CN1789362A - One-step preparation process of organic-montmorillonite modified ethylene-vinyl acetate hot-melt adhesive - Google Patents
One-step preparation process of organic-montmorillonite modified ethylene-vinyl acetate hot-melt adhesive Download PDFInfo
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- CN1789362A CN1789362A CN 200510112141 CN200510112141A CN1789362A CN 1789362 A CN1789362 A CN 1789362A CN 200510112141 CN200510112141 CN 200510112141 CN 200510112141 A CN200510112141 A CN 200510112141A CN 1789362 A CN1789362 A CN 1789362A
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Abstract
The invention discloses the one-step method of ethylene-vinyl acetate hot melt adhesive modified by organic montmorillonite, comprising the following steps: putting 1-12wt% montmorillonite, 0.5-8wt% organic intercalating agent, 15-30wt% tackifying resin, 5-15wt% plasticity agent and 0.1-0.5wt% anti-oxidant into rapid mixer at 100-200Deg.C, stirring them, then adding 30-50wt% ethylene-vinyl acetate, cooling and getting the product. The method simplifies the preparing technology of EVA hot melt adhesive modified by OMMT, and the peel bond strength of EVA hot melt adhesive is up to 5.25/kN/m at 180 deg.
Description
Technical field
The present invention relates to a kind of hot melt adhesive that contains ethene-vinyl acetate, the present invention relates to a kind of method of utilizing a step fusion intercalation composite algorithm to prepare organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive in particular.
Background technology
Ethene-vinyl acetate (EVA) hot melt adhesive is most widely used, that consumption is maximum a kind of hot melt adhesive.It has excellent cementing property, and nearly all material is all had the hot glue relay; Its resistance to chemical reagents, weathering resistance, winter hardiness, excellent electrical properties; Melt viscosity is low, and applying glue is convenient; Good with the consistency of Synergist S-421 95, the Synergist S-421 95 range of choice is wide, can be according to service requirements preparation performance/price than rational hot melt adhesive.The EVA hot melt adhesive not only is used for shoemaking and clothes in a large number to be pasted, and also is widely used in the unsewn binding of books, and the timber laminated plates is made, and non-woven fabrics is made or the like.The EVA hot melt adhesive also has application at aspects such as automobile, electronics, electrical equipment and cigarette, system jars.But it is lower that the shortcoming of EVA hot melt adhesive is a bonding strength, thermo-labile, and not anti-fatty oil needs that it is carried out modification and could adapt to Application Areas widely.A spot of layered silicate such as organic montmorillonoid (OMMT) are filled in the hot melt adhesive component, can improve some performance of EVA hot melt adhesive.Polynite (MMT) has typical 2: 1 type laminate structures, is that silicate lamella about 1nm piles up and forms by thickness.The processing that organises of MMT is the important step of the good polymer nanocomposites of processability.Use long chain alkyl ammonium salt to MMT processings that organise, make the increase of MMT sheet interlayer spacing, and become lipophilicity, become OMMT, can increase consistency with polymkeric substance such as EVA by wetting ability.Compound by fusion intercalation, the EVA hot melt adhesive of preparation OMMT modification.But the processing that organises of MMT exists technical process long, the power consumption water wasting, and efficient is low, shortcomings such as aftertreatment complexity.
Summary of the invention
Technical problem to be solved by this invention provides an a kind of one-step preparation method of the easy compound montmorillonite modified ethylene that organises of fusion intercalation-vinyl acetate between to for plastic hot melt adhesive, the present invention has simplified the preparation technology of the EVA hot melt adhesive of preparation OMMT modification, the technical process that has overcome the existence of organ-mmt process is long, the power consumption water wasting, efficient is low, shortcomings such as aftertreatment complexity make the ethene-vinyl acetate hot melt adhesive have good bonding strength simultaneously.
The technical solution used in the present invention: an a kind of one-step preparation method of organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive: polynite 1～12 (weight percent), organic intercalation agent 0.5～8 (weight percent), tackifying resin 15～30 (weight percent), softening agent 5～15 (weight percent) and oxidation inhibitor 0.1～0.5 (weight percent) together joined in 100～200 ℃ the super mixer, stir, mix, add ethene-vinyl acetate 30～50 (weight percent) then, after fully mediating, cooling, discharging, granulation.
Described polynite is a sodium-based montmorillonite.
Described organic intercalation agent is selected from Dodecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyl trimethyl ammonium chloride, two octadecyl dimethyl brometo de amonio.
Described tackifying resin is selected from one or more the mixture in coumarone indene resin, Gum Rosin, petroleum resin, the styrene-isoprene-phenylethene.
