CN101724373A - Preparation method of hot-melt reaction type adhesive for composite material - Google Patents
Preparation method of hot-melt reaction type adhesive for composite material Download PDFInfo
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- CN101724373A CN101724373A CN200910237969A CN200910237969A CN101724373A CN 101724373 A CN101724373 A CN 101724373A CN 200910237969 A CN200910237969 A CN 200910237969A CN 200910237969 A CN200910237969 A CN 200910237969A CN 101724373 A CN101724373 A CN 101724373A
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Abstract
The invention discloses a preparation method of a hot-melt reaction type adhesive for a composite material, belonging to the field of adhesive preparation. The method comprises the following steps of: preparing polyester polyol: esterifying and poly-condensing dimethyl terephthalate, glycol, hexane diacid, decanedioic acid and 1,4-butanediol under a certain condition to obtain polyester polyol; and mixing the prepared polyester polyol and polyether glycol, heating and formulating the prepared polyester polyol and polyether glycol by using MDI (diphenyl-methane-diisocyanate), tackifying resin and organosilicon coupling agent in proportion to obtain the hot-melt reaction type adhesive. Through the structural design of polyester segmer and the introduction of a polyether glycol segmer unit, the produced adhesive has very high combined strength and wide technical applicability for various composite base materials; and various composite materials can be produced through the adhesive. The composite materials made of the adhesive have excellent weather-resistant performance and excellent outdoor applicability.
Description
Technical field
The present invention relates to the preparation field of tackiness agent, particularly relate to a kind of preparation method of hot-melt reaction type adhesive for composite material.
Background technology
At present, the material of different two kinds of character is combined with each other, makes it to become a kind of have special performance and the cheap advanced composite material of cost value, be commonly referred to as the hot-melt reaction type matrix material by using tackiness agent.In such matrix material, inner layer material is mainly from Wood fiber composite material, PVC extruded material and aluminum alloy materials, compound plastic basis material scope is then quite extensive with it, mainly be the Plastic Resin film, as all thickness, versicolor composite polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC) etc.Advantages such as such composite material has environmental protection, processing characteristics is excellent and with low cost.This class matrix material is mainly used in building and decoration industry: as composite door and window, composite floor board, compound furred ceiling and the aspects such as decoration buckle and finishing material of house ornamentation.Composite wood is just the same with the wood products outward appearance behind fitting operation, available nail or bolting, and sawing, and be easy to paint and dyeing, and possess inaccessiable mechanics of solid wood products and anti-marquis, and water-fast, heat resistance.
Above-mentioned performance of composites is by the bonding realization of tackiness agent, and coating method is mainly the form of blade coating or showering.Adhesive for composite material is mainly based on Solvent Adhesive at present, and system is based on urethane, polyester, acrylic resin etc.Have problems in the adhesive for composite material at present, it mainly is the material environment friendly poor performance, and in the process of operation, need the mixing cooperation of two kinds of components just can carry out bonding, cause the hot-melt reaction type adhesive for composite material operating environment bad, various in style, increased unnecessary difficulty for the operation time spent.
Summary of the invention
Based on above-mentioned existing in prior technology problem, the embodiment of the invention provides a kind of preparation method of hot-melt reaction type adhesive for composite material, and purpose provides the tackiness agent that is used for matrix material of a kind of environmental protection, alternative Solvent Adhesive easy to use.
