US Pat. No. 10,190,242

METHOD OF PREPARING OF NATURAL GRAPHENE CELLULOSE BLENDED SPUNBOND NONWOVEN FABRIC

ACELON CHEMICALS AND FIBE...

1. A method of preparing natural graphene cellulose blended spunbond nonwoven fabric, which comprises the following steps:(a) combining a graphite powder with a solution comprising 1 to 10 wt. % of a first compound selected from the group consisting of sulfuric acid (H2SO4), hydrochloric acid (HCl), perchloric acid (HClO4), hydrogen iodide (HI), hydrofluoric acid (HF), and nitric acid (HNO3), then stirring for 30 minutes in an ice bath environment;
(b) adding a solution comprising 1 to 20 wt. % potassium permanganate (KMnO4) to the product of step (a), stirring for 1 to 2 hours, and adding distilled water, wherein the potassium permanganate solution is continuously added until reaction of the potassium permanganate and the product of step (a) and the distilled water is complete;
(c) adding a solution comprising 1 to 10 wt. % hydrogen peroxide (H2O2) to the product of step (b), wherein the hydrogen peroxide solution is added until reaction between the hydrogen peroxide and the product step (b) is complete and the mixture becomes green, then filtering the green solution into a cake;
(d) rinsing the cake of step (c) with a solution comprising 5 wt. % hydrochloric acid (HCl) to remove sulfate ions, then washing the cake with distilled water;
(e) drying the cake of step (d) in an oven at 40° C. for 2 hrs to obtain a dried solid graphite oxide;
(f) adding distilled water to the dried solid graphite oxide of step (e), wherein the distilled water is added up to 200 mls per 0.06 to 1.0 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 wt. % to 0.5 wt. %;
(g) adding a solution comprising 1 to 10 wt. % of a second compound selected from the group consisting of sodium borohydride (NaBH4), potassium borohydride (KBH4), lithium aluminum hydride (LiAlH4), and sodium citrate (C6H5Na3O7) to the graphite oxide solution of step (f), then treating by ultrasonic vibration for 30 to 60 minutes, wherein in the resulting solution, the ratio of graphene oxide to the second compound is 1:1 to 1:5 by weight;
(h) filtrating the product of step (g), washing the filtrate with water 3 to 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 to 80° C., wherein the graphene solution of step (h) is added in a ratio of 0.11 to 5.0 wt. %, the pulp is selected from the group consisting of wood pulp, cotton pulp, bamboo pulp and a mixture of cotton and bamboo pulp, the pulp comprises ?-cellulose in an amount of 65% or more with a polymerization degree of 500 to 1500; and the NMMO has a concentration of 50% to 78%;
(j) removing water from the product of step (i) using a Thin Film Evaporator (TFE) and heating at 80 to 130° C., wherein the water is removed to 5% to 13% within 5 minutes and the cellulose is dissolved to form a spinning dope, and the amount ratio of each component among the components comprised in the dope is: water (H2O) 5% to 15%, N-methylmorpholine N-oxide (NMMO) 70% to 90%, and cellulose 5% to 15%;
(k) Squeezing the spinning dope of step (j) from a spinning orifice by using a spunbond process to form a natural graphene cellulose blended filament strand, which comprises pressuring the spinning dope by a metering pump, filtering and degassing by a continuous filter (CPF), transporting the spinning dope into a spinning tank, and stretching the spinning dope outward by air gap cooling through the spinning orifice, to form a natural graphene cellulose blended filament strand; and
(l) feeding the natural graphene cellulose blended filament strand of step (k) into a coagulation liquid, solidifying and regenerating the filament strand, stretching the filament strand under high pressure and high speed by an air stream drafting device, stacking the filament strand on a collection web to form a fibrous network structure, and washing, water needle punching, drying, oiling and coiling the fibrous network structure to form a natural graphene cellulose blended spunbond nonwoven fabric, wherein the concentration of the coagulation liquid is between 2.0% to 10.0%, and after washing, the amount of residual NMMO solvent is less than 0.1%.

US Pat. No. 9,745,673

SPUNBOND METHOD FOR PRODUCING NON-WOVEN FABRICS WITH HYGROSCOPIC METASTATIC FEATURE

ACELON CHEMICALS AND FIBE...

