Progress 07/01/10 to 06/30/14
Outputs
Target Audience: US wood composite board manufacturing industry and related university researchers. US Government authorities dealing with the formaldehyde emission problem of wood composite boards. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided? One graduate studenttrained in the projectwas graduated with a Ph. D. degree. How have the results been disseminated to communities of interest? Three large chemcial companies were contacted and the information was submitted for consideration forlarge scale production of Dand DF resins. One company informedthey do not have the capability or not want to pursue;othercompanies have not replied yet. Two wood compositemanufacturing companies wereinformed ofDF resin'sperformance potentials: they want to have the resin tested in their plants,but for the plant trial testing, each plantrequiresat least ten (10) drums of liquid resin, which is outside of the range of our laboratory capability.The final report is written ahead of the planned research period because ofP.I.'s retirement. What do you plan to do during the next reporting period to accomplish the goals?
Nothing Reported
Impacts
What was accomplished under these goals?
The planned conversion reactions of using a 200-L reactor was not accomplished due to the lack of funding, which was sought with research proposalssubmitted to the USDA foundational program. However, we continued the 25-L reactor reactions and improved the conversion efficiencyand further clarifiedthe effects ofsolvent level, catalysts level, temperature, and reaction time.We have also tested the resulting materials (D) by synthesizingDF resins and then by making and testing a series of 28" x 28" x 0.75" laboratory particleboards.We verified the efficacy of DF resins as low formaldehyde emitting particleboard binder resins and alsodiscoveredhow to detect the end-point of the conversion reactionin terms of the performance of resultant D as a component of DF resins: the melting point ofD must bein the range of 213oC -216oC.Materials having lower melting pointsobtaineddue toinappropriate reaction variables used in the reaction were found to have a signficant adverse effect of DF resin's binder performance. Overall, the data obtained through this research appear to providean adequate basis for future larger scale-up experiments.
Publications
- Type:
Journal Articles
Status:
Published
Year Published:
2013
Citation:
1.Mao, A., Hassan, E. B., and Kim, M. G. 2013. Investigation of low mole ratio UF and UMF resins aimed at lowering the formaldehyde emission potential of wood composite boards. BioResources 8(2), 2453-2469.
2.Mao, A., Hassan, E. B., and Kim, M. G. 2013. Low mole ratio UF and UMF resins entailing uron-type methylene-ether groups and their low formladehyde emmission potentials. BioResources 8(2), 2470-2486.
3.Mao, A., Hassan, E. B., and Kim, M. G. 2013. Low mole ratio urea-melamine-formaldehyde resins entailing increased methylene-ether group contents and their formaldehyde emissison potentials of wood composite boards. BioResources 8(3), 4659-4675.
4.Mao, A., Hassan, E. B., and Kim, M. G. 2013. The effects of adding melamine at different resin synthesis points of low mole ratio urea-melamine-formaldehyde (UMF) resins. BioResosurces 8(4), 5733-5748.
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Progress 01/01/12 to 12/31/12
Outputs
OUTPUTS: This annual report covers the period of October 1, 2011 to December 31, 2012. Synthesis procedure of D, starting material of DF resins, was carried out in a 25-L reactor, by varying reaction time length, mole ratio, and addition rate of one reaction component. The reaction products were then worked up to obtain yields of D, quality and quantity of recovered solvent and un-reacted residual components. The resultant data were evaluated to obtain the optimum and economic reaction procedure. Also, DF resins synthesis procedures were repeated at varying mole ratios and tested by making small particleboard samples and testing the boards for formaldehyde emission potentials and water soak properties. The results were analyzed and the optimum hot-pressing time and temperature was found, significantly improving the wood bonding performance of DF resins. Also, a comparative study is in progress on melamine-modified urea-formaldehyde resins, which thus far ascertains the comparative advantages of DF resins. The patent application of DF resins needed a revision and was followed up. PARTICIPANTS: One Ph. D. level graduate student, An Mao, participated in this project in the comparative study on melamine-modified urea-formaldehyde resins. TARGET AUDIENCES: The project results and other contents have been prepared to be communicated to USDA AFRI programs as research proposals for possible funding for scale up experiments to 50 drum quantities and testing the resins in particleboard manufacturing plants. Results on the DF resin development have been communicated to open innovation channels (Nine-Sigma). PROJECT MODIFICATIONS: Nothing significant to report during this reporting period.
