can partly or entirely replace the phenolic substances in the phenolic resin of one of Wood in Common Use adhesive to prepare tannin base in industry
Wood adhesive.
Chemical structure 1:
Tannin and formaldehyde carry out polycondensation and form intensive reticular structure, so that tannin base adhesive has glue performance
And it is directly used as wood adhesive, but formaldehyde, as a kind of toxic chemical substance, it is ground by World Health Organization's international cancer
Study carefully mechanism and be classified as a kind of carcinogenic substance, is unfavorable for human health；According to glyoxal, glutaraldehyde, trishydroxymethylnitromethane, six times
The substitution formaldehyde such as tetramine can prepare environment-friendly type tannin base timber work glue as curing agent, but water resistance is undesirable, makes
The popularization and application for obtaining the biolobic material glue are restricted.
Chitosan (chitosan) is also known as chitosan, is chitin (chitin) warp being widely present by nature
Cross the natural polymer that deacetylation obtains, be present in the shell of the shellfish such as shrimp crab, the crust of insect and
In the cell wall of fungi, content is laid in nature and is only second to cellulose.Due to its biological functionality and compatibility, blood compatibility
The excellent performances such as property, safety, microbic resolvability are by all trades and professions extensive concern, in medicine, food, chemical industry, cosmetics, water
The application study of the numerous areas such as processing, METAL EXTRACTION and recycling, biochemistry and biomedical engineering achieves major progress.
Chemical structure 2:
As shown in chemical structure 2, the amido in chitosan molecule has compared with high reaction activity, can react with tannin, and shape
At the dense mesh structure of intertexture, and then it is made to have glue performance, this makes it possible chitin modified Tannin adhesive.This
Outside, chitosan molecule is insoluble in water, may make the adhesive after solidifying to be not easily decomposed under water effect, has preferable water resistance
Energy.
Patent No. CN200810032289.X discloses the excellent wood adhesive of a kind of formaldehydeless release, hot water resistance, should
Adhesive at room temperature, while stirring by the raw material containing protein, acidity regulator, aromatic compound, curing agent, anti-corrosion
Agent, viscosity modifier, filler, drier are added to the water, and novel timber adhesive, the selection packet of the viscosity modifier is made
Chitosan is included, the selection of the aromatic compound includes tannin, but the adhesive components are complicated, are unfavorable for mass production,
And production cost is higher.
Patent No. CN200810181549.X discloses a kind of adhesion agent for artificial board of formaldehydeless release, the adhesive
Specific step is as follows for manufacturing process: water intaking, acid and soft segments are added in stainless steel kettle, 10 DEG C -80 DEG C of temperature, start blender
It being stirred evenly with the speed of 400r/min, phenol stirring is added, adjusting pH is 3-8, enzyme is added and continues to stir, the enzymatic treatment reaction time
It is -48 hours 0.1 minute, when adhesive viscosity applies 4 glasss 20-100 seconds, stops stirring, sealing saves, and the soft segments are
Chitosan, chitin, soybean protein, wheat gluten；The selection of the phenol includes tannin, but the adhesive components are complicated, at enzyme
Reason is difficult to control, and is unfavorable for industrial production control.
Summary of the invention
The present invention is in order to solve the above technical problems, provide a kind of environment-friendly type tannin-chitosan-based adhesive.
It is realized particular by following technical scheme:
A kind of environment-friendly type tannin-chitosan-based adhesive, including following parts by weight component: 30-50 parts of condensed tannin, low viscous
Spend chitosan 15-35 parts, 1-5 parts of acid, 1-5 parts of curing agent, 500-700 parts of water.
Further, the environment-friendly type tannin-chitosan-based adhesive, including following parts by weight component: 40 parts of condensed tannin,
25 parts of low viscosity chitosan, sour 3 parts, 3 parts of curing agent, 600 parts of water.
The condensed tannin is from Black Wattle, hard ebon skin, pine bark, english walnut bark, oak bark, Chinese waxmyrtle bark
One of or multiple combinations.
