News Details
Polythiol coating crosslinking agent
2017-7-13 19:23:15
Polythiol coating crosslinking agent
The application development and performance of epoxy resin depend on the development of new crosslinking agent. With 2, 2-2 thiol sulfur ethyl ether (MES) and trimethylolpropane acrylate (TMPTA) as raw materials, polymerization step by step is the preparation with multiple branched structure and the thiol, and studied the poly mercaptan kind of crosslinking agent and the room temperature of epoxy resin crosslinking process.
The sulfhydryl value, branching degree and molecular weight of polythiol crosslinking agent were determined by magnetic resonance spectroscopy (1HNMR) and gel permeation chromatography (GPC). Using real-time infrared (rt-ir), the crosslinking process of polysulfide/epoxy resin was studied, and the thermal stability of the crosslinked products was characterized by thermal weightloss analysis (TGA).
Results show that the poly mercaptan kind of crosslinking agent crosslinking system compared with the traditional amine room temperature crosslinking system, obviously improve the speed before crosslinking, 80 min of thiol and epoxy conversion rate can reach 48% and 36% respectively, and the thermal stability increased slightly, the initial decomposition temperature of 322 degrees Celsius.
Epoxy resin has good stability, low cross - linking rate, high mechanical strength and fine processing technology. Therefore, it is widely used in various fields of national economy.
The commonly used crosslinking agents of epoxy resin are amines, anhydride and mimidazolines, and their research is also more in-depth. At room temperature and low temperature crosslinking areas, however, mercaptan kind of crosslinking agent has unique advantages, not only crosslinking speed, but also because of the existence of flexible chain segment and high sulfur refractive index, and transparency in toughening resin resin has great application value.
Chinese name: Diethyl toluene diamine(DETDA)
Diethyltoluenediamine Raw material ：
TDA industrial, Sichuan production
Ethylene (Et) polymer grade, Shanghai production
TEA industrial imports
The application development and performance of epoxy resin depend on the development of new crosslinking agent. With 2, 2-2 thiol sulfur ethyl ether (MES) and trimethylolpropane acrylate (TMPTA) as raw materials, polymerization step by step is the preparation with multiple branched structure and the thiol, and studied the poly mercaptan kind of crosslinking agent and the room temperature of epoxy resin crosslinking process.
The sulfhydryl value, branching degree and molecular weight of polythiol crosslinking agent were determined by magnetic resonance spectroscopy (1HNMR) and gel permeation chromatography (GPC). Using real-time infrared (rt-ir), the crosslinking process of polysulfide/epoxy resin was studied, and the thermal stability of the crosslinked products was characterized by thermal weightloss analysis (TGA).
Results show that the poly mercaptan kind of crosslinking agent crosslinking system compared with the traditional amine room temperature crosslinking system, obviously improve the speed before crosslinking, 80 min of thiol and epoxy conversion rate can reach 48% and 36% respectively, and the thermal stability increased slightly, the initial decomposition temperature of 322 degrees Celsius.
Epoxy resin has good stability, low cross - linking rate, high mechanical strength and fine processing technology. Therefore, it is widely used in various fields of national economy.
The commonly used crosslinking agents of epoxy resin are amines, anhydride and mimidazolines, and their research is also more in-depth. At room temperature and low temperature crosslinking areas, however, mercaptan kind of crosslinking agent has unique advantages, not only crosslinking speed, but also because of the existence of flexible chain segment and high sulfur refractive index, and transparency in toughening resin resin has great application value.
Chinese name: Diethyl toluene diamine(DETDA)Diethyltoluenediamine Raw material ：
TDA industrial, Sichuan production
Ethylene (Et) polymer grade, Shanghai production
TEA industrial imports
A reagent grade additives
In this paper, the polythiol crosslinking agent with multi-branched structure was synthesized by simple experiment device and operation method using 2, 2-disulfyl ethyl sulfide (MES) and trimethyl-propane trimethacrylate (TMPTA). In this paper, the temperature of the crosslinking agent with the epoxy resin e-51 was tracked by the real-time infrared (rt-ir) method, and the thermal performance of the crosslinking product was characterized by thermal loss (TGA).
Experimental raw materials: 2, 2-disulfyl ethyl sulfide (MES) : 98% purity; Trimethyl-propane triacrylate (TMPTA); Bisphenol A type epoxy resin: e-51; Triethylamine (Et3N) : analytical pure.
