CN112745660A - Polyol modified toughening pre-dispersed master batch and preparation method thereof - Google Patents
Polyol modified toughening pre-dispersed master batch and preparation method thereof Download PDFInfo
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- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 60
- 229920005862 polyol Polymers 0.000 title claims abstract description 20
- 150000003077 polyols Chemical class 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 32
- 229920002635 polyurethane Polymers 0.000 claims abstract description 37
- 239000004814 polyurethane Substances 0.000 claims abstract description 37
- 239000012745 toughening agent Substances 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000000945 filler Substances 0.000 claims abstract description 31
- 239000004970 Chain extender Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 37
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 33
- 239000002202 Polyethylene glycol Substances 0.000 claims description 32
- 239000003054 catalyst Substances 0.000 claims description 32
- 229920001223 polyethylene glycol Polymers 0.000 claims description 32
- 239000000839 emulsion Substances 0.000 claims description 26
- 229920001228 polyisocyanate Polymers 0.000 claims description 24
- 239000005056 polyisocyanate Substances 0.000 claims description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Natural products CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 20
- 229920005749 polyurethane resin Polymers 0.000 claims description 20
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical group CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 claims description 18
- 238000007789 sealing Methods 0.000 claims description 12
- -1 morpholinyl diethyl ether Chemical compound 0.000 claims description 11
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 10
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 10
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 10
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 claims description 10
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- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
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- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 6
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
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- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 3
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
The invention relates to the technical field of modified pre-dispersed master batches, in particular to a polyol modified toughening pre-dispersed master batch and a preparation method thereof. The feed comprises the following raw materials: the toughening mother material modified by polyol prepared by the invention adopts the chain extender to be gradually added into the polyurethane solution, the reaction is stable, the hard chain segment and the hard chain segment as well as the soft chain segment and the soft chain segment are easy to form ordered arrangement, the macromolecules have larger interaction and better microphase separation degree and are used for improving the mechanical property and the process property of a polyurethane product, the toughening agent contains an active group and can chemically react with the polyurethane, the thermal deformation temperature is not changed or slightly reduced, the strength, the toughness, the brittleness and the impact resistance are obviously improved, and the addition of the filler has the main function of improving the strong tensile property and the impact strength of the plastic besides reducing the cost.
Description
Technical Field
The invention relates to the technical field of modified pre-dispersed master batches, in particular to a polyol modified toughening pre-dispersed master batch and a preparation method thereof.
Background
The polyurethane mainly has a thermoplastic linear structure, and has better stability, chemical resistance, rebound resilience and mechanical property and smaller compression deformability than a PVC foaming material. The polyurethane elastomer has the advantages of excellent heat insulation, sound insulation, shock resistance and gas defense properties, so that the polyurethane elastomer is used as a packaging, sound insulation and filtering material, is light in weight, excellent in sound insulation and heat insulation properties, chemical resistant, good in electrical property, easy to process and low in water absorption rate, is mainly used for building, automobile and aviation industries and heat insulation structural materials, has the properties of the polyurethane elastomer between plastic and rubber, is oil-resistant, wear-resistant, low-temperature resistant, ageing-resistant, high in hardness and elastic, is mainly used for the shoe manufacturing industry and the medical industry, and can be used for preparing adhesives, coatings, synthetic leather and the like;
the existing polyurethane resin predispersed master batch has insufficient flexibility and poor mechanical properties such as impact strength, tensile strength and the like, so that the processing performance of the master batch is influenced, and the application range is greatly reduced.
Disclosure of Invention
The invention aims to provide a toughening pre-dispersed master batch modified by polyol and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the above object, in one aspect, the present invention provides a polyol-modified toughening predispersion master batch, which comprises the following raw materials: 70-100 parts of polyurethane prepolymer, 7-15 parts of chain extender, 10-20 parts of flexibilizer and 20-30 parts of filler.
As a further improvement of the technical scheme, the polyurethane prepolymer is prepared by the prepolymerization reaction of 30-40 parts of polyethylene glycol, 40-60 parts of polyisocyanate and 1-5 parts of catalyst;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction;
the pre-polymerization reaction of the polyurethane prepolymer comprises the following steps:
s1.1, placing polyethylene glycol in a reactor, heating, vacuumizing, dehydrating, cooling, and sealing for later use;
s1.2, adding polyisocyanate into the polyethylene glycol solution, adding a catalyst, and uniformly stirring;
and S1.3, heating, reacting at constant temperature for timing to obtain a polyurethane prepolymer, and sealing and storing.
