CN105754524A - Preparation method for corn starch based wood adhesive - Google Patents
Preparation method for corn starch based wood adhesive Download PDFInfo
- Publication number
- CN105754524A CN105754524A CN201610110641.1A CN201610110641A CN105754524A CN 105754524 A CN105754524 A CN 105754524A CN 201610110641 A CN201610110641 A CN 201610110641A CN 105754524 A CN105754524 A CN 105754524A
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- mass parts
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Classifications
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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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/02—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to polysaccharides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a preparation method for a corn starch based wood adhesive. The preparation method comprises the following steps: oxidizing the corn starch by use of sodium hypochlorite; co-polymerizing the oxidized corn starch with N-hydroxymethyl acrylamide and acrylic acid to obtain a copolymer; modifying the copolymer by use of polyvinyl alcohol; and adding epoxy chloropropane into the copolymer to etherify, graft and cross-link, thereby obtaining the corn based starch glue. According to the preparation method, the N-hydroxymethyl acrylamide is adopted to replace the conventional acrylamide to copolymerize with the starch; the acrylic acid is added to provide protons for being beneficial for the starch to form the copolymer; the reaction is stable; the starch grafting effect is good; the adhesive prepared by the preparation method is free from formaldehyde, is safe, and is good in bonding performance, and the problems such as poor water resistance of common starch adhesive are solved.
Description
Technical field
The present invention relates to the preparing technical field of adhesive, be specifically related to the preparation side of a kind of corn starch base based Wood Adhesives
Method.
Background technology
Existing domestic wood uses in adhesive, Lauxite, amino resins, melamine resin and phenolic resin glue
Glutinous agent is widely used, and its raw material is cheap, area is wide, of good quality, but containing substantial amounts of free formaldehyde in resin, not only to ring
Border pollutes, and has an effect on health.Along with increasingly stringent and the raising of health of people consciousness of environmental law, produce environment-friendly type
Adhesive, the exploitation adhesive without free formaldehyde is a kind of trend.
In based Wood Adhesives field, people gradually develop the adhesive with natural polymer as primary raw material, as vegetable protein,
Starch etc..Starch adhesive extensive, efficient can produce and purify, and cheap, but in use, amylan
Glutinous agent easily precipitates, high temperature is the most mouldy, bond properties is the highest, poor water resistance, in order to improve the applicability of starch and adhesive, right
Starch is modified, and prepares comprehensive excellent Starch Based Wood Adhesives.
Summary of the invention
It is an object of the invention to, for prior art, it is provided that the preparation method of a kind of corn starch base based Wood Adhesives.
For achieving the above object, the present invention takes techniques below scheme: the preparation method of a kind of corn starch base based Wood Adhesives,
Comprise the following steps:
(1) oxidation of cornstarch: the cornstarch of 75～85 mass parts and the water of 100～150 mass parts are stirred and make starch
Breast, adds sodium hydroxide solution while stirring, and the pH value of regulation starch solution is 7.0～8.0, adds 20～25 mass parts
8～10% liquor natrii hypochloritis, the PH maintaining reaction solution with sodium hydroxide solution is 7.0～7.5, and reacts 1～6h at 30 DEG C；
(2) activation of cornstarch: the pH value at room temperature regulating oxidized starch with sodium hydroxide solution is 6.0～6.5, adds
Ammonium sulfate activation 30min, adds the sodium hydrogensulfite activation 30min of 0.01～0.1 mass parts；
(3) starch-grafted: after cornstarch is heated to 50～55 DEG C, be slowly added in 1h 12～16 mass parts acrylic acid and
The N hydroxymethyl acrylamide of 18～25 mass parts, continues reaction 2h at such a temperature after having added；
(4) etherificate crosslinking: the dodecyl sodium sulfonate ammonium of 0.05～0.1 mass parts and the polyvinyl alcohol of 1～10 mass parts are dissolved in 40～50
After the water of mass parts, limit stirring just adds in starch solution, is further continued for stirring 20min, adds 0.5～5 mass parts after adding
Epoxychloropropane, 20～25 anhydrous sodium sulfates and 0.05～the sodium hydrate solid of O.1 mass parts of mass parts, anti-at 25 DEG C
Answer 1h, be 6 with sulfuric acid regulation PH, obtain product.
