CN102443135A - 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
- Publication number
- CN102443135A CN102443135A CN2011103357568A CN201110335756A CN102443135A CN 102443135 A CN102443135 A CN 102443135A CN 2011103357568 A CN2011103357568 A CN 2011103357568A CN 201110335756 A CN201110335756 A CN 201110335756A CN 102443135 A CN102443135 A CN 102443135A
- Authority
- CN
- China
- Prior art keywords
- solidifying agent
- low temperature
- deblocking
- preparation
- component solidifying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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 low temperature deblocking single-component solidifying agent, in particular to single component solidifying agent and preparation and application.
Background technology
Compare with other dip-coating, spraying watersoluble baking lacquer with traditional solvent based coating, low-temperature curing cathode electrophoresis coating has unrivaled meliority: 1. bake out temperature is low, the fuel saving expense.After adopting the low temperature curing type cathode electrophoresis dope, can make weight of coated paint reduce about 10%; The low-temperature curing baking, temperature reduces by 10%, can save energy 10%. Do not produce cigarette and tobacco tar when 2. drying.Alleviate the electrophoresis stoving oven and pollute, reduce discharge amount of exhaust gas, help environmental protection; 3. can not produce strain during large-scale workpiece such as application automobile chassis, reduce paint film and become, thereby improve film quality because of the look of baking; 4. can whole application plastics, rubber and steel plate assembled workpiece; But the 5. workpiece of wall thickness such as application foundry goods.Corrosion resistance coating can be good, and covering power is good, and the coating equipment level of automation is high, and utilization efficiency of coatings is high.Yet, obtain low temperature deblocking cathode electrodip painting, at first to prepare a kind of single-component solidifying agent of deblocking at low temperatures.
The invention discloses a kind of hexanolactam as the low temperature deblocking single-component solidifying agent that encapsulant sealing TDI obtains, have do soon, advantages such as high firmness, 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 low temperature deblocking single-component solidifying agent, the present invention adopts following technical scheme:
One aspect of the present invention relates to a kind of low temperature deblocking single-component solidifying agent, it is characterized in that it being as the end capped polymethyl benzene vulcabond of encapsulant with hexanolactam.
In a preferred implementation of the present invention, its characteristic obtains low temperature deblocking single-component solidifying agent of the present invention at the end capping that ethylene glycol monobutyl ether carries out the single component solidifying agent.
The invention still further relates to the preparation method of above-mentioned low temperature deblocking single-component solidifying agent, it is characterized in that comprising the steps: adding tolylene diisocyanate and catalyzer in (1) container, heating container and controlled temperature are between 50 ℃ to 55 ℃; (2) in container, add the mixing solutions that contains methyl alcohol, ethylene glycol monobutyl ether and hexanolactam; (3) add a certain amount of trihydroxy-propane in the reaction vessel.
In a preferred implementation of the present invention, it is characterized in that the catalyzer in the step (1) is a dibutyl tin laurate.
In a preferred implementation of the present invention, it is characterized in that the mixing solutions in the step (2) slowly is added drop-wise in the reaction vessel, in step (3), add after the TriMethylolPropane(TMP), reaction system is warmed up between 75-95 ℃ reacts.
In a preferred implementation of the present invention, it is characterized in that also comprising the step of judging the reaction performance with the content of Di-n-Butyl Amine method mensuration-NCO.
The invention still further relates to of the application of above-mentioned low temperature deblocking single-component solidifying agent as solidifying agent.
Description of drawings:
Fig. 1: the ir spectra of low temperature deblocking single-component solidifying agent;
Fig. 2: low temperature deblocking single-component solidifying agent deblocking temperature and thermogravimetric analysis thereof.
Embodiment
Embodiment 1:
1.1 raw material
Preparation process
(1) in the 250ml there-necked flask of TM, whisking appliance, prolong is housed, add tolylene diisocyanate (TDI) and a spot of catalyzer dibutyl tin laurate, there-necked flask is placed in the constant temperature water bath, temperature is controlled between 50 ℃ to 55 ℃;
(2) under 50 ℃ to 55 ℃, in there-necked flask, slowly drip the mixing solutions of anhydrous methanol, ethylene glycol monobutyl ether, hexanolactam, drip in 30 minutes. be warmed up to 60 ℃ and be incubated 3 hours.
In there-necked flask, add quantitative TriMethylolPropane(TMP) after (3) 3 hours, be warming up to 80 ℃ and be incubated 2 hours. with the content of Di-n-Butyl Amine method mensuration-NCO, reach the requirement cooling discharge.
2. discussion of results
2.1 Di-n-Butyl Amine method survey-NCO content delta data in time sees 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 |
The masked isocyanate solidifying agent is elevated to certain temperature, and the encapsulant small molecules splits away off from macromole, produces weightlessness, discharges-the NCO group.The isocyanate curing agent of above-mentioned encapsulant sealing has been carried out thermogravimetric analysis, and the deblocking temperature that draws conforms to IR spectroscopy.Wherein accompanying drawing 2 is seen in the thermogravimetric analysis of ethylene glycol monobutyl ether blocked isocyanate curing agent, can be known when temperature reaches 130 ℃ the small molecules fracture by accompanying drawing 2.So the deblocking temperature of ethylene glycol monobutyl ether blocked isocyanate curing agent is 130 ℃
Through the ir spectra shown in the accompanying drawing 1, its initial deblocking temperature that shows solidifying agent is 105 ℃, and when best deblocking temperature was 130 ℃, the deblocking time was 20min.