As a further improvement of the technical scheme, in the S1.1, the internal temperature of the reactor is 100-.
As a further improvement of the technical scheme, in the S1.3, the temperature is increased for 0.5 to 1 hour, the temperature is 80 to 90 ℃, and the constant-temperature reaction time is 1.5 to 2 hours.
As a further improvement of the technical scheme, the chain extender is at least one of 1, 4-butanediol, 1, 6-hexanediol, dimethylolbutyric acid and trimethylolpropane, in the polyester processing technology, the molecular weight is reduced and the number of terminal carboxyl groups is increased due to the reduction of molecular weight caused by thermal degradation and hydrolysis, so that the mechanical and chemical properties of the polymer are reduced, and the chain extender is a substance which can react with functional groups on a linear polymer chain to expand the molecular chain and increase the molecular weight and is used for improving the mechanical property and the technological property of a polyurethane product.
As a further improvement of the technical scheme, the toughening agent is at least one of polyvinyl butyral, polyvinyl acetate and chlorinated polyethylene, and the toughening agent is a substance capable of increasing the flexibility of an adhesive film layer, so that the effect of increasing the strength, toughness, brittleness and impact resistance of the polyurethane resin is achieved.
As a further improvement of the technical scheme, the filler is at least one of calcium carbonate, titanium dioxide, carbon black, kaolin, diatomite, wood powder, clay, silica and talcum powder, and in order to reduce the cost of the polyurethane resin product, the bulk strength, the adhesive strength and the heat resistance of the polyurethane resin product are improved, or the expansion and shrinkage rates or other functions of a cured product are improved.
On the other hand, the invention provides a preparation method of the polyol modified toughening pre-dispersion master batch, which comprises the polyol modified toughening pre-dispersion master batch, and comprises the following operation steps:
s2.1, cooling the polyurethane prepolymer solution, gradually adding a chain extender, and stirring;
s2.2, heating, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction;
s2.3, cooling again, adding a neutralizing agent, and adding water for emulsification to prepare an aqueous polyurethane emulsion;
s2.4, heating and melting the toughening agent, and taking out for later use after the toughening agent reaches a flowing state;
s2.5, adding the filler into a dryer, removing surface moisture, and taking out for later use;
s2.6, adding a toughening agent and a filler into the polyurethane emulsion, and uniformly stirring;
and S2.7, vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
Preferably, the temperature in S2.1 is reduced to 50-70 ℃ and the temperature in S2.2 is increased to 80-100 ℃.
Preferably, the temperature in the S2.3 is reduced to 30-50 ℃, the neutralizer is dibutylamine, and the emulsifying time is 0.5-1 h.
Compared with the prior art, the invention has the beneficial effects that:
1. in the polyol modified toughening pre-dispersion master batch and the preparation method thereof, a chain extender is gradually added into a polyurethane solution, the reaction is stable, the hard chain segments and the soft chain segments are easily arranged in a relatively ordered way, and macromolecules have relatively large interaction and relatively good microphase separation degree and are used for improving the mechanical property and the process property of a polyurethane product.
2. In the polyol modified toughening pre-dispersed master batch and the preparation method thereof, the toughening agent contains active groups, can chemically react with polyurethane, is not completely compatible after curing, sometimes needs phase splitting, can obtain ideal toughening effect, enables the thermal deformation temperature not to be changed or to be slightly reduced, and obviously improves the strength, toughness, brittleness and impact resistance.
3. In the toughening pre-dispersion master batch modified by the polyol and the preparation method thereof, the filler is added, so that the temperature dependence of the density, hardness, elastic modulus and mechanical property of the thermoplastic plastic is changed, and the toughening pre-dispersion master batch mainly has the effect of improving the tensile property and impact strength of the plastic besides reducing the cost.
