CN108192062A - The preparation method of super branched polyurethane - Google Patents
The preparation method of super branched polyurethane Download PDFInfo
- Publication number
- CN108192062A CN108192062A CN201711361157.7A CN201711361157A CN108192062A CN 108192062 A CN108192062 A CN 108192062A CN 201711361157 A CN201711361157 A CN 201711361157A CN 108192062 A CN108192062 A CN 108192062A
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- CN
- China
- Prior art keywords
- preparation
- diisocyanate
- super branched
- branched polyurethane
- organic solvent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a kind of preparation method of super branched polyurethane, including step：(1) 2,2 dihydromethyl propionic acids, diisocyanate and pentaerythrite are dissolved in organic solvent, obtain mixed solution；(2) mixed solution obtained in step (1) under conditions of 65 75 DEG C is reacted into 5 7h, obtains prepolymer；(3) triethylamine is added in the prepolymer obtained into step (2), after reacting 2 3h, organic solvent is removed in vacuo, obtains the super branched polyurethane.The preparation method mild condition of the present invention is easily realized；The hyperbranched aqueous polyurethane viscosity of preparation is low, active height；With preferable water resistance, mechanical performance and heat resistance.
Description
Technical field
The present invention relates to polyurethane preparation field more particularly to a kind of preparation methods of super branched polyurethane.
Background technology
Polyurethane is used as roller, conveyer belt, hose, auto parts, sole, synthetic leather, electric wire and medical artificial
Internal organs etc., flexible foam for vehicle, room, clothes liner, hard foam be used as heat-insulated, sound-absorbing, packaging, insulation with
And low ratio foamed synthetic wood, coating are used for advanced vehicle, furniture, wood and metal protection, pond dam and building anti-seepage material,
And fabric coating etc..Adhesive has good adhesion strength to metal, glass, ceramics, leather, fiber etc..In addition polyurethane
It may also be fabricated which lotion, magnetic material etc..
As aqueous polyurethane develops, its application range constantly expands, but shortcoming is also more and more apparent, such as water-fast
Property, mechanical performance and heat resistance are poor, limit the application of polyurethane.
Super branched polyurethane is a kind of novel high polymer material that latest developments are got up, and has highly branched molecule knot
Structure, it is intermolecular that there is less chain entanglement, containing a large amount of functional end-group, have viscosity it is low, it is active it is high, that dissolubility is good etc. is excellent
Point.
Invention content
Goal of the invention：The present invention provides a kind of preparation methods of super branched polyurethane, and the preparation method step is simple, system
Standby super branched polyurethane viscosity is low, active height, and with preferable water resistance, mechanical performance and heat resistance.
Technical solution：The preparation method of the super branched polyurethane of the present invention, includes the following steps：
(1) 2,2- dihydromethyl propionic acids, diisocyanate and pentaerythrite are dissolved in organic solvent, obtain mixing molten
Liquid；
(2) mixed solution obtained in step (1) under conditions of 65-75 DEG C is reacted into 5-7h, obtains prepolymer；
(3) triethylamine is added in the prepolymer obtained into step (2), after reacting 2-3h, organic solvent is removed in vacuo, obtains
To the super branched polyurethane.
In step (1), the diisocyanate is 1, hexamethylene-diisocyanate, isophorone diisocyanate and two hexamethylenes
One or more of dicyclohexylmethane diisocyanate.
The molar ratio of the 2,2- dihydromethyl propionic acids, diisocyanate and pentaerythrite is
1:0.8-1.2:0.25-0.4。
A concentration of 0.2-0.4mol/L of the 2,2- dihydromethyl propionic acids.
The organic solvent is one or more of acetone, dichloromethane and ethyl acetate.
In step (3), the molar ratio of the triethylamine and 2,2- dihydromethyl propionic acid is 3-6:1.
Advantageous effect：1st, preparation method mild condition of the invention, easily realization；2nd, step is simple, easy to operate；3rd, raw material is easy
, it is at low cost；4th, the hyperbranched aqueous polyurethane viscosity for preparing is low, active height；5th, have preferable water resistance, mechanical performance and
Heat resistance；6th, simultaneously, tensile strength and acid-proof alkaline obtain a degree of promotion.
Specific embodiment
Embodiment 1
The preparation method of super branched polyurethane, includes the following steps：
(1) by 0.02mol 2,2- dihydromethyl propionic acids, 0.016mol hexamethylene diisocyanates and 0.005mol seasons penta
Tetrol is dissolved in 100ml ethyl acetate, obtains mixed solution；
(2) mixed solution obtained in step (1) is reacted into 5h under conditions of 65 DEG C, obtains prepolymer；
(3) 0.06mol triethylamines are added in the prepolymer obtained into step (2), after reacting 2h, acetic acid second is removed in vacuo
Ester obtains the super branched polyurethane.
