CN102757546A - Preparation method of self-crosslinking aqueous polyurethane for terrace - Google Patents
Preparation method of self-crosslinking aqueous polyurethane for terrace Download PDFInfo
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- CN102757546A CN102757546A CN201210267256XA CN201210267256A CN102757546A CN 102757546 A CN102757546 A CN 102757546A CN 201210267256X A CN201210267256X A CN 201210267256XA CN 201210267256 A CN201210267256 A CN 201210267256A CN 102757546 A CN102757546 A CN 102757546A
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Abstract
The invention discloses a preparation method of self-crosslinking aqueous polyurethane for a terrace, which belongs to the field of chemical materials for buildings. The method comprises the following steps of: dehydrating a mixture of hydrophilic macromolecular polyatomic alcohol and castor oil at the temperature of 80-100 DEG C in vacuum, preserving heat at the temperature of 50-95 DEG C for reacting diisocyanate under the condition of introducing nitrogen gas for 3-4 hours, adding a polyfunctional hydroxyl-containing chain extender and a catalyst, and preserving heat at the temperature of 50-90 DEG C for reacting for 3-5 hours to obtain a polyurethane prepolymer of which the chain end is provided with isocyanate and the molecular chain contains a hydrophilic group; and cooling the polyurethane prepolymer to 40-55 DEG C, rapidly stirring and dispersing into deionized water containing neutralizing amine, and adding a ketone hydrazine self-crosslinking chain extender to a dispersoid for performing a chain extending reaction to obtain the self-crosslinking aqueous polyurethane for the terrace after reacting.
Description
Technical field
The present invention relates to chemical material field for building, relate in particular to the preparation method of a kind of terrace with self-crosslinking aqueous polyurethane.
Background technology
At present in the resin that the terrace of building uses, commonly used have epoxy resin, monocomponent polyurethane and a bi-component resin etc., and epoxy resin exists weathering resistance poor; The monocomponent polyurethane poor water resistance; And there is the problem of using validity period short in components resin in pairs.
Summary of the invention
Embodiment of the present invention provides the preparation method of a kind of terrace with self-crosslinking aqueous polyurethane, and it is poor to solve the epoxy resin weathering resistance, can not be used for outdoor shortcoming, and its wear resistance of filming, weathering resistance and water-whitening resistance are excellent.
Following for addressing the above problem technical scheme provided by the invention:
Embodiment of the present invention provides the preparation method of a kind of terrace with self-crosslinking aqueous polyurethane, comprising:
The wetting ability macromolecular polyol mixed with Viscotrol C the mixture that forms after the vacuum hydro-extraction under 80～100 ℃ of temperature with vulcabond under logical condition of nitrogen gas under 50～95 ℃ of temperature insulation reaction 3～4 hours; Add polyfunctionality hydroxyl chainextender and catalyzer again; Insulation reaction is 3～5 hours under 50～90 ℃ of temperature, and obtaining the end of the chain is the base polyurethane prepolymer for use as that contains hydrophilic radical on NCO and the molecular chain;
Said base polyurethane prepolymer for use as is cooled to 40～55 ℃; Join in the deionized water that contains with the neutralizing amine of the hydrophilic radical equimolar amount of said base polyurethane prepolymer for use as and disperse to form dispersion-s with the rotating speed THE ADIABATIC SHEAR IN of 3000～3500r/min; And ketone hydrazine self-crosslinking chainextender joined carry out chain extending reaction in the said dispersion-s, promptly make terrace after the reaction and use self-crosslinking aqueous polyurethane.
Technical scheme by the invention described above provides can be found out, the method that embodiment of the present invention provides adopts the renewable resources Viscotrol C to prepare aqueous polyurethane, has improved the feature of environmental protection and economizes on resources; Adopting macromole to contain the carboxyl polyvalent alcohol can solve and adopt common small molecules hydrophilic monomer to cause hydrophilic radical problem of uneven distribution on molecular chain easily.
Embodiment
Below in conjunction with specific embodiment the technical scheme among the present invention is carried out clear, intactly description, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on embodiments of the invention, those of ordinary skills belong to protection scope of the present invention not making the every other embodiment that is obtained under the creative work prerequisite.
Do to describe in detail further in the face of the embodiment of the invention down.
