CN104974683B - The preparation method of adhesive is blended in a kind of konjaku flour-chitosan-PVA - Google Patents
The preparation method of adhesive is blended in a kind of konjaku flour-chitosan-PVA Download PDFInfo
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Abstract
The invention discloses the preparation methods that adhesive is blended in a kind of konjaku flour-chitosan-PVA, are related to adhesive preparing technical field.This method includes the following steps（1）Preparation mass fraction is 10%PVA solution；（2）Blending polymerization reacts in the solution for konjaku flour and chitosan；（3）PVA solution and crosslinking agent epoxychloropropane solution are added into polymer blend, 1.5-2h is stirred at 60-70 DEG C must be blended adhesive.The konjaku flour of the present invention-chitosan-PVA blending adhesive has the advantages that adhesion strength height, water-tolerant, stability are good, may be used as adhesive and is widely used in timber assembly, wood-based plate manufacture field, applies also for waterproof, packaging field.
Description
Technical field
The present invention relates to chemical field, the preparation of adhesive is blended in especially a kind of konjaku flour-chitosan-PVA
Method.
Background technology
In wood adhesive used at present, many is three-aldehyde glue --- Lauxite (UF), the phenolic resin of solvent
(PF) and melamine resin (VIF), this " three-aldehyde glue " in addition to poor water resistance, Storage period are short, in the mistake for producing and using
A large amount of formaldehyde is released in journey, environmental pollution causes prodigious influence, mankind's Long Term Contact that can also cause to suffer from respiratory tract disease
The danger of the diseases such as disease, malignant tumour, leukaemia.With the proposition of the theories such as environmentally friendly and energy saving, timber industry is also carried with glue
Go out higher requirement, this requires reduction formaldehyde monomers and dosages, and content of free aldehyde in adhesive is made to reach minimum standard, or
Seek suitable raw material and formula to replace three formaldehyde resins, thoroughly solves free aldehyde and discharge the environmental problem brought.
Natural adhesive raw material sources are extensive, at low cost, easy to use, asepsis environment-protecting, as petroleum-based energy is nervous and glue
Stick theoretical research is goed deep into, it is often more important that and the enhancing of people's environmental consciousness, natural adhesive are taken seriously again, to
Give full play to its natural environmental-protective and reproducible advantage.
Konjaku glucomannan is a kind of deposit polysaccharide extracted from Araeceae konjac tuber, is a kind of renewable day
Right high score child resource, derives from a wealth of sources, and has biodegradability, and water-soluble gumminess is high, can thicken, gel and film forming.Shell is poly-
Sugared (chitosan, CA) is in the large biological molecule and nature that chitin (Chitin) deacetylation is transformed
Unique natural alkaline polysaccharide.Contain abundant hydroxyl and amino in chitosan molecule structure, makes it easy to be chemically modified
And modification, application field are very extensive.In recent years, chitosan is widely used in the industries such as medicine, food, chemical industry, environmental protection.Shell
Glycan all has very strong hydrophily by a series of modified derivatives generated, can be degraded by biology, is a kind of nontoxic, nothing
The high molecular material of pollution.Polyvinyl alcohol (polyvinyl alcohol, PVA) is white obtained by being hydrolyzed by polyvinyl acetate
Powdery, water-soluble macromolecule resin, nontoxic, cheap, the glued membrane intensity of good film-forming property and generation is high, is suitable for viscous
Splicing, fabric and timber etc..The auxiliary agent that PVA is also used as many adhesives uses, and gluing power and moisture-proof can be improved.
But the konjaku flour obtained of research at present-chitosan-PVA blendings adhesive adhesion strength is not good enough, constrains its
Development.
Invention content
The goal of the invention of the present invention is：In view of the above problems, it is high, water-tolerant to provide a kind of glue-joint strength
The preparation method of adhesive is blended in konjaku flour-chitosan-PVA.