Wherein, in described step (1), reporting of stirring is 250～300r/min.
Wherein, in described sodium hydroxide solution, the mass fraction of NaOH is 2%.
Wherein, the concentration of described ammonium persulfate solution is 2.0～8.0 × 10-3Mol/L, the volume that ammonium persulfate solution adds
Score ratio 5～10, in the present invention, mass fraction calculates than with g, and Volume fraction calculates with ml.
Wherein, the concentration of described sulfuric acid is 2mol/L.
Further, the ammonium persulfate in the present invention is initiator, and ammonium persulfate has easy to control, the advantage of favorable reproducibility.
Further, in the present invention, epoxychloropropane is crosslinking agent, and cross-linking effect is good, and reaction temperature change is mild, easily-controllable
System, and the ether formed is strong stable.
Further, in the present invention, N hydroxymethyl acrylamide molecule has amide group, and also have with carbonyl conjugation is double
Key and rich reactive methylol, it can be with starch-grafted introducing amide group, and acrylic acid can provide proton simultaneously, it is possible to decrease
The temperature of reaction, graft effect is good.
Further, the hydroxyl in starch agent can be combined with water with the likeness in form of hydrogen bond, and causing hydrolysis to analyse adhesive is to viscous
The suction-operated of glue material, destroys glue and intensity, and the present invention uniformly implants the appropriate change being firmly combined with between starch molecular chain
Learn key, enhance the adhesion of molecule interchain, stop the entrance of hydrone, prevent Hydrogenbond to be destroyed.
Further, the starch after sex change of the present invention is grafted, and introduces amide group, and the space of starch is direct-connected to become more
By force, then the starch after grafting is carried out cross-linking reaction with epoxychloropropane, enables starch polymer to form three closed structures of complexity,
Can effectively prevent the entrance of hydrone, improve the resistance to water of adhesive.
The invention has the beneficial effects as follows:
1, the present invention uses N hydroxymethyl acrylamide to replace conventional acrylamide and starch copolymerization, because of N hydroxymethyl acrylamide carbonyl
The double bond of base conjugation and rich reactive methylol, provide proton plus acrylic acid again, it is easy to Starch formation copolymer, starch
Graft effect is good, stable reaction.
2, the adhesive being made up of the present invention is formaldehydeless, safety, solves the problems such as common starch adhesive poor water resistance, and glue performance is good.
Detailed description of the invention
Below in conjunction with specific embodiment, to further instruction of the present invention.
Embodiment 1
The preparation method of a kind of corn starch base based Wood Adhesives, comprises the following steps:
(1) oxidation of cornstarch: the cornstarch of 80 mass parts and the water of 120 mass parts are stirred and make starch milk, with
The addition mass fraction while stirring of reporting of 280r/min is the sodium hydroxide solution of 2%, and the pH value of regulation starch solution is 8.0,
Add 9% liquor natrii hypochloritis of 24 mass parts, with the PH of the sodium hydroxide solution maintenance reaction solution that mass fraction is 2% be
7.0, and at 30 DEG C, react 4h；
(2) activation of cornstarch: the pH value at room temperature regulating oxidized starch with the sodium hydroxide solution that mass fraction is 2% is 6.0,
The concentration adding 8 volume fractions is 5.0 × 10-3Mol/L ammonium persulfate solution activation 30min, adds the Asia of 0.05 mass parts
Niter cake activation 30min；
(3) starch-grafted: after cornstarch is heated to 53 DEG C, in 1h, it is slowly added to acrylic acid and 20 mass of 15 mass parts
The N hydroxymethyl acrylamide of part, continues reaction 2h at such a temperature after having added；
(4) etherificate crosslinking: the dodecyl sodium sulfonate ammonium of 0.09 mass parts and the polyvinyl alcohol of 5 mass parts are dissolved in 45 mass parts
After water, limit stirring just add in starch solution, be further continued for after adding stir 20min, add 3 mass parts epoxychloropropane,
The anhydrous sodium sulfate of 24 mass parts and the sodium hydrate solid of 0.08 mass parts, react 1h at 25 DEG C, be 2mol/L by concentration
Sulfuric acid regulation PH be 6, obtain product.