Embodiment 2
The preparation method of super branched polyurethane, includes the following steps：
(1) by 0.03mol 2,2- dihydromethyl propionic acids, 0.03mol isophorone diisocyanate and 0.009mol seasons penta
Tetrol is dissolved in 100ml dichloromethane, obtains mixed solution；
(2) mixed solution obtained in step (1) is reacted into 6h under conditions of 70 DEG C, obtains prepolymer；
(3) 0.12mol triethylamines are added in the prepolymer obtained into step (2), after reacting 2.5h, dichloro is removed in vacuo
Methane obtains the super branched polyurethane.
Embodiment 3
The preparation method of super branched polyurethane, includes the following steps：
(1) by 0.04mol 2,2- dihydromethyl propionic acids, 0.048mol dicyclohexyl methyl hydride diisocyanates and
0.016mol pentaerythrites are dissolved in acetone, obtain mixed solution；
(2) mixed solution obtained in step (1) is reacted into 7h under conditions of 75 DEG C, obtains prepolymer；
(3) 0.24mol triethylamines are added in the prepolymer obtained into step (2), after reacting 3h, acetone is removed in vacuo,
Obtain the super branched polyurethane.
Claims (6)
1. a kind of preparation method of super branched polyurethane, which is characterized in that include the following steps：
(1) 2,2- dihydromethyl propionic acids, diisocyanate and pentaerythrite are dissolved in organic solvent, obtain mixed solution；
(2) mixed solution obtained in step (1) under conditions of 65-75 DEG C is reacted into 5-7h, obtains prepolymer；
(3) triethylamine is added in the prepolymer obtained into step (2), after reacting 2-3h, organic solvent is removed in vacuo, obtains institute
State super branched polyurethane.
2. preparation method according to claim 1, it is characterised in that：In step (1), the diisocyanate for 1,6- oneself
One or more of diisocyanate, isophorone diisocyanate and dicyclohexyl methyl hydride diisocyanate.
3. preparation method according to claim 1, it is characterised in that：The 2,2- dihydromethyl propionic acids, diisocyanate
Molar ratio with pentaerythrite is 1:0.8-1.2:0.25-0.4.
4. preparation method according to claim 1, it is characterised in that：A concentration of 0.2- of the 2,2- dihydromethyl propionic acids
0.4mol/L。
5. preparation method according to claim 1, it is characterised in that：The organic solvent is acetone, dichloromethane and second
One or more of acetoacetic ester.
6. preparation method according to claim 1, it is characterised in that：In step (3), the triethylamine and 2,2- dihydroxy first
The molar ratio of base propionic acid is 3-6:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711361157.7A CN108192062A (en) | 2017-12-18 | 2017-12-18 | The preparation method of super branched polyurethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711361157.7A CN108192062A (en) | 2017-12-18 | 2017-12-18 | The preparation method of super branched polyurethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108192062A true CN108192062A (en) | 2018-06-22 |
Family
ID=62576875
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711361157.7A Withdrawn CN108192062A (en) | 2017-12-18 | 2017-12-18 | The preparation method of super branched polyurethane |
Country Status (1)
| Country | Link |
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| CN (1) | CN108192062A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109486285A (en) * | 2018-10-30 | 2019-03-19 | 浙江蓝宇数码科技股份有限公司 | A kind of paint ink and preparation method of the dispersing agent containing super branched polyurethane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942664A (en) * | 2012-11-28 | 2013-02-27 | 安徽大学 | Preparation method of hydroxyl-terminated hyperbranched polyurethane |
| CN107353387A (en) * | 2017-08-03 | 2017-11-17 | 山东天庆科技发展有限公司 | A kind of aqueous anionic polyurethane emulsion and preparation method and application |
-
2017
- 2017-12-18 CN CN201711361157.7A patent/CN108192062A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942664A (en) * | 2012-11-28 | 2013-02-27 | 安徽大学 | Preparation method of hydroxyl-terminated hyperbranched polyurethane |
| CN107353387A (en) * | 2017-08-03 | 2017-11-17 | 山东天庆科技发展有限公司 | A kind of aqueous anionic polyurethane emulsion and preparation method and application |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109486285A (en) * | 2018-10-30 | 2019-03-19 | 浙江蓝宇数码科技股份有限公司 | A kind of paint ink and preparation method of the dispersing agent containing super branched polyurethane |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180622 |