The preparation method of adhesive is blended in a kind of konjaku flour-chitosan-PVA, it is characterised in that includes the following steps：
(1) it is 10%PVA solution to prepare mass fraction；
(2) 40-60 portions of konjaku flours and 200-300 parts of deionized waters are added in a reservoir, 65-75 DEG C are warming up to, in rotating speed
To be stirred into konjaku solution under the stirring condition of 200-220r/min, 40-60 parts of chitosans are added into konjaku solution, no
Disconnected stirring makes chitosan dissolve or fully be swollen, and the initiator stirring of 2-3 parts by weight is added in the range of 4~6 in adjustment pH value
30-40min obtains polymer blend；
(3) PVA solution that 30-40 parts of mass concentrations are 10% is added into polymer blend, 10-20 parts by weight quality is dense
Degree is 4% epoxychloropropane solution, and 1.5-2h is stirred at 60-70 DEG C must be blended adhesive；Then with 30% NaOH solution
The pH value of glue is adjusted to 6~7, after being warming up to 85 DEG C the reaction was continued 5min, cooling discharge, up to gluing after standing and defoaming
Agent.
Further, the preparation method of the 10%PVA solution is：By PVA and pure water in mass ratio 1：9 is molten at normal temperatures
Then solution after swelling is warming up to 90 DEG C of constant temperature and keeps 20~30min, is allowed to after being completely dissolved, then drop by swollen 5~10min
Temperature is sealed to 25 DEG C, that is, the PVA solution that mass fraction is 10% is made.
Further, the degree of polymerization >=1700 of PVA of the present invention, alcoholysis degree 97%.
Further, the initiator is the ammonium persulfate or potassium persulfate solution that mass concentration is 10%.
By adopting the above-described technical solution, the beneficial effects of the invention are as follows：The preferred epoxychloropropane of the present invention is crosslinked
Agent, epoxychloropropane are a kind of cyclic annular oxygenatedchemicals, easily crosslink and react with graft starch molecule, make between chemical bond that
This combine form a kind of high polymer of reticular structure seemingly, and make crosslinking points segment have better ductility, flexibility, because
This its mechanical property is more preferable, and due to epoxychloropropane cross-linking reaction mild condition, easily controllable, chemical stability is high,
Gained cross-linking products are antiacid, alkali, anti-shearing effect stability higher.The preparation process of the present invention by preferred copolymerization units,
Initiator, controls the temperature condition of reaction, for the more existing adhesive of gained adhesive, does not contain organic volatile, pollution
Small more environmentally friendly, adhesion strength is stronger, water resistance higher, while production cost is low, is easy to mass produce, and is nontoxic dirt
Contaminate few adhesive.
Specific implementation mode
By the following examples, the invention will be further described：
Embodiment 1
The preparation method of adhesive is blended in a kind of konjaku flour-chitosan-PVA, includes the following steps：
(1) it is 10%PVA solution to prepare mass fraction：By PVA and pure water in mass ratio 1：9 are swollen 5min at normal temperatures,
Then the solution after swelling is warming up to 90 DEG C of constant temperature and keeps 20min, be allowed to after being completely dissolved, then to be cooled to 25 DEG C of progress close
The PVA solution that mass fraction is 10% is made in envelope；Wherein, the degree of polymerization >=1700 of selected PVA, alcoholysis degree 97%.
(2) 40 portions of konjaku flours and 300 parts of deionized waters are added in a reservoir, are warming up to 65 DEG C, are 200r/min in rotating speed
Stirring condition under be stirred into konjaku solution, into konjaku solution be added 40 parts of chitosans, being stirred continuously keeps chitosan molten
Solution or fully swelling, adjustment pH value are 4, and the initiator stirring 30min that 2 parts by weight are added obtains polymer blend；Initiation used
Agent is the ammonium persulfate solution that mass concentration is 10%；
(3) PVA solution that 40 parts of mass concentrations are 10% is added into polymer blend, 20 parts by weight mass concentrations are
4% epoxychloropropane solution, 1.5h is stirred at 70 DEG C must be blended adhesive；Then with 30% NaOH solution by the pH of glue
Value is adjusted to 6, after being warming up to 85 DEG C the reaction was continued 5min, cooling discharge, up to adhesive after standing and defoaming.