Condensed tannin of the invention is extracted from bark, relative to root, stem, leaf, kind skin, kind shell and kernel, bark
Middle condensed tannin content is higher；Most importantly from Black Wattle, hard ebon skin, pine bark, english walnut bark, oak bark, poplar
The degree of polymerization distribution for the condensed tannin that Japanese apricot skin obtains constitutes structural unit and includes catechin, epicatechin, amasses wealth by heavy taxation to a variety of aggressiveness
Catechin, afzelechin etc., therefore there is excellent space structure and Physiology and biochemistry activity, improve the stabilization of adhesive
Property, it is therefore prevented that harmful bacteria moth erosion and caused by degumming phenomenon.
The viscosity of the low viscosity chitosan is 50-100mPas (1wt.%, in 1% acetum, 25 DEG C).
The present invention uses condensed tannin, can combine with multiple sites on chitosan, so that the space conformation of chitosan
It changes, chitosan is prevented to be degraded, improve its anti-microbial property and stability；Pass through containing for control polymer carbohydrate
Amount, helps to improve bonding force.The present invention uses low viscosity chitosan, and Hyarogen-bonding weakens, and molecule can be in loose condition (of surface),
Can be preferably compatible with tannin structure when stirring, condensation degree of dissolved is improved, while chitosan itself positive charge density is small, with moisture
Son interaction, can reduce the activity of water, avoid the chemical reaction of OH- participation Various Complex in hydrone.
The granularity of the low viscosity chitosan is 200-400 mesh；Granularity of the present invention by control chitosan, cooperation stirring
The excitation of power promotes it to be uniformly dispersed and improve dispersion rate so that the activity of chitosan occurs to increase in short-term, shortens
Mixing time, thereby reduces stirring energy consumption and mechanical damage rate, while Control granularity, is conducive to adjust glue consistency,
Prevent extremely thick or extremely dilute state.
The acid is selected from one of p-methyl benzenesulfonic acid, formic acid, acetic acid, hydrochloric acid, sulfuric acid, citric acid or a variety of.
The curing agent is selected from trishydroxymethylnitromethane, trimethylolpropane, hexamethylenetetramine, glyoxal, penta 2
One of aldehyde is a variety of.
The present invention also provides environment-friendly type tannin-chitosan-based adhesive preparation methods, are made of following steps: In
Under room temperature, condensed tannin, low viscosity chitosan, water are added into blender, opens stirring, acid adding stirs 25-35min
Afterwards, add curing agent stirring 3-8min to get.
Condensed tannin, low viscosity chitosan, water are first sufficiently mixed by the present invention, are added acid, are dissolved chitosan sufficiently
And it is woven into dense mesh structure with tannin, sour effect goes back solidification agent activity, reinforces the curing performance of curing agent, not only
The water resistance of adhesive is improved, loose chitosan space structure is shunk, effectively control the hygroscopicity of product and is contained
Water.
The utility model has the advantages that
The present invention prepares the chitosan-based adhesive of tannin-using renewable native compound tannin and chitosan as raw material, fits
For plywood production in wood-based plate, obtained adhesive has good glue-joint strength and water resistance, and performance indicator is full
The requirement of II class glued board specified in sufficient standard GB/T/T9846.3-2004.
Compared with prior art, the present invention has a characteristic that
1. material source is wide, component is simple, is easy to implement mass production, and cost of material is low.
2. preparation process is simple；Room temperature preparation is realized, the energy consumption generated in production because heating up heating is greatly reduced,
Energy conservation and environmental protection simultaneously reduces production cost, at the same avoid heating damage tannin, chitosan activity cause the stability of adhesive
Decline with bonding force.
3. environmentally protective；The adhesive main raw material(s) derives from agricultural product waste (bark, leaf) and fishing animal husbandry shrimp
The shell-fish such as crab belong to renewable biomass natural polymer, and advantageously reduce timber industry is to fossil resources
The degree of dependence of the synthetic resin on basis, and the formaldehydeless release of product.
