Preparation of Glutaraldehyde Cross-Linked Chitosan Beads Under Microwave Irradiation and Properties of Urease Immobilized onto the Beads

The glutaraldehyde cross-linked chitosan beads were prepared under microwave irradiation and urease was immobilized onto the beads. The activity and the yield of enzyme activity of the immobilized urease were 10.83 U/g carrier and 47.700, respectively. The optimum conditions of immobilization were 100 of glutaraldehyde volume fraction, 10 mg/g of urease/beads weight ratio, 24 h of the processing time and pH 6.5 of the reaction medium for immobilization. The properties of the immobilized urease were investigated and compared with those of the free enzyme. The optimum pH values were 6.5 and 7.0 for the immobilized and free urease, respectively. The optimum temperature was 60 ℃ for the free urease, while it shifted to 65 ℃ for the immobilized enzyme. The Michaelis constant Km was 9.1 mmol/L for the immobilized and 12.5 mmol/L for the free urease. The immobilized urease retained 4000 of its initial enzyme activity even after 10 repeated uses. The immobilized urease stored at 4 ℃ retained 4600 of its initial activity even after 35 d.

A Facile Route for the Large Scale Fabrication of Graphene Oxide Papers and Their Mechanical Enhancement by Cross-linking with Glutaraldehyde

A facile route for the large scale production of graphene oxide(GO) papers and their mechanical enhancement has been presented in this work. The novel paper-like GO made from individual GO sheets in aqueous suspension can be achieved in large scale by a simple drop casting method on hydrophobic substrates.Significant enhancement in mechanical stiffness(341%) and fracture strength(234%) of GO paper have been achieved upon modification with a small amount(less than 10 wt%) of glutaraldehyde(GA). The cross-linking reaction takes place between hydroxyl groups on the surface of GO and aldehyde groups of GA, through forming hemiacetal structure, which can result in distinct mechanical enhancement of the GO papers.

One-pot synthesis of a hierarchical microporous-mesoporous phosphotungstic acid-HKUST-1 catalyst and its application in the selective oxidation of cyclopentene to glutaraldehyde

A hierarchical microporous-mesoporous metal-organic framework of HKUST-l（Cu）-encapsulated phosphotungstic acid （HPW） material, referred to as HPWs@Meso-HKUST-1, is prepared by a one-pot synthesis method using cetyltrimethylammonium bromide as the supramolecular template. The addition of HPWs to the synthesis mixture of hierarchical porous HKUST-1 results in the direct encapsulation of HPWs inside the mesopores of the HKUST-1 structure, with a homogeneous distribution over the HKUST-1 crystals, which is confirmed by XRD, FT-IR, N2 adsorption, UV-Vis DRS, and TEM. FT-IR-CO adsorption experiments indicated that additional Lewis acid sites were present in the HPWs@Meso-HKUST-1 sample. The novel heterogeneous catalyst demonstrates excellent catalytic performance for the selective oxidation of cyclopentene （CPE） to glutaraldehyde CGA） using tert-butyl hydroperoxide and acetonitrile （MeCN） as the oxidant and solvent, respectively. The high activity of the catalyst is attributed to the mesostructure of the catalyst and the nature and appropriate abundance of the HPWs--being highly dispersed with the addition of Lewis sites. After a reaction for 36 h, the 30% wt% HPWs@Meso-HKUST-1 catalyst exhibits a CPE conversion of 92.5% and a high GA yield of 73%. Furthermore, the HPWs@Meso-HKUST-1 material is sufficiently stable to prevent the leaching of HPWs, and behaves as a true heterogeneous catalyst that can be repeatedly recycled without sustaining a loss of activity and selectivity in the selective oxidation of CPE.

Coating performance on glutaraldehyde-modified wood

Scots pine(Pinus sylvestris L.) panels were modified with glutaraldehyde(GA) to various weight percent gains and subsequently coated with several commercial coatings. The drying rate and adhesion of the coatings on the modified wood were measured; the coated/modified woods were exposed outdoors to analyze how the wood modifications influence the coating deterioration. The results showed that GA modification caused an increase in the drying rate of the waterborne coatings, but had no influence on drying of tested solvent-borne coatings. GAmodification did not change the dry adhesion but reduced the wood strength in a pull-off test. Wet adhesion of waterborne coatings was improved, while that of the solvent-borne coatings tended to be somewhat reduced. During 22 months of outdoor weathering, the coated/modified samples exhibited lower moisture content than the coated/unmodified samples, but GA modification didn't contribute a substantially synergistic effect with surface coatings on resistance to weathering.