Embodiment 2
The preparation method of adhesive is blended in a kind of konjaku flour-chitosan-PVA, includes the following steps：
(1) it is 10%PVA solution to prepare mass fraction：By PVA and pure water in mass ratio 1：9 are swollen 10min at normal temperatures,
Then the solution after swelling is warming up to 90 DEG C of constant temperature and keeps 30min, be allowed to after being completely dissolved, then to be cooled to 25 DEG C of progress close
The PVA solution that mass fraction is 10% is made in envelope；Wherein, the degree of polymerization >=1700 of selected PVA, alcoholysis degree 97%；
(2) 60 portions of konjaku flours and 200 parts of deionized waters are added in a reservoir, are warming up to 75 DEG C, are 220r/min in rotating speed
Stirring condition under be stirred into konjaku solution, into konjaku solution be added 60 parts of chitosans, being stirred continuously keeps chitosan molten
Solution or fully swelling, adjustment pH value are 6, and the initiator stirring 40min that 3 parts by weight are added obtains polymer blend；Initiation used
Agent is the ammonium persulfate solution that mass concentration is 10%；
(3) PVA solution that 30 parts of mass concentrations are 10% is added into polymer blend, 10 parts by weight mass concentrations are
4% epoxychloropropane solution, 2h is stirred at 60 DEG C must be blended adhesive；Then with 30% NaOH solution by the pH value of glue
It adjusts to 7, after being warming up to 85 DEG C the reaction was continued 5min, cooling discharge, up to adhesive after standing and defoaming.
Embodiment 3
The preparation method of adhesive is blended in a kind of konjaku flour-chitosan-PVA, includes the following steps：
(1) it is 10%PVA solution to prepare mass fraction：By PVA and pure water in mass ratio 1：9 are swollen 8min at normal temperatures,
Then the solution after swelling is warming up to 90 DEG C of constant temperature and keeps 25min, be allowed to after being completely dissolved, then to be cooled to 25 DEG C of progress close
The PVA solution that mass fraction is 10% is made in envelope；Wherein, the degree of polymerization >=1700 of selected PVA, alcoholysis degree 97%.
(2) 50 portions of konjaku flours and 250 parts of deionized waters are added in a reservoir, are warming up to 70 DEG C, are 210r/min in rotating speed
Stirring condition under be stirred into konjaku solution, into konjaku solution be added 50 parts of chitosans, being stirred continuously keeps chitosan molten
Solution or fully swelling, adjustment pH value are 5, and the initiator stirring 35min that 2-3 parts by weight are added obtains polymer blend；It is used to draw
Hair agent is the ammonium persulfate or potassium persulfate solution that mass concentration is 10%；
(3) PVA solution that 35 parts of mass concentrations are 10% is added into polymer blend, 15 parts by weight mass concentrations are
4% epoxychloropropane solution, 2h is stirred at 65 DEG C must be blended adhesive；Then with 30% NaOH solution by the pH value of glue
It adjusts to 6.5, after being warming up to 85 DEG C the reaction was continued 5min, cooling discharge, up to adhesive after standing and defoaming.
3 performance test of embodiment
Following testing performance index is done to the adhesive obtained by embodiment 1,2 or 3, test result is as follows shown in table 1：
| Index | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Shear strength/MPa | 28 | 30 | 31 |
| Tensile strength/MPa | 26 | 27 | 27 |
| Peel strength/MPa | 46 | 50 | 48 |
From test result as can be seen that the blending adhesive adhesion strength obtained by the present invention is big, various aspects of performance can
Meet the use standard of wood adhesive, assembled, wood-based plate manufacture field can be used in timber.
Claims (2)
1. the preparation method of adhesive is blended in a kind of konjaku flour-chitosan-PVA, it is characterised in that include the following steps：
(1) it is 10%PVA solution to prepare mass fraction；
(2) 40-60 portions of konjaku flours and 200-300 parts of deionized waters are added in a reservoir, is warming up to 65-75 DEG C, is in rotating speed
It is stirred into konjaku solution under the stirring condition of 200-220r/min, 40-60 parts of chitosans are added into konjaku solution, constantly
Stirring makes chitosan dissolve or fully be swollen, and the initiator stirring of 2-3 parts by weight is added in the range of 4~6 in adjustment pH value
30-40min obtains polymer blend；
(3) PVA solution that 30-40 parts of mass concentrations are 10% is added into polymer blend, 10-20 parts by weight mass concentrations are
4% epoxychloropropane solution, 1.5-2h is stirred at 60-70 DEG C must be blended adhesive；Then with 30% NaOH solution by glue
The pH value of liquid is adjusted to 6~7, after being warming up to 85 DEG C the reaction was continued 5min, cooling discharge, up to adhesive after standing and defoaming；
The initiator is the ammonium persulfate or potassium persulfate solution that mass concentration is 10%；The degree of polymerization >=1700 of the PVA,
Alcoholysis degree is 97%.