Specific embodiment
Specific embodiments of the present invention will be described in further detail below, but the invention is not limited to these realities
Mode is applied, it is claimed to still fall within the claims in the present invention for any improvement or replacement on the present embodiment essence spirit
Range.
Embodiment 1
A kind of environment-friendly type tannin-chitosan-based adhesive, including following parts by weight component: 50 parts of condensed tannin, low viscosity
35 parts of chitosan, sour 5 parts, 5 parts of curing agent, 700 parts of water；
The condensed tannin derives from pine bark；
The viscosity of the low viscosity chitosan is 100mPas (1wt.%, in 1% acetum, 25 DEG C)；
The granularity of the low viscosity chitosan is 400 mesh；
The acid is selected from p-methyl benzenesulfonic acid；
The curing agent is selected from trishydroxymethylnitromethane.
Embodiment 2
A kind of environment-friendly type tannin-chitosan-based adhesive, including following parts by weight component: 30 parts of condensed tannin, low viscosity
15 parts of chitosan, sour 1 part, 1 part of curing agent, 500 parts of water；
The condensed tannin derives from Black Wattle；
The viscosity of the low viscosity chitosan is 50mPas (1wt.%, in 1% acetum, 25 DEG C)；
The granularity of the low viscosity chitosan is 200 mesh；
The mass ratioes compositions such as the acid is formic acid, acetic acid, hydrochloric acid, sulfuric acid are pressed；
The curing agent is trishydroxymethylnitromethane, trimethylolpropane, hexamethylenetetramine, glyoxal, glutaraldehyde
By equal mass ratioes composition.
Embodiment 3
A kind of environment-friendly type tannin-chitosan-based adhesive, including following parts by weight component: 40 parts of condensed tannin, low viscosity
25 parts of chitosan, sour 3 parts, 3 parts of curing agent, 600 parts of water；
The mass ratioes compositions such as the condensed tannin is pine bark, english walnut bark, oak bark are pressed.
The viscosity of the low viscosity chitosan is 80mPas (1wt.%, in 1% acetum, 25 DEG C)；
The granularity of the low viscosity chitosan is 300 mesh；
The acid is selected from acetic acid；
The mass ratioes compositions such as the curing agent is hexamethylenetetramine, glyoxal, glutaraldehyde are pressed.
Embodiment 4
A kind of environment-friendly type tannin-chitosan-based adhesive, which is characterized in that including following parts by weight component: condensed tannin
40 parts, 25 parts of low viscosity chitosan, sour 3 parts, 3 parts of curing agent, 600 parts of water；
The condensed tannin Black Wattle, hard ebon skin, oak bark by etc. mass ratioes composition.
The viscosity of the low viscosity chitosan is 50mPas (1wt.%, in 1% acetum, 25 DEG C)；
The granularity of the low viscosity chitosan is 400 mesh；
The acid is selected from hydrochloric acid；
The mass ratioes compositions such as the curing agent is trishydroxymethylnitromethane, trimethylolpropane is pressed.
Embodiment 5-8
Embodiment 5-8 provides the preparation method of the adhesive on the basis of examples 1 to 4 respectively, using following step
Suddenly it is made: at room temperature, condensed tannin, low viscosity chitosan, water being added into blender, open stirring, acid adding stirring
After 30min, add curing agent stirring 5min to get.
Glue-line shear strength and resistance to is carried out according to the adhesive that the method for GB/T9846.3-2004 prepares embodiment 5-8
Aqueous detection, effect are as follows:
The dry shape shear strength of 1 each group adhesive of table
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | |
| Shear strength/MPa | 2.0 | 1.9 | 2.2 | 2.2 |
2 each group adhesive of table, 63 ± 3 DEG C of water impregnate the wet strength after 3h
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | |
| Shear strength/MPa | 1.3 | 1.0 | 1.5 | 1.4 |
Present invention discover that adhesive is without phenomenon of coming unglued, and shear strength is greater than national standard under above-mentioned disposition
0.70MPa.