The present invention is achieved by the following technical solutions:
The embodiment of the invention provides a kind of preparation method of hot-melt reaction type adhesive for composite material, comprising:
Preparation polyester polyols ester:
A, esterification:
With 1 of the sebacic acid of the hexanodioic acid of the ethylene glycol of the dimethyl terephthalate (DMT) of 10～20 mass parts, 25～35 mass parts, 15～30 mass parts, 5～10 mass parts, 25～35 mass parts, 4 butyleneglycols join in the polyester synthesis reactor, be warming up to 210～240 ℃, reacted 6～8 hours, esterification is finished;
B, polycondensation:
Long vacuumizing in the polyester synthesis reactor that esterification is finished, the long vacuum tightness that vacuumizes reaches-0.095Mpa, and the long pumpdown time is 2～4 hours; Length vacuumizes aftercondensated and finishes, and the polycondensation product that obtains is a polyester polyol;
Composite:
The polyester polyol that makes in the above-mentioned preparation polyester polyols ester step with 30～40 mass parts, the polyether glycol of 30～40 mass parts, after the organo-silicon coupling agent of the tackifying resin of the diphenylmethanediisocyanate of 5～15 mass parts, 5～10 mass parts, 0.5～1 mass parts mixes, under 100 ℃ environment, mixed 4～8 hours, make promptly that to contain admittedly be that viscosity is the hot-melt reaction type adhesive for composite material of 10000～30000mPas under 100%, 120 ℃ of temperature condition.
The technical scheme that provides by the invention described above embodiment as can be seen, pass through in the embodiment of the invention polyester segment structure design and the unitary introducing of polyether glycol segment, and, the equal nontoxicity of urethane raw of reaction and chain extension effect in the raw material that uses, virose diphenylmethanediisocyanate (MDI) with other raw material reactions after after, become nontoxic, nonirritant, therefore, make the tackiness agent that makes in use can not distribute poison gas, has environmental-protecting performance completely, high compound fastness, good operational stability and to the broad applicability of various composite base materials can prepare various environment friendly composite materials by this tackiness agent.The hot-melt reaction type composite prod weather resistance excellence that this tackiness agent is made has good suitability.
Embodiment
For ease of understanding, the invention will be further described below in conjunction with specific embodiment.
Embodiment one
This embodiment one provides a kind of preparation method of hot-melt reaction type adhesive for composite material, and just viscosity fastness is big for the tackiness agent that makes, and stable performance is applicable to that various composite base materials prepare environment friendly composite material, and this preparation method specifically comprises:
The preparation polyester polyol:
A, esterification:
With 1 of the sebacic acid of the hexanodioic acid of the ethylene glycol of the dimethyl terephthalate (DMT) of 10～20 mass parts, 25～35 mass parts, 15～30 mass parts, 5～10 mass parts, 25～35 mass parts, 4 butyleneglycols join in the polyester synthesis reactor, be warming up to 210～240 ℃, reacted 6～8 hours, esterification is finished;
In above-mentioned esterif iotacation step, the quantity of distillate that keeps the overhead product of polyester synthesis reactor be 1～3 mass parts/hour; After treating that esterification finishes, sampling detecting acid number confirms whether esterification is qualified, if the acid number≤25mgKOH/g of sampling confirms that then esterification is qualified.
B, polycondensation:
Long vacuumizing in the polyester synthesis reactor that esterification is finished, the long vacuum tightness that vacuumizes reaches-0.095Mpa, and the long pumpdown time is 2～4 hours; Length vacuumizes aftercondensated and finishes, and the polycondensation product that obtains is a polyester polyol;
In above-mentioned polycondensation steps, after long vacuumizing, feeding nitrogen in the polyester synthesis reactor takes a sample to 0.02Mpa, and confirm by viscosity, hydroxyl value and the acid number of test sampling whether the polyester polyol that makes is qualified, if the acid number of test sampling is that 3～5mgKOH/g, the viscosity under 60 ℃ of temperature condition are 20000～50000mPas, then confirm to make qualified polyester polyol.
Composite:
The polyester polyol that makes in the above-mentioned preparation polyester polyol step with 30～40 mass parts, the polyether glycol of 30～40 mass parts, after the tackifying resin of the diphenylmethanediisocyanate of 5～15 mass parts (MDI), 5～10 mass parts, the organo-silicon coupling agent of 0.5～1 mass parts mix, under 100 ℃ environment, mixed 4～8 hours, make promptly that to contain admittedly be that viscosity is the hot-melt reaction type adhesive for composite material of 10000～30000mPas under 100%, 120 ℃ of temperature condition.
