(2) 6a om m wy wo ay @ 6) (2 68) United States Patent Abu-Jdayil et BIODEGRADABLE COMPOSITE INSULATION MATERIAL AND METHOD OF MAKING THE SAME, Applicant: UNITED ARAB EMIRATES UNIVERSITY, Al Ain (AE) Basi Waleed Khalil Ahmed, Al Ain (AP); Amged Ethassan, Al Ain (AF) Molisin Raza, Al Ain (AP) Inventors Assignee: UNITED ARAB EMIRATES UNIVERSITY, A Ain (AE) Notice: Subject to any disclaimer, the term ofthis pateat is extended of adjusted under 35 USC. 154(b) by 0 days. Appl. No. 17/833,107 Filed: Nov. 22, 2021 Int. 298 13/10 (2006.01) Cast, 99/00 (2006.01) 298 1306 (2005.01), 29 43700 (2006.01) F048 78 (2005.01) oss 3/12 (2006.01) sb 174 (2006.01) 229K 1/00 (2006.01) Us. c. cre C081, 99/00 (2013.01), B29B 13706 (2013.01); 8298 13/10 (2013.01); B29C 481003 (2013.01); COBY 3/12 (2013.01), BOMB {1/78 (2013.01); B29K 2001/00 (2013.01): 829K 29951006 (2013.01); B29K 2995/0015. (2013.01); COSY 2399/00 201801); Cos 2493/00 2013.01); COSL. 2201/06 (2013.01) COSE 22051025 (2013.01); COS. 220916 (2013.01); £osB 20017745 (3013.01) Field of Classification Search oc CO8t, 99/00; COST, 2201/06; COR 22051025; Col. 205/16; 298 13/06; US 11,359,095 B1 Jun, 14, 2022 USO 1135909SB (10) Patent No.: (4s) Date of Patent: 18208 13/10, B29C 43/003; COB V1 (C0 2399100; ORS 2499/00; FOSD 1/78; [EO 2001/745; 29K 2001/00: 29K 2095/0015; B29K 2995/005 ‘See application file for complete seurc history 60) References Cited u PATENT DOCUMEt S $2020, Abu-Sdayi ea FOREIGN PATENT DOCUMENTS ew lorsssas © 92017 cN Hogeaosd a” 11/2019 (OTHER PUBLICATIONS ‘han, Gasi Mil otal “Okra fibers pots material for biocomposites" Gren biocompesites. Springer, Chan, 2017. 261 * cited by examiner Irina S Zemel Nath, Goldberg & Primary Bsaminer (74) Attornes, Agent, or Firm Meyer: Richard €. Titman on ABSTRACT The biodegradable composite insulation material is made From date pam leat fibers and powdered oka, The date palm leaf fihers have a concentration of between $0 Wt No aid 50 ‘wt % of the biodegradable composite insulation material, ‘nd the powdered ok has a concentration of between 10 wt % and 80 wi % of the biodegradable composite insulation material. The biodegradable composite insulation material is prepared by mixing date palm lea fibers and powdered okra, Jn the ubove concentrations, to form a mixture This mixture is then wetted with water, ale to a mold, and heated under pressure to form a compressed article. The compressed file is then dred to form the biodegradable composite insulation material. 13 Claims, 4 Drawing SheetsUS 11,359,095 B1 Sheet 1 of 4 Jun, 14, 2022 U.S. Patent WHO 40 %0S ~ VaHO 40 KO « WaHO 40 %0E == WSO 40 4002 WYHO 40 %00 b ‘Old (0) 3unuvuadWVSL NV&WN so $900 900 S900 100 00 (yum) GNOOU.S. Patent Jun, 14, 2022 Sheet 2 of 4 US 11,359,095 B1 60% 40% 30% OKRA % FIG. 2 0% 10% 0% geeese¢sesae 2° (ed) HLONZULS SLYWILINU.S. Patent Jun, 14, 2022 Sheet 3 of 4 US 11,359,095 B1 50% 0% OKRA % FIG. 3 | | | # (ea) SANGON DLLS3T3U.S. Patent Jun, 14, 2022 Sheet 4 of 4 US 11,359,095 B1 50% 30% OKRA % FIG. 4 10% eesesese e828 AdniwonaUS 11,359,095 BL 1 BIODEGRADABLE COMPOSITE INSULATION MATERIAL AND METHOD OF MAKING THE SAME, BACKGROUND 1. Field “The disclosure ofthe present patent application relates to thermal insulation materials, ancl particularly to a biodeprad- able, thermally insulating composite made from date palm Jeaves and okra 2. Description of the Related Art ‘Thermal insulators are found in most moslem buildings since they significantly reduce the need to artificially heat fand cool the interiors of the buildings. Such insulators are traditionally fabricated from petrochemical materials, hov- ‘ever, the negative environmental impact of such materials, has given rise to an interest in alternative types of insulators. Natural fiberreinforced polymer composite materials, in particular, are gaining in popularity in a wide variety of Industries, including the construction and automotive fields ‘A ull-cale replacement of petrochemical-based insula tors by natural fiber-reinforced polymer composites has not ‘et taken place because research has shown that the addition ‘of natural fibers to polymer matrices decreases the overall, mechanical strength. Developing a composite in which the mechanical strength docs not sulle from such a decrease would be of great interes, particularly since natural fibers have numerous advantages over conventional and synthetic fibers, including their environmental friendliness and