CN110358048B - Preparation method of waterborne polyurethane emulsion for temperature-resistant transfer coating - Google Patents
Preparation method of waterborne polyurethane emulsion for temperature-resistant transfer coating Download PDFInfo
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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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/758—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing two or more cycloaliphatic rings
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/06—Polyurethanes from polyesters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
Abstract
The invention discloses a preparation method of waterborne polyurethane emulsion for temperature-resistant transfer paint, which has the technical scheme key points that the preparation method comprises the following steps: under the protection of dry nitrogen, 6-14% of oligomer polyol is dehydrated and vacuumized for 1 hour at the temperature of 100-110 ℃, and then cooled to 50-60 ℃; adding 10-12% of diisocyanate, automatically releasing heat, heating to 85 +/-3 ℃, reacting for 2 hours, and cooling to 52-54 ℃; mixing 12-16% of hydrophilic chain extender, 1.5-3% of cross-linking agent and 2-4% of NMP, and reacting for 1 hour at 70-75 ℃; adding 0.006-0.012% of catalyst, and reacting for 2 hours at 60-65 ℃; cooling, adding 12-18% of acetone, cooling to below 30-35 ℃, adding an amine chain extender, and dispersing for 1 minute; adding a neutralizing agent and ice pure water within 1 minute, and dispersing at a high speed for 20 minutes; vacuumizing and removing the solvent to obtain the waterborne polyurethane emulsion for the temperature-resistant transfer coating; the synthesis process is simple, the particle size of the emulsion is appropriate, the production quality is good, and the heat resistance is good.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to a preparation method of a waterborne polyurethane emulsion for a temperature-resistant transfer coating, belonging to the technical field of coatings.
[ background of the invention ]
The PET is coated with a layer of solvent-based transfer coating, then aluminized and then transferred onto paper through water-based wet composite glue, which is a great reform in the cigarette packet industry because the PET is more environment-friendly and more easily degraded than the PET directly plated with aluminum. However, in recent years, as domestic environmental regulations become more stringent, solvent-based transfer coatings are increasingly limited due to their high VOC emission, odor, flammability, and explosiveness. Therefore, the trend of requiring water-based paint is more and more obvious, but at present, two water-based products are mainly used in the market to replace the solvent-based transfer paint, one water-based transfer paint using water-based acrylic emulsion as a bonding material is used to replace the solvent-based transfer paint, and the other way is to replace the solvent-based transfer paint by the water-based transfer paint using water-based polyurethane as a bonding material. However, the waterborne transfer coating using the waterborne acrylic emulsion as a binder has good printability and good temperature resistance, but has poor stripping property; the water-based transfer coating using the water-based polyurethane as the bonding material has good stripping performance and poor temperature resistance.
[ summary of the invention ]
The invention aims to provide the aqueous polyurethane emulsion for the temperature-resistant transfer coating, which has good transferability and good temperature resistance on the premise of not increasing the cost of raw materials by using main raw materials such as low polymer polyol, diisocyanate, a hydrophilic chain extender, a cross-linking agent, an amine chain extender and the like and using a two-step method of a prepolymer method.
The invention also aims to provide a preparation method of the waterborne polyurethane emulsion for the temperature-resistant transfer coating.
The waterborne polyurethane emulsion for the temperature-resistant transfer coating comprises the following components in parts by weight:
preferably, the oligomer polyol is any one of polycarbonate diol (PCDL), neopentyl glycol adipate diol (PNA) and polytetrahydrofuran ether glycol (PTMG).
Preferably, the diisocyanate is any one of H12MDI and IPDI.
Preferably, the hydrophilic chain extender is any one of dimethylolpropionic acid (DMPA) and dihydroxybutyric acid.
Preferably, the cross-linking agent is a mixture of trimethylolpropane, CHDM and BEPD.
Preferably, the catalyst is stannous octoate.
Preferably, the amine chain extender is a solution obtained by dissolving DMEA in 3% ice pure water, and the ice pure water is water at 0-4 ℃.
Preferably, the neutralizing agent is any one of triethylamine and hexamethylene diamine.