14. A spunbond method for producing nonwoven fabrics with hygroscopic metastatic feature comprises following steps:
a. Prepare macromolecule polymer of bio-polyamide 6,10 as raw material;
b. Fuse the bio-polyamide 6,10 into a melt of molten substance under high temperature in range of 250-280 degree centigrade
(250-280° C.);

c. Via melt spinning method, the melt is firstly fed into and extruded out of an extruder with extruding quantity in range
of 100-50,000 c.c./min, next the melt is fed into a spin-pack and forcedly spun out of spin heads into filaments, then external
compressed quenching air with temperature range of 15-25 degrees centigrade (15-25° C.) is continuously blown through for
cooling and drawing the filaments into fibrous tow of bio-polyamide 6,10 by collecting means;

d. Extend the fibrous tow of bio-polyamide 6,10 into certain specification of fiber size, then cut the filaments in the fibrous
tow of bio-polyamide 6,10 into staples of bio-polyamide 6,10 with specific length;

e. Card and spread the staples of bio-polyamide 6,10 on a conveyer to form a substrate fibrous web with thickness in range
of 0.3-2.5 mm;

f. Prepare pulp as raw material with content cellulose over 65% and degree of polymerization (DP) in range of 500-1500;
g. By putting N-methylmorpholine N-oxide (NMMO) as dissolving solvent into prepared pulp for high speed blending and dissolving
under low temperature in range from 60-90 degrees centigrade (60-90° C.), then dehydrate it via heating up to temperature
in range from 80-120 degrees centigrade (80-120° C.) for 5 minutes to decrease water content thereof down to 5-13% so that
a homogenized mucilaginous dope is formed;

h. Via spunbond method, the dope is forcedly spun out of spin nozzles for converting it into natural cellulose filaments,
and draw the natural cellulose filaments by an airflow draw jet device or airflow draw stretcher to become uniform fine natural
cellulose filaments, then bond and overlay these fine natural cellulose filaments on existing substrate fibrous web of natural
bio-polyamide 6,10 filaments on the conveyer in step e to form an overlaid fibrous web;

i. The fine fibrous web of the bio-polyamide 6,10 and natural cellulose is coagulated with regeneration by means of ejecting
mist aerosol of water to become fibrous composite web, then the dissolving solvent of N-methylmorpholine N-oxide (NMMO) is
washed out by water rinsing; and

j. After post treatments of hydro-entangled needle punching, drying, winding-up processes have been orderly applied, then
the fibrous composite web of the bio-polyamide 6,10 and natural cellulose is converted into nonwoven fabric of continuous
filament with hygroscopic metastatic feature.

US Pat. No. 9,573,308

MELTBLOWN METHOD FOR PRODUCING NONWOVEN FABRICS WITH HYGROSCOPIC METASTATIC FEATURE

ACELON CHEMICALS AND FIBE...

1. A meltblown method for producing a nonwoven fabric with hygroscopic metastatic features comprising the following steps:
a. preparing a raw material comprising a macromolecule polymer of bio-polyamide 6,10;
b. fusing the macromolecule polymer of bio-polyamide 6,10 of step a. into a melt at a temperature of 250-280° C.;
c. melt blowing the melt of step b. by blowing the melt from spinnerets to form bio-polyamide 6,10 filaments;
d. blowing the bio-polyamide 6,10 filaments of step c. onto a conveyer to form a substrate fibrous web with a thickness of
0.3-2.5 mm;

e. preparing a raw material comprising pulp with a cellulose content of over 65% and a degree of polymerization (DP) of 500-1500;
f. dissolving the pulp of step e. with N-methylmorpholine N-oxide (NMMO) by blending the pulp with NMMO at a temperature of
60° C.-90° C., then dehydrating the dissolved pulp by heating to 80° C.-120° C. to form a homogenized mucilaginous dope;

g. melt blowing the dope of step f. by blowing the dope from spinnerets and laying up over the substrate fibrous web of step
d. to form a fibrous composite web of the bio-polyamide 6,10 and cellulose in overlaid lamination;

h. regenerating the fibrous composite web of step f. by misting the web with aerosolized water, then washing out the NMMO
by rinsing with water;

i. treating the regenerated fibrous composite web of step h. by needle punching, drying, and winding-up to obtain the nonwoven
fabric with hygroscopic metastatic features.

US Pat. No. 10,190,243

METHOD OF PREPARING OF NATURAL GRAPHENE CELLULOSE BLENDED MELTBLOWN NONWOVEN FABRIC

ACELON CHEMICALS AND FIBE...