As the reaction progresses, the strength of the epoxy base at the sulfhydryl peak and 916cm-1 at 2561cm-1 is decreasing, while the intensity of hydroxyl peaks at 3500cm-1 is increasing. Thiol functional groups and epoxy functional groups according to the formula (3) the conversion calculation: (t) = 1 - A (t) (I)/(O) iA A 2966 / A (t) (O), 2966 (3), A for absorbance, the peak A point method to determine in the Supreme Court: A = log101T, namely by the transmittance of t wave number analysis on directly determine.
The conversion rate of the functional groups at the time of t is related to the absorption of a (t) with its infrared signature absorption peak at 2966cm-1.
The conversion rate of sulfhydryl and epoxies at different moments in polymercaptan/e-51 crosslinking system. The conversion rate of the reaction in an s-shaped type: the top 50 min, although the concentration of thiol and epoxide group is the largest, but the response is slow, this may be due to the polymerization system contains the function of material, so the conversion rate is small (10%) did not meet; As the reaction was carried out, the resistance was consumed, and the reaction rate was significantly accelerated after 50min, and the conversion rate of sulfhydryl and epoxy group increased rapidly in 30min, reaching the maximum value. After 80 min, along with the increase of the system viscosity of polymer chain segment decreased activity, thiol and epoxy group of contact decreases, and the reaction rate is slow again, to terminate the infrared tracking thiol conversion rate of 48%, the epoxy group is 36%.
This indicates that the polythiol/e-51 crosslinking system should have a post-crosslinking process so that the reaction groups can fully respond and form highly crosslinked thermosetting resins. Compared with the traditional fatty polyamines, such as triethylene tetramine (TETA), the anterior crosslinking speed of the crosslinking system is significantly faster than the cross-linking time of the 4-d + 100-30min.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
In this paper, the polythiol crosslinking agent with multi-branched structure was synthesized by simple experiment device and operation method using 2, 2-disulfyl ethyl sulfide (MES) and trimethyl-propane trimethacrylate (TMPTA). In this paper, the temperature of the crosslinking agent with the epoxy resin e-51 was tracked by the real-time infrared (rt-ir) method, and the thermal performance of the crosslinking product was characterized by thermal loss (TGA).
Experimental raw materials: 2, 2-disulfyl ethyl sulfide (MES) : 98% purity; Trimethyl-propane triacrylate (TMPTA); Bisphenol A type epoxy resin: e-51; Triethylamine (Et3N) : analytical pure.
As the reaction progresses, the strength of the epoxy base at the sulfhydryl peak and 916cm-1 at 2561cm-1 is decreasing, while the intensity of hydroxyl peaks at 3500cm-1 is increasing. Thiol functional groups and epoxy functional groups according to the formula (3) the conversion calculation: (t) = 1 - A (t) (I)/(O) iA A 2966 / A (t) (O), 2966 (3), A for absorbance, the peak A point method to determine in the Supreme Court: A = log101T, namely by the transmittance of t wave number analysis on directly determine.
The conversion rate of the functional groups at the time of t is related to the absorption of a (t) with its infrared signature absorption peak at 2966cm-1.
The conversion rate of sulfhydryl and epoxies at different moments in polymercaptan/e-51 crosslinking system. The conversion rate of the reaction in an s-shaped type: the top 50 min, although the concentration of thiol and epoxide group is the largest, but the response is slow, this may be due to the polymerization system contains the function of material, so the conversion rate is small (10%) did not meet; As the reaction was carried out, the resistance was consumed, and the reaction rate was significantly accelerated after 50min, and the conversion rate of sulfhydryl and epoxy group increased rapidly in 30min, reaching the maximum value. After 80 min, along with the increase of the system viscosity of polymer chain segment decreased activity, thiol and epoxy group of contact decreases, and the reaction rate is slow again, to terminate the infrared tracking thiol conversion rate of 48%, the epoxy group is 36%.
This indicates that the polythiol/e-51 crosslinking system should have a post-crosslinking process so that the reaction groups can fully respond and form highly crosslinked thermosetting resins. Compared with the traditional fatty polyamines, such as triethylene tetramine (TETA), the anterior crosslinking speed of the crosslinking system is significantly faster than the cross-linking time of the 4-d + 100-30min.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
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