CN102477273A - Preparation method of polyurethane hot melt adhesive - Google Patents
Preparation method of polyurethane hot melt adhesive Download PDFInfo
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- CN102477273A CN102477273A CN2010105672401A CN201010567240A CN102477273A CN 102477273 A CN102477273 A CN 102477273A CN 2010105672401 A CN2010105672401 A CN 2010105672401A CN 201010567240 A CN201010567240 A CN 201010567240A CN 102477273 A CN102477273 A CN 102477273A
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Abstract
The invention relates to a preparation method of a polyurethane hot melt adhesive. The preparation method comprises the following steps: 1, weighing 50-70 wt% of polyaryl polymethylene isocyanate, 20-30 wt% of a crystallized polymer polyol, 1-2 wt% of a blocking agent, 5-15 wt% of a tackifying resin and 5-10 wt% of a filler; 2, putting the weighed crystallized polymer polyol into a 100DEG C vacuum drying box, carrying out vacuum dehydration for 2h, and cooling to 50-60DEG C; and 3, adding the polyaryl polymethylene isocyanate during addition of the obtained product into a split type reaction vessel, buckling a reaction vessel cover, heating the reaction product with slowly stirring, and keeping the temperature at 95-100DEG C for 20-30min with stirring at a uniform speed until the reaction terminal point is reached. The adhesive has the advantages of excellent initial strength and final strength, low coating temperature and melting viscosity, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of sizing agent, belong to the sizing agent field, particularly a kind of preparation method of polyurethane thermosol.
Background technology
Thermosol is a kind ofly under melting condition, to be coated with, and produces the sizing agent of intensity through sclerosis or crystallization.The coating of thermosol does not need solvent, and the market demand of thermosol is in continuous increase.
For general purpose thermosol, it is normally thermoplastic, but an one of which subject matter is that its infiltration for water and solvent is also very responsive.In the curing thermosol, the most frequently used reaction is exactly the moisture curing of isocyanic ester.Use chainextender to have following drawback: lower fusion speed; Low initial strength: the open hour are longer: package stability is relatively poor; In 90-100 ℃ use temperature scope, the thermostability of sizing agent is relatively poor.Therefore, still there is certain drawback in the hard segment content that increases urethane by chainextender in wet solidified polyurethane thermosol.Wet solidified polyurethane thermosol by the preparation of this type material not only can harden by rapid crystallization, produce intensity just, and the internal cohesive energy of its cured product is also higher relatively, so the whole intensity after this thermosol completely solidified also is very high.Though some technology has successfully been prepared wet solidified polyurethane thermosol; But mostly the POLYMETHYLENE POLYPHENYLISOCYANATE raw material that it adopted is expensive diphenylmethanediisocyanate; And its use properties is uneven, shows that mainly just intensity is low, the open hour are short, the slow aspect of curing speed.
Summary of the invention
The technical problem that the present invention will solve is: the preparation method that a kind of new green environment protection sizing agent is provided; Its sizing agent of preparing has excellent first intensity and whole intensity; Lower coating temperature and melting viscosity, and the advantage of good thermotolerance and package stability.
In order to solve the problems of the technologies described above, the present invention provides a kind of preparation method of polyurethane thermosol, gets following composition at first by weight percentage:
Poly methylene poly phenyl poly isocyanate: 50-70%, crystalline polymer polyvalent alcohol: 20-30%, end-capping reagent: 1-2%, increase glutinous resin: 5-15%, filler: 5-10%, acid stabilizer: 0.001-0.01%, moisture curing catalysts diether: 0.02-0.1%
The vacuum drying oven that the crystalline polymer polyvalent alcohol of being got is put into 100 ℃ carries out 2 hours vacuum hydro-extraction, is cooled to 50～60 ℃ then, product is joined in the split type reaction kettle again, adds poly methylene poly phenyl poly isocyanate simultaneously; Subsequently, buckle the reaction kettle cover, reaction product is heated up; And slowly stir, when treating that temperature rises to 95-100 ℃, pick up counting, be incubated 20-30 minute; At the uniform velocity stir simultaneously, until reaching reaction end, then; Continue to be warming up to 100-110 ℃, add end-capping reagent, increase glutinous resin, filler, acid stabilizer and moisture curing catalysts, the back discharging that stirs gets final product.