1. A method of preparing natural graphene cellulose blended meltblown nonwoven fabric, which comprises the following steps:(a) combining a graphite powder with a solution comprising 1 to 10 wt. % of a first compound selected from the group consisting of sulfuric acid (H2SO4), hydrochloric acid (HCl), perchloric acid (HClO4), hydrogen iodide (HI), hydrofluoric acid (HF), and nitric acid (HNO3), then stirring for 30 minutes in an ice bath environment;
(b) adding a solution comprising 1 to 20 wt. % potassium permanganate (KMnO4) to the product of step (a), stirring for 1 to 2 hours, and adding distilled water, wherein the potassium permanganate solution is continuously added until reaction of the potassium permanganate and the product of step (a) and the distilled water is complete;
(c) adding a solution comprising 1 to 10 wt. % hydrogen peroxide (H2O2) to the product of step (b), wherein the hydrogen peroxide solution is added until reaction between the hydrogen peroxide and the product step (b) is complete and the mixture becomes green, then filtering the green solution into a cake;
(d) rinsing the cake of step (c) with a solution comprising 5 wt. % hydrochloric acid (HCl) to remove sulfate ions, then washing the cake with distilled water;
(e) drying the cake of step (d) in an oven at 40° C. for 2 hrs to obtain a dried solid graphite oxide;
(f) adding distilled water to the dried solid graphite oxide of step (e), wherein the distilled water is added up to 200 mls per 0.06 to 1.0 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 wt. % to 0.5 wt. %;
(g) adding a solution comprising 1 to 10 wt. % of a second compound selected from the group consisting of sodium borohydride (NaBH4), potassium borohydride (KBH4), lithium aluminum hydride (LiAlH4), and sodium citrate (C6H5Na3O7) to the graphite oxide solution of step (f), then treating by ultrasonic vibration for 30 to 60 minutes, wherein in the resulting solution, the ratio of graphene oxide to the second compound is 1:1 to 1:5 by weight;
(h) filtrating the product of step (g), washing the filtrate with water 3 to 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 to 80° C., wherein the graphene solution of step (h) is added in a ratio of 0.11 to 5.0 wt. %, the pulp is selected from the group consisting of wood pulp, cotton pulp, bamboo pulp and a mixture of cotton and bamboo pulp, the pulp comprises ?-cellulose in an amount of 65% or more with a polymerization degree of 500 to 1500; and the NMMO has a concentration of 50% to 78%;
(j) removing water from the product of step (i) using a Thin Film Evaporator (TFE) and heating at 80 to 130° C., wherein the water is removed to 5% to 13% within 5 minutes and the cellulose is dissolved to form a spinning dope, and the amount ratio of each component among the components comprised in the dope is: water (H2O) 5% to 15%, N-methylmorpholine N-oxide (NMMO) 70% to 90%, and cellulose 5% to 15%;
(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 on a collector, which comprises pressuring the spinning dope by a metering pump, filtrating and degassing by a continuous filter (CPF), 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, wherein the concentration of the coagulation liquid is between 2.0% to 10.0%, and after washing, the amount of residual NMMO solvent is less than 0.1%.

US Pat. No. 9,868,240

SPUNBOND METHOD FOR PRODUCING NON-WOVEN FABRIC WITH DEODORANT FEATURE FROM BAMBOO CELLULOSE

ACELON CHEMICALS AND FIBE...

1. A spunbond method for producing non-woven fabric with deodorant feature from bamboo cellulose comprises the following process
steps:
a. selecting bamboo pulp and wasted coffee residue as raw materials to blend together mutually into a bamboo pulp mixture,
wherein a cellulose content of the bamboo pulp is over 50% and a range for degree of polymerization (DP) is 350-750, and said
wasted coffee residue having been ground into a size range of 500-900 nm granules in high speed mode;

b. putting N-methylmorpholine N-oxide (NMMO) as a primary dissolving solvent and 1,3-phenylene-bis 2-oxazoline (BOX) as an
additive stabilizer into the bamboo pulp mixture for blending and dissolving under low temperature in a range of 50-70 degree
centigrade (50-70° C. ) via rapid grinding using a horizontal dope blending machine; and, by means of cellulose features of
high expanding, moistening and dissolving ability as well as high rate of dissolving speed affected by the NMMO to expedite
a mutually blending and dissolving effect for forming a slurry; then, dehydrating the slurry via heating up to a temperature
in a range of 80-100 degree centigrade (80-100° C. ) using a vacuum thin film evaporator (TFE) for 5 minutes to decrease a
water content thereof to an range down to 5-13% so that a homogenized mucilaginous dope is formed;