Drawings
FIG. 1 is an overall flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1 a method for preparing a polyol-modified toughening predispersion master batch, comprising:
preparation of polyurethane prepolymer
Placing 40 parts of polyethylene glycol in a reactor, heating to 120 ℃ at 100-; adding 40 parts of polyisocyanate into the polyethylene glycol solution, adding 1 part of catalyst, and uniformly stirring; heating for 0.5-1h at 80-90 deg.C, maintaining the temperature for 1.5-2h to obtain polyurethane prepolymer, and sealing for storage;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction.
Preparation of polyurethane emulsion
Cooling 80 parts of solution of polyurethane prepolymer to 50-70 ℃, gradually adding 7 parts of chain extender, and stirring; heating to 80-100 ℃, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction; and cooling, adding dibutylamine for neutralization, and adding water for emulsification for 0.5-1h to obtain the waterborne polyurethane emulsion.
Preparation of modified predispersed masterbatch
Heating and melting 20 parts of toughening agent, and taking out for later use after the toughening agent reaches a flowing state; adding 30 parts of filler into a dryer, removing surface moisture, and taking out for later use; adding a toughening agent and a filler into the polyurethane emulsion, and uniformly stirring; vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
Embodiment 2 a method for preparing a polyol-modified toughening predispersion master batch, comprising:
preparation of polyurethane prepolymer
Placing 37.5 parts of polyethylene glycol in a reactor, heating to 120 ℃ at 100-; adding 45 parts of polyisocyanate into the polyethylene glycol solution, adding 2 parts of catalyst, and uniformly stirring; heating for 0.5-1h at 80-90 deg.C, maintaining the temperature for 1.5-2h to obtain polyurethane prepolymer, and sealing for storage;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction.
Preparation of polyurethane emulsion
Cooling 82.5 parts of solution of polyurethane prepolymer to 50-70 ℃, gradually adding 9 parts of chain extender, and stirring; heating to 80-100 ℃, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction; and cooling, adding dibutylamine for neutralization, and adding water for emulsification for 0.5-1h to obtain the waterborne polyurethane emulsion.
Preparation of modified predispersed masterbatch
Heating and melting 17.5 parts of toughening agent, and taking out for later use after the toughening agent reaches a flowing state; adding 27.5 parts of filler into a dryer, removing surface moisture, and taking out for later use; adding a toughening agent and a filler into the polyurethane emulsion, and uniformly stirring; vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
Embodiment 3 a method of preparing a polyol-modified toughening predispersion masterbatch, comprising:
preparation of polyurethane prepolymer
Placing 35 parts of polyethylene glycol in a reactor, heating to 120 ℃ at 100-; adding 50 parts of polyisocyanate into the polyethylene glycol solution, adding 3 parts of catalyst, and uniformly stirring; heating for 0.5-1h at 80-90 deg.C, maintaining the temperature for 1.5-2h to obtain polyurethane prepolymer, and sealing for storage;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction.
Preparation of polyurethane emulsion
Cooling 85 parts of solution of polyurethane prepolymer to 50-70 ℃, gradually adding 11 parts of chain extender, and stirring; heating to 80-100 ℃, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction; and cooling, adding dibutylamine for neutralization, and adding water for emulsification for 0.5-1h to obtain the waterborne polyurethane emulsion.
Preparation of modified predispersed masterbatch
Heating and melting 15 parts of toughening agent, and taking out for later use after the toughening agent reaches a flowing state; adding 25 parts of filler into a dryer, removing surface moisture, and taking out for later use; adding a toughening agent and a filler into the polyurethane emulsion, and uniformly stirring; vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
Embodiment 4 a method of preparing a polyol-modified toughening pre-dispersed masterbatch, comprising:
preparation of polyurethane prepolymer
32.5 parts of polyethylene glycol is placed in a reactor, the temperature is raised to 120 ℃ for 100-; adding 55 parts of polyisocyanate into the polyethylene glycol solution, adding 4 parts of catalyst, and uniformly stirring; heating for 0.5-1h at 80-90 deg.C, maintaining the temperature for 1.5-2h to obtain polyurethane prepolymer, and sealing for storage;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction.