The embodiment of the invention provides the preparation method of a kind of terrace with self-crosslinking aqueous polyurethane; May further comprise the steps: the wetting ability macromolecular polyol is mixed with Viscotrol C the mixture that forms after the vacuum hydro-extraction under 80～100 ℃ of temperature with vulcabond under logical condition of nitrogen gas under 50～95 ℃ of temperature insulation reaction 3～4 hours; Add polyfunctionality hydroxyl chainextender and catalyzer again; Insulation reaction is 3～5 hours under 50～90 ℃ of temperature, and obtaining the end of the chain is the base polyurethane prepolymer for use as that contains hydrophilic radical on NCO and the molecular chain;
Said base polyurethane prepolymer for use as is cooled to 40～55 ℃; Join in the deionized water that contains with the neutralizing amine of the hydrophilic radical equimolar amount of said base polyurethane prepolymer for use as and disperse to form dispersion-s with the rotating speed THE ADIABATIC SHEAR IN of 3000～3500r/min; And ketone hydrazine self-crosslinking chainextender joined carry out chain extending reaction in the said dispersion-s, promptly make terrace after the reaction and use self-crosslinking aqueous polyurethane.
In the aforesaid method, the consumption of each raw material by mass parts is:
Wetting ability macromolecular polyol consumption is: 80～100 parts;
The Viscotrol C consumption is: 5～10 parts;
The vulcabond consumption is: 48 parts;
Polyfunctionality hydroxyl chainextender consumption is: 7 parts;
Catalyst levels is: 0.04 part;
Ketone hydrazine self-crosslinking chainextender consumption is: 25.7 parts～35 parts.
In the aforesaid method, the relative molecular weight of wetting ability macromolecular polyol is 400～4000.
In the aforesaid method, contain on the wetting ability macromolecular polyol molecular chain-OH and-COOH functional group.
In the aforesaid method, the functionality of Viscotrol C is 2～3, and molecular weight is 200～600.
In the aforesaid method, vulcabond is one or several in hexamethylene diisocyanate, isofoer diisocyanate, the tolylene diisocyanate.
In the aforesaid method, polyfunctionality hydroxyl chainextender is 1, one or several in 4-butyleneglycol, tetramethylolmethane, NSC 6366, the TriMethylolPropane(TMP).
In the aforesaid method, catalyzer is a dibutyl tin laurate.
In the aforesaid method, neutralizing amine is triethylamine or Tri N-Propyl Amine.
In the aforesaid method, the agent of ketone hydrazine self-crosslinking is diacetone-acryloamide(DAA) and adipic dihydrazide.
The terrace of embodiment of the invention method preparation is used self-crosslinking aqueous polyurethane; Be by isocyanic ester; The wetting ability macromolecular polyol, Viscotrol C, polyfunctionality hydroxyl chainextender synthesis of polyurethane performed polymer; Through the THE ADIABATIC SHEAR IN stirring and emulsifying in containing the water of neutralizing amine, after ketone hydrazine self-cross linking monomer chain extension be prepared from.This emulsion has package stability preferably under normal temperature sealing, along with the volatilization of moisture, the reduction of pH value and crosslinked voluntarily can form bigger the filming of cross-linking density in the use.
Below in conjunction with specific embodiment aforesaid method is described further.
Embodiment 1
Present embodiment provides the preparation method of a kind of terrace with self-crosslinking aqueous polyurethane, may further comprise the steps:
According to the form below is got preparation terrace each raw material with self-crosslinking aqueous polyurethane:
| Raw material type | Mass fraction |
| Wetting ability macromolecular polyol 2000 | 80 |
| Viscotrol C (CO) | 10 |
| Isofoer diisocyanate (IPDI) | 48 |
| TriMethylolPropane(TMP) (TMP) | 2 |
| NSC 6366 (NPG) | 5 |
| Dibutyl tin laurate (DBTDL) | 0.04 |
| Triethylamine (TEA) | 6 |
| Adipic dihydrazide (ADH) | 18.9 |
| Diacetone-acryloamide(DAA) (DAAM) | 9.5 |
Concrete preparation process is: with molecular weight is that 2000 wetting ability macromolecular polyol and Viscotrol C were 80～100 ℃ of following vacuum hydro-extractions 1.5 hours; Reduce to room temperature; Add IPDI and be warming up to 50～95 ℃, insulation reaction 3 hours is introduced NPG, TMP and DBTDL; Insulation reaction 3.5 hours makes base polyurethane prepolymer for use as;
The base polyurethane prepolymer for use as that makes is reduced to 40～55 ℃, and the rotating speed THE ADIABATIC SHEAR IN with 3000～3500r/min in the deionized water that contains neutralizing agent triethylamine (consumption of triethylamine and base polyurethane prepolymer for use as are equimolar amount) stirs the acquisition aqueous polyurethane emulsion.Add ADH and DAAM at last, promptly make terrace and use self-crosslinking aqueous polyurethane.