Among the preparation method of described polyurethane thermosol, described poly methylene poly phenyl poly isocyanate accounts for 55%, the crystalline polymer polyvalent alcohol accounts for 25%, end-capping reagent accounts for 1%, increase that glutinous resin accounts for 5%, filler accounts for 5%, acid stabilizer accounts for 0.001%, moisture curing catalysts diether accounts for 0.02%.
Among the preparation method of described polyurethane thermosol, described poly methylene poly phenyl poly isocyanate accounts for 65%, the crystalline polymer polyvalent alcohol accounts for 28%, end-capping reagent accounts for 2%, increase that glutinous resin accounts for 15%, filler accounts for 10%, acid stabilizer accounts for 0.01%, moisture curing catalysts diether accounts for 0.1%.
Embodiment
Below, with embodiment the present invention is made more detailed description.These embodiment only are the descriptions to best mode for carrying out the invention, scope of the present invention are not had any restriction.
Embodiment 1
This embodiment is processed by following composition by weight percentage: poly methylene poly phenyl poly isocyanate: 50-70%, crystalline polymer polyvalent alcohol: 20-30%, end-capping reagent: 1-2%, increase glutinous resin: 5-15%, filler: 5-10%, acid stabilizer: 0-001-0.01%, moisture curing catalysts diether: 0.02-0.1%; Described crystalline polymer polyvalent alcohol is for gathering hexanodioic acid 1; 6-pinakon esterdiol, gather hexanodioic acid 1; 4-butanediol ester glycol, polyethylene glycol adipate glycol, polycaprolactone or gather 2; 3-dimethyl--2; 3-butyleneglycol (40～60 ℃ of Tcs, molecular weight 1500-3000): described end-capping reagent is organoalkoxysilane or vinyltrimethoxy silane; Described increase glutinous resin be not with isocyanic ester radical reaction, and hydrogenated rosin glyceride, terpine resin, t-butyl styrene or the terpenes-phenol copolymer resins that has good consistency with matrix resin; Described filler is precipitated silica, superfine silicon dioxide or the active carbon white that can not have a negative impact to the melt stability and the package stability of constituent; Described acid stabilizer is phosphoric acid or Benzoyl chloride 99min..
Embodiment 2
Compare with embodiment 1, this embodiment is processed by following composition by weight percentage: described poly methylene poly phenyl poly isocyanate accounts for 55%, the crystalline polymer polyvalent alcohol accounts for 25%, end-capping reagent accounts for 1%, increase that glutinous resin accounts for 5%, filler accounts for 5%, acid stabilizer accounts for 0.001%, moisture curing catalysts diether accounts for 0.02%.
Embodiment 3
Compare with embodiment 1; This embodiment is processed by following composition by weight percentage: among the preparation method of described polyurethane thermosol, described poly methylene poly phenyl poly isocyanate accounts for 65%, the crystalline polymer polyvalent alcohol accounts for 28%, end-capping reagent accounts for 2%, increase that glutinous resin accounts for 15%, filler accounts for 10%, acid stabilizer accounts for 0.01%, moisture curing catalysts diether accounts for 0.1%.
Claims (3)
1. the preparation method of a polyurethane thermosol is characterized in that:
Get following composition at first by weight percentage:
Poly methylene poly phenyl poly isocyanate: 50-70%, crystalline polymer polyvalent alcohol: 20-30%, end-capping reagent: 1-2%, increase glutinous resin: 5-15%, filler: 5-10%, acid stabilizer: 0.001-0.01%, moisture curing catalysts diether: 0.02-0.1%
The vacuum drying oven that the crystalline polymer polyvalent alcohol of being got is put into 100 ℃ carries out 2 hours vacuum hydro-extraction, is cooled to 50～60 ℃ then, product is joined in the split type reaction kettle again, adds poly methylene poly phenyl poly isocyanate simultaneously; Subsequently, buckle the reaction kettle cover, reaction product is heated up; And slowly stir, when treating that temperature rises to 95-100 ℃, pick up counting, be incubated 20-30 minute; At the uniform velocity stir simultaneously, until reaching reaction end, then; Continue to be warming up to 100-110 ℃, add end-capping reagent, increase glutinous resin, filler, acid stabilizer and moisture curing catalysts, the back discharging that stirs gets final product.