c. via a spunbond method, the mucilaginous dope is firstly fed into and extruded out of an extruder, henceforth the mucilaginous
dope is fed into a spin-pack and forcedly spun out of spin nozzles by means of a gear pump, afterward external compressed
quenching air is continuously blown through for cooling and preliminarily drawing the mucilaginous dope for converting the
mucilaginous dope into bamboo cellulose filaments by means of an air gap by latterly drawing the bamboo cellulose filaments
using an airflow draw jet device to become bamboo filaments of fibrous strand, wherein the ranges for distance of the air
gap, temperature and relative humidity of the quenching air are 2-30 cm, 5-35 degrees centigrade (5-35° C. ) and 60-90% respectively;

d. coagulating and regenerating the bamboo filaments of fibrous strand in a coagulating liquid, by drawing the bamboo filaments
of fibrous strand using the airflow draw jet device with drawing speed thereof in a range of 20-3000 m/min to become uniform
fine bamboo cellulose filaments, then bonding and laying said bamboo filaments of fibrous strand on a belt collector to form
a webbed nonwoven wherein the ranges for temperature of the coagulating liquid and concentration for existing NMMO of dissolving
solvent are 5-30 degrees centigrade (5-30° C. ) and 0-30 wt % respectively; and

e. in after post treatments of water rinsing, orderly applying hydro-entangled needle punching and drying, wherein a resultant
nonwoven fabric having continuous filament of bamboo cellulose with deodorant feature is produced from the webbed nonwoven,

wherein the viscosity of cellulose for the dope in step b is in range of 6800-7600 poise,
wherein the non-woven fabric of bamboo cellulose in above step d, a fineness (or fiber number) for fiber in range of 15-30
?m, and

wherein the resultant nonwoven fabric has a deodorant capability of absorbing between 52.8 and 68.3%.

US Pat. No. 9,869,042

SPUNBOND METHOD FOR PRODUCING NON-WOVEN FABRIC OF NATURAL CELLULOSE WITH FLAME-RETARDING FEATURE

ACELON CHEMICALS AND FIBE...

1. A spunbond method for producing non-woven fabric of natural cellulose with flame-retarding feature comprises following
process steps:
a. preparing pulp of soft wood pulp or hard wood pulp as a raw material with content cellulose over 65% and degree of polymerization
(DP) in range of 450-1050;

b. blending and dissolving the pulp by putting N-methylmorpholine N-oxide (NMMO) as a dissolving solvent into the prepared
pulp for dissolving it into a slurry, and high speed blending under low temperature in a range of 50-80 degrees centigrade
(50-80° C.) by using a horizontal blending machine, wherein the concentration of the NMMO is in a percentage range of 45-78%;

c. evaporating extra water content from the prepared slurry by using a Thin Film Vacuum Evaporator (TFE) under temperature
in a range of 80-120 degrees centigrade (80-120° C.) and heated for 10 minutes for decreasing a water content thereof down
to 5-13% so that a homogenized mucilaginous dope is formed;

d. via a spunbond method, the dope is firstly fed into and extruded out of an extruder, henceforth the dope is fed into a
spin-pack and forcedly spun out of spin nozzles by means of a gear pump, afterward external compressed quenching air is continuously
blown through for cooling and preliminarily drawing the dope for converting it into natural cellulose filaments by means of
air gap, latterly drawing the natural cellulose filaments by using an airflow draw jet device or airflow draw stretcher to
become natural filaments of fibrous strand, wherein the ranges for distance of the air gap, temperature and relative humidity
of the quenching air are 0.5-30 cm, 5-35 degrees centigrade (5-35° C.) and 60-99% respectively;

e. coagulating and regenerating the natural filaments of fibrous strand in a coagulating liquid, and drawing the natural filaments
of fibrous strand by using an airflow draw jet device or airflow draw stretcher with drawing speed thereof in a range of 20-3000
m/min to form uniform fine natural cellulose filaments, then bonding and laying these natural filaments of fibrous strand
on a belt collector to form a webbed nonwoven, wherein the ranges for temperature of the coagulating liquid and concentration
for existing NMMO of dissolving solvent are 5-30 degrees centigrade (5-30° C.) and 0-30 wt % respectively;

