CN112500551B - PU curing agent and preparation method thereof - Google Patents
PU curing agent and preparation method thereof Download PDFInfo
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- CN112500551B CN112500551B CN202011289388.3A CN202011289388A CN112500551B CN 112500551 B CN112500551 B CN 112500551B CN 202011289388 A CN202011289388 A CN 202011289388A CN 112500551 B CN112500551 B CN 112500551B
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- Prior art keywords
- curing agent
- stirring
- drier
- water absorbent
- hexamethylene diisocyanate
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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
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/791—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups
- C08G18/792—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups formed by oligomerisation of aliphatic and/or cycloaliphatic isocyanates or isothiocyanates
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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
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a PU curing agent, and relates to the technical field of curing agents. The PU curing agent comprises hexamethylene diisocyanate tripolymer, isophorone diisocyanate tripolymer, drier, butyl acetate, water absorbent and dehydrating agent. The conventional PU finishing paint is matched with the PU curing agent, so that the drying speed is high, the defect that the reaction rate of the conventional PU finishing paint curing agent is low at low temperature can be overcome, the drying speed can be increased by 50 percent, the construction efficiency of the coating can be effectively improved, and the hardness of a prepared paint film is also high.
Description
Technical Field
The invention relates to the technical field of curing agents, and particularly relates to a PU curing agent and a preparation method thereof.
Background
Polyurethane has good physical and chemical properties and mechanical properties, and is widely used in various fields. However, the isocyanate curing agent used in the current market has insufficient stability and slow drying speed, and particularly, the reaction rate is too slow at low temperature, so that the construction efficiency is seriously influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the PU curing agent which can be dried quickly, has higher hardness and is environment-friendly and the preparation method thereof.
In order to realize the purpose, the technical scheme adopted by the invention is as follows: the PU curing agent is characterized by comprising hexamethylene diisocyanate tripolymer, isophorone diisocyanate tripolymer, drier, butyl acetate, water absorbent and dehydrating agent.
Preferably, the drier is dibutyltin dilaurate, the dehydrating agent is p-toluenesulfonyl isocyanate, and the water absorbent is triethyl orthoformate.
Preferably, the PU curing agent comprises the following components in percentage by mass: 50-60% of hexamethylene diisocyanate tripolymer, 30-40% of isophorone diisocyanate tripolymer, 0.1-1% of drier, 5-10% of butyl acetate, 0.15-0.25% of dehydrating agent and 0.05-0.15% of water absorbent.
Preferably, the PU curing agent comprises the following components in percentage by mass: 50% of hexamethylene diisocyanate tripolymer, 40% of isophorone diisocyanate tripolymer, 0.5% of drier, 9.2% of butyl acetate, 0.2% of dehydrating agent and 0.1% of water absorbent.
Meanwhile, the invention also discloses a preparation method of the PU curing agent, which comprises the following steps:
(1) filling nitrogen or inert gas into the material cylinder (continuously filling nitrogen or inert gas in the whole charging process);
(2) adding butyl acetate into a material cylinder filled with nitrogen or inert gas, stirring and adding a dehydrating agent;
(3) quality inspection: ensuring that the water content is less than or equal to 450ppm (when the water content does not meet the requirement, adding a dehydrating agent, stirring for 5min, and detecting the water content again);
(4) after the water content is qualified, adding hexamethylene diisocyanate tripolymer and isophorone diisocyanate tripolymer and stirring;
(5) adding a water absorbent and stirring;
(6) adding a drier, and stirring to obtain the PU curing agent.
Preferably, the nitrogen or the inert gas is continuously filled into the material cylinder in the whole feeding process, and the flow rate of the gas is 140-160 mL/min.
Preferably, the stirring speed in the steps (2) and (4) - (6) is 45-55 rpm, the stirring time after the dehydrating agent is added in the step (2) is 4-6 min, the stirring time in the step (5) is 4-6 min, and the stirring time in the step (6) is 14-16 min.