theie ability o create composites with low densities, low costs, and comparable specific strengths. Although different types of natural filers, such as the fibers from flax, hemp, jute, Kenaf, sisal, abaca, pineapple leaf, ramie, coir, bamboo, rice Iusk, oil palm, and bagasse have boea investigated, fibers from date palm bas, thus far received litle attention. It would be desirable to be able to make use of date palms, given how widely they are pro- ‘duoed, particularly in Arabian Gulf countries. The United Arab Emirates, for example, has about 40 million date palms. Fach palm generates about 15 kilograms of biomass ‘waste anntally langely made up of date wood (DW), where DW typically includes material from the petiole, rachis, leaflets, thorns. spathe, bunch, pedicels, and fibrilium Accordingly, DW makes up a significant source of waste or ow value produet at present, and represents a curently underutilized! material resource, Given the abundance of date palm, and the great potential foe natural fiber fillers, i would bo desirable to be able to use date palm waste inan environmentally fend alternative to traditional petrochemical-hased insulating material, paricu- larly without a loss of mechanical strength in the composite product. Thus, a biodegradable composite insulation mate- Fial and a method of making the same solving the afore- mentioned problems are desired SUMMARY ‘The biodegradable composite insulation material is made from date palin leaf fibers and powdered okra, The date palm Jeaf fibers have a concentration ranging from about 50 Wt % to about 0 wt % of the biodegradable composite insulation ‘material, and the powdered ok has a concentration maging from about 10 wt % to about $0 Wi % of the biodepradable 0 o 2 ‘composite insulation material, The biodegradable composite insulation material is prepared by mixing date palm leat {hers and powdered okra, in the above concentrations, 10 form a mixture. This mixture is then wetted with water, fadded to @ mold, and heated under pressure to form compressed article. The compressed article is then dried to {orm the biodegradable composite inslation material These and other features ofthe present subject matter will become really apparent upon further review ofthe fall ing specification BRIEF DESCRIPTION OF THE DRAWINGS PIG. 1is« graph showing the measured thermal conduc- tivity for a biodegradable composite insulation material prepared with varying weight ratios of powdered okra to ‘dae palm leaf fibers FIG. 2 is @ graph showing the measured compressive strength for the biodegradable composite insolation material prepared with varying weight ratios of powdered oka to ate palm leaf fibers. PIG. 36a graph showing the measured elastic modulus for the biodegradable composite insulation material pre- pared with varying weight ratios of powdered okra to date palm lea fibers. FIG. 4 isa graph showing the measured ductility forthe biodegradable composite insulation material prepared with varying weight ratios of powdered okra to date palm leat sihors. ‘Similar reference characters denote corresponding fea. tures consistently throughout the attached drawings DETAILED DESCRIPTION OF THE. PREFERRED EMBODIMENTS ‘The biodepradable composite insulation material is made from date palm leaf fibers and powdered okra, The date palm Ieaf fibers have a concentration ranging from about 50 wt % to about 90 wt % ofthe biodegmdable composite insulation ‘material, and the powdered okra has a concentration ranging from about 10 wt 26 to about $0 wt % ofthe biodegradable ‘composite insulation material. The biodegradable composite insulation material is prepared by mixing date palm leat iihers and powdered okra, in the above concentrations, 10 {om a mixture. As a non-limiting example, mixing may be performed using a eommereal mixer or the fke for appro ‘mately I minute. This mixture is then wetted with water. The wetting may be performed by, for example, gradually spray~ ‘ng pure water ver the mixture unt it becomes wet AS @ ‘non-limiting example, a weight of the sprayed water may range from about 10% to about 20% of the weight of the mixture. As used herein, the term “about” when used 10 modify aumber means within 10% of the modified number, "The wetted mixture is then added to a mold. As 3 ‘non-limiting example, the wetted mixture may be alded 10 ‘stainless see! mold. The wetted mixture in the mois then heated under pressure to form a compressed