Described softening agent is selected from alicyclic mineral oil, liquid wax or stearic acid.
Described oxidation inhibitor is selected from Hinered phenols antioxidant, as antioxidant 1010, oxidation inhibitor 168.
One of beneficial effect of the present invention is: omitted the MMT process that organises, simplified the preparation technology of the EVA hot melt adhesive of preparation OMMT modification; Two of beneficial effect is: add the bonding strength that a spot of OMMT just can improve the EVA hot melt adhesive significantly.The present invention prepares the EVA hot melt adhesive of OMMT modification by a step fusion intercalation composite methods.This modified EVA hot-melt adhesive stick is through 180 ° of stripping strengths (canvas-canvas) experiment test, and stripping strength reaches 5.25kN/m, has good bonding strength.
Embodiment
By embodiment the present invention is described in further detail, an a kind of one-step preparation method of organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive: with polynite 1～12 (weight percent), organic intercalation agent 0.5～8 (weight percent), tackifying resin 15～30 (weight percent), softening agent 5～15 (weight percent) and oxidation inhibitor 0.1～0.5 (weight percent) together join in 100～200 ℃ the super mixer, stir, mix, add ethene-vinyl acetate 30～50 (weight percent) then, after fully mediating, cooling, discharging, granulation.Described polynite is a sodium-based montmorillonite.Described organic intercalation agent is selected from Dodecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyl trimethyl ammonium chloride, two octadecyl dimethyl brometo de amonio.Described tackifying resin is selected from one or more the mixture in coumarone indene resin, Gum Rosin, petroleum resin, the styrene-isoprene-phenylethene.Described softening agent is selected from alicyclic mineral oil, liquid wax or stearic acid.Described oxidation inhibitor is selected from Hinered phenols antioxidant, as antioxidant 1010, oxidation inhibitor 168 etc.
Embodiment
EVA hot melt adhesive component: EVA 40 (weight percent), Gum Rosin GA-90 32 (weight percent), naphthenic oil 8 (weight percent), stearic acid 6 (weight percent), paraffin 1.5 (weight percent), sodium base MMT 8% (weight percent), cetyl trimethylammonium bromide 4 (weight percent), antioxidant 1010 0.5 (weight percent).Above-mentioned MMT, cetyl trimethylammonium bromide, GA-90, stearic acid, naphthenic oil, oxidation inhibitor after 5 minutes, are obtained pre-composition in 150 ℃ of mixing in high-speed mixer.The EVA elastomerics is joined in the mixing machine, with pre-composition thorough mixing 30 minutes.Cooling.Granulation obtains the EVA hot melt adhesive of the OMMT modification of step fusion intercalation composite algorithm preparation.
Comparative example one:
EVA hot melt adhesive component: EVA 42 (weight percent), Gum Rosin GA-90 33 (weight percent), naphthenic oil 8.3 (weight percent), stearic acid 6.7 (weight percent), paraffin 1.5 (weight percent), sodium base MMT 8% (weight percent), antioxidant 1010 0.5 (weight percent).Above-mentioned MMT, GA-90, stearic acid, naphthenic oil, oxidation inhibitor after 5 minutes, are obtained pre-composition in 150 ℃ of mixing in high-speed mixer.The EVA elastomerics is joined in the mixing machine, with pre-composition thorough mixing 30 minutes.Cooling.Granulation obtains the EVA hot melt adhesive of MMT modification.
Comparative example two (two step method):
EVA hot melt adhesive component: EVA 40 (weight percent), Gum Rosin GA-90 32 (weight percent), naphthenic oil 8 (weight percent), stearic acid 6 (weight percent), paraffin 1.5 (weight percent), sodium base MMT 8% (weight percent), cetyl trimethylammonium bromide 4 (weight percent), antioxidant 1010 0.5 (weight percent).
Processing at first organises MMT.Treatment process is: by mass ratio is to take by weighing MMT and cetyl trimethylammonium bromide at 1: 1 in beaker, adds an amount of distilled water, stirs down at 50 ℃, after question response is finished, is cooled to room temperature.Decompress filter, the throw out that obtains uses the deionized water repetitive scrubbing.It is dry that milky white precipitate thing filter cake is put into baking oven, until constant weight, ground 80 mesh sieves.With the white organic montmorillonoid powder that obtains, sealing is preserved.
The polynite (OMMT) that has organised, GA-90, stearic acid, naphthenic oil, oxidation inhibitor in high-speed mixer in 150 ℃ mix 5 minutes after, obtain pre-composition.The EVA elastomerics is joined in the mixing machine, with pre-composition thorough mixing 30 minutes.Cooling.Granulation.Obtain the EVA hot melt adhesive of OMMT modification.