Used polyether glycol comprises in above-mentioned preparation method's the composite step: any of polyoxypropyleneglycol, polytetrahydrofuran diol, tetrahydrofuran (THF)-propylene oxide copolymerization glycol.
Used tackifying resin comprises in above-mentioned preparation method's the composite step: any in terpine resin, terpenes-resol, aromatic modified terpine resin, the Gum Rosin.
Used organo-silicon coupling agent comprises in above-mentioned preparation method's the composite step: any in γ-An Bingjisanyiyangjiguiwan, γ-An Bingjisanjiayangjiguiwan, the γ-sulfydryl triethoxyl silane.
Pass through in the embodiment of the invention polyester segment structure design and the unitary introducing of polyether glycol segment, and, the equal nontoxicity of urethane raw of reaction and chain extension effect in the raw material that uses, virose diphenylmethanediisocyanate (MDI) with other raw material reactions after after, become nontoxic, nonirritant, therefore, make the tackiness agent that makes in use can not distribute poison gas, has environmental-protecting performance completely, high compound fastness, good operational stability and to the broad applicability of various composite base materials can prepare various environment friendly composite materials by this tackiness agent.The hot-melt reaction type composite prod weather resistance excellence that this tackiness agent is made has good suitability.
Embodiment two
Present embodiment two provides a kind of preparation method of hot-melt reaction type adhesive for composite material, and just viscosity fastness is big for the tackiness agent that makes, and stable performance is applicable to that various composite base materials prepare the hot-melt reaction type environment-friendly composite material, and this preparation method specifically comprises:
(1) preparation polyester polyol:
Get each raw material by following proportioning:
Proportioning raw materials (mass parts)
Dimethyl terephthalate (DMT) 15
Ethylene glycol 25
Hexanodioic acid 26
Sebacic acid 6
1,4 butyleneglycol 28
The preparation method of polyester polyol:
A, an esterification:
The dimethyl terephthalate (DMT) of 15 mass parts, the ethylene glycol of 25 mass parts, the hexanodioic acid of 6 mass parts, the sebacic acid of 6 mass parts, 1,4 butyleneglycol of 28 mass parts are all joined in the polyester synthesis reactor, be warming up to 220 ℃, reacted 8 hours, finish esterification; In the esterification process, note to observe the overhead product situation of polyester synthesis reactor, keep the quantity of distillate of overhead product be stabilized in 2～3 mass parts/hour, treat that esterification finishes, the measurement acid number be 22mgKOH/g (≤25mgKOH/g), can confirm that then esterification is qualified;
C, polycondensation:
Polyester synthesis reactor after above-mentioned esterification finished is grown and is taken out, and the vacuum tightness of vacuum will reach-0.095Mpa, and the long pumpdown time is 4 hours, and the overhead product of polyester synthesis reactor is about 15 mass parts; After long the vacuumizing, promptly make polyester polyol;
After long vacuumizing, in the polyester synthesis reactor, feed nitrogen and to 0.02Mpa, take a sample, test sampling viscosity and acid number, the viscosity that records sampling is 30000mPas (under 60 ℃ of temperature), acid number is 3mgKOH/g, confirms that then the polyester polyol that makes is qualified;
(2) composite:
Get each raw material by following proportioning:
Proportioning raw materials (mass parts)
The polyester polyol 38 of above-mentioned steps (1) preparation
Polyoxypropyleneglycol 30
Diphenylmethanediisocyanate (MDI) 10
Gum Rosin 8
γ-sulfydryl triethoxyl silane (KH560) 1
The preparation method:
With after γ-sulfydryl triethoxyl silane (KH560) mixes of the Gum Rosin of the diphenylmethanediisocyanate (MDI) of the polyoxypropyleneglycol of the polyester polyol of the above-mentioned steps (1) of 38 mass parts preparation and 38 mass parts, 15 mass parts, 6 mass parts, 1 mass parts, under 90 ℃ situation, react 6h, make tackiness agent.Testing that it contains admittedly is 100%, and viscosity is 16000mPas (under 120 ℃ of temperature).