A preparation method of waterborne polyurethane emulsion for temperature-resistant transfer paint comprises the following steps:
1) under the protection of dry nitrogen, 6-14% of oligomer polyol is dehydrated and vacuumized for 1 hour at the temperature of 100-110 ℃, and then cooled to 50-60 ℃;
2) adding 10-12% of diisocyanate, automatically releasing heat, heating to 85 +/-3 ℃, reacting for 2 hours, and cooling to 52-54 ℃;
3) mixing 12-16% of hydrophilic chain extender, 1.5-3% of cross-linking agent and 2-4% of NMP, adding, paying attention to the fact that the temperature can not rise too fast, and reacting for 1 hour at 70-75 ℃;
4) adding 0.006-0.012% of catalyst, and reacting for 2 hours at 60-65 ℃;
5) adding 12-18% of acetone while cooling, and cooling to below 30-35 ℃;
6) discharging the prepolymer into a dispersing barrel, quickly adding an amine chain extender, and dispersing at a high speed for 1 minute;
7) quickly adding a neutralizing agent and ice pure water within 1 minute, and dispersing at a high speed for 20 minutes;
8) and vacuumizing at 57-60 ℃ for desolventizing for 1 hour to obtain the waterborne polyurethane emulsion for the temperature-resistant transfer coating.
The viscosity of the aqueous polyurethane emulsion for the temperature-resistant transfer coating is 14 +/-2 seconds/25 ℃.
Compared with the prior art, the invention has the following advantages:
1. the waterborne polyurethane emulsion for the temperature-resistant transfer coating adopts oligomer polyol, diisocyanate, a hydrophilic chain extender, a cross-linking agent and an amine chain extender, prepares a prepolymer by a two-step method of a prepolymer method, quickly stirs, emulsifies, vacuumizes and desolventizes, and generates the waterborne polyurethane emulsion with larger molecular weight by controlling the reaction temperature, the cross-linking density and the chain extension degree;
2. according to the waterborne polyurethane emulsion for the temperature-resistant transfer coating, a proper hydrophilic chain extender and a proper proportion are adopted, so that the comprehensive indexes of small particle size and good leveling property of the waterborne polyurethane emulsion are achieved, a proper cross-linking agent combination and a proper proportion are adopted to achieve a proper molecular weight, so that the product has good heat resistance and simultaneously has the characteristic of easy stripping, the prepared waterborne polyurethane emulsion for the temperature-resistant transfer coating has excellent performance, can be easily stripped after film forming, can resist the temperature of 160 ℃, has no yellowing and sticking phenomenon, and is superior to similar products abroad;
3. the preparation method of the aqueous polyurethane emulsion for the temperature-resistant transfer coating has the advantages of simple synthesis process, easy reaction control, good repeatability, proper emulsion particle size, good production quality, good heat resistance, environment-friendly and safe process synthesis and little smell;
4. according to the preparation method of the waterborne polyurethane emulsion for the temperature-resistant transfer coating, disclosed by the invention, the prepolymer is prepared by adopting a two-step method of a prepolymer method, so that a plurality of defects of large particle size range, coarse particle size, poor storage stability, poor physical properties of a film-forming material and the like of the traditional polyurethane emulsion are overcome.
[ detailed description ] embodiments
The invention is further described below with reference to specific examples:
example 1:
the waterborne polyurethane emulsion for the temperature-resistant transfer coating comprises the following components in parts by weight:
the preparation method of the aqueous polyurethane emulsion for the temperature-resistant transfer paint in the embodiment 1 comprises the following steps:
1) under the protection of dry nitrogen, dehydrating and vacuumizing polycarbonate diol (PCDL) at 110 ℃ for 1 hour, and cooling to 60 ℃;
2) adding H12MDI, heating to 88 ℃ from self-heat release, reacting for 2 hours, and cooling to 54 ℃;
3) mixing dimethylolpropionic acid (DMPA) with cross-linking agents of TMP, CHDM and BEPD and NMP, adding the mixture, wherein the temperature cannot be increased too fast, and reacting for 1 hour at 75 ℃;
4) adding a catalyst, and reacting for 2 hours at 65 ℃;
5) adding acetone while cooling, and cooling to 35 ℃;
6) discharging the prepolymer into a dispersing barrel, quickly adding DMEA, and dispersing at a high speed for 1 minute;
7) quickly adding triethylamine and ice pure water within 1 minute, and dispersing at high speed for 20 minutes;
8) and vacuumizing at 60 ℃ for desolventizing for 1 hour to obtain the waterborne polyurethane emulsion for the temperature-resistant transfer coating.