Embodiment 2
(1) oxidation of cornstarch: the cornstarch of 75 mass parts and the water of 100 mass parts are stirred and make starch
Breast, is the sodium hydroxide solution of 2% with the addition mass fraction while stirring of reporting of 250r/min, the pH value of regulation starch solution
It is 7.0, adds 8% liquor natrii hypochloritis of 20 mass parts, maintain reaction molten with the sodium hydroxide solution that mass fraction is 2%
The PH of liquid is 7.0, and reacts 1h at 30 DEG C；
(2) activation of cornstarch: the pH value at room temperature regulating oxidized starch with the sodium hydroxide solution that mass fraction is 2% is 6.0,
The concentration adding 5～10 volume fractions is 2.0 × 10-3Mol/L ammonium persulfate solution activation 30min, adds 0.01 mass parts
Sodium hydrogensulfite activation 30min；
(3) starch-grafted: after cornstarch is heated to 50 DEG C, in 1h, it is slowly added to acrylic acid and 18 mass of 12 mass parts
The N hydroxymethyl acrylamide of part, continues reaction 2h at such a temperature after having added；
(4) etherificate crosslinking: the dodecyl sodium sulfonate ammonium of 0.05 mass parts and the polyvinyl alcohol of 1 mass parts are dissolved in 40 mass parts
After water, limit stirring just adds in starch solution, is further continued for stirring 20min, adds the epoxy chloropropionate of 0.5 mass parts after adding
Alkane, the anhydrous sodium sulfate of 20 mass parts and the sodium hydrate solid of 0.05 mass parts, react 1h at 25 DEG C, by concentration be
The sulfuric acid regulation PH of 2mol/L is 6, obtains product.
Embodiment 3
(1) oxidation of cornstarch: the cornstarch of 85 mass parts and the water of 150 mass parts are stirred and make starch
Breast, is the sodium hydroxide solution of 2% with the addition mass fraction while stirring of reporting of 300r/min, the pH value of regulation starch solution
It is 8.0, adds 10% liquor natrii hypochloritis of 25 mass parts, maintain reaction molten with the sodium hydroxide solution that mass fraction is 2%
The PH of liquid is 7.5, and reacts 6h at 30 DEG C；
(2) activation of cornstarch: the pH value at room temperature regulating oxidized starch with the sodium hydroxide solution that mass fraction is 2% is 6.5,
The concentration adding 10 volume fractions is 8.0 × 10-3Mol/L ammonium persulfate solution activation 30min, adds the Asia of 0.1 mass parts
Niter cake activation 30min；
(3) starch-grafted: after cornstarch is heated to 55 DEG C, in 1h, it is slowly added to acrylic acid and 25 mass of 16 mass parts
The N hydroxymethyl acrylamide of part, continues reaction 2h at such a temperature after having added；
(4) etherificate crosslinking: the dodecyl sodium sulfonate ammonium of 0.1 mass parts and the polyvinyl alcohol of 10 mass parts are dissolved in 50 mass parts
After water, limit stirring just add in starch solution, be further continued for after adding stir 20min, add 5 mass parts epoxychloropropane,
The sodium hydrate solid of the anhydrous sodium sulfate of 25 mass parts and O.1 mass parts, reacts 1h at 25 DEG C, is 2mol/L by concentration
Sulfuric acid regulation PH be 6, obtain product.