Peel strength test:
The EVA hot melt adhesive of the modification that makes is in 150 ℃ of following fusions, and the employing temperature is that 110 ℃ coating machine is coated in fused EVA hot melt adhesive on the canvas.Two 20mm * 30mm canvas that one side is scribbled hot melt adhesive is fitted mutually, places 110 ℃ of baking ovens hot-forming 5 minutes, cooling.Make the batten that is used for 180 ° of peel strength tests.Adopt the test of electron detachment trier BLD-200S electronic stripping tester, draw speed is 50mm/min.Test result sees Table 1.
180 ° of stripping strengths (canvas-canvas) of table 1 EVA hot melt adhesive
| The glue sample | Stripping strength/kN/m |
| The EVA hot melt adhesive (two step method) of EVA hot melt adhesive (single stage method) the OMMT modification of unmodified EVA hot melt adhesive OMMT modification | 2.37 5.25 5.53 |
By table 1 as seen, add the bonding strength that a spot of OMMT can improve the EVA hot melt adhesive significantly.The EVA hot melt adhesive of the OMMT modification of one step fusion intercalation composite algorithm preparation, omitted the process that organises of MMT, simplified the preparation technology of the EVA hot melt adhesive of preparation OMMT modification, and with elder generation MMT is organised, the modified EVA hot-melt adhesive stick with the compound preparation of EVA hot melt adhesive has good equally bonding strength again.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (6)
1. an one-step preparation method of an organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive: polynite 1～12 (weight percent), organic intercalation agent 0.5～8 (weight percent), tackifying resin 15～30 (weight percent), softening agent 5～15 (weight percent) and oxidation inhibitor 0.1～0.5 (weight percent) together joined in 100～200 ℃ the super mixer, stir, mix, add ethene-vinyl acetate 30～50 (weight percent) then, after fully mediating, cooling, discharging, granulation.
2. according to an one-step preparation method of the described a kind of organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive of claim 1, it is characterized in that: described polynite is a sodium-based montmorillonite.
3. according to an one-step preparation method of the described a kind of organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive of claim 1, it is characterized in that: described organic intercalation agent is selected from Dodecyl trimethyl ammonium chloride or cetyl trimethylammonium bromide.
4. according to an one-step preparation method of the described a kind of organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive of claim 1, it is characterized in that: described tackifying resin is selected from one or more the mixture in coumarone indene resin, Gum Rosin, petroleum resin, the styrene-isoprene-phenylethene.
5. according to an one-step preparation method of the described a kind of organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive of claim 1, it is characterized in that: described softening agent is selected from alicyclic mineral oil, liquid wax or stearic acid.
6. according to an one-step preparation method of the described a kind of organic montmorrilonite modified ethene-vinyl acetate hot melt adhesive of claim 1, it is characterized in that: described oxidation inhibitor is selected from Hinered phenols antioxidant.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005101121413A CN100350011C (en) | 2005-12-28 | 2005-12-28 | One-step preparation process of organic-montmorillonite modified ethylene-vinyl acetate hot-melt adhesive |
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| CNB2005101121413A CN100350011C (en) | 2005-12-28 | 2005-12-28 | One-step preparation process of organic-montmorillonite modified ethylene-vinyl acetate hot-melt adhesive |
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| CN1789362A true CN1789362A (en) | 2006-06-21 |
| CN100350011C CN100350011C (en) | 2007-11-21 |
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| CN100395301C (en) * | 2006-07-18 | 2008-06-18 | 山东久隆高分子材料有限公司 | Nanometer composite hot melt adhesive for sealing joint in heavy caliber polyethylene pipeline |
| CN101838511A (en) * | 2010-03-31 | 2010-09-22 | 鲁泰纺织股份有限公司 | Heat-resistant clothing hot melt adhesive and preparation method thereof |
| JP2011148876A (en) * | 2010-01-20 | 2011-08-04 | Tosoh Corp | Ethylene-vinyl acetate copolymer resin composition and hot-melt adhesive comprising the same |