Example 2:
the waterborne polyurethane emulsion for the temperature-resistant transfer coating comprises the following components in parts by weight:
the preparation method of the aqueous polyurethane emulsion for the temperature-resistant transfer paint in the embodiment 2 comprises the following steps:
1) under the protection of dry nitrogen, dehydrating and vacuumizing polycarbonate diol (PCDL) at 105 ℃ for 1 hour, and cooling to 55 ℃;
2) adding H12MDI, heating to 86 ℃ from self-heat release, reacting for 2 hours, and cooling to 53 ℃;
3) mixing dimethylolpropionic acid (DMPA) with cross-linking agents of TMP, CHDM and BEPD and NMP, adding the mixture, wherein the temperature cannot be increased too fast, and reacting at 72 ℃ for 1 hour;
4) adding a catalyst, reacting at 63 ℃ for 2 hours,
5) Adding acetone while cooling, and cooling to 33 ℃;
6) discharging the prepolymer into a dispersing barrel, quickly adding a DMEA aqueous solution, and dispersing at a high speed for 1 minute;
7) quickly adding triethylamine and ice pure water within 1 minute, and dispersing at high speed for 20 minutes;
8) and vacuumizing at 58 ℃ for desolventizing for 1 hour to obtain the waterborne polyurethane emulsion for the temperature-resistant transfer coating.
Example 3:
the waterborne polyurethane emulsion for the temperature-resistant transfer coating comprises the following components in parts by weight:
the preparation method of the aqueous polyurethane emulsion for the temperature-resistant transfer paint in the embodiment 3 comprises the following steps:
1) under the protection of dry nitrogen, dehydrating neopentyl glycol adipic acid diol (PNA) at 108 ℃, vacuumizing for 1 hour, and cooling to 55 ℃;
2) adding H12MDI, heating to 85 ℃ from self-heat release, reacting for 2 hours, and cooling to 52 ℃;
3) mixing dimethylolpropionic acid (DMPA) with cross-linking agents of TMP, CHDM and BEPD and NMP, adding the mixture, wherein the temperature cannot be increased too fast, and reacting at 72 ℃ for 1 hour;
4) adding a catalyst, and reacting for 2 hours at 62 ℃;
5) adding acetone while cooling, and cooling to 32 ℃;
6) discharging the prepolymer into a dispersing barrel, quickly adding a DMEA aqueous solution, and dispersing at a high speed for 1 minute;
7) quickly adding triethylamine and ice pure water within 1 minute, and dispersing at high speed for 20 minutes;
8) and vacuumizing at 58 ℃ for desolventizing for 1 hour to obtain the waterborne polyurethane emulsion for the temperature-resistant transfer coating.
Example 4:
the waterborne polyurethane emulsion for the temperature-resistant transfer coating comprises the following components in parts by weight:
the preparation method of the aqueous polyurethane emulsion for the temperature-resistant transfer paint in the embodiment 4 comprises the following steps:
1) under the protection of dry nitrogen, dehydrating neopentyl glycol adipic acid diol (PNA) at 103 ℃, vacuumizing for 1 hour, and cooling to 52 ℃;
2) adding IPDI, heating to 84 ℃ from self-heat release, reacting for 2 hours, and cooling to 53 ℃;
3) mixing dimethylolpropionic acid (DMPA), a cross-linking agent of TMP1, CHDM and BEPD and NMP, adding the mixture, wherein the temperature cannot be increased too fast, and reacting for 1 hour at 71 ℃;
4) then adding a catalyst, and reacting for 2 hours at 62 ℃;
5) adding acetone while cooling, and cooling to 31 ℃;
6) discharging the prepolymer into a dispersing barrel, quickly adding a DMEA aqueous solution, and dispersing at a high speed for 1 minute;
7) and quickly adding triethylamine and ice pure water within 1 minute, and dispersing at a high speed for 20 minutes.
8) And vacuumizing at 59 ℃ for desolventizing for 1 hour to obtain the waterborne polyurethane emulsion for the temperature-resistant transfer coating.
Example 5:
the waterborne polyurethane emulsion for the temperature-resistant transfer coating comprises the following components in parts by weight:
the preparation method of the aqueous polyurethane emulsion for the temperature-resistant transfer paint in the embodiment 5 comprises the following steps:
1) under the protection of dry nitrogen, dehydrating and vacuumizing polytetrahydrofuran ether glycol (PTMG) at 100 ℃ for 1 hour, and cooling to 50 ℃;
2) adding H12MDI, heating to 83 ℃ from self-heat release, reacting for 2 hours, and cooling to 52 ℃;
3) mixing dimethylolbutyric acid with cross-linking agents of TMP, CHDM and BEPD and NMP, adding, and reacting at 70 ℃ for 1 hour, wherein the temperature can not be increased too fast;
4) adding a catalyst, and reacting for 2 hours at 60 ℃;
5) adding acetone while cooling, and cooling to 30 ℃;
6) discharging the prepolymer into a dispersing barrel, quickly adding a DMEA aqueous solution, and dispersing at a high speed for 1 minute;
7) quickly adding hexamethylene diamine and ice pure water within 1 minute, and dispersing at high speed for 20 minutes;
8) and vacuumizing at 57 ℃ for desolventizing for 1 hour to obtain the waterborne polyurethane emulsion for the temperature-resistant transfer coating.