Characterization of Tungsten-Based Catalyst Used for Selective Oxidation of Cyclopentene to Glutaraldehyde

Tungsten-containing hexagonal mesoporous silica （W-HMS） supported tungsten oxide catalysts （WOx/W-HMS） was prepared for the selective oxidation of cyclopentene with aqueous hydrogen peroxide to glutaraldehyde. X-ray diffraction （XRD） results indicated that the crystal form of the active phase （tungsten oxide） of the WOx/W-HMS catalysts was dependent on the W loading and calcination temperature. X-ray photoelectron spec- troscopy （XPS） analysis revealed that the dispersed tungsten oxides on the surface of W-HMS support consisted of a mixture of W（V） and W（VI）. It was found that a high content of amorphous W species in （5＋） oxidation state resuited in the high catalytic activity. When the W loading was up to 12% （by mass） or the catalyst precursor was treated at temperature of 623 K, the catalytic activity decreased due to the presence of WO3 crystallites and the oxidation of W（V） to W（VI） on the catalyst surface. Furthermore, NH3-temperature-programmed-desorption （NH3-TPD） analysis showed that the effects of W loading and calcination temperature on the acidity of the catalysts were related to the catalytic activity. A high selectivity of 80.2% for glutaraldehyde with a complete conversion of cyclopentene was obtained over 8%WOx/W-HMS catalyst calcined at 573 K after 14 h of reaction.

Immobilization of laccase on amine-terminated magnetic nano-composite by glutaraldehyde crosslinking method

The immobilizing procedure has great influence on the activity of the immobilized laccase. The laccase was immobilized on copper tetraaminophthalocyanine (CuTAPc)-Fe3O4 magnetic nano-composite by glutaraldehyde crosslinking method via a two-step reaction. For 1 g nano-composite, the optimum pH value, the quantity, the concentration and reaction time of glutaraldehyde are 7.0, 10 mL, 10% and 4 h, respectively. In the second step the optimum pH value, reaction temperature and reaction time of laccase are 5.0, 0 ℃ and 2 h, respectively. The average diameter of the immobilized laccase is 78 nm, the saturation magnetization (Ms) of the immobilize laccase is 23.45 A·m2/kg and the surface area of the immobilized laccase is 115.03 m2/g. When 2.0 mg/mL laccase solution is used under optimum conditions and 2, 2′-azino-bis-(3-ethylbenzothiazoling-6-sulphonic acid) is used as substrate, the activity of immobilized laccase reaches 1 430 U/g (nano-composite) and the Michealis-Menten constant(Km) of the immobilized laccase is 2.38×10?5 mol/L.

PREPARATION AND ADSORPTION OF THIOUREA MODIFIED GLUTARALDEHYDE-CROSSLINKED CHITOSAN RESINS

The preparation and adsorption of thiourea modified glutaraldehyde-crosslinked chitosan resin （Thio-chitosan） using cyanuric chloride as activator was studied. The adsorptive capacity of thio-chitosan with 15% apparent degree of crosslinking （DC, mass ration of glutaraldehyde to chitosan） to Cu（Ⅱ） was 160mg/g （dry weight）. The adsorption of Cu（Ⅱ） was correlated with Freundlich and Langmuir isotherm equation. Cu（Ⅱ） adsorbed on thio-chitosan column （ 1cm×10cm） was eluted with 0.5mol/L H2SO4, 6mol/L HCI and 3% thiourea solution with the recovery of 88.3%, 86.1% and 95.3%, respectively. The thio-chitosan resin can be applied to the separation and recovery of metal ions.

The Stabilization Effect of Glutaraldehyde on the Spirulina platensis Phycobilisomes

The spectral properties of the glutaraldehyde-treated phycobilisomes were studied. The results showed that glutaraldehyde was effective in preventing phycobilisomes from dilution- induced dissociation and preserving the intra-phycobilisomes energy transfer.

