CN107400494A - A kind of wheat stalk-konjaku flour composite adhesive and preparation method thereof - Google Patents

A kind of wheat stalk-konjaku flour composite adhesive and preparation method thereof Download PDF

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Publication number
CN107400494A
CN107400494A CN201610333132.5A CN201610333132A CN107400494A CN 107400494 A CN107400494 A CN 107400494A CN 201610333132 A CN201610333132 A CN 201610333132A CN 107400494 A CN107400494 A CN 107400494A
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China
Prior art keywords
wheat stalk
konjaku flour
preparation
adhesive
add
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CN201610333132.5A
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Chinese (zh)
Inventor
蒲德兴
黄朋勉
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Changsha Huihua Adhesive And Technology Co Ltd
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Changsha Huihua Adhesive And Technology Co Ltd
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Priority to CN201610333132.5A priority Critical patent/CN107400494A/en
Publication of CN107400494A publication Critical patent/CN107400494A/en
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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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/06—Polyurethanes from polyesters
    • 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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
    • C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
    • 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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
    • C08G18/6484—Polysaccharides and derivatives thereof
    • 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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
    • C08G18/6492—Lignin containing materials; Wood resins; Wood tars; Derivatives thereof
    • 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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes

Abstract

The invention discloses a kind of wheat stalk konjaku flour composite adhesive and preparation method thereof, it is related to technical field of adhesive preparation.The product of the present invention is a kind of composite adhesive, colloid coordinates other auxiliary materials to be made using wheat stalk, konjaku flour as primary raw material, and cohesive is good, intensity is high, and cost is low, manufacture craft is simple, without the harmful substance composition such as formaldehyde and fragrant class, it is free from environmental pollution, for the adhesive of degradable environmentally-friendly, as adhesive particularly suitable for glued board, core-board, the production field of carton.This method comprises the following steps（1）Prepare plant base PEPA；（2）Prepare Polymer Composite Emulsion；（3）Macromolecule composite aqueous emulsion is stirred at room temperature in proportion with isocyanates and mixed, produces macromolecule composite adhesive.