article. AS a on-imiting. example, the mixture may be heated in the sold at 80° C. under 250 MPa, using a hot press for Approximately 15 minutes It should be understood thatthe ‘mold may have any desired shape, such as evlindecal ‘mold, a flat mold, ete, dependent upon the desired shape of the end product. Additionally, prior to adding the wetted ‘mixture tothe mold, it may ist be mixed in a Bow! at low speed for, for example, 10 minutes. "The compressed article is then dried to form the biode- aradable composite insulation material. As @-noa-limitingUS 11,359,095 BL 3 ‘example, the drying may be performed by deying the co pressed article, still inthe mol, in an air oven at 80°C. for 24 thous. Following dying, the biodegradable composite ‘insulation material may he removed from the oven and fet to cool at room temperature. As a non-limiting example the initial powdered okra may be prepared by grinding fresh green okra using @ grinding machine or the like. The ground okra may then by dried using, for example, spray drying sta temperature between 55°C. and 65° C. for between 10 hours and 12 hours. The ‘ried, grouncl okra is thea filtered to produce the powdered ‘okra, Asa non-limiting example, the dried, ground okra may be filtered through an 80 mesh sieve to produce 10-1 soluble ‘okra exircts powder, ‘Asa non-limiting example, the initial date palm leaf fibers may be prepared by peeling the date palm leaves from a date palm tree using a seraper or the like, ‘The date palm leat fibers may then be cleaned, for example, using dry air and water The date palm lea fibers are then soaked! in water at ‘temperature between 110° C. and 125°C. for two hours, tnd then cleaned with water. As a non-limiting example, “drying ofthe soaked date palm lea bers may take place as fa two-step process, beginning with drying the sled date palm leaf fibers at room temperature for one hour, followed by dying the soaked date palm leaf fibers ata temperature ‘of approximately 110° C. for 24 hours. The second drying step may'be periormed in an aleatrying oven or the like. The ried dae palm lea fibers are thea ground using commer. JI mixer, shredder othe like for two minutes to produce ‘hors having lengths between approximately S mm and 7 The mechanical properties of biodegradable compenite insulation materials produced by’ the above method are shown below in Table 1 for varying concentrations of the date palm leaf fibers and the okra powder. ABLE 1 Neh apt oft Regie Comat Power Urine asic Dac paim eat "sk Dasiy —commmene) oa hem tees) gets) eas) Additionally, the biodegradable composite insulation ‘materials found to have afow thermal condvetivity, ranging from about 0.06013 Win K to about 0.06938 WiavK. FIG. | shows the thermal condoetivity as 2 function of tenpera= ture for the biodegradable composite insulation material ‘with powdered okra concentrations of O-wt 9, 20 wt %, 30 1%, 40 wt %, and $0 wi %e (and comesponding respective date palm leaf fiber concentrations of 100 wt %, 80 wt %, 70, 1w1%6, 60 1 %, and 0 WE), As can be seen, the messed thermal conductivity is consistently Hinear for the composite ‘over the varying ratios of powdered okra to date palm leat fibers. FIG. 2 shows the ultimate (compressive) strength for the composite with powdered okra concentrations of 0 wt %, 20 %, 30 wt %, 40 wt 9, and S0-wt % (and corresponding respective date palm lea fiber concentrations of 100 wt % BO wt %, 70 wt Ho, 60 wt %, and $0 wt). AS shown, the compressive strength increases with a comesponding increase ofthe powered okra concentration (up 0 50 wt %). ACSO wt%, the compressive strength is preater than 70 Mp, 0 o 4 whieh approaches the compressive strength associated with common wood building and insulation materials FIG. 3 shows the measured elastic modulus for the composite with powdered okra concentrations of 0 wt %, 20 1w1 %, 30-61 %, 40 we 95 and 50 6 % (and eovtesponding respoctive date palm leat ber eoncentrations of 100 wt %, BOWE %, 70 wt M60 wt %, and 50 wr %). AS shown, the clastic mods has a substantially linear behavior, with an clastic modulus range within those associated with comamer= cially available polymeric insulating materials. FIG. 4 shows the measured ductility forthe composite with powdered okra concentrations oF 0 wi %, 20 wt %, 30 wt %, 40 wt, and ‘50 wt % (and corresponding respective date palm leaf fiber concentrations of 100 wt %, 80 wt %, 70 41%, 60 wi %,and 50 wi %). AS shown, the