1 raw material proportioning screening experiment of test example
The present inventor in order to study the science and reasonability of raw material proportioning, with condensed tannin, low viscosity chitosan, acid,
Curing agent, water are tested, and are prepared as follows adhesive on the basis of table 4 is formulated: at room temperature, to organic
Condensed tannin, low viscosity chitosan end, water are added in the beaker of tool stirring rod, turn on agitator is added hydrochloric acid, and stirs
Hexamethylenetetramine is added in 30min, continues to stir 5min；
Each group of formula of table 4
| Condensed tannin/g | Low viscosity chitosan/g | Water/g | Hydrochloric acid/g | Hexamethylenetetramine/g | |
| A group 1 | 40 | 25 | 600 | -- | 3 |
| A group 2 | 40 | 25 | 600 | 3 | -- |
| A group 3 | 28 | 25 | 600 | 3 | 3 |
| A group 4 | 52 | 25 | 600 | 3 | 3 |
| A group 5 | 40 | 14 | 600 | 3 | 3 |
| A group 6 | 40 | 36 | 600 | 3 | 3 |
| A group 7 | 40 | 25 | 600 | 0.8 | 3 |
| A group 8 | 40 | 25 | 600 | 3.2 | 3 |
| A group 9 | 40 | 25 | 600 | 3 | 0.8 |
| A group 10 | 40 | 25 | 600 | 3 | 3.2 |
Each group adhesive prepares poplar gluing in 130 DEG C of hot pressing temperature, hot pressing time 1min/mm, hot pressing pressure 1.0MPa
Plate.Then it is sawn into sample dimensions required by shear strength test respectively.Shear strength test relates generally to dry shape shear strength
With resistance to warm water intensity (63 DEG C of warm water impregnate 3h), the results are shown in Table 5；
The measurement of the shear strength of each group under 5 different ratio of table
The experiment of 2 craft screening of test example
The present inventor is in order to study the science and reasonability that technique is arranged, based on the formula of embodiment 3, using not
Same process, and the test of glue-line shear strength, water-fast removing rate is carried out, it is specific as follows:
Technique groups 1: it is poly- that condensed tannin, low viscosity shell are added at room temperature, in the beaker of Xiang Peiyou mechanical stirring stick
Sugared end, water, acid, curing agent, turn on agitator stir 45min；
Technique groups 2: it is poly- that condensed tannin, low viscosity shell are added at room temperature, in the beaker of Xiang Peiyou mechanical stirring stick
Sugared end, water, acid, turn on agitator stir 45min, add curing agent stirring 5min；
Technique groups 3: at room temperature, in the beaker of Xiang Peiyou mechanical stirring stick be added low viscosity chitosan end, water,
Acid, turn on agitator stir 30min, and condensed tannin is added and stirs 30min, add curing agent stirring 5min；
Technique groups 4: at room temperature, in the beaker of Xiang Peiyou mechanical stirring stick be added low viscosity chitosan end, water,
Acid, turn on agitator stir 30min, and curing agent is added and stirs 5min, add condensed tannin stirring 30min；
Technique groups 5: it is poly- that condensed tannin, low viscosity shell are added at room temperature, in the beaker of Xiang Peiyou mechanical stirring stick
Sugared end, water, curing agent, turn on agitator stir 30min, and acid stirring 30min is added；
The measurement of the shear strength of each group under 6 different process of table
| Dry shape shear strength/MPa | Warm water impregnates shear strength/MPa | |
| Technique groups 1 | 1.9 | 0.9 |
| Technique groups 2 | 2.0 | 1.1 |
| Technique groups 3 | 1.8 | 1.1 |
| Technique groups 4 | 1.7 | 0.8 |
| Technique groups 5 | 1.9 | 0.9 |
3 Viscosity of Chitosan screening experiment of test example
The present inventor controls Viscosity of Chitosan on the basis of embodiment 7, set gradually 30mPas,
50mPa·s、100mPa·s、200mPa·s、500mPa·s、800mPa·s、1000mPa·s、1500mPa·s、
2000mPas, 2600mPas, 3200mPas, 4000mPas multiple groups, according to the method for GB/T9846.3-2004 to each
Group adhesive carries out the detection of glue-line shear strength, and research is found: Viscosity of Chitosan is affected to adhesive, significant difference,
There is preferable dry strong, about 2.3MPa in 50-100mPas, be below the numerical value in the case of remaining；In addition, using GB/
The method of T14074-2006 tests adhesive viscosity, and research is found: the chitosan within the scope of 50-100mPas can
Gelatin viscosity is reduced, this may be that chitosan has biggish space structure, cross-linked network can be better achieved, while in net
Shape prevents agglomeration when being crosslinked, and improves mobility, shortens the reaction active sites distance retained in molecule.