Effects of albumin/glutaraldehyde glue on healing of colonic anastomosis in rats

To evaluate the effect of local surgical adhesive glue (albumin/glutaraldehyde-Bioglue) on the healing of colonic anastomoses in rats. METHODSForty Albino-Wistar male rats were randomly divided into two groups, with two subgroups of ten animals each. In the control group, an end-to-end colonic anastomosis was performed after segmental resection. In the Bioglue group, the anastomosis was protected with extraluminar application of adhesive glue containing albumin and glutaraldehyde. Half of the rats were sacrificed on the fourth and the rest on the eighth postoperative day. Anastomoses were resected and macroscopically examined. Bursting pressures were calculated and histological features were graded. Other parameters of healing, such as hydroxyproline and collagenase concentrations, were evaluated. The experimental data were summarized and computed from the results of a one-way ANOVA. Fisher’s exact test was applied to compare percentages. RESULTSBursting pressures, adhesion formation, inflammatory cell infiltration, and collagen deposition were significantly higher on the fourth postoperative day in the albumin/glutaraldehyde group than in the control group. Furthermore, albumin/glutaraldehyde significantly increased adhesion formation, inflammatory cell infiltration, neoangiogenesis, and collagen deposition on the eighth postoperative day. There was no difference in fibroblast activity or hydroxyproline and collagenase concentrations. CONCLUSIONAlbumin/glutaraldehyde, when applied on colonic anastomoses, promotes their healing in rats. Therefore, the application of protective local agents in colonic anastomoses leads to better outcomes.

Suture-Less Circumcision by Glutaraldehyde Albumin Glue Enhanced Laser Tissue Welding—A Comparative Study

Background: Suture-less circumcision by Feracrylate glue creates a weak and non waterproob bond. Hence, there is wound dehiscence and delayed healing which favor infection in many patients. I am describing a new technique for suture-less circumcision which is free from above limitations. Methods: In my center in the time span of 2 years, I did 51 cases of circumcision with Laser tissue welding technique (group A). Age range was 5 months to 21 years. During the same time span, in 56 patients circumcision was done by Feracrylate glue (group B). The age range was 3 months to 22 years. This group was kept as a control. Patients in both groups were randomly distributed. The technique of circumcision by Laser tissue welding is as follows. Patient is under short GA, the prepuce above the artery forceps is chopped off by scissors and bleeders are coagulated by bipolar cautery. Now, 0.9 ml 40% human albumin is taken in 1 ml syringe and mixed with 0.1 ml of 10% glutaraldehyde solution. The syringe is shaken vigorously to mix both the components. The skin and mucosa of penis are held by tooth forceps and a thin layer of this mixture is layered over it all around. Infrared Laser of 5 watts power and 850 nm illuminated over this bond for 60 seconds to polymerize it. Results: In group A, 2 (3.9%) patients developed partial wound gape, no patient had complete wound gape. 3 (5.88%) patients had grade 2 infections which settled with conservative treatment of oral antibiotics. In group B, 6 (10.71%) patients had partial wound gape and 8 (14.28%) patients had complete wound gapping. 11 (19.64%) patients developed grade 2 and 8 (14.28%) patients grade 3 wound infection. All these 19 patients’ post-operative antibiotics were started and given for 7 - 10 days. The Glutaraldehyde albumin mixture bond is already described in medical literature (Bioglue) for its use to seal coronary anastomosis after CABG operation, to seal sutures of cardiac surgery and for aortic dissection, etc. It is a surgical adhesive composed of purified bovine serum albumin (BSA) and glutaraldehyde and is already American FDA approved. It creates a flexible mechanical seal independently of the body’s clotting mechanism. In my technique, 0.9 ml of 40% human albumin is mixed with 0.1 ml 10% glutaraldehyde solution which costs only 50 cents which is a massive 1000 times cost reduction. Laser application polymerizes the glue and forms a waterproob bond in less than a minute. In my technique, percentage of glutaraldehyde used is only 10% compared to 50% in bioglue, hence it is non-toxic to the tissues. Conclusion: Suture-less circumcision by glutaraldehyde albumin glue enhanced Laser tissue welding is a safe, cheap and effective technique of performing circumcision. It is an important advance in circumcision surgery after a long time. The technique becomes a foundation for its vast application in other areas of surgery.