| CN102643617A (en) * | 2012-04-20 | 2012-08-22 | 北京益达装饰材料有限公司 | Ultraviolet radiation based bonding process for EVA (ethylene vinyl acetate) hot melt adhesive on decorative edge bands |
| CN103101281A (en) * | 2013-01-31 | 2013-05-15 | 北京工业大学 | Laser square light spot thermal radiation-based process for adhering EVA (Ethylene-Vinyl Acetate) hot melt adhesive on decorative edge band |
| CN103468171A (en) * | 2013-08-13 | 2013-12-25 | 安徽东方金河精密机械制造有限公司 | Hot melt adhesive used for automobile interior decoration parts |
| CN103509495A (en) * | 2013-09-18 | 2014-01-15 | 滁州市光威化工有限公司 | Hot melt adhesive for cable accessories |
| CN103571381A (en) * | 2013-10-24 | 2014-02-12 | 芜湖众力部件有限公司 | Waterproof hot melt adhesive |
| CN103571380A (en) * | 2013-10-24 | 2014-02-12 | 芜湖众力部件有限公司 | Hot melt adhesive with low odor |
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| CN105219306A (en) * | 2015-10-23 | 2016-01-06 | 台州市顶立胶粘剂有限公司 | A kind of organo montmorillonite and application thereof |
| CN105838298A (en) * | 2016-04-14 | 2016-08-10 | 上海政太纳米科技股份有限公司 | EVA hot melt adhesive used for fixing electronic element |
| CN105936814A (en) * | 2016-06-07 | 2016-09-14 | 刘伟 | Anti-ultraviolet plate adhesive |
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| CN100395301C (en) * | 2006-07-18 | 2008-06-18 | 山东久隆高分子材料有限公司 | Nanometer composite hot melt adhesive for sealing joint in heavy caliber polyethylene pipeline |
| JP2011148876A (en) * | 2010-01-20 | 2011-08-04 | Tosoh Corp | Ethylene-vinyl acetate copolymer resin composition and hot-melt adhesive comprising the same |
| CN101838511A (en) * | 2010-03-31 | 2010-09-22 | 鲁泰纺织股份有限公司 | Heat-resistant clothing hot melt adhesive and preparation method thereof |
| CN101838511B (en) * | 2010-03-31 | 2012-09-12 | 鲁泰纺织股份有限公司 | Heat-resistant clothing hot melt adhesive and preparation method thereof |
| CN102643617A (en) * | 2012-04-20 | 2012-08-22 | 北京益达装饰材料有限公司 | Ultraviolet radiation based bonding process for EVA (ethylene vinyl acetate) hot melt adhesive on decorative edge bands |
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| US9536637B2 (en) | 2012-12-20 | 2017-01-03 | Sumitomo Electric Industries, Ltd. | Multilayered heat-recoverable article, wire splice, and wire harness |
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| CN103468171A (en) * | 2013-08-13 | 2013-12-25 | 安徽东方金河精密机械制造有限公司 | Hot melt adhesive used for automobile interior decoration parts |
| CN103509495A (en) * | 2013-09-18 | 2014-01-15 | 滁州市光威化工有限公司 | Hot melt adhesive for cable accessories |
| CN103571381A (en) * | 2013-10-24 | 2014-02-12 | 芜湖众力部件有限公司 | Waterproof hot melt adhesive |
| CN103571380A (en) * | 2013-10-24 | 2014-02-12 | 芜湖众力部件有限公司 | Hot melt adhesive with low odor |
| CN105219306A (en) * | 2015-10-23 | 2016-01-06 | 台州市顶立胶粘剂有限公司 | A kind of organo montmorillonite and application thereof |
| CN105838298A (en) * | 2016-04-14 | 2016-08-10 | 上海政太纳米科技股份有限公司 | EVA hot melt adhesive used for fixing electronic element |
| CN106010367A (en) * | 2016-06-07 | 2016-10-12 | 刘伟 | Board adhesive with great bonding strength |
| CN106010393A (en) * | 2016-06-07 | 2016-10-12 | 刘伟 | Board adhesive with good resistance to water penetration |
| CN105936814A (en) * | 2016-06-07 | 2016-09-14 | 刘伟 | Anti-ultraviolet plate adhesive |
| CN106252442A (en) * | 2016-08-31 | 2016-12-21 | 乐凯胶片股份有限公司 | A kind of solar cell backboard |
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Assignee: Ningbo Songhe Stationery Co., Ltd. Assignor: Shanghai Institute of Technology Contract fulfillment period: 2009.3.13 to 2012.3.12 contract change Contract record no.: 2009330000806 Denomination of invention: One-step preparation process of organic-montmorillonite modified ethylene-vinyl acetate hot-melt adhesive Granted publication date: 20071121 License type: Exclusive license Record date: 2009.4.29 |
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Assignee: Ningbo Songhe Stationery Co., Ltd. Assignor: Shanghai Institute of Technology Contract fulfillment period: 2009.3.13 to 2015.3.12 contract change Contract record no.: 2009330000806 Denomination of invention: One-step preparation process of organic-montmorillonite modified ethylene-vinyl acetate hot-melt adhesive Granted publication date: 20071121 License type: Exclusive license Record date: 2009.4.29 |
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