f. after post treatments of water rinsing, hydro-entangled needle punching and drying have been orderly applied, then a normal
nonwoven fabric of natural cellulose is produced from the webbed nonwoven;

g. soaking a roll of the normal natural cellulose nonwoven in a flame retardant of N-hydroxymethyl-3-(dimethoxy-phosphate
acyl) propyl amide with concentration thereof in a range of 350-500 grams per liter (g/L); and

h. orderly baking, alkaline cleaning, water rinsing and drying, then winding up the soaking rolled normal natural cellulose
nonwoven to produce modified natural cellulose nonwoven of long-acting flame retarding feature, wherein the baking is performed
under temperature of 180 degree centigrade (180° C.) with baking time in a range of 120-240 seconds, the alkaline cleaning
is performed in an alkaline solution of sodium hydroxide (NaOH) with concentration of 50 grams per liter (g/L); and the coiling
speed is in a range of 2-200 meters per minute,

wherein the fineness of fiber for the modified natural cellulose nonwoven produced from spunbond process in step g is greater
than 15 and less than 50 ?m,

wherein the basis weight for the modified natural cellulose nonwoven produced from spunbond process in step g is in range
of 100-300 g/m2, and

wherein the modified natural cellulose nonwoven has a limit of oxygen index between 25 to 35 after 50 water rinsings.

US Pat. No. 10,132,007

FABRICATING METHOD FOR MELTBLOWN NONWOVEN FROM NATURAL CELLULOSE FIBER BLENDED WITH NANO SILVER

ACELON CHEMICALS AND FIBE...

1. A fabricating method for meltblown nonwoven from natural cellulose fiber blended with nano silver comprises following steps:(a) Put partially alkalized polyvinyl alcohol (PVA) power together with silver nitrate (AgNO3) solution as precursor thereof into pure water for agitating to form polyvinyl alcohol (PVA) solution in gel state such that the alkalization degree and the molecular weight of partially alkalized polyvinyl alcohol (PVA) power added is 86-89 mole % and 14,700-98,000 respectively while the weight percentage of polyvinyl alcohol (PVA) solution is 5-12 wt %, and the silver nitrate (AgNO3) solution is created by dissolving the silver nitrate (AgNO3) crystal into pure water;
(b) Put sodium borohydride (NaBH4) into the gel state polyvinyl alcohol (PVA) solution for reduction titration by agitating to form nano silver colloidal sol such that the reduction titration is performed by sodium borohydride (NaBH4) with mole ratio in range of 1:4-1:8, titration speed in range of 5-15 ml/min, agitating frequency about 200 rpm, and titration time in range of 10-20 minutes, and the concentration of produced nano silver sol is in range of 500-20,000 ppm while the diameter of the nano silver particle is in range of 10-150 nm;
(c) Put the nano silver colloidal sol into a mixing cellulose serum of wood pulp raw material and N-methylmorpholine N-oxide (NMMO) solvent for blending process to prepare blending mucilage such that the blending process is performed by putting raw material of chipped wood pulp, solvent of N-methylmorpholine N-oxide (NMMO), and stabilizer together into an expansion dissolving tank with constant temperature in range of 60-80 degrees centigrade (° C.) for blending agitation, and in association of dehydration in a vacuum condensing equipment with vacuum about 933 micro-Pa. Wherein, the weight percentage for the nano silver sol in the prepared blending mucilage is in range of 5-30 wt % while the concentration of the nano silver particle therein is in range of 100-5000 ppm;
(d) Evaporate water contained in the blending mucilage of nano silver colloidal sol and natural cellulose of wood pulp to form spinning dope by heating via a Thin Film Evaporator (TFE) under vacuum in range of 939-926 micro-Pa, heating temperature in range of 80-130 degrees centigrade (° C.) to dehydrate water down to range of 5-15% in 5 minutes so that the wood cellulose is dissolved into spinning dope, wherein the percentage of water (H2O) is in range of 9-18%, the percentage of N-methylmorpholine N-oxide (NMMO) is in range of 75-87%, and the percentage of cellulose is in range of 6-11%;
(e) Spin the spinning dope via “meltblown spinning method” by means of firstly conveying the spinning dope via boosted pressure to a continuous polymer filter (CPF) for filtration and defoaming treatment, secondly feeding the spinning dope into a spinning block for heating to melt the spinning dope by means of constantly blowing hot air into the spinning block, and finally meltblown extruding the melted spinning dope out of spinnerets to form into fibrous tow to form molten filament tow by means of jetting the hot air through circular air gaps the spinnerets;
(f) By means of ejecting mist aerosol of water, feed the molten filament tow into coagulation bath for coagulation, regeneration in coagulation liquid therein, and water rinse such that the concentration of the coagulation liquid is in range of 2.5-7.0%, and the residual quantity percentage of the N-methylmorpholine N-oxide (NMMO) solvent is less than 0.1% while the residual quantity percentage of the polyvinyl alcohol (PVA) solution is less than 0.3%, both of which become leftover mixture of residual N-methylmorpholine N-oxide (NMMO) solvent and residual polyvinyl alcohol (PVA) solution; and
(g) Lay and stack the molten filament tow out of coagulation bath onto a collecting net to form a fibrous web of nonwoven substrate, and after post treatments of hydro-entangled needle punching, drying, winding-up processes have been orderly applied on the fibrous web of nonwoven substrate, then the meltblown nonwoven of natural cellulose fiber blended with nano silver is fabricated completely.