2. the preparation method of polyurethane thermosol according to claim 1 is characterized in that described poly methylene poly phenyl poly isocyanate accounts for 55%, the crystalline polymer polyvalent alcohol accounts for 25%, end-capping reagent accounts for 1%, increase that glutinous resin accounts for 5%, filler accounts for 5%, acid stabilizer accounts for 0.001%, moisture curing catalysts diether accounts for 0.02%.
3. the preparation method of polyurethane thermosol according to claim 1 is characterized in that described poly methylene poly phenyl poly isocyanate accounts for 65%, the crystalline polymer polyvalent alcohol accounts for 28%, end-capping reagent accounts for 2%, increase that glutinous resin accounts for 15%, filler accounts for 10%, acid stabilizer accounts for 0.01%, moisture curing catalysts diether accounts for 0.1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105672401A CN102477273A (en) | 2010-11-26 | 2010-11-26 | Preparation method of polyurethane hot melt adhesive |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105672401A CN102477273A (en) | 2010-11-26 | 2010-11-26 | Preparation method of polyurethane hot melt adhesive |
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| CN102477273A true CN102477273A (en) | 2012-05-30 |
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| CN2010105672401A Pending CN102477273A (en) | 2010-11-26 | 2010-11-26 | Preparation method of polyurethane hot melt adhesive |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660217A (en) * | 2012-06-08 | 2012-09-12 | 舒跃辉 | Polyurethane moisture-curing hot melt coating glue, as well as preparation method and application thereof |
| CN109321191A (en) * | 2018-08-22 | 2019-02-12 | 上海天洋热熔粘接材料股份有限公司 | A kind of preparation method of moisture-curable polyurethane hot melt adhesive |
| US10800957B2 (en) | 2015-12-23 | 2020-10-13 | Sika Technology Ag | Polyurethane hot melt adhesive based on polyacrylates with high heat resistance |
| CN112375533A (en) * | 2020-11-27 | 2021-02-19 | 帅山 | Pressure-maintaining-free reactive polyurethane hot melt adhesive and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06234184A (en) * | 1993-02-09 | 1994-08-23 | Toyo Seikan Kaisha Ltd | Flexible packaging laminate, method for production thereof and adhesive agent for use in the method |
| CN1236382A (en) * | 1996-11-08 | 1999-11-24 | 美国3M公司 | Moisture-curable, hot-melt composition |
| CN1752169A (en) * | 2005-09-28 | 2006-03-29 | 东北林业大学 | Wet solidified polyurethane thermosol and preparing process thereof |
-
2010
- 2010-11-26 CN CN2010105672401A patent/CN102477273A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06234184A (en) * | 1993-02-09 | 1994-08-23 | Toyo Seikan Kaisha Ltd | Flexible packaging laminate, method for production thereof and adhesive agent for use in the method |
| CN1236382A (en) * | 1996-11-08 | 1999-11-24 | 美国3M公司 | Moisture-curable, hot-melt composition |
| CN1752169A (en) * | 2005-09-28 | 2006-03-29 | 东北林业大学 | Wet solidified polyurethane thermosol and preparing process thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660217A (en) * | 2012-06-08 | 2012-09-12 | 舒跃辉 | Polyurethane moisture-curing hot melt coating glue, as well as preparation method and application thereof |
| US10800957B2 (en) | 2015-12-23 | 2020-10-13 | Sika Technology Ag | Polyurethane hot melt adhesive based on polyacrylates with high heat resistance |
| CN109321191A (en) * | 2018-08-22 | 2019-02-12 | 上海天洋热熔粘接材料股份有限公司 | A kind of preparation method of moisture-curable polyurethane hot melt adhesive |
| CN112375533A (en) * | 2020-11-27 | 2021-02-19 | 帅山 | Pressure-maintaining-free reactive polyurethane hot melt adhesive and preparation method thereof |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120530 |