Compared with the prior art, the invention has the beneficial effects that:
1) the materials of hexamethylene diisocyanate tripolymer and isophorone diisocyanate tripolymer are selected, and the drying speed is high. The conventional PU finishing paint is matched with the PU curing agent, so that the drying speed is high, particularly, the defect that the reaction rate of the conventional PU finishing paint curing agent is low at low temperature is overcome in a low-temperature environment, the drying rate is increased by 50 percent, and the construction efficiency of the paint can be effectively improved.
2) The composite material of hexamethylene diisocyanate trimer and isophorone diisocyanate trimer and the conventional PU finishing paint have high reaction crosslinking density, compared with the conventional PU curing agent, the hardness of the paint film is obviously improved, and the HB of the paint film of the conventional PU curing agent is improved to 3H.
3) The proper metal drier is selected, the reaction rate of PU in a low-temperature environment is improved, and the condition that gel appears in the storage process of adding the traditional hexamethylene diisocyanate curing agent into the metal drier is also improved.
4) Nitrogen is filled in the whole production process, so that no moisture exists in a production cylinder, a dehydrating agent and a water absorbent are added, the moisture of a solvent is ensured to be in a qualified range, and the condition that the curing agent resin is not reacted with water in the storage process to cause gel is also ensured.
5) The solid content of the PU curing agent prepared by the invention is 73 percent, the content of Volatile Organic Compounds (VOC) is less than or equal to 300g/L, the VOC content is low, and the PU curing agent meets the requirement of environmental protection.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Hexamethylene Diisocyanate (HDI) tripolymer used in the experiment is Corsika 3300 and Corsika 3790; isophorone diisocyanate (IPDI) trimer is Corsai 4470, dehydrating agent is p-toluenesulfonyl isocyanate of OMGB Borchers GmbH, and water absorbent is triethyl orthoformate of OMG.
Example 1
In an embodiment of the PU curing agent of the present invention, the preparation method of the PU curing agent of the present embodiment includes the following steps:
(1) filling nitrogen into the material cylinder (the nitrogen is continuously filled in the whole feeding process, and the flow rate of the nitrogen is 150 mL/min);
(2) adding butyl acetate into a material cylinder filled with nitrogen, stirring, adding a dehydrating agent, and stirring at 50rpm for 5 min;
(3) quality inspection: ensuring that the water content is less than or equal to 450ppm (when the water content does not meet the requirement, adding a dehydrating agent, stirring for 5min, and detecting the water content again);
(4) after the water content is qualified, adding polyisocyanate trimer and stirring at the rotating speed of 50 rpm;
(5) adding water absorbent, and stirring at 50rpm for 5 min;
(6) adding a drier, and stirring at the rotating speed of 50rpm for 15min to obtain the PU curing agent.
The formulation of the PU curing agent described in this example is shown in Table 1.
Examples 2 to 4
Examples 2 to 4 are all the PU curing agents of the present invention, the preparation methods are the same as in example 1, and the formulations are shown in Table 1.
Comparative examples 1 to 5
The PU curing agent prepared according to the formulation different from the present invention was prepared in the same manner as in example 1, and the formulation thereof is shown in Table 1.
TABLE 1 formulation of PU curing agent (% by mass)
The PU curing agents prepared in examples 1-4 and comparative examples 2-5 were subjected to performance tests, and the test results of examples 1-4 are shown in Table 2, and the test results of comparative examples 1-5 are shown in Table 3.
DOI is the numerical value of the distinctness of image of the paint film;
the glossiness is tested according to GB/T9754, and the testing angle is 60 degrees;
testing the water resistance by referring to GB/T5209;
the color difference was evaluated with reference to GB/T1766.