Description

A kind of wheat stalk-konjaku flour composite adhesive and preparation method thereof
Technical field
The present invention relates to chemical field, especially a kind of wheat stalk-konjaku flour composite adhesive and its preparation Method.
Background technology
It is well known that wood industry, packed in cases, house ornamentation field need to use substantial amounts of adhesive to be used for Product processing. In the wood adhesive used at present, many is the three-aldehyde glue ----Lauxite of solvent（UF）, phenolic resin（PF）With Melamine resin（VIF）, this " three-aldehyde glue " discharges in the production and use process in addition to poor water resistance, storage period are short Go out substantial amounts of formaldehyde, environmental pollution causes very big influence, and mankind's Long Term Contact can also cause breathing problem, pernicious swollen The danger of the diseases such as knurl, leukaemia.With the proposition of the theory such as environmental protection and energy-conservation, timber industry it is also proposed with glue higher It is required that this requires to reduce formaldehyde monomers and dosage, content of free aldehyde in adhesive is reached minimum standard, or seek suitably Raw material substitutes " three-aldehyde glue " with formula, thoroughly solves the next environmental problem of free aldehyde release band.
In recent years, as the reinforcement of environmental consciousness, people increasingly increase to the demand of environment-friendly adhesive.The U.S. in 2007 CARB has strict environmental protection standard to the adhesive used in woodwork, and implements in 2013.US7,722,712 B2 and Dolbey seminars（Dolbey R. etc.Recent developments in epoxy resins. Rapra Rev. Rep. 8:176pp,1996）Develop and be based on natural bean gum adhesive, bonding strength and water resistance are above urea-formaldehyde glue, but deposit In the high deficiency of product price.Natural adhesive raw material sources are extensive, and cost is low, easy to use, asepsis environment-protecting, with room-mate's energy It is nervous and adhesive theoretical research to go deep into, it is often more important that the enhancing of mankind's environmental consciousness, natural adhesive again by Pay attention to, its naturally environmentally friendly and reproducible advantage is given full play to it.
Wheat stalk is discarded serious in China, the direct burn-up having, and has both wasted or polluting weather, haze is caused, with wheat Stalk prepares macromolecule for raw material and meets adhesive, turns waste into wealth, has both made full use of discarded wheat stalk, and cost is cheap, and And provide one and solve the approach that wheat stalk pollution environment is burned in rural area.Konjaku glucomannan（KGM）It is to extract from day south A kind of deposit property polysaccharide in star section konjac tuber, is a kind of renewable natural polymer child resource, its wide material sources, has biology Degradability, water-soluble adhesiveness is high, can thicken, gel and film forming.The report of adhesive is developed in research using konjaku as raw material at present Road is few.CN104974683A reports " a kind of preparation of konjaku flour-chitosan-PVA blending adhesive ", with konjaku flour, shell gathers Sugar and PVA are raw material, are made and are applied to timber assembly, wood-based plate manufacture field, the deficiency of high expensive be present. CN104800813A reports " a kind of konjaku glucomannan car sickness therapeutic plaster and preparation method thereof ", using Glucomannan as main raw material(s), Coordinate other auxiliary materials that adhesive is made, then along with Chinese medicinal formulae, have and alleviate carsick effect, but the adhesive equally has The deficiency of high expensive.The compound research for preparing adhesive of wheat stalk and konjaku flour is had no into report, the present invention is based on small Wheat Straw and konjaku flour prepare the research of adhesive.
The content of the invention
It is an object of the invention to：For above-mentioned problem, there is provided a kind of adhesion strength is high, the wheat of water-tolerant The preparation method of stalk-konjaku flour composite adhesive.
The preparation method of a kind of wheat stalk-konjaku flour composite adhesive, it is characterised in that including following steps：
（1) plant base PEPA is prepared
Into 100g dihydric alcohol, under agitation, add 10 mesh below wheat stalk powder 15-20g, catalyst lean sulfuric acid 2~ 3g, after blending uniformly, 160~180 DEG C are heated to, is incubated 30min, the 15~20g of wheat stalk powder added below 10 mesh, after Continue and be incubated 60~90min at 160~180 DEG C, vegetable based polyol is made, add 20~30g of glutaric anhydride, in 150 DEG C of insulations 30min, temperature is risen to 190~210 DEG C, 120~150min is incubated, is cooled to normal temperature, plant base PEPA is made；
（2）Prepare Polymer Composite Emulsion