The performance test of the waterborne polyurethane emulsion for the temperature-resistant transfer coating in the embodiment 1-5 after curing and film forming is shown in the following table 1:
1. the preparation process of the water-based temperature-resistant transfer coating comprises the following steps: 70 parts of waterborne polyurethane emulsion for temperature-resistant transfer coating are respectively taken and added into a glass with the volume of 150ml, then 27 parts of distilled water, 1 part of film forming additive, 1 part of wear-resisting agent and 0.6 part of wetting agent are added, 0.2 part of waterborne flatting agent (polyether modified organic silicon) and 0.2 part of waterborne defoaming agent are added, the mixture is stirred for 15-30 minutes at the rotating speed of 350-550 r/min until the system is uniform, a filter screen with 250 meshes is used for filtering, and the filtrate is poured into a black glue tank for later use.
2. And (3) curing and film forming processes: respectively coating the water-based temperature-resistant transfer coating on the front surfaces of the PET films by using a No. 2 scraper in numbers of 1, 2, 3, 4 and 5, setting the temperature of an oven at 105 ℃ and the humidity at 10%, respectively standing the films 1, 2, 3, 4 and 5 for 3 hours, and curing to form the film.
Table 1:
the results obtained from the above tests show that:
1) the waterborne polyurethane emulsion for the temperature-resistant transfer coating has good leveling property, easy stripping and high temperature resistance.
2) The waterborne polyurethane emulsion for the temperature-resistant transfer coating is a water dispersion system, has no adverse effect on human bodies and the environment, and meets the requirements of national and industrial environmental protection standards.
Claims (1)
1. A preparation method of waterborne polyurethane emulsion for temperature-resistant transfer paint is characterized by comprising the following steps:
1) under the protection of dry nitrogen, dehydrating and vacuumizing polycarbonate diol (PCDL) at 110 ℃ for 1 hour, and cooling to 60 ℃;
2) adding H12MDI, heating to 88 ℃ from self-heat release, reacting for 2 hours, and cooling to 54 ℃;
3) mixing dimethylolpropionic acid (DMPA) with cross-linking agents of TMP, CHDM and BEPD and NMP, adding the mixture, wherein the temperature cannot be increased too fast, and reacting for 1 hour at 75 ℃;
4) adding a catalyst, and reacting for 2 hours at 65 ℃;
5) adding acetone while cooling, and cooling to 35 ℃;
6) discharging the prepolymer into a dispersing barrel, quickly adding DMEA, and dispersing at a high speed for 1 minute;
7) quickly adding triethylamine and ice pure water within 1 minute, and dispersing at high speed for 20 minutes;
8) vacuumizing at 60 ℃ for desolventizing for 1 hour to obtain the waterborne polyurethane emulsion for the temperature-resistant transfer coating;
the preparation method comprises the following components in parts by weight:
7.4% of polycarbonate diol
H12MDI 12%
1.5% of dimethylolpropionic acid
TMP 1%
CHDM 0.8%
BEPD 0.2%
18 percent of acetone
NMP 2.7%
DMEA 4.1%
0.01 percent of stannous octoate
51.49 percent of ice pure water
And 0.8 percent of neutralizer.