Impacts
The findings are that the synthesis procedure of D can be done safely, efficiently (8 hours), in high yields (96-99 percent) at 25-L reaction levels. The optimum DF resins were found to bond particleboard well with about 5 percent higher wood moisture content than with UF resins and also at a hot-pressing temperature of about 300F in comparison to 350F for UF resins, in addition to maintaining the lower formaldehyde potentials of particleboards reported last year. In conclusion, the DF resin technology is considered to be safely scalable up to 25-L reactions and beyond and also, with the wood bonding performance improvements achieved in this reporting period, the DF resin technology deserves further scale up evaluation experiments. The results of the comparative study on melamine-modified urea-formaldehyde resins have reinforced the performance and emission advantages of DF resins and also resulted in three articles submitted for publication in 2012.
Publications
- Kim, M. G. 2012. Diethylene tricarbamide and diethylene tricarbamide-formaldehyde resins. U. S. Patent Office. Publication No. 2012-0316270-A1. (12/13/2012).
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Progress 01/01/11 to 09/30/11
Outputs
OUTPUTS: Synthesis procedure of D, starting material of DF resins, was repeated about 30 times in a 5-L reactor, by varying reaction time length, mole ratio, and addition rate of one reaction component. The reaction products were then worked up to obtain yields of D, quality and quantity of recovered solvent, and unreacted residual components. The resultant data were evaluated to obtain the optimum and economic reaction procedure that is considered to be safe to scale-up to 20-30 gallon quantities. Also, DF resins synthesis procedures were repeated about 30 times by varying the mole ratio and an additive content and tested by making small particleboard samples and testing the boards for formaldehyd emission potentials and water soak properties. The results were analyzed and obtained the optimum resin synthesis procedure that gives the lowest formaldehyde emission potential and is safe to scale-up to 20-30 gallon quantities. PARTICIPANTS: Nothing significant to report during this reporting period. TARGET AUDIENCES: The project contents were communicated to USDA AFRI programs as research proposals for possible funding for scale up experiments to 50 drum quantities and testing the resins in particleboard manufatcuring plants, but funding was rejected. PROJECT MODIFICATIONS: One year extention of project time has been requested. More time is needed to more fully explore the commercial possibility of DF resin technology.
Impacts
The findings are that the synthesis procedure of D can be done safely, efficiently (6 hours), in high yields (96-99 percent), and with only minor loss of materials due to breakdown from decomposition at 5-L reaction levels. Similarly, DF resin synthesis procedure was found to be safe to scale up and to require a very short reaction time of about 2 hours. The optimum DF resins made at 5-L reaction levels were found to be stable for more than 4 weeks at room temperature and gave formaldehyde contents of about 3 mg per 100 gram of particleboard compared to about 8 mg per 100 gram of particleboard bonded with current UF resins. In conclusion, the DF resin technology is considered to be safely scalable up to 20-30-L reactions and beyond and also, the wood bonding performances are promising and considered to deserve further scale up evaluation experiments.
Publications
- Kim, M. G. 2011. Renewable Polyol-Based Polycarbamates and Polycarbamate-Formaldehyde Thermosetting Resins. J. Applied Polymer Science, Vol 122, 2209-2220.
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Progress 07/01/10 to 12/31/10
Outputs
OUTPUTS: Several scale-up synthesis experiments of resin raw material D were carried out using a 5L reactor and one reagent pump recently purchased which is suitable for controlling the addition rate of one starting material (DA). Since the addition rate of DA is considered to be one key to further increasing of the reaction yield and leaving the least amount of waste byproducts in the recovered reaction solvent system, various addition rates were used in the synthesis experiments and the yields and amounts of waste byproducts were determiend. Also, preparations have been made for larger scale experiments up to a 25L reactor size and several solicitations were made to attract interests on DF resins from the wood composite board manufacturing industry. PARTICIPANTS: Nothing significant to report during this reporting period. TARGET AUDIENCES: Nothing significant to report during this reporting period. PROJECT MODIFICATIONS: Not relevant to this project.
Impacts
The results of synthesis experiments using the controlled addition pump resulted in improving the overall reaction pattern to give cleaner products (D) and cleaner recovered solvent system. The actual yields of D were similar at about 99%, but the recovered solvent system was clean enough to allow reuse two more times without going through a purification process.
Publications
- No publications reported this period
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