2.5~3.0g konjaku flour is added in 100g water, 30~40 DEG C of 20~30min of stirring are allowed to be swelled, and use quality Fraction is that to adjust pH be 8~10 to 5% sodium hydrate aqueous solution, adds hydrogen peroxide solution 2.5~3.0g of mass fraction 30%, 40~50 DEG C alkaline oxygenated 40~50min, it is 6.5 to adjust pH with watery hydrochloric acid, cooling discharging, oxidized konjac glucomannan aqueous emulsion is made；Will Oxidized konjac glucomannan aqueous emulsion and step（1）Obtained plant base PEPA in mass ratio 100:15~25 blendings 30min, macromolecule compound aqueous solution is made；
（3）The preparation of wheat stalk-konjaku flour composite adhesive
Macromolecule composite aqueous emulsion and diisocyanate are pressed 100:Mixing is stirred at room temperature in 7~10 ratio, produce wheat stalk- Konjaku flour composite adhesive.
By adopting the above-described technical solution, the beneficial effects of the invention are as follows：The present invention uses diisocyanate（IPDI). Isocyanates（—NCO）With high reactivity, easily produced containing-OH compounds with polyalcohol, water and wood surface Raw cross-linking reaction.Isocyanates can typically use phenols, alcohols etc. to be closed, and can also use isocyanates auto polymerization, water The methods of emulsification, is handled.NCO majorities after being closed using the above method need just discharge at very high temperatures. This experiment is closed using low temperature sodium bisulfite method to isocyanates, and the isocyanates after closing will seal in 60 DEG C of cans The NCO closed is discharged.Production of the method particularly suitable for glued board, core-board.The preparation technology of the present invention passes through Preferred feedstock, controls the temperature conditionss of reaction, for the more existing adhesive of gained adhesive, does not contain organic volatile, pollutes Small more environmentally friendly, adhesion strength is stronger, and water resistance is higher, while production cost is low, is easy to mass produce, and is nontoxic dirt Contaminate few adhesive.Glue-spread is 180g/m2。
Embodiment
By the following examples, the invention will be further described：
Embodiment 1
A kind of preparation method of wheat stalk-konjaku flour composite adhesive, comprises the following steps：（1）100g glycerine is weighed to add Enter in 1L round-bottomed flasks, weigh 16g wheat stalk powders and add in flask, 160 DEG C are heated to oil bath pan, add the 4g concentrated sulfuric acids and make Catalyst, the mechanical agitation 1.5h at 160 DEG C；Weigh 14g wheat stalk powders add flask at 160 DEG C mechanical agitation 2h； Weigh 20g glutaric anhydrides to add in flask, react to obtain PEPA mechanical agitation 3h at 150 DEG C.
（2）Weigh 3g konjaku flours to add in 100g water, mechanical agitation 1h at 35 DEG C；Add 5%NaOH solution and adjust pH to 9, then Add 3g30%H2O2Solution, oxidation, mechanical agitation 1h is into aqueous emulsion at 45 DEG C；Take the above-mentioned aqueous emulsions of 100g and 20g polyester polyols Alcohol, which is blended in mechanical agitation 1h at 25 DEG C, must mix Polymer Composite Emulsion.
（3）Above-mentioned mixing aqueous emulsion 30g is taken, 4.5gIPDI is added, mixing, Wheat Straw is obtained in 20 DEG C of mechanical agitation 0.5h Stalk-konjaku flour composite adhesive.
Embodiment 2
A kind of preparation method of wheat stalk-konjaku flour composite adhesive, comprises the following steps：（1）100g glycerine is weighed to add Enter in 1L round-bottomed flasks, weigh 19g wheat stalk powders and add in flask, 170 DEG C are heated to oil bath pan, add the 5g concentrated sulfuric acids and make Catalyst, the mechanical agitation 1.0h at 160 DEG C；Weigh 15g wheat stalk powders add flask at 170 DEG C mechanical agitation 2h； Weigh 21g glutaric anhydrides to add in flask, react to obtain PEPA mechanical agitation 4h at 140 DEG C.
（2）Weigh 3g konjaku flours to add in 100g water, mechanical agitation 1h at 40 DEG C；Add 5%NaOH solution and adjust pH to 9, then Add 3.5g30%H2O2Solution, oxidation, mechanical agitation 1h is into aqueous emulsion at 45 DEG C；Take the above-mentioned aqueous emulsions of 100g and 22g polyester more First alcohol, which is blended in mechanical agitation 1h at 25 DEG C, must mix Polymer Composite Emulsion.
（3）Above-mentioned mixing aqueous emulsion 30g is taken, 4.2gIPDI is added, mixing, Wheat Straw is obtained in 20 DEG C of mechanical agitation 1.0h Stalk-konjaku flour composite adhesive.
Following testing performance index is done to the adhesive obtained by embodiment 1 or 2, bonding step refers to GB/T 15104- 2006《Decorative veneered woodbased panel》Carry out.Will be using sheet of veneer single spreading stick as panel, glue-spread 180g/m2, The existing pressure with 1.0MPa is cold-pressed 20min after gluing, then in the favorite 1.0MPa of hot press pressure, with 115 DEG C of uniform pressurizations 3min, the sheet material after compacting are aged 24h at room temperature.Test specimen is made in sheet material after ageing, surveys its surface bonding intensity.Test knot Fruit is as follows：
Index Embodiment 1 Embodiment 2
Shear strength/MPa 31 33
Tensile strength/MPa 28 29
Peel strength/MPa 45 50
From test result as can be seen that the adhesive adhesive strength obtained by the present invention is big, reach the standard of wood adhesive, fit Share in timber assembly, wood-based plate manufacture field, due to environmental protection, be also applied for interior decoration wallpaper adhesive area.