US Pat. No. 10,132,009

FABRICATING METHOD FOR NATURAL CELLULOSE FIBER BLENDED WITH NANO SILVER

ACELON CHEMICALS AND FIBE...

1. A fabricating method for natural cellulose fiber blended with nano silver comprises following steps:(a) Put partially alkalized polyvinyl alcohol (PVA) power together with silver nitrate (AgNO3) solution as precursor thereof into pure water for agitating to form polyvinyl alcohol (PVA) solution in gel state such that the alkalization degree and the molecular weight of partially alkalized polyvinyl alcohol (PVA) power added is 86-89 mole % and 14,700-98,000 respectively while the weight percentage of polyvinyl alcohol (PVA) solution is 3-12 wt %, and the concentration of polyvinyl alcohol (PVA) solution is good enough to enclose and protect the micro silver particles formed therein because the polyvinyl alcohol (PVA) features in low polymerization degree and water-solubility at low temperature, and the silver nitrate (AgNO3) solution is created by dissolving the silver nitrate (AgNO3) crystal into pure water;
(b) Put sodium borohydride (NaBH4) into the gel state polyvinyl alcohol (PVA) solution for reduction titration by agitating to form nano silver colloidal sol such that the reduction titration is performed by sodium borohydride (NaBH4) with mole ratio in range of 1:4-1:8, titration speed in range of 5-15 ml/min, agitating frequency about 200 rpm, and titration time about 10 minutes, and the concentration of produced nano silver sol is in range of 500-20,000 ppm while the diameter of the nano silver particle is in range of 10-150 nm;
(c) Put the nano silver colloidal sol into a mixing cellulose serum of wood pulp raw material and N-methylmorpholine N-oxide (NMMO) solvent for blending process to prepare blending mucilage such that the blending process is performed by putting raw material of chipped wood pulp, solvent of N-methylmorpholine N-oxide (NMMO), and stabilizer together into an expansion dissolving tank with constant temperature in range of 60-80 degrees centigrade (° C.) for blending agitation, and in association of dehydration in a vacuum condensing equipment with vacuum about 933 micro-Pa. such that the content of ?-cellulose is over 85% while the polymerization degree for the cellulose of wood pulp is in range of 500-1200, and the weight percentage for the nano silver sol in the prepared blending mucilage is in range of 5-35 wt % while the concentration of the nano silver particle therein is in range of 100-5000 ppm;
(d) Evaporate water contained in the blending mucilage of nano silver colloidal sol and natural cellulose of wood pulp to form spinning dope by heating via a Thin Film Evaporator (TFE) under vacuum in range of 939-926 micro-Pa, heating temperature in range of 80-130 degrees centigrade (° C.) to dehydrate water down to range of 5-13% in 5 minutes so that the wood cellulose is dissolved into spinning dope with the composition percentages for all constituents in the spinning dope are as following: the percentage of water (H2O) is in range of 9-18%, the percentage of N-methylmorpholine N-oxide (NMMO) is in range of 75-87%, and the percentage of cellulose is in range of 6-11%;
(e) Spin the spinning dope via “Dry-Jet Wet Spinning Method” by means of conveying the spinning dope via boosted pressure to a continuous polymer filter (CPF) for filtration and defoaming treatment, feeding the spinning dope into a spinning block for extruding out as melt trickle via spinnerets therein, and thinning the melt trickle into fibrous tow by stretching it through an air gap