Embodiment three
This embodiment two provides a kind of preparation method of hot-melt reaction type adhesive for composite material, and just viscosity fastness is big for the tackiness agent that makes, and stable performance is applicable to that various composite base materials prepare the hot-melt reaction type environment-friendly composite material, and this preparation method specifically comprises:
(1) preparation polyester polyol:
Get each raw material by following quality proportioning:
Proportioning raw materials (mass parts)
Dimethyl terephthalate (DMT) 20
Ethylene glycol 30
Hexanodioic acid 15
Sebacic acid 10
1,4 butyleneglycol 25
It is basic identical to prepare the method for polyester polyol and the method for preparing polyester polyol that embodiment two provides in the present embodiment, can be referring to embodiment two, in this no longer repeat specification.
(2) composite:
Get each raw material by following proportioning:
Proportioning raw materials (quality proportioning)
The polyester polyol 30 that above-mentioned steps (1) makes
Polytetrahydrofuran diol 40
Diphenylmethanediisocyanate (MDI) 5
Aromatic modified terpine resin 10
γ-An Bingjisanyiyangjiguiwan (KH550) 0.7
The preparation method:
After the γ-An Bingjisanyiyangjiguiwan (KH550) of the aromatic modified terpine resin of the diphenylmethanediisocyanate (MDI) of the polytetrahydrofuran diol of the polyester polyol of the above-mentioned steps (1) of 35 mass parts preparation and 40 mass parts, 15 mass parts, 10 mass parts, 1 mass parts mixed, reaction is 6 hours under 100 ℃ situation, make tackiness agent, it is 100% that test makes that consolidating of tackiness agent contain, and viscosity is 25000mPas (under 120 ℃ of temperature).
Embodiment four
This embodiment two provides a kind of preparation method of hot-melt reaction type adhesive for composite material, and just viscosity fastness is big for the tackiness agent that makes, and stable performance is applicable to that various composite base materials prepare the hot-melt reaction type environment-friendly composite material, and this preparation method specifically comprises:
(1) preparation polyester polyol:
Get each raw material by following quality proportioning:
Proportioning raw materials (mass parts)
Dimethyl terephthalate (DMT) 10
Ethylene glycol 35
Hexanodioic acid 30
Sebacic acid 5
1,4 butyleneglycol 35
It is basic identical to prepare the method for preparing polyester polyol that provides among the method for polyester polyol and the embodiment two in the present embodiment, can be referring to embodiment two, in this no longer repeat specification.
(2) composite:
Proportioning raw materials (mass parts)
The polyester polyol 40 that above-mentioned steps (1) makes
Polyoxypropyleneglycol 35
Diphenylmethanediisocyanate (MDI) 15
Terpenes-resol 5
γ-An Bingjisanjiayangjiguiwan (KH551) 0.5
Preparation method:
After the γ-An Bingjisanjiayangjiguiwan (KH551) of the terpenes-resol of the diphenylmethanediisocyanate (MDI) of the polyether glycol of the polyester polyol of the above-mentioned steps (1) of 40 mass parts preparation and 35 mass parts, 15 mass parts, 6 mass parts, 0.5 mass parts mixed, after reacting 8 hours under 105 ℃ the situation, make tackiness agent, it is 100% that test makes that consolidating of tackiness agent contain, and viscosity is 20000mPas (under 120 ℃ of temperature).