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| CN201910677751.XA CN110358048B (en) | 2017-02-14 | 2017-02-14 | Preparation method of waterborne polyurethane emulsion for temperature-resistant transfer coating |
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| CN201710077579.5A CN106589310B (en) | 2017-02-14 | 2017-02-14 | A kind of heatproof transfer coatings aqueous polyurethane emulsion and preparation method thereof |
| CN201910677751.XA CN110358048B (en) | 2017-02-14 | 2017-02-14 | Preparation method of waterborne polyurethane emulsion for temperature-resistant transfer coating |
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| CN201910677750.5A Active CN110358047B (en) | 2017-02-14 | 2017-02-14 | Waterborne polyurethane coating for environment-friendly temperature-resistant transfer coating and preparation method thereof |
| CN201910677751.XA Active CN110358048B (en) | 2017-02-14 | 2017-02-14 | Preparation method of waterborne polyurethane emulsion for temperature-resistant transfer coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| DE3741538A1 (en) * | 1987-12-08 | 1989-06-22 | Bayer Ag | POLYURETHANE URBS |
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| WO1999060046A1 (en) * | 1998-12-30 | 1999-11-25 | Eastman Chemical Company | Gel resistant, hydrolytically stable polyester resins with high hydroxyl functionality and carboxylic acid functionality for isocyanate cross-linkable, waterborne coatings |
| JP4557517B2 (en) * | 2002-08-09 | 2010-10-06 | 三菱樹脂株式会社 | Release agent and release film |
| SE528577C2 (en) * | 2005-03-23 | 2006-12-19 | Perstorp Specialty Chem Ab | Waterborne polyurethane dispersion and its use |
| CN101760121A (en) * | 2009-12-14 | 2010-06-30 | 上海维凯化学品有限公司 | Temperature-resistance environmental-protection aqueous transfer coating and preparation method thereof |
| CN101948659B (en) * | 2010-09-17 | 2013-01-09 | 淄博奥德美高分子材料有限公司 | Aqueous polyurethane resin and preparation method thereof |
| CN102363708A (en) * | 2011-06-30 | 2012-02-29 | 上海乘鹰新材料有限公司 | Transferring and compounding dual-purpose coating for waterborne polyurethane, preparation method and application thereof |
| CN102719185B (en) * | 2012-06-27 | 2015-02-11 | 安徽灵达化工科技有限公司 | waterborne polyurethane laser transfer coating free of benzene and homolog and preparation method thereof |
| CN103173185B (en) * | 2013-04-07 | 2014-03-12 | 江苏华信塑业发展有限公司 | Preparation method of waterborne polyurethane adhesive for card matrix material |
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| CN103360934B (en) * | 2013-07-31 | 2016-04-13 | 常德市武陵金德镭射科技有限公司 | Mute silver-colored transfer coatings of a kind of water-based and preparation method thereof |
| JP6122368B2 (en) * | 2013-09-24 | 2017-04-26 | リンテック株式会社 | Release sheet and adhesive sheet |
| CN104311777A (en) * | 2014-09-28 | 2015-01-28 | 上海乘鹰新材料有限公司 | Low-stripping-force water-based polyurethane emulsion composition for transfer paints and preparation method thereof |
| CN104403544A (en) * | 2014-12-11 | 2015-03-11 | 广州慧谷化学有限公司 | Water-based heat transfer printing release coating, and preparation method and application thereof |
| CN104497743A (en) * | 2014-12-14 | 2015-04-08 | 安徽顺彤包装材料有限公司 | Environment-friendly waterborne transfer coating |
| CN104594119B (en) * | 2014-12-26 | 2016-12-07 | 上海乘鹰新材料有限公司 | A kind of direct vacuum aluminum-coated aqueous basecoat coating composition and preparation method thereof |
| CN105440244A (en) * | 2016-01-08 | 2016-03-30 | 广东邦固化学科技有限公司 | High-film-forming-property aqueous polyurethane resin as well as preparation method and use method of high-film-forming-property aqueous polyurethane resin |
| CN105542111A (en) * | 2016-01-29 | 2016-05-04 | 西安大天新材料有限公司 | High-temperature-resistant transfer aluminized waterborne polyurethane emulsion and preparation method thereof |
| CN106118428A (en) * | 2016-07-28 | 2016-11-16 | 上海乘鹰新材料有限公司 | A kind of waterproof scratch resistant aqueous polyurethane coating and preparation method thereof |
| CN106589310B (en) * | 2017-02-14 | 2019-09-06 | 广东博海化工科技有限公司 | A kind of heatproof transfer coatings aqueous polyurethane emulsion and preparation method thereof |
-
2017
- 2017-02-14 CN CN201710077579.5A patent/CN106589310B/en active Active
- 2017-02-14 CN CN201910677750.5A patent/CN110358047B/en active Active
- 2017-02-14 CN CN201910677751.XA patent/CN110358048B/en active Active
- 2017-02-14 CN CN201910677749.2A patent/CN110358046A/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| CN110358048A (en) | 2019-10-22 |
| CN110358047A (en) | 2019-10-22 |
| CN110358046A (en) | 2019-10-22 |
| CN106589310A (en) | 2017-04-26 |
| CN110358047B (en) | 2021-08-10 |
| CN106589310B (en) | 2019-09-06 |
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