• 专利标题:   Making natural graphene cellulose blended meltblown nonwoven fabric involves e.g. combining graphite powder with solution comprising e.g. sulfuric acid, stirring in ice bath environment, and adding solution comprising potassium permanganate.
  • 专利号:   US2017107650-A1, TW201714822-A, TW588089-B1, US10190243-B2
  • 发明人:   CHOU W, LAI M, HUANG K, CHOU S, HSU C, CHOU W T, LAI M Y, HUANG K S, CHOU S H, HSU C Y
  • 专利权人:   ACELON CHEM FIBERS CORP, ACELON CHEM FIBERS CORP
  • 国际专利分类:   D01D001/02, D01D005/098, D01F008/02, D01F008/18, D04H001/485, D04H001/49, D04H001/56, C01B031/04, D01F001/02, D04H001/04, D04H001/492, C01B032/192, C01B032/23, D01D010/06, D01F001/10, D01F013/00, D01F002/00, D04H001/4258, D04H003/013, D04H003/16
  • 专利详细信息:   US2017107650-A1 20 Apr 2017 D04H-001/485 201728 Pages: 15 English
  • 申请详细信息:   US2017107650-A1 US283472 03 Oct 2016
  • 优先权号:   TW134352

▎ 摘  要

NOVELTY - Preparing natural graphene cellulose blended meltblown nonwoven fabric, comprises: e.g. (a) combining a graphite powder with a solution comprising 1-10 wt.% of a first compound comprising sulfuric acid, hydrochloric acid, perchloric acid, hydrogen iodide, hydrofluoric acid or nitric acid, then stirring for 30 minutes in an ice bath environment; and (b) adding a solution comprising 1-20 wt.% potassium permanganate to the product of step (a), stirring for 1-2 hours, and adding distilled water. USE - The method is useful for preparing natural graphene cellulose blended meltblown nonwoven fabric. ADVANTAGE - The method: provides the recycle ratio of NMMO of 99.5% or more, and the usage of the condensed recycled water of 100% (claimed); does not require a highly toxic hydrazine hydrate solution which is required in a reduction process, and thus provides no occurrence of health hazards e.g. dizziness, nausea and others resulting from operator exposure through inhalation or skin contact with a highly toxic hydrazine hydrate solution, and thus the preparation method is a safe and harmless to operators; controls the antistatic properties and thermal transferring function by increasing the adding ratio of the graphene solution in the manufacturing process, and thus various requirements of different consumers can be satisfied; and provides the fabric which can be decomposed naturally after being used, and thus the product is harmless, natural, and environmentally friendly. DETAILED DESCRIPTION - Preparing natural graphene cellulose blended meltblown nonwoven fabric, comprises: (a) combining a graphite powder with a solution comprising 1-10 wt.% of a first compound comprising sulfuric acid, hydrochloric acid, perchloric acid, hydrogen iodide, hydrofluoric acid or nitric acid, then stirring for 30 minutes in an ice bath environment; (b) adding a solution comprising 1-20 wt.% potassium permanganate to the product of step (a), stirring for 1-2 hours, and adding distilled water, where the potassium permanganate solution is continuously added until none of the purple smoke generated by reacting with the potassium permanganate is formed from the distilled water; (c) adding a solution comprising 1-10 wt.% hydrogen peroxide to the product of step (b), where the hydrogen peroxide solution is added until no bubbles are formed and the mixture becomes dark green, then filtering the dark green solution into a cake; (d) rinsing the cake of step (c) with a solution comprising 5 wt.% hydrochloric acid to remove sulfate ions, then washing the cake with distilled water; (e) drying the cake of step (d) in an oven at 40 degrees C for 2 hours to obtain a dried solid graphite oxide; (f) adding distilled water to the dried solid graphite oxide of step (e), where the distilled water is added up to 200 mls per 0.06-1 g of the dried solid graphite oxide, then treating by ultrasonic vibration for 30 minutes to obtain a graphite oxide solution having a graphite oxide concentration of 0.03-0.5 wt.%; (g) adding a solution comprising 1-10 wt.% of a second compound comprising sodium borohydride, potassium borohydride, lithium aluminum hydride or sodium citrate to the graphite oxide solution of step (f), then treating by ultrasonic vibration for 30-60 minutes, where in the resulting solution, the ratio of graphene oxide to the second compound is 1:1-1:5 by weight; (h) filtrating the product of step (g), washing the filtrate with water 3-5 times to remove the second compound, then back-filtrating to obtain a graphene solution; (i) adding the graphene solution of step (h) to a slurry solution formed by mixing a pulp with N-methylmorpholine N-oxide (NMMO) and a stabilizer in an expansion dissolving tank, then mixing at 60-80 degrees C, where the graphene solution of step (h) is added in a ratio of 0.11-5 wt.%, the pulp is wood pulp, cotton pulp, bamboo pulp or a mixture of cotton and bamboo pulp, the pulp comprises alpha -cellulose in an amount of 65% or more with a polymerization degree of 500-1500, and the NMMO has a concentration of 50-78%; (j) removing water from the product of step (i) using a thin film evaporator and heating at 80-130 degrees C, where the water is removed to 5-13% within 5 minutes and the cellulose is dissolved to form a spinning dope, and the dope comprises 5-15% water, 70-90% NMMO and 5-15% cellulose; (k) squeezing the spinning dope of step (j) from a spinning orifice using a meltblown process to form a natural graphene cellulose blended filament strand and piling into a fibrous network structure (5) on a collector (4), which comprises pressuring the spinning dope by a metering pump, filtrating and degassing by a continuous filter, transporting the spinning dope into a spinning tank, continuously blowing hot air into the spinning orifice and outputting an air stream from the area surrounding the spinning orifice, forcing the spinning dope to be molten and squeezed to the outside of the spinning orifice to form a uniform natural graphene cellulose blended filament strand, and piling the filament strand onto a fibrous network structure on a collector; and (l) spraying a water mist to force the natural graphene cellulose blended filament strand of step (k) into a coagulation liquid, solidifying, regenerating and washing the filament strand, and water needle punching, drying, oiling and coiling the filament strand to form a natural graphene cellulose blended meltblown nonwoven fabric, where the concentration of the coagulation liquid is 2-10%, and after washing, the amount of residual NMMO solvent is less than 0.1%. DESCRIPTION OF DRAWING(S) - The figure shows a schematic view of meltblowing natural graphene cellulose blended fabric. Gear pump (1) Spinning orifice mold (2) Spinning orifice tube (3) Collector (4) Fibrous network structure (5)