Influence of Glutaraldehyde on the Properties and Release Kinetic of α-Tocopherol from Chitosan-based Film

A crosslinked chitosan film with α-tocopherol was produced by a solution casting method. The appearance, mechanical properties, morphology, barrier properties and release kinetics of the α-tocopherol were evaluated. The addition of glutaraldehyde and α-tocopherol decreased the lightness and greenness and increased the yellowness of the chitosan-based film. Moreover, it also affected the compatibility of the film due to a decrease in the opacity values. The elongation at break(EB) and tensile strength(TS) values of the film decreased when the glutaraldehyde and α-tocopherol were added. In contrast, the Young’s modulus(YM) values increased. SEM micrographs showed coarse spots and pores on the surface and cross-section of the film when compared with the chitosan film. Based on the results, it was indicated that the chitosan structure was disconnected by the α-tocopherol, and the glutaraldehyde as a crosslinking agent generated a link between the chitosan network, which could be the cause of the reduced flexibility and the increased surface roughness of the film. However, the glutaraldehyde and α-tocopherol did not result in a significant difference in water vapour permeability(WVP) values. The glutaraldehyde influenced the release kinetics of the α-tocopherol as seen by the decrease of the diffusion coefficient values that were calculated using the Fickian diffusion model.

Mechanism of high Li-ion conductivity in poly(vinylene carbonate)-poly(ethylene oxide)cross-linked network based electrolyte revealed by solid-state NMR

Solid polymer electrolytes(SPEs)have become increasingly important in advanced lithium-ion batteries(LIBs)due to their improved safety and mechanical properties compared to organic liquid electrolytes.Cross-linked polymers have the potential to further improve the mechanical property without trading off Li-ion conductivity.In this study,focusing on a recently developed cross-linked SPE,i.e.,the one based on poly(vinylene carbonate)-poly(ethylene oxide)cross-linked network(PVCN),we used solid-state nuclear magnetic resonance(NMR)techniques to investigate the fundamental interaction between the chain segments and Li ions,as well as the lithium-ion motion.By utilizing homonuclear/heteronuclear correlation,CP(cross-polarization)kinetics,and spin-lattice relaxation experiments,etc.,we revealed the structural characteristics and their relations to lithium-ion mobilities.It is found that the network formation prevents poly(ethylene oxide)chains from crystallization,which could create sufficient space for segmental tumbling and Li-ion co nductio n.As such,the mechanical property is greatly improved with even higher Li-ion mobilities compared to the poly(vinylene carbonate)or poly(ethylene oxide)based SPE analogues.

Residual alkali-evoked cross-linked polymer layer for anti-air-sensitivity LiNi_(0.89)Co_(0.06)Mn_(0.05)O_(2)cathode

High-energy density lithium-ion batteries(LIBs)with layered high-nickel oxide cathodes(LiNi_(x)Co_(y)Mn_(1-x-y)O_(2),x≥0.8)show great promise in consumer electronics and vehicular applications.However,LiNi_(x)Co_(y)Mn_(1-x-y)O_(2)faces challenges related to capacity decay caused by residual alkalis owing to high sensitivity to air.To address this issue,we propose a hazardous substances upcycling method that fundamentally mitigates alkali content and concurrently induces the emergence of an anti-air-sensitive layer on the cathode surface.Through the neutralization of polyacrylic acid(PAA)with residual alkalis and then coupling it with 3-aminopropyl triethoxysilane(KH550),a stable and ion-conductive cross-linked polymer layer is in situ integrated into the LiNi_(0.89)Co_(0.06)Mn_(0.05)O_(2)(NCM)cathode.Our characterization and measurements demonstrate its effectiveness.The NCM material exhibits impressive cycling performance,retaining 88.4%of its capacity after 200 cycles at 5 C and achieving an extraordinary specific capacity of 170.0 mA h g^(-1) at 10 C.Importantly,this layer on the NCM efficiently suppresses unfavorable phase transitions,severe electrolyte degradation,and CO_(2)gas evolution,while maintaining commendable resistance to air exposure.This surface modification strategy shows widespread potential for creating air-stable LiNi_(x)Co_(y)Mn_(1-x-y)O_(2)cathodes,thereby advancing high-performance LIBs.