In sum, the preparation method of the embodiment of the invention, by better simply technology, to polyester segment structure design and the unitary introducing of polyether glycol segment, and the equal nontoxicity of urethane raw of reaction and chain extension effect in the material therefor, virose diphenylmethanediisocyanate (MDI) with other raw material reactions after after, become nontoxic, nonirritant, therefore, make the tackiness agent that makes in use can not distribute poison gas, and have high compound fastness and the broad applicability of various polarity composite base materials.When utilizing this tackiness agent to prepare the hot-melt reaction type matrix material, after applying glue, the composition operation environmental friendliness, the hot-melt reaction type matrix material weather resisteant that utilizes tackiness agent to make can be excellent, has good outdoor suitability.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. the preparation method of a hot-melt reaction type adhesive for composite material is characterized in that, comprising:
Preparation polyester polyols ester:
A, esterification:
With 1 of the sebacic acid of the hexanodioic acid of the ethylene glycol of the dimethyl terephthalate (DMT) of 10～20 mass parts, 25～35 mass parts, 15～30 mass parts, 5～10 mass parts, 25～35 mass parts, 4 butyleneglycols join in the polyester synthesis reactor, be warming up to 210～240 ℃, reacted 6～8 hours, esterification is finished;
B, polycondensation:
Long vacuumizing in the polyester synthesis reactor that esterification is finished, the long vacuum tightness that vacuumizes reaches-0.095Mpa, and the long pumpdown time is 2～4 hours; Length vacuumizes aftercondensated and finishes, and the polycondensation product that obtains is a polyester polyol;
Composite:
The polyester polyol that makes in the above-mentioned preparation polyester polyols ester step with 30～40 mass parts, the polyether glycol of 30～40 mass parts, after the organo-silicon coupling agent of the tackifying resin of the diphenylmethanediisocyanate of 5～15 mass parts, 5～10 mass parts, 0.5～1 mass parts mixes, under 90 ℃～105 ℃ environment, mixed 4～8 hours, make promptly that to contain admittedly be that viscosity is the hot-melt reaction type adhesive for composite material of 10000～30000mPas under 100%, 120 ℃ of temperature condition.
2. the preparation method of hot-melt reaction type adhesive for composite material as claimed in claim 1 is characterized in that, in the esterif iotacation step of described preparation polyester polyol, the quantity of distillate that keeps the overhead product of polyester synthesis reactor be 1～3 mass parts/hour; After treating that esterification finishes, sampling detecting acid number confirms whether esterification is qualified, if the acid number≤25mgKOH/g of sampling confirms that then esterification is qualified.
3. the preparation method of hot-melt reaction type adhesive for composite material as claimed in claim 1, it is characterized in that, in the polycondensation steps of described preparation polyester polyols ester, after long vacuumizing, feeding nitrogen in the polyester synthesis reactor takes a sample to 0.02Mpa, and confirm by viscosity, hydroxyl value and the acid number of test sampling whether the polyester polyol that makes is qualified, if the acid number of test sampling is that 3～5mgKOH/g, the viscosity under 60 ℃ of temperature condition are 20000～50000mPas, then confirm to make qualified polyester polyol.
4. the preparation method of hot-melt reaction type adhesive for composite material as claimed in claim 1 is characterized in that, used polyether glycol comprises in the described composite step:
Any of polyoxypropyleneglycol, polytetrahydrofuran diol, tetrahydrofuran (THF)-propylene oxide copolymerization glycol.
5. the preparation method of hot-melt reaction type adhesive for composite material as claimed in claim 1 is characterized in that, used tackifying resin comprises in the described composite step:
In terpine resin, terpenes-resol, aromatic modified terpine resin, the Gum Rosin any.
6. the preparation method of hot-melt reaction type adhesive for composite material as claimed in claim 1 is characterized in that, used organo-silicon coupling agent comprises in the described composite step:
In γ-An Bingjisanyiyangjiguiwan, γ-An Bingjisanjiayangjiguiwan, the γ-sulfydryl triethoxyl silane any.