2. the preparation method of adhesive is blended in a kind of konjaku flour according to claim 1-chitosan-PVA, it is characterised in that
The preparation method of the 10%PVA solution is：By PVA and pure water in mass ratio 1：9 are swollen 5~10min at normal temperatures, then will
Solution after swelling is warming up to 90 DEG C of constant temperature and keeps 20~30min, is allowed to after being completely dissolved, then be cooled to 25 DEG C and be sealed,
The PVA solution that mass fraction is 10% is made.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107400477A (en) * | 2016-05-19 | 2017-11-28 | 长沙市汇华胶粘剂科技有限公司 | A kind of preparation method of konjac glucomannan-polyvinyl alcohol-dipotassium hydrogen phosphate blending green environment protection adhesion agent |
| CN106047221A (en) * | 2016-06-15 | 2016-10-26 | 安徽扬帆充气游乐设备制造有限公司 | Adhesive with excellent adhesive property for inflatable boats |
| CN106047222A (en) * | 2016-06-15 | 2016-10-26 | 安徽扬帆充气游乐设备制造有限公司 | High adhesive strength adhesive for inflatable boat |
| CN106118551A (en) * | 2016-06-26 | 2016-11-16 | 欧振云 | A kind of forest-friendly building timbers adhesive |
| CN106566440A (en) * | 2016-10-28 | 2017-04-19 | 无锡市永兴金属软管有限公司 | Composite modified environment-friendly metal corrugated pipe adhesive and preparation method thereof |
| CN107446523B (en) * | 2017-08-30 | 2018-08-21 | 阜南盛原木业有限公司 | A kind of glued board adhesive |
| CN107828284B (en) * | 2017-10-24 | 2020-05-12 | 沈阳顺风新材料有限公司 | Interface agent and preparation method thereof |
| CN107903847A (en) * | 2017-11-20 | 2018-04-13 | 苏州甫众塑胶有限公司 | A kind of compound wooden case adhesive and preparation method thereof |
| CN110037293A (en) * | 2019-04-02 | 2019-07-23 | 安徽雁飞粮油有限责任公司 | A kind of wheat compound nutritional particle and preparation method thereof |
| CN117599753B (en) * | 2023-12-29 | 2024-05-24 | 广东微方程新材料有限公司 | Adsorption material based on molecular sieve and preparation method thereof |
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| CN102952496A (en) * | 2012-11-26 | 2013-03-06 | 山东泰德新能源有限公司 | Non-toxic adhesive and preparation method thereof |
| CN102994006A (en) * | 2012-11-26 | 2013-03-27 | 山东泰德新能源有限公司 | Nontoxic adhesive and method for preparing same |
| CN103013380A (en) * | 2012-11-26 | 2013-04-03 | 山东泰德新能源有限公司 | Non-toxic adhesive and preparation method thereof |
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| US5264569A (en) * | 1990-06-12 | 1993-11-23 | E. I. Du Pont De Nemours And Company | Purified fungal spore tip mucilage |
| CN101824286A (en) * | 2010-03-31 | 2010-09-08 | 西北农林科技大学 | Wood adhesive and preparation method thereof |
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Effective date of registration: 20180914 Address after: 221300 Sheng Qiang Road, New River Town, Pizhou, Jiangsu Applicant after: Pizhou Jinfeng wood fiber powder Co., Ltd. Address before: 530004 100 East University Road, Nanning, the Guangxi Zhuang Autonomous Region Applicant before: Guangxi University |
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Address after: 221300 Sheng Qiang Road, New River Town, Pizhou, Jiangsu Patentee after: Jiangsu jinyufeng New Material Co., Ltd Address before: 221300 Sheng Qiang Road, New River Town, Pizhou, Jiangsu Patentee before: PIZHOU JINFENG WOOD FIBER POWDER Co.,Ltd. |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of konjac powder chitosan PVA blend adhesive Effective date of registration: 20210809 Granted publication date: 20181026 Pledgee: China Construction Bank Corporation Pizhou sub branch Pledgor: Jiangsu jinyufeng New Material Co.,Ltd. Registration number: Y2021980007390 |
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