TABLE 2 Performance test results of examples 1 to 4
TABLE 3 Performance test results for comparative examples 1-5
As can be seen from Table 2, the hardness of the paint film pencil prepared from the PU curing agent of example 2 of the present invention can exceed that of the imported curing agent Acksolcis 720 curing agent, the surface drying time and the polishing time are shorter than those of the imported curing agent, and other properties are equivalent to those of the imported curing agent. As can be seen from the comparison between tables 2 and 3, the PU curing agent prepared by the formula disclosed by the invention has faster drying time when being used with PU finishing paint, and the pencil hardness of a paint film can be improved from the traditional H to 3H.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The PU curing agent is characterized by comprising the following components in percentage by mass: 50-60% of hexamethylene diisocyanate tripolymer, 30-40% of isophorone diisocyanate tripolymer, 0.1-1% of drier, 5-10% of butyl acetate, 0.15-0.25% of dehydrating agent and 0.05-0.15% of water absorbent; the drier is dibutyltin dilaurate, the dehydrating agent is p-toluenesulfonyl isocyanate, and the water absorbent is triethyl orthoformate; the hexamethylene diisocyanate trimer is kesichun 3790; the isophorone diisocyanate trimer is Coximato 4470.
2. The PU curing agent according to claim 1, wherein the PU curing agent comprises the following components in percentage by mass: 50% of hexamethylene diisocyanate trimer, 40% of isophorone diisocyanate trimer, 0.5% of drier, 9.2% of butyl acetate, 0.2% of dehydrating agent and 0.1% of water absorbent.
3. The method for preparing the PU curing agent according to any one of claims 1 to 2, comprising the steps of:
(1) filling nitrogen or inert gas into the material cylinder;
(2) adding butyl acetate into a material cylinder filled with nitrogen or inert gas, stirring and adding a dehydrating agent;
(3) quality inspection: ensuring that the water content is less than or equal to 450 ppm;
(4) after the water content is qualified, adding hexamethylene diisocyanate tripolymer and isophorone diisocyanate tripolymer and stirring;
(5) adding a water absorbent and stirring;
(6) and adding a drier, and stirring to obtain the PU curing agent.
4. The method for preparing PU curing agent according to claim 3, wherein the nitrogen or inert gas is continuously filled into the material cylinder during the whole feeding process, and the flow rate of the gas is 140-160 mL/min.
5. The method for preparing the PU curing agent according to claim 3, wherein in the step (2), the mixture is stirred at a rotation speed of 45-55 rpm, and the stirring is continued for 4-6 min after the dehydrating agent is added.
6. The method of claim 3, wherein in the step (4), the stirring is performed at a rotation speed of 45 to 55 rpm.
7. The method of claim 3, wherein in the step (5), the mixture is stirred at 45 to 55rpm for 4 to 6 minutes.
8. The method of claim 3, wherein the stirring time in step (6) is 14-16 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011289388.3A CN112500551B (en) | 2020-11-17 | 2020-11-17 | PU curing agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011289388.3A CN112500551B (en) | 2020-11-17 | 2020-11-17 | PU curing agent and preparation method thereof |
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| Publication Number | Publication Date |
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| CN112500551A CN112500551A (en) | 2021-03-16 |
| CN112500551B true CN112500551B (en) | 2022-07-12 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239987A (en) * | 2008-01-23 | 2008-08-13 | 湖北德邦化工新材料有限公司 | Siloxane modifying polyisocyanate trimer curing agent containing sulphydryl or hydroxyl |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101469248B (en) * | 2007-12-30 | 2012-01-25 | 比亚迪股份有限公司 | Bicomponent polyurethane coating and preparation thereof |
| CN101792639B (en) * | 2010-04-02 | 2012-09-05 | 德莱特恩环保涂料(北京)有限公司 | Wear-resisting scratch-resisting weather-proof polyurethane coating and preparation method thereof |
| US8859710B2 (en) * | 2013-03-15 | 2014-10-14 | Jones-Blair Company | Polysiloxane modified polyisocyanates for use in coatings |
| KR102095020B1 (en) * | 2019-08-21 | 2020-03-30 | 주식회사 정석케미칼 | 2-component polyurea resin composition excellent in durability and visibility for a road marking and method for a road marking using the same |
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- 2020-11-17 CN CN202011289388.3A patent/CN112500551B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239987A (en) * | 2008-01-23 | 2008-08-13 | 湖北德邦化工新材料有限公司 | Siloxane modifying polyisocyanate trimer curing agent containing sulphydryl or hydroxyl |
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