Claims (6)
1. the preparation method of a corn starch base based Wood Adhesives, it is characterised in that comprise the following steps:
(1) oxidation of cornstarch: the cornstarch of 75～85 mass parts and the water of 100～150 mass parts are stirred and make starch
Breast, adds sodium hydroxide solution while stirring, and the pH value of regulation starch solution is 7.0～8.0, adds 20～25 mass parts
8～10% liquor natrii hypochloritis, the PH maintaining reaction solution with sodium hydroxide solution is 7.0～7.5, and reacts 1～6h at 30 DEG C；
(2) activation of cornstarch: the pH value at room temperature regulating oxidized starch with sodium hydroxide solution is 6.0～6.5, adds
Ammonium sulfate activation 30min, adds the sodium hydrogensulfite activation 30min of 0.01～0.1 mass parts；
(3) starch-grafted: after cornstarch is heated to 50～55 DEG C, be slowly added in 1h 12～16 mass parts acrylic acid and
The N hydroxymethyl acrylamide of 18～25 mass parts, continues reaction 2h at such a temperature after having added；
(4) etherificate crosslinking: the dodecyl sodium sulfonate ammonium of 0.05～0.1 mass parts and the polyvinyl alcohol of 1～10 mass parts are dissolved in 40～50
After the water of mass parts, limit stirring just adds in starch solution, is further continued for stirring 20min, adds 0.5～5 mass parts after adding
Epoxychloropropane, 20～25 anhydrous sodium sulfates and 0.05～the sodium hydrate solid of O.1 mass parts of mass parts, anti-at 25 DEG C
Answer 1h, be 6 with sulfuric acid regulation PH, obtain product.
The preparation method of a kind of corn starch base based Wood Adhesives the most according to claim 1, it is characterised in that: described step
(1), in, reporting of stirring is 250～300r/min.
The preparation method of a kind of corn starch base based Wood Adhesives the most according to claim 1, it is characterised in that: described hydrogen-oxygen
Changing the mass fraction of NaOH in sodium solution is 2%.
The preparation method of a kind of corn starch base based Wood Adhesives the most according to claim 1, it is characterised in that: described over cure
The concentration of acid ammonium solution is 2.0～8.0 × 10-3mol/L。
The preparation method of a kind of corn starch base based Wood Adhesives the most according to claim 1, it is characterised in that: step (2)
In, the Volume fraction 5～10 that described ammonium persulfate solution adds.
The preparation method of a kind of corn starch base based Wood Adhesives the most according to claim 1, it is characterised in that: described sulfuric acid
Concentration be 2mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610110641.1A CN105754524A (en) | 2016-02-29 | 2016-02-29 | Preparation method for corn starch based wood adhesive |
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| CN201610110641.1A CN105754524A (en) | 2016-02-29 | 2016-02-29 | Preparation method for corn starch based wood adhesive |
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| CN201610110641.1A Pending CN105754524A (en) | 2016-02-29 | 2016-02-29 | Preparation method for corn starch based wood adhesive |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106085286A (en) * | 2016-08-10 | 2016-11-09 | 南宁市邦得力木业有限责任公司 | A kind of Environment-friendlyadhesive adhesive |
| CN106085284A (en) * | 2016-08-10 | 2016-11-09 | 南宁市邦得力木业有限责任公司 | A kind of novel timber adhesive |
| CN106085285A (en) * | 2016-08-10 | 2016-11-09 | 南宁市邦得力木业有限责任公司 | A kind of based Wood Adhesives |