Embodiment 2
Present embodiment provides the preparation method of a kind of terrace with self-crosslinking aqueous polyurethane, may further comprise the steps:
According to the form below is got preparation terrace each raw material with self-crosslinking aqueous polyurethane:
| Raw material type | Mass fraction |
| Wetting ability macromolecular polyol 2000 | 80 |
| Viscotrol C (CO) | 5 |
| Isofoer diisocyanate (IPDI) | 48 |
| TriMethylolPropane(TMP) (TMP) | 2 |
| NSC 6366 (NPG) | 5 |
| Dibutyl tin laurate (DBTDL) | 0.04 |
| Triethylamine (TEA) | 6 |
| Adipic dihydrazide (ADH) | 23.5 |
| Diacetone-acryloamide(DAA) (DAAM) | 11.5 |
Concrete preparation process and embodiment 1 are basic identical, can be referring to the preparation process of embodiment 1.
Embodiment 3
Present embodiment provides the preparation method of a kind of terrace with self-crosslinking aqueous polyurethane, may further comprise the steps:
According to the form below is got preparation terrace each raw material with self-crosslinking aqueous polyurethane:
| Raw material type | Mass fraction |
| Wetting ability macromolecular polyol 2000 | 100 |
| Viscotrol C (CO) | 10 |
| Isofoer diisocyanate (IPDI) | 48 |
| TriMethylolPropane(TMP) (TMP) | 2 |
| NSC 6366 (NPG) | 5 |
| Dibutyl tin laurate (DBTDL) | 0.04 |
| Triethylamine (TEA) | 7.5 |
| AH (ADH) | 17.2 |
| Diacetone-acryloamide(DAA) (DAAM) | 8.5 |
Concrete preparation process and embodiment 1 are basic identical, can be referring to the preparation process of embodiment 1.
In sum, the embodiment of the invention prepare the method for terrace with self-crosslinking aqueous polyurethane, adopt the renewable resources Viscotrol C to prepare aqueous polyurethane, improved the feature of environmental protection and economized on resources; Adopting macromole to contain the carboxyl polyvalent alcohol can solve and adopt common small molecules hydrophilic monomer to cause hydrophilic radical problem of uneven distribution on molecular chain easily.
The above; Be merely the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is 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 (10)
1. a terrace is characterized in that with the preparation method of self-crosslinking aqueous polyurethane, comprising:
The wetting ability macromolecular polyol mixed with Viscotrol C the mixture that forms after the vacuum hydro-extraction under 80～100 ℃ of temperature with vulcabond under logical condition of nitrogen gas under 50～95 ℃ of temperature insulation reaction 3～4 hours; Add polyfunctionality hydroxyl chainextender and catalyzer again; Insulation reaction is 3～5 hours under 50～90 ℃ of temperature, and obtaining the end of the chain is the base polyurethane prepolymer for use as that contains hydrophilic radical on NCO and the molecular chain;
Said base polyurethane prepolymer for use as is cooled to 40～55 ℃; Join in the deionized water that contains with the neutralizing amine of the hydrophilic radical equimolar amount of said base polyurethane prepolymer for use as and disperse to form dispersion-s with the rotating speed THE ADIABATIC SHEAR IN of 3000～3500r/min; And ketone hydrazine self-crosslinking chainextender joined carry out chain extending reaction in the said dispersion-s, promptly make terrace after the reaction and use self-crosslinking aqueous polyurethane.