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Cited By (7)
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| CN102010687A (en) * | 2010-10-28 | 2011-04-13 | 华南理工大学 | Fast curing reaction type hot melt adhesive and preparation method thereof |
| CN102766430A (en) * | 2012-08-03 | 2012-11-07 | 北京高盟新材料股份有限公司 | Adhesive of hot melting coating for laminated steel process and preparation method thereof |
| CN103437194A (en) * | 2013-08-16 | 2013-12-11 | 东莞市雄林新材料科技有限公司 | Sewing-free hot melt adhesive TPU leather and preparation method thereof |
| CN104531038A (en) * | 2014-12-24 | 2015-04-22 | 广州市白云化工实业有限公司 | Reaction type polyurethane hot-melt adhesive and preparation method thereof |
| CN106566459A (en) * | 2016-10-26 | 2017-04-19 | 江苏宏腾运动场地新材料有限公司 | Adhesive free from free toluene diisocynate, and preparation method thereof |
| CN109440483A (en) * | 2018-09-11 | 2019-03-08 | 东莞市雄林新材料科技股份有限公司 | A kind of high scratch resistance mirror surface super fiber leather and preparation method thereof |
| CN114437361A (en) * | 2021-12-24 | 2022-05-06 | 中国科学院福建物质结构研究所 | Inorganic-organic hybrid material, preparation method thereof and application of modified polyurethane prepared from inorganic-organic hybrid material as adhesive |
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| CN1229827A (en) * | 1998-03-23 | 1999-09-29 | 庄建元 | Compsn. of reacting polyurethane thermosol |
| CN1322085C (en) * | 2005-09-21 | 2007-06-20 | 北京高盟化工有限公司 | Single-copmonent no-solvent polyurethane adhesive for low temperature painting and its prepn process |
| CN101353562B (en) * | 2007-07-25 | 2012-01-25 | 比亚迪股份有限公司 | Preparation of polyester hot-melt adhesive |
| CN101245230A (en) * | 2008-02-21 | 2008-08-20 | 上海天洋热熔胶有限公司 | Method for manufacturing linear copolyester hot melt adhesive |
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- 2009-11-19 CN CN200910237969XA patent/CN101724373B/en not_active Expired - Fee Related
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| CN102010687A (en) * | 2010-10-28 | 2011-04-13 | 华南理工大学 | Fast curing reaction type hot melt adhesive and preparation method thereof |
| CN102010687B (en) * | 2010-10-28 | 2013-04-17 | 华南理工大学 | Fast curing reaction type hot melt adhesive and preparation method thereof |
| CN102766430A (en) * | 2012-08-03 | 2012-11-07 | 北京高盟新材料股份有限公司 | Adhesive of hot melting coating for laminated steel process and preparation method thereof |
| CN102766430B (en) * | 2012-08-03 | 2015-10-28 | 北京高盟新材料股份有限公司 | Multiple film iron process hot melt coating tackiness agent and preparation method thereof |
| CN103437194A (en) * | 2013-08-16 | 2013-12-11 | 东莞市雄林新材料科技有限公司 | Sewing-free hot melt adhesive TPU leather and preparation method thereof |
| CN103437194B (en) * | 2013-08-16 | 2015-04-08 | 东莞市雄林新材料科技股份有限公司 | Sewing-free hot melt adhesive TPU leather and preparation method thereof |
| CN104531038A (en) * | 2014-12-24 | 2015-04-22 | 广州市白云化工实业有限公司 | Reaction type polyurethane hot-melt adhesive and preparation method thereof |
| CN104531038B (en) * | 2014-12-24 | 2016-11-23 | 广州市白云化工实业有限公司 | Reaction type polyurethane hot-melt adhesive and preparation method thereof |
| CN106566459A (en) * | 2016-10-26 | 2017-04-19 | 江苏宏腾运动场地新材料有限公司 | Adhesive free from free toluene diisocynate, and preparation method thereof |
| CN109440483A (en) * | 2018-09-11 | 2019-03-08 | 东莞市雄林新材料科技股份有限公司 | A kind of high scratch resistance mirror surface super fiber leather and preparation method thereof |
| CN114437361A (en) * | 2021-12-24 | 2022-05-06 | 中国科学院福建物质结构研究所 | Inorganic-organic hybrid material, preparation method thereof and application of modified polyurethane prepared from inorganic-organic hybrid material as adhesive |
| CN114437361B (en) * | 2021-12-24 | 2022-12-06 | 中国科学院福建物质结构研究所 | Inorganic-organic hybrid material, preparation method thereof and application of modified polyurethane prepared from inorganic-organic hybrid material as adhesive |
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| CN101724373B (en) | 2012-07-04 |
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