Claims (6)

1. the preparation method of a kind of wheat stalk-konjaku flour composite adhesive, it is characterised in that comprise the following steps：
（1) plant base PEPA is prepared
Into 100g dihydric alcohol, under agitation, wheat stalk powder 15-20g, the 2~3g of catalyst added below 10 mesh, blending After uniformly, 160~180 DEG C are heated to, 30min is incubated, the 15~20g of wheat stalk powder added below 10 mesh, continues 160 ~180 DEG C of 60~90min of insulation, are made vegetable based polyol, add 20~30g of glutaric anhydride, and 30min is incubated at 150 DEG C, will Temperature rises to 190~210 DEG C, is incubated 120~150min, is cooled to normal temperature, and plant base PEPA is made；
The catalyst is the concentrated sulfuric acid, p-methyl benzenesulfonic acid.
2. the dihydric alcohol is ethylene glycol, propane diols, butanediol.
3. prepare Polymer Composite Emulsion
3.0g konjaku flour is added in 100g water, 30~40 DEG C of 20~60min of stirring are allowed to be swelled, and are with mass fraction It is 8~10 that 5% sodium hydrate aqueous solution, which adjusts pH, adds 0.2~1.0g of hydrogen peroxide solution of mass fraction 30%, 40~50 DEG C of alkalescence 40~50min is aoxidized, it is 6.5 to adjust pH with watery hydrochloric acid, cooling discharging, oxidized konjac glucomannan aqueous emulsion is made；Will oxidation evil spirit Taro Glucomannan aqueous emulsion and step（1）Obtained plant base PEPA in mass ratio 100:15~25 blending 30min, system Secure satisfactory grades sub- compound aqueous solution；
The preparation of wheat stalk-konjaku flour composite adhesive
By macromolecule composite aqueous emulsion and diisocyanate（IPDI 100) are pressed:Mixing is stirred at room temperature in 7~10 ratio, produces small Wheat Straw-konjaku flour composite adhesive.
A kind of 4. preparation method of wheat stalk-konjaku flour composite adhesive according to claim 1, it is characterised in that institute The preparation for the plant base PEPA stated：
（1）Weigh 100g ethylene glycol to add in 1L round-bottomed flasks, weigh 16g wheat stalk powders and add in flask, with oil bath pan plus Heat adds the 4g concentrated sulfuric acids and makees catalyst to 160 DEG C, the mechanical agitation 1.5h at 160 DEG C；
（2）Weigh 14g wheat stalk powders add flask at 160 DEG C mechanical agitation 2h；
（3）Weigh 20g glutaric anhydrides to add in flask, react to obtain PEPA mechanical agitation 3h at 150 DEG C.
A kind of 5. preparation method of wheat stalk-konjaku flour composite adhesive according to claim 1, it is characterised in that institute The preparation for the Polymer Composite Emulsion stated：
Weigh 3g konjaku flours to add in 100g water, mechanical agitation 1h at 35 DEG C；
Add 5%NaOH solution and adjust pH to 9, add 3g30%H2O2Solution, oxidation, mechanical agitation 1h is into aqueous emulsion at 45 DEG C；
Polymer Composite Emulsion must be mixed by taking the above-mentioned aqueous emulsions of 100g to be blended in mechanical agitation 1h at 25 DEG C with 20g PEPAs；
The preparation method of a kind of wheat stalk-konjaku flour composite adhesive according to claim 1, it is characterised in that described Wheat stalk-konjaku flour composite adhesive preparation：Above-mentioned mixing aqueous emulsion 30g is taken, adds 4.5gIPDI, mixing, 20 DEG C mechanical agitation 0.5h obtains wheat stalk-konjaku flour composite adhesive.
6. wheat stalk-konjaku flour the composite adhesive prepared as the either method described in right 1 ~ 4.
CN201610333132.5A 2016-05-19 2016-05-19 A kind of wheat stalk-konjaku flour composite adhesive and preparation method thereof Pending CN107400494A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109628014A (en) * 2018-12-04 2019-04-16 任国斌 A kind of environmentally protective Wall paper adhesive and preparation method thereof
CN110078883A (en) * 2019-05-22 2019-08-02 西华大学 A kind of water paint resin, preparation method and composition based on konjaku flour

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103320078A (en) * 2013-05-23 2013-09-25 济南大学 Plant-based polyester polyol-chitosan adhesive, and preparation method and application thereof
CN103320081A (en) * 2013-05-23 2013-09-25 济南大学 High-molecular composite adhesive, and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103320078A (en) * 2013-05-23 2013-09-25 济南大学 Plant-based polyester polyol-chitosan adhesive, and preparation method and application thereof
CN103320081A (en) * 2013-05-23 2013-09-25 济南大学 High-molecular composite adhesive, and preparation method and application thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109628014A (en) * 2018-12-04 2019-04-16 任国斌 A kind of environmentally protective Wall paper adhesive and preparation method thereof
CN110078883A (en) * 2019-05-22 2019-08-02 西华大学 A kind of water paint resin, preparation method and composition based on konjaku flour
CN110078883B (en) * 2019-05-22 2021-08-03 西华大学 Water-based paint resin based on konjac flour, preparation method and composition thereof

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Application publication date: 20171128