The experiment of 4 chitosan particle filter of test example
The present inventor controls chitosan granularity on the basis of embodiment 7, sets gradually 50 mesh, 100 mesh, 200
Mesh, 400 mesh, 600 mesh, 1200 mesh, 3000 mesh multiple groups carry out glue to each group adhesive according to the method for GB/T9846.3-2004
Layer shear strength detection, research are found: chitosan granularity is in adhesive bonding strength correlation, in 100 to 200 mesh
Now rapidly rise, the rate of climb obviously slows down after 200 mesh, and climbing is about between 1-4%, and adhesive is dry when 100 mesh is by force
1.95MPa, it is 2.36MPa that adhesive is dry when 200 mesh by force, it is contemplated that cost and energy consumption problem select 600 mesh powder below,
And powder size, when being higher than 600 mesh, extremely thick gel elastomer is presented in glue, it is difficult to be glued.
Claims (8)
1. a kind of environment-friendly type tannin-chitosan-based adhesive, which is characterized in that including following parts by weight component: condensed tannin 30-
50 parts, 15-35 parts of low viscosity chitosan, 1-5 parts of acid, 1-5 parts of curing agent, 500-700 parts of water.
2. environment-friendly type tannin as described in claim 1-chitosan-based adhesive, which is characterized in that including following parts by weight component:
40 parts of condensed tannin, 25 parts of low viscosity chitosan, sour 3 parts, 3 parts of curing agent, 600 parts of water.
3. environment-friendly type tannin as claimed in claim 1 or 2-chitosan-based adhesive, which is characterized in that the condensed tannin source
In one of Black Wattle, hard ebon skin, pine bark, english walnut bark, oak bark, Chinese waxmyrtle bark or multiple combinations.
4. environment-friendly type tannin-chitosan-based adhesive as claimed in claim 1 or 2, which is characterized in that the low viscosity chitosan
Viscosity be 50-100mPas.
5. environment-friendly type tannin as claimed in claim 1 or 2-chitosan-based adhesive, which is characterized in that the low viscosity chitosan
Granularity be 200-400 mesh.
6. environment-friendly type tannin as claimed in claim 1 or 2-chitosan-based adhesive, which is characterized in that the acid is selected to toluene
One of sulfonic acid, formic acid, acetic acid, hydrochloric acid, sulfuric acid are a variety of.
7. environment-friendly type tannin as claimed in claim 1 or 2-chitosan-based adhesive, which is characterized in that the curing agent is selected from three
One of methylol nitromethane, trimethylolpropane, hexamethylenetetramine, glyoxal, glutaraldehyde are a variety of.
8. environment-friendly type tannin as described in claim 1-chitosan-based adhesive, which is characterized in that the preparation side of the adhesive
Method is made of following steps: at room temperature, condensed tannin, low viscosity chitosan, water being added into blender, is opened
Stirring, acid adding stir 25-35min after, add curing agent stirring 3-8min to get.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114672281A (en) * | 2022-04-18 | 2022-06-28 | 北京京都大成新材料科技有限公司 | Bio-based adhesive for laminating kraft paper to metal plate and preparation method and application thereof |
| CN114672281B (en) * | 2022-04-18 | 2024-03-08 | 北京京都大成新材料科技有限公司 | Bio-based adhesive for laminating kraft paper to metal plate, and preparation method and application thereof |
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| CN110452635B (en) | 2020-12-22 |
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