Preparation of polyurethane emulsion
Cooling 87.5 parts of solution of polyurethane prepolymer to 50-70 ℃, gradually adding 13 parts of chain extender, and stirring; heating to 80-100 ℃, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction; and cooling, adding dibutylamine for neutralization, and adding water for emulsification for 0.5-1h to obtain the waterborne polyurethane emulsion.
Preparation of modified predispersed masterbatch
Heating and melting 12.5 parts of toughening agent, and taking out for later use after the toughening agent reaches a flowing state; adding 22.5 parts of filler into a dryer, removing surface moisture, and taking out for later use; adding a toughening agent and a filler into the polyurethane emulsion, and uniformly stirring; vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
Embodiment 5 a method of preparing a polyol-modified toughening predispersion masterbatch, comprising:
preparation of polyurethane prepolymer
Placing 30 parts of polyethylene glycol in a reactor, heating to 120 ℃ at 100-; adding 60 parts of polyisocyanate into the polyethylene glycol solution, adding 5 parts of catalyst, and uniformly stirring; heating for 0.5-1h at 80-90 deg.C, maintaining the temperature for 1.5-2h to obtain polyurethane prepolymer, and sealing for storage;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction.
Preparation of polyurethane emulsion
Cooling 90 parts of the solution of the polyurethane prepolymer to 50-70 ℃, gradually adding 15 parts of the chain extender, and stirring; heating to 80-100 ℃, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction; and cooling, adding dibutylamine for neutralization, and adding water for emulsification for 0.5-1h to obtain the waterborne polyurethane emulsion.
Preparation of modified predispersed masterbatch
Heating and melting 10 parts of toughening agent, and taking out for later use after the toughening agent reaches a flowing state; adding 20 parts of filler into a dryer, removing surface moisture, and taking out for later use; adding a toughening agent and a filler into the polyurethane emulsion, and uniformly stirring; vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
In examples 1-5 above:
the chain extender is at least one of 1, 4-butanediol, 1, 6-hexanediol, dimethylolbutyric acid and trimethylolpropane, in the polyester processing technology, the molecular weight is reduced due to thermal degradation and hydrolysis, the number of terminal carboxyl groups is increased, so that the mechanical and chemical properties of the polymer are reduced, and the chain extender is a substance which can react with functional groups on a linear polymer chain to expand the molecular chain and increase the molecular weight and is used for improving the mechanical property and the technological property of a polyurethane product;
the toughening agent is at least one of polyvinyl butyral, polyvinyl acetate and chlorinated polyethylene, and the toughening agent is a substance capable of increasing the flexibility of an adhesive film layer, and plays a role in increasing the strength, toughness, brittleness and impact resistance of the polyurethane resin;
the filler is at least one of calcium carbonate, titanium dioxide, carbon black, kaolin, diatomite, wood flour, clay, silicon dioxide and talcum powder, and is used for reducing the cost of the polyurethane resin product, improving the bulk strength, the adhesive strength and the heat resistance of the polyurethane resin product, or improving the expansion and shrinkage rate or other functions of a cured product.
The polyol modified toughening pre-dispersed master batch prepared by the invention has better mechanical property, and the detection indexes of the polyol modified toughening pre-dispersed master batch prepared by the invention are shown in table 1:
TABLE 1
| Tensile strength (Mpa) | Elongation at Break (%) | Flexibility | Impact strength (J/m) | |
| Example 1 | 40 | 375 | In general | 355 |
| Example 2 | 42 | 390 | Good effect | 370 |
| Example 3 | 50 | 415 | Is preferably used | 385 |
| Example 4 | 48 | 410 | Good taste | 380 |
| Example 5 | 45 | 400 | Good effect | 365 |
According to table 1, the polyol modified toughening pre-dispersed master batch prepared by the invention has the advantages that in examples 1-5, when 35 parts of polyethylene glycol, 50 parts of polyisocyanate, 3 parts of catalyst, 11 parts of chain extender, 15 parts of toughening agent and 25 parts of filler are used, the tensile strength, elongation at break, flexibility and impact strength of the polyurethane resin pre-dispersed master batch are all the best, and when too much or too little polyisocyanate is used, the mechanical properties of polyurethane are affected, and meanwhile, the polyurethane blended by the chain extender, the toughening agent and the filler has better mechanical properties.