Tuning the cross-linked structure of basic poly(ionic liquid)to develop an efficient catalyst for the conversion of vinyl carbonate to dimethyl carbonate

Dimethyl carbonate(DMC)is a crucial chemical raw material widely used in organic synthesis,lithiumion battery electrolytes,and various other fields.The current primary industrial process employs a conventional sodium methoxide basic catalyst to produce DMC through the transesterification reaction between vinyl carbonate and methanol.However,the utilization of this catalyst presents several challenges during the process,including equipment corrosion,the generation of solid waste,susceptibility to deactivation,and complexities in separation and recovery.To address these limitations,a series of alkaline poly(ionic liquid)s,i.e.[DVBPIL][PHO],[DVCPIL][PHO],and[TBVPIL][PHO],with different crosslinking degrees and structures,were synthesized through the construction of cross-linked polymeric monomers and functionalization.These poly(ionic liquid)s exhibit cross-linked structures and controllable cationic and anionic characteristics.Research was conducted to investigate the effect of the cross-linking degree and structure on the catalytic performance of transesterification in synthesizing DMC.It was discovered that the appropriate cross-linking degree and structure of the[DVCPIL][PHO]catalyst resulted in a DMC yield of up to 80.6%.Furthermore,this catalyst material exhibited good stability,maintaining its catalytic activity after repeated use five times without significant changes.The results of this study demonstrate the potential for using alkaline poly(ionic liquid)s as a highly efficient and sustainable alternative to traditional catalysts for the transesterification synthesis of DMC.

Solid-state NMR of vulcanized natural rubber/butadiene rubber blends:Local organization and cross-linking heterogeneities This article is part of the virtual special issue“Solid-state NMR studies on polymers and biological solids”

Elastomer blends,among which natural rubber(NR)and butadiene rubber(BR),are involved in many components of the automotive/tire industry.A comprehensive understanding of their mechanical behavior requires,among other features,a detailed description of the crosslink density in these mixtures.In the case of vulcanized immiscible blends,the distribution of the cross-link density within each of the NR-and BR-rich domains is key information,but difficult to determine using the conventional approaches used for one-component crosslinked elastomers.In this study,the vulcanization within NR/BR blends is investigated using a robust^(1)H double-quantum(DQ)MAS recoupling experiment,BaBa-xy16.Two kinds of cross-linked NR/BR blends were considered with two different microstructures for the BR component.The bulk organization of the resulting blends was first probed by analyzing the^(1)H spin-lattice relaxation behavior.In a second step,BaBa-xy16 was used to investigate,in a selective way,the cross-link heterogeneities within NR/BR blends.In particular,for immiscible NR/BR mixtures,the distribution of the cross-link density between both phases was compared and the observed differences were discussed.

Early changes in corneal densitometry after FS-LASIK combined with accelerated corneal cross-linking for correction of high myopia

AIM:To observe the effects of femtosecond laserassisted excimer laser in situ keratomileusis combined with accelerated corneal cross-linking(FS-LASIK Xtra)on corneal densitometry after correcting for high myopia.METHODS:In this prospectively study,130 patients underwent FS-LASIK or FS-LASIK Xtra for high myopia.Their right eyes were selected for inclusion in the study,of which 65 cases of 65 eyes in the FS-LASIK group,65 patients with 65 eyes in the FS-LASIK Xtra group.Patients were evaluated for corneal densitometry at 1,3,and 6mo postoperatively using Pentacam Scheimpflug imaging.RESULTS:Preoperative differences in corneal densitometry between the FS-LASIK and FS-LASIK Xtra groups in different ranges were not statistically significant(P>0.05).Layer-by-layer analysis revealed statistically significant differences in the anterior(120μm),central,and total layer corneal densitometry between the FS-LASIK and FS-LASIK Xtra groups at 1 and 3mo postoperatively(all P<0.05),the FS-LASIK Xtra group is higher than that of the FS-LASIK group.Analysis of different diameter ranges showed statistically significant differences between the FS-LASIK group and the FS-LASIK Xtra group at 1mo postoperatively in the ranges of 0–2,2–6,and 6–10 mm(both P<0.05);At 3mo postoperatively,the FS-LASIK Xtra group is higher than that of the FS-LASIK group in the ranges of 0–2 and 2–6 mm(P<0.05).At 6mo postoperatively,there were no statistically significant differences in corneal densitometry between the FS-LASIK group and the FS-LASIK Xtra group in different diameter ranges(all P>0.05).CONCLUSION:There is an increase in internal corneal densitometry during the early postoperative period after FS-LASIK Xtra for correction of high myopia.However,the densitometry values decreased to the level of conventional FS-LASIK at 6mo after surgery,with the most significant changes observed in the superficial central zone.

