CN102443135B - Single-component curing agent capable of being deblocked at low temperature - Google Patents
Single-component curing agent capable of being deblocked at low temperature Download PDFInfo
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- CN102443135B CN102443135B CN201110335756.8A CN201110335756A CN102443135B CN 102443135 B CN102443135 B CN 102443135B CN 201110335756 A CN201110335756 A CN 201110335756A CN 102443135 B CN102443135 B CN 102443135B
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- curing agent
- deblocked
- component curing
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Abstract
The invention discloses a single-component curing agent capable of being deblocked at a low temperature, which is obtained by sealing TDI (Toluene Diisocyanate) with caprolactam as a sealant. The single-component curing agent has the advantages of rapidness in drying, high hardness, strong adhesivity and the like, the compatibility of the single-component curing agent with hydroxy resins is improved and the use range of the single-component curing agent is expanded.
Description
Technical field
The present invention relates to a kind of single-component curing agent capable of being deblocked at low temperature, in particular to single component solidifying agent and preparation and application.
Background technology
Compare with other dip-coating, spraying watersoluble baking paint with traditional solvent based coating, low-temperature curing cathode electrophoresis coating has unrivaled superiority: 1. bake out temperature is low, fuel saving expense.Adopt after low temperature curing type cathode electrophoresis dope, can make weight of coated paint reduce approximately 10%; Low-temperature curing baking, temperature reduces by 10%, can save energy 10%.; While 2. drying, do not produce cigarette and tobacco tar.Alleviate electrophoresis stoving oven and pollute, reduce discharge amount of exhaust gas, be conducive to environmental protection; 3. can not produce strain during the large-scale workpiece such as application automobile chassis, reduce paint film and become because of the look of baking, thereby improve film quality; 4. can whole application plastics, rubber and steel plate assembled workpiece; 5. can application foundry goods etc. the workpiece of wall thickness.Corrosion resistance coating can be good, and covering power is good, and coating equipment level of automation is high, and utilization efficiency of coatings is high.Yet, obtain low temperature deblocking cathode electrodip painting, first to prepare a kind of single-component solidifying agent of deblocking at low temperatures.
The invention discloses the single-component curing agent capable of being deblocked at low temperature that a kind of hexanolactam obtains as encapsulant blocked TDI, there is the advantages such as quick-drying, high rigidity, strong adhesion, and can improve the consistency of itself and hydroxy resin, expand its use range.
Summary of the invention
For can obtain can be compatible with hydroxyl numerical value single-component curing agent capable of being deblocked at low temperature, the present invention adopts following technical scheme:
One aspect of the present invention relates to a kind of single-component curing agent capable of being deblocked at low temperature, it is characterized in that usining the polymethyl benzene vulcabond of hexanolactam as encapsulant end-blocking.
In a preferred embodiment of the present invention, the end capping that its feature is carried out single component solidifying agent at ethylene glycol monobutyl ether obtains single-component curing agent capable of being deblocked at low temperature of the present invention.
The invention still further relates to the preparation method of above-mentioned single-component curing agent capable of being deblocked at low temperature, it is characterized in that comprising the steps: adding tolylene diisocyanate and catalyzer in (1) container, heating container is also controlled temperature between 50 ℃ to 55 ℃; (2) in container, add the mixing solutions that contains methyl alcohol, ethylene glycol monobutyl ether and hexanolactam; (3) in reaction vessel, add a certain amount of Glycerin.
In a preferred embodiment of the present invention, it is characterized in that the catalyzer in step (1) is dibutyl tin laurate.
In a preferred embodiment of the present invention, it is characterized in that the mixing solutions in step (2) is slowly added drop-wise in reaction vessel, add TriMethylolPropane(TMP) in step (3) after, reaction system is warmed up between 75-95 ℃ and is reacted.
In a preferred embodiment of the present invention, characterized by further comprising the step that judges reaction performance with the content of Di-n-Butyl Amine method mensuration-NCO.
The invention still further relates to above-mentioned single-component curing agent capable of being deblocked at low temperature as the application of solidifying agent.
Accompanying drawing explanation:
Fig. 1: the infrared spectra of single-component curing agent capable of being deblocked at low temperature;
Fig. 2: single-component curing agent capable of being deblocked at low temperature deblocking temperature and thermogravimetric analysis thereof.
Embodiment
Embodiment 1:
1.1 raw material
Preparation process
(1) in being housed, the 250ml there-necked flask of thermometer, agitator, prolong adds tolylene diisocyanate (TDI) and a small amount of catalyzer dibutyl tin laurate, there-necked flask is placed in constant temperature water bath, and temperature is controlled between 50 ℃ to 55 ℃;
(2) at 50 ℃ to 55 ℃ to slowly dripping the mixing solutions of anhydrous methanol, ethylene glycol monobutyl ether, hexanolactam in there-necked flask, in 30 minutes, drip. be warmed up to 60 ℃ and be incubated 3 hours.
In (3) 3 hours backward there-necked flasks, adding quantitative TriMethylolPropane(TMP), be warming up to 80 ℃ and be incubated 2 hours. the content with Di-n-Butyl Amine method mensuration-NCO, reaches requirement cooling discharge.