2. method according to claim 1 is characterized in that, the consumption of said each raw material by mass parts is:
Wetting ability macromolecular polyol consumption is: 80～100 parts;
The Viscotrol C consumption is: 5～10 parts;
The vulcabond consumption is: 48 parts;
Polyfunctionality hydroxyl chainextender consumption is: 7 parts;
Catalyst levels is: 0.04 part;
Ketone hydrazine self-crosslinking chainextender consumption is: 25.7 parts～35 parts.
3. method according to claim 1 and 2 is characterized in that, the relative molecular weight of said wetting ability macromolecular polyol is 400～4000.
4. method according to claim 1 and 2 is characterized in that, contains on the said wetting ability macromolecular polyol molecular chain-OH and-COOH functional group.
5. method according to claim 1 and 2 is characterized in that, the functionality of said Viscotrol C is 2～3, and molecular weight is 200～600.
6. method according to claim 1 and 2 is characterized in that, said vulcabond is one or several in hexamethylene diisocyanate, isofoer diisocyanate, the tolylene diisocyanate.
7. method according to claim 1 and 2 is characterized in that, said polyfunctionality hydroxyl chainextender is 1, one or several in 4-butyleneglycol, tetramethylolmethane, NSC 6366, the TriMethylolPropane(TMP).
8. method according to claim 1 and 2 is characterized in that, said catalyzer is a dibutyl tin laurate.
9. method according to claim 1 and 2 is characterized in that, said neutralizing amine is triethylamine or Tri N-Propyl Amine.
10. method according to claim 1 and 2 is characterized in that, the agent of said ketone hydrazine self-crosslinking is diacetone-acryloamide(DAA) and adipic dihydrazide.
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Cited By (5)
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| CN104761993A (en) * | 2015-04-09 | 2015-07-08 | 广西吉顺能源科技有限公司 | Polyurethane anticorrosive thermal-insulation paint and preparation method thereof |
| CN107177303A (en) * | 2017-06-12 | 2017-09-19 | 芜湖天航科技（集团）股份有限公司 | Polyurethane coating and preparation method thereof |
| CN108977035A (en) * | 2018-08-07 | 2018-12-11 | 广州立邦涂料有限公司 | Low-VOC aqueous polyurethane floor coatings and preparation method thereof |
| CN112266460A (en) * | 2020-11-06 | 2021-01-26 | 安徽聚合辐化化工有限公司 | Thermosetting polyurethane and preparation method thereof |
| CN116675826A (en) * | 2023-06-05 | 2023-09-01 | 京准化工技术(上海)有限公司 | Polyurethane waterproof agent for fabric and preparation process thereof |
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| CN101270259A (en) * | 2008-04-22 | 2008-09-24 | 上海阳森精细化工有限公司 | Solvent-free polyurethane gravity flow self-leveling floor material and preparing method |
| CN101759861A (en) * | 2010-02-02 | 2010-06-30 | 陕西科技大学 | Method for preparing waterborne polyurethane emulsion capable of self-crosslinking at normal temperature |
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| CN101759861A (en) * | 2010-02-02 | 2010-06-30 | 陕西科技大学 | Method for preparing waterborne polyurethane emulsion capable of self-crosslinking at normal temperature |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104761993A (en) * | 2015-04-09 | 2015-07-08 | 广西吉顺能源科技有限公司 | Polyurethane anticorrosive thermal-insulation paint and preparation method thereof |
| CN104761993B (en) * | 2015-04-09 | 2017-12-29 | 广西吉顺能源科技有限公司 | Polyurethane anticorrosion insulating mold coating and preparation method thereof |
| CN107177303A (en) * | 2017-06-12 | 2017-09-19 | 芜湖天航科技（集团）股份有限公司 | Polyurethane coating and preparation method thereof |
| CN108977035A (en) * | 2018-08-07 | 2018-12-11 | 广州立邦涂料有限公司 | Low-VOC aqueous polyurethane floor coatings and preparation method thereof |
| CN112266460A (en) * | 2020-11-06 | 2021-01-26 | 安徽聚合辐化化工有限公司 | Thermosetting polyurethane and preparation method thereof |
| CN116675826A (en) * | 2023-06-05 | 2023-09-01 | 京准化工技术(上海)有限公司 | Polyurethane waterproof agent for fabric and preparation process thereof |
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