When being understood that, concerning those of ordinary skills, can improve or conversion, and all these improvement and conversion all should belong to the protection domain of accompanying claims of the present invention according to above-mentioned explanation.
Claims (7)
1. low temperature deblocking single-component solidifying agent is characterized in that it being as the end capped polymethyl benzene vulcabond of encapsulant with hexanolactam.
2. low temperature deblocking single-component solidifying agent according to claim 1 is characterized in that with the ethylene glycol monobutyl ether being the end capping that solvent carries out the single component solidifying agent.
3. the preparation method of low temperature deblocking single-component solidifying agent according to claim 2 is characterized in that comprising the steps: adding tolylene diisocyanate and catalyzer in (1) container, and heating container and controlled temperature are between 50 ℃ to 55 ℃; (2) in container, add the mixing solutions that contains methyl alcohol, ethylene glycol monobutyl ether and hexanolactam; (3) add a certain amount of trihydroxy-propane in the reaction vessel.
4. preparation method according to claim 3 is characterized in that the catalyzer in the step (1) is a dibutyl tin laurate.
5. preparation method according to claim 3 is characterized in that the mixing solutions in the step (2) slowly is added drop-wise in the reaction vessel, in step (3), adds after the TriMethylolPropane(TMP), reaction system is warmed up between 75-95 ℃ reacts.
6. preparation method according to claim 3 is characterized in that also comprising the step of judging the reaction performance with the content of Di-n-Butyl Amine method mensuration-NCO.
7. low temperature deblocking single-component solidifying agent according to claim 1 and 2 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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102443135A true CN102443135A (en) | 2012-05-09 |
| CN102443135B CN102443135B (en) | 2014-05-07 |
Family
ID=46006103
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110335756.8A Expired - Fee Related CN102443135B (en) | 2011-10-31 | 2011-10-31 | Single-component curing agent capable of being deblocked at low temperature |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102443135B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437408A (en) * | 2019-07-19 | 2019-11-12 | 中国石油集团川庆钻探工程有限公司 | High temperature excitated type oil base drilling fluid curing agent and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030060541A1 (en) * | 2001-03-28 | 2003-03-27 | Yoshio Kojima | Lead-free cationic electrodeposition coating composition, electrodeposition coating process, and process for forming double layered coated film |
| 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 |
-
2011
- 2011-10-31 CN CN201110335756.8A patent/CN102443135B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030060541A1 (en) * | 2001-03-28 | 2003-03-27 | Yoshio Kojima | Lead-free cationic electrodeposition coating composition, electrodeposition coating process, and process for forming double layered coated film |
| 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 (3)
| Title |
|---|
| 付荣兴等: "《封端化TMP－TDI型反应物的研究》", 《江苏化工》 * |
| 余新利等: "《阴极电泳涂料用新型交联剂的制备》", 《涂料工业》 * |
| 陈龙等: "《封端型多异氰酸酯加成物的合成》", 《聚氨酯工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437408A (en) * | 2019-07-19 | 2019-11-12 | 中国石油集团川庆钻探工程有限公司 | High temperature excitated type oil base drilling fluid curing agent and preparation method thereof |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102443135B (en) | 2014-05-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101602854B (en) | Polyamide epoxy hardener and preparation method thereof | |
| CN103305110B (en) | A kind of low-temperature curing cathode electrophoresis coating and preparation method thereof | |
| CN113956756B (en) | Quaternary ammonium salt antibacterial anticorrosive paint, preparation method, coating preparation method and application | |
| CN105820320A (en) | Alkyd resin for woodware primer and synthesis method of alkyd resin | |
| CN104861821A (en) | Anticorrosive heat dissipation coating and production method thereof | |
| CN107987298B (en) | Flame-retardant electric vehicle plastic shell | |
| CN108250904B (en) | Epoxy storage tank coating, coating matching system and application thereof | |
| CN105482757A (en) | High-strength multifunctional polyurea adhesive and preparation method thereof | |
| CN112011250A (en) | Low-temperature fast-curing environment-friendly insulating coating for non-oriented electrical steel | |
| CN111073459A (en) | Energy-saving and environment-friendly cathode electrophoretic coating | |
| CN110396178A (en) | A kind of large arch dam water paint curing agent | |
| CN102443135B (en) | Single-component curing agent capable of being deblocked at low temperature | |
| WO2013099750A1 (en) | Electrodeposition coating composition, and dissociation catalyst therefor | |
| CN105244455A (en) | Anti-corrosion protective film for soft package lithium battery and preparation method and application thereof | |
| CN106752934B (en) | Fluorubber-silicon rubber interpenetrating polymer network anticorrosion paint and preparation method thereof | |
| CN110804364B (en) | Preparation method of high throwing power emulsion | |
| CN112375208A (en) | High-throwing-power toughened cathode electrophoresis resin and preparation method thereof, and electrophoresis emulsion and preparation method thereof | |
| CN105907283A (en) | Process for producing high-polymer explosion-proof paint | |
| CN105368260A (en) | Permeable epoxy seal primer and preparing method and using method thereof | |
| CN202142548U (en) | Installation support of single/dual-axis tracking system of solar photovoltaic plate | |
| CN112094540B (en) | Special rubber protective primer | |
| CN111393683B (en) | Modified cationic microgel and preparation method and application thereof | |
| CN103483934A (en) | Low-cost anticorrosive antirust primer and preparation method thereof | |
| CN103131219A (en) | Glasses frame coating and preparation method thereof | |
| CN114686072B (en) | Preparation method of epoxy tree composition for high-temperature-resistant anti-corrosion coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140507 Termination date: 20151031 |
|
| EXPY | Termination of patent right or utility model |