Comparative example 1 a method of preparing a polyol modified toughening predispersion masterbatch, comprising:
preparation of polyurethane prepolymer
Placing 35 parts of polyethylene glycol in a reactor, heating to 120 ℃ at 100-; adding 50 parts of polyisocyanate into the polyethylene glycol solution, adding 3 parts of catalyst, and uniformly stirring; heating for 0.5-1h at 80-90 deg.C, maintaining the temperature for 1.5-2h to obtain polyurethane prepolymer, and sealing for storage;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction.
Preparation of modified pre-dispersed master batch
Heating and melting 15 parts of toughening agent to a flowing state for later use; adding 25 parts of filler into a dryer, and removing surface moisture for later use; adding a toughening agent and a filler into the polyurethane emulsion, and uniformly stirring; vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
Comparative example 2 a method of preparing a polyol modified toughening predispersion masterbatch, comprising:
preparation of polyurethane prepolymer
Placing 35 parts of polyethylene glycol in a reactor, heating to 120 ℃ at 100-; adding 50 parts of polyisocyanate into the polyethylene glycol solution, adding 3 parts of catalyst, and uniformly stirring; heating for 0.5-1h at 80-90 deg.C, maintaining the temperature for 1.5-2h to obtain polyurethane prepolymer, and sealing for storage;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction.
Preparation of polyurethane emulsion
Cooling 85 parts of solution of polyurethane prepolymer to 50-70 ℃, gradually adding 11 parts of chain extender, and stirring; heating to 80-100 ℃, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction; and cooling, adding dibutylamine for neutralization, and adding water for emulsification for 0.5-1h to obtain the waterborne polyurethane emulsion.
Preparation of modified predispersed masterbatch
Adding 25 parts of filler into a dryer, and removing surface moisture for later use; adding the filler into the polyurethane emulsion, and uniformly stirring; vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
Comparative example 3 a method of preparing a polyol modified toughening predispersion masterbatch, comprising:
preparation of polyurethane prepolymer
Placing 35 parts of polyethylene glycol in a reactor, heating to 120 ℃ at 100-; adding 50 parts of polyisocyanate into the polyethylene glycol solution, adding 3 parts of catalyst, and uniformly stirring; heating for 0.5-1h at 80-90 deg.C, maintaining the temperature for 1.5-2h to obtain polyurethane prepolymer, and sealing for storage;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate, the reactivity of the polyethylene glycol is low, and the addition of the catalyst can reduce the reaction activity, accelerate the reaction process and control the occurrence of-OH side reaction.
Preparation of polyurethane emulsion
Cooling 85 parts of solution of polyurethane prepolymer to 50-70 ℃, gradually adding 11 parts of chain extender, and stirring; heating to 80-100 ℃, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction; and cooling, adding dibutylamine for neutralization, and adding water for emulsification for 0.5-1h to obtain the waterborne polyurethane emulsion.
Preparation of modified predispersed masterbatch
Heating and melting 15 parts of toughening agent to a flowing state for later use; adding a toughening agent into the polyurethane emulsion, and uniformly stirring; vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
The polyol modified toughening predispersed master batch prepared by the invention has good flexibility and strong mechanical properties such as tensile strength, and has a large relationship with a chain extender, a toughening agent and a filler added in the master batch, and in order to verify the related technical scheme, the applicant performs the following tests:
comparative examples 1 to 3: by adopting the method of the embodiment 3, under the condition of removing the chain extender, the flexibilizer and the filler, the related indexes of the prepared polyol modified toughening pre-dispersion master batch are detected, and the concrete indexes are shown in table 2:
TABLE 2
| Tensile strength (Mpa) | Elongation at Break (%) | Flexibility | Impact strength (J/m) | |
| Comparative example 1 | 28 | 180 | Difference (D) | 220 |
| Comparative example 2 | 23 | 171 | Is poor | 190 |
| Comparative example 3 | 19 | 166 | Difference (D) | 150 |
| Example 4 | 50 | 415 | Is preferably used | 385 |
According to table 2, in comparative examples 1 to 3, under the condition of removing the chain extender, the toughening agent and the filler, the tensile strength of the polyurethane resin pre-dispersed master batch is lower than 30Mpa, the elongation at break is less than 200%, and the flexibility and the impact strength are greatly reduced, so that it can be seen that the added chain extender, toughening agent and filler are important factors influencing the mechanical properties of the polyurethane resin pre-dispersed master batch.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A polyol modified toughening pre-dispersing master batch comprises the following raw materials: 70-100 parts of polyurethane prepolymer, 7-15 parts of chain extender, 10-20 parts of flexibilizer and 20-30 parts of filler.