Molecule‑Level Multiscale Design of Nonflammable Gel Polymer Electrolyte to Build Stable SEI/CEI for Lithium Metal Battery

The risk of flammability is an unavoidable issue for gel polymer electrolytes(GPEs).Usually,flameretardant solvents are necessary to be used,but most of them would react with anode/cathode easily and cause serious interfacial instability,which is a big challenge for design and application of nonflammable GPEs.Here,a nonflammable GPE(SGPE)is developed by in situ polymerizing trifluoroethyl methacrylate(TFMA)monomers with flame-retardant triethyl phosphate(TEP)solvents and LiTFSI–LiDFOB dual lithium salts.TEP is strongly anchored to PTFMA matrix via polarity interaction between-P=O and-CH_(2)CF_(3).It reduces free TEP molecules,which obviously mitigates interfacial reactions,and enhances flame-retardant performance of TEP surprisingly.Anchored TEP molecules are also inhibited in solvation of Li^(+),leading to anion-dominated solvation sheath,which creates inorganic-rich solid electrolyte interface/cathode electrolyte interface layers.Such coordination structure changes Li^(+)transport from sluggish vehicular to fast structural transport,raising ionic conductivity to 1.03 mS cm^(-1) and transfer number to 0.41 at 30℃.The Li|SGPE|Li cell presents highly reversible Li stripping/plating performance for over 1000 h at 0.1 mA cm^(−2),and 4.2 V LiCoO_(2)|SGPE|Li battery delivers high average specific capacity>120 mAh g^(−1) over 200 cycles.This study paves a new way to make nonflammable GPE that is compatible with Li metal anode.

Study on the Soy Protein-Based Adhesive Cross-Linked by Glyoxal

Based on the ESI-MS and ^(13)C-NMR analysis of the forms of glyoxal in acidic and alkaline solutions,the soy-based adhesive cross-linked by glyoxal was prepared in this work.The results showed that glyoxal existed in water in different forms at different pH levels.Under alkaline conditions,glyoxal transformed to glycolate through the intramolecular disproportionation reaction.Under acidic conditions,although some of glyoxal transformed to glycolate as what happened under alkaline conditions,most of glyoxal molecules existed in the form of fiveor six-membered cyclic ether structure.No ethylene tetraol or free aldehyde group was actually detected under these conditions.Although glyoxal reacted with soy protein under both acidic and alkaline conditions,alkaline conditions were more favorable for the improvement of mechanical performance and water resistance of soybased adhesives than acid conditions.

PERVAPORATION PROPERTIES OF PDMS MEMBRANES CURED WITH DIFFERENT CROSS-LINKING REAGENTS FOR ETHANOL CONCENTRATION FROM AQUEOUS SOLUTIONS

Ethanol perm-selective PDMS/PVDF composite membranes were prepared by curing polydimethylsiloxane (PDMS) with various cross-linking reagents,such as tetraethoxylsilane(TEOS),γ-aminopropyltriethoxylsilane(APTEOS), phenyltrimethoxylsilane(PTMOS) and octyltrimethoxylsilane(OTMOS) as well.The cross-linking density and surface properties of the PDMS active layer were adjusted by varying cross-linking reagents.The pervaporation performance of PDMS membranes cured with different cross-linking reagents was investig...