ductility is substantially linear, approaching 80% at a powdered okra concentration of 50 wt % Its to be understood thit the biodegradable composite insulation material and method of making the same are not limited to the specific embodiments deseribed above, but encompasses any and all embodiments within the scope of the generic langage of the Following claims enabled by the embodiments deseribed herein, or otherwise shown in the ‘drawings or described above in ermssuficient to enable one of ordinary skill in the art to make and use the claimed subject mater We clin 1A biodegradable composite insulation material, com- rising: dat palm laf fibers having a concentration ranging from ‘shout 50 wi % to about 90 wt % of the biodegradable ‘composite instlation material; and powdered okra having a concentration ranging from about 10 wt % to about 50 wt % of the biodegradable ‘composite insulation material, 2. Amethod of making a biodegredable composite inst Jation material, comprising the steps of: ‘mixing date palm leaf fibers and powered okra to form ‘2 mixture, wherein the date palm leaf fibers have a ‘concentration ranging from about $0 wt % to about 90 ‘wt % of the mixture, and the powdered okra has a ‘concentration ranging from about 10 wt % to about $0 ‘0% of the mixture; welling the mixture with water adding the mixture to a mold; Dheatng the mixture under pressure in the mold fo form a ‘compressed article; eying the compressed article to form the biodegradable ‘composite insulation material 3. The method of making a biodegradable composite insulation material as ected in claim 2, wherein a weight of the Waler in the step of Welling the mixture ranges Irom bout 10% to about 20% of @ weight of the mixture. 4. The method of making a biodegradable composite insulation material as recited in claim 2, wherein the step oF beating the mixture under pressure in the mold comprises Dating the mixture at temperature of about 80° C. under about 250 MPa, 5. The method of making « biodegradable composite insulation material as recited in elaim 4, wherein the step of heating the mixtore under pressure in the mold comprises Doeating the mixture under pressure in the mold for about 1S 6. The method of making a biodegradable composite insulation material as recited in claim 2, further comprising the step of mixing the mixture for about 10 minutes follow-US 11,359,095 BL 5 ing the step of wetting the mixture and prior to the step of ‘adding the mixture to the mold 7. The method of making a biodegradable componite insulation material as recited in claim 2, wherein the step of drying the compressed article comprises drying the com- pressed article in the mold within an oven, 8. The method of making a biodegradsble compowite insulation material as cited in claim 7, wherein the step of drying the compressed article comprises drying the com= pressed artiele at about 80° C. for about 24 hos 9. The method of making a biodegradable composite insulation material as recited in claim 2, further comprising the steps o: srinding fresh green okra: tying the ground okra; and illering the dried, ground okra to produce the powdered okra, 10, The method of making a biodegradable composite insolation material as recited in claim 9, wherein the step of drying the ground okra comprises spray drying the ground ‘okra at a temperature ranging from about 55° C. to about 65° (C.for about 10 hours to about 12 hours. 6 11. The method of making a biodeuradable composite insulation material as recited in claim 10, wherein the step of filtering the dried, ground okra comprises fering the ried, ground okra through an 80 mesh sieve. 12, The method of making a biodegradable composite ‘insulation material as recited in claim 2, wherein, prior tothe sep of mixing the date palm lea fibers and the powsdered okra to form the mixture, the method further comprises: cleaning the date palin leaf fibers; soaking the date palm lel fibers ia water at a temperature ‘ranging {rom about 110° C. to about 125° C. for about two hours; eying the soaked date palm leaf fibers; and farinding the dried date pal lea fibers. 13. The method of making a biodegradable composite insulation material as recited in claim 12, wherein the step of drying the soaked date palm leaf fibers comprises drying the soaked date pal loaf fibers at oom tempers ture for one hour: and eying the soaked dae pal leaf bers ata temperature of "approximately 110°C, for 24 hours,