2. discussion of results
2.1 Di-n-Butyl Amine method survey-NCO content temporal evolution data see the following form
| Time/h | 0.5 | 1.0 | 1.5 | 2.0 | 2.5 |
| -NCO content/% | 68.2 | 31.0 | 14.9 | 7.4 | 2.1 |
Blocked Isocyanate Curing Agents is elevated to certain temperature, and encapsulant small molecules splits away off from macromole, produces weightlessness, discharge-NCO group.The isocyanate curing agent of above-mentioned encapsulant sealing has been carried out to thermogravimetric analysis, and the deblocking temperature drawing conforms to Infrared spectroscopy.Wherein accompanying drawing 2 is shown in the thermogravimetric analysis of ethylene glycol monobutyl ether blocked isocyanate curing agent, known when temperature reaches 130 ℃ by accompanying drawing 2, small molecules fracture.Therefore the deblocking temperature of ethylene glycol monobutyl ether blocked isocyanate curing agent is 130 ℃
By the infrared spectra shown in accompanying drawing 1, its initial deblocking temperature that shows solidifying agent is 105 ℃, and when best deblocking temperature is 130 ℃, the deblocking time is 20min.
When understanding, for those of ordinary skills, can be improved according to the above description or convert, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (5)
1. a preparation method for single-component curing agent capable of being deblocked at low temperature, is characterized in that comprising the steps: adding tolylene diisocyanate and catalyzer in (1) container, and heating container is also controlled temperature between 50 ℃ to 55 ℃; (2) in container, add the mixing solutions that contains methyl alcohol, ethylene glycol monobutyl ether and hexanolactam; (3) in reaction vessel, add a certain amount of Glycerin.
2. preparation method according to claim 1, is characterized in that the catalyzer in step (1) is dibutyl tin laurate.
3. preparation method according to claim 1, is characterized in that the mixing solutions in step (2) is slowly added drop-wise in reaction vessel, after adding TriMethylolPropane(TMP), reaction system is warmed up between 75-95 ℃ and is reacted in step (3).
4. preparation method according to claim 1, characterized by further comprising the step that judges reaction performance with the content of Di-n-Butyl Amine method mensuration-NCO.
5. the single-component curing agent capable of being deblocked at low temperature that according to claim 1 prepared by method is as the application of solidifying agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110335756.8A CN102443135B (en) | 2011-10-31 | 2011-10-31 | Single-component curing agent capable of being deblocked at low temperature |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110335756.8A CN102443135B (en) | 2011-10-31 | 2011-10-31 | Single-component curing agent capable of being deblocked at low temperature |
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| Publication Number | Publication Date |
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| CN102443135A CN102443135A (en) | 2012-05-09 |
| CN102443135B true CN102443135B (en) | 2014-05-07 |
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Families Citing this family (1)
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| CN110437408B (en) * | 2019-07-19 | 2021-07-23 | 中国石油集团川庆钻探工程有限公司 | Curing agent for high-temperature excitation type oil-based drilling fluid and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1665793A (en) * | 2002-04-30 | 2005-09-07 | 拜尔材料科学股份公司 | Ionic liquids |
| CN1675004A (en) * | 2002-08-13 | 2005-09-28 | 阿克佐诺贝尔国际涂料股份有限公司 | Multilayer coating system comprising thiol-functional compounds |
| CN1865328A (en) * | 2006-04-27 | 2006-11-22 | 中国科学院广州化学研究所 | Water dispersible end capping diisocyanate cross-linking agent and its preparation method |
| TWI289599B (en) * | 2004-02-12 | 2007-11-11 | Jintex Corp Ltd | Solvent base fluorine water-repellent and oil-repellent agent and manufacturing method thereof |
| CN101619128A (en) * | 2009-07-31 | 2010-01-06 | 中国科学院广州化学研究所 | Amido end-blocking non-ionic water-based isocyanate, preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020077156A (en) * | 2001-03-28 | 2002-10-11 | 닛본 페인트 가부시끼가이샤 | Lead-free cataionic electrodeposition coating composition, electrodeposition coating process, and process for forming double layered coated film |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1665793A (en) * | 2002-04-30 | 2005-09-07 | 拜尔材料科学股份公司 | Ionic liquids |
| CN1675004A (en) * | 2002-08-13 | 2005-09-28 | 阿克佐诺贝尔国际涂料股份有限公司 | Multilayer coating system comprising thiol-functional compounds |
| TWI289599B (en) * | 2004-02-12 | 2007-11-11 | Jintex Corp Ltd | Solvent base fluorine water-repellent and oil-repellent agent and manufacturing method thereof |
| CN1865328A (en) * | 2006-04-27 | 2006-11-22 | 中国科学院广州化学研究所 | Water dispersible end capping diisocyanate cross-linking agent and its preparation method |
| CN101619128A (en) * | 2009-07-31 | 2010-01-06 | 中国科学院广州化学研究所 | Amido end-blocking non-ionic water-based isocyanate, preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《阴极电泳涂料用新型交联剂的制备》;余新利等;《涂料工业》;20020731;第23－24页 * |
| 余新利等.《阴极电泳涂料用新型交联剂的制备》.《涂料工业》.2002, |
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