2. The polyol-modified toughening predispersion masterbatch of claim 1, characterized in that: the polyurethane prepolymer is prepared by the prepolymerization reaction of 30-40 parts of polyethylene glycol, 40-60 parts of polyisocyanate and 1-5 parts of catalyst;
the polyisocyanate is selected from at least one of 2, 4-toluene diisocyanate and 2, 6-toluene diisocyanate;
the catalyst is at least one of stannous octoate, morpholinyl diethyl ether and dibutyltin dilaurate;
the pre-polymerization reaction of the polyurethane prepolymer comprises the following steps:
s1.1, placing polyethylene glycol in a reactor, heating, vacuumizing, dehydrating, cooling, and sealing for later use;
s1.2, adding polyisocyanate into the polyethylene glycol solution, adding a catalyst, and uniformly stirring;
and S1.3, heating, reacting at constant temperature for timing to obtain a polyurethane prepolymer, and sealing and storing.
3. The polyol-modified toughening predispersion masterbatch of claim 2, wherein: in the S1.1, the temperature in the reactor is 100-.
4. The polyol-modified toughening predispersion masterbatch of claim 2, wherein: and in the S1.3, the temperature is increased for 0.5 to 1 hour, the temperature is 80 to 90 ℃, and the constant-temperature reaction time is 1.5 to 2 hours.
5. The polyol-modified toughening predispersion masterbatch of claim 1, characterized in that: the chain extender is at least one of 1, 4-butanediol, 1, 6-hexanediol, dimethylolbutyric acid and trimethylolpropane.
6. The polyol-modified toughening predispersion masterbatch of claim 1, characterized in that: the toughening agent is at least one of polyvinyl butyral, polyvinyl acetate and chlorinated polyethylene.
7. The polyol-modified toughening predispersion masterbatch of claim 1, characterized in that: the filler is at least one of calcium carbonate, titanium dioxide, carbon black, kaolin, diatomite, wood powder, clay, silicon dioxide and talcum powder.
8. A method for preparing a polyol-modified toughening predispersion master batch, comprising the polyol-modified toughening predispersion master batch of any one of claims 1 to 7, comprising the following steps:
s2.1, cooling the polyurethane prepolymer solution, gradually adding a chain extender, and stirring;
s2.2, heating, stopping stirring, vacuumizing to remove bubbles, and carrying out chain extension reaction;
s2.3, cooling again, adding a neutralizing agent, and adding water for emulsification to prepare an aqueous polyurethane emulsion;
s2.4, heating and melting the toughening agent, and taking out for later use after the toughening agent reaches a flowing state;
s2.5, adding the filler into a dryer, removing surface moisture, and taking out for later use;
s2.6, adding a toughening agent and a filler into the polyurethane emulsion, and uniformly stirring;
and S2.7, vacuumizing and defoaming for 10-15min, stopping stirring, relieving vacuum, and performing extrusion molding to obtain the polyurethane resin pre-dispersed master batch.
9. The method for preparing the polyol-modified toughening predispersion master batch according to claim 8, wherein the method comprises the following steps: the temperature in the S2.1 is reduced to 50-70 ℃, and the temperature in the S2.2 is increased to 80-100 ℃.
10. The method for preparing the polyol-modified toughening predispersion master batch according to claim 8, wherein the method comprises the following steps: the temperature in the S2.3 is reduced to 30-50 ℃, the neutralizer is dibutylamine, and the emulsifying time is 0.5-1 h.
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| US5344882A (en) * | 1990-06-22 | 1994-09-06 | E. I. Du Pont De Nemours And Company | Polyacetal blends |
| US20150051306A1 (en) * | 2011-11-16 | 2015-02-19 | Singtex Industrial Co., Ltd. | Method for preparing a coffee polyol and compositions and materials containing the same |
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