| CN106147650A (en) * | 2016-08-10 | 2016-11-23 | 南宁市邦得力木业有限责任公司 | A kind of environment-friendly type based Wood Adhesives |
| CN106221610A (en) * | 2016-08-10 | 2016-12-14 | 南宁市邦得力木业有限责任公司 | A kind of timber environment-protective adhesive |
| CN107286866A (en) * | 2017-07-11 | 2017-10-24 | 合肥龙发包装有限公司 | A kind of Packaging Box amylum adhesive |
| CN107502229A (en) * | 2017-09-07 | 2017-12-22 | 滁州市光威化工有限公司 | A kind of nanocrystal cellulose enhancing maize-starch adhesive modified with oxidizing for making-cigarette and preparation method |
| CN108641640A (en) * | 2018-04-18 | 2018-10-12 | 海宁玖洲家具有限公司 | The preparation method of furniture environment-friendly adhesive |
| CN108841341A (en) * | 2018-05-25 | 2018-11-20 | 钱万琦 | A kind of preparation method of wood adhesive |
| CN111278866A (en) * | 2017-08-11 | 2020-06-12 | 瑞典淀粉生产者协会 | Process for preparing inhibited starch |
| WO2021036197A1 (en) * | 2019-08-30 | 2021-03-04 | 齐鲁工业大学 | Preparation method for starch-based adhesive |
| CN113088222A (en) * | 2021-04-30 | 2021-07-09 | 南宁市磨氏林圣木业有限公司 | Adhesive for preventing plate from warping and preparation method thereof |
| CN113461853A (en) * | 2021-06-25 | 2021-10-01 | 山东顶立新材料科技有限公司 | Environment-friendly plate alignment adhesive polymerization emulsion and preparation method thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106085284A (en) * | 2016-08-10 | 2016-11-09 | 南宁市邦得力木业有限责任公司 | A kind of novel timber adhesive |
| CN106085285A (en) * | 2016-08-10 | 2016-11-09 | 南宁市邦得力木业有限责任公司 | A kind of based Wood Adhesives |
| CN106147650A (en) * | 2016-08-10 | 2016-11-23 | 南宁市邦得力木业有限责任公司 | A kind of environment-friendly type based Wood Adhesives |
| CN106221610A (en) * | 2016-08-10 | 2016-12-14 | 南宁市邦得力木业有限责任公司 | A kind of timber environment-protective adhesive |
| CN106085286A (en) * | 2016-08-10 | 2016-11-09 | 南宁市邦得力木业有限责任公司 | A kind of Environment-friendlyadhesive adhesive |
| CN107286866A (en) * | 2017-07-11 | 2017-10-24 | 合肥龙发包装有限公司 | A kind of Packaging Box amylum adhesive |
| CN111278866B (en) * | 2017-08-11 | 2022-03-25 | 瑞典淀粉生产者协会 | Process for preparing inhibited starch |
| CN111278866A (en) * | 2017-08-11 | 2020-06-12 | 瑞典淀粉生产者协会 | Process for preparing inhibited starch |
| US11566084B2 (en) | 2017-08-11 | 2023-01-31 | Sveriges Stärkelseproducenter, förening u.p.a. | Method for preparing an inhibited starch |
| CN107502229A (en) * | 2017-09-07 | 2017-12-22 | 滁州市光威化工有限公司 | A kind of nanocrystal cellulose enhancing maize-starch adhesive modified with oxidizing for making-cigarette and preparation method |
| CN108641640A (en) * | 2018-04-18 | 2018-10-12 | 海宁玖洲家具有限公司 | The preparation method of furniture environment-friendly adhesive |
| CN108841341A (en) * | 2018-05-25 | 2018-11-20 | 钱万琦 | A kind of preparation method of wood adhesive |
| WO2021036197A1 (en) * | 2019-08-30 | 2021-03-04 | 齐鲁工业大学 | Preparation method for starch-based adhesive |
| CN113088222A (en) * | 2021-04-30 | 2021-07-09 | 南宁市磨氏林圣木业有限公司 | Adhesive for preventing plate from warping and preparation method thereof |
| CN113088222B (en) * | 2021-04-30 | 2022-08-23 | 南宁市磨氏林圣木业有限公司 | Adhesive for preventing plate from warping and preparation method thereof |
| CN113461853A (en) * | 2021-06-25 | 2021-10-01 | 山东顶立新材料科技有限公司 | Environment-friendly plate alignment adhesive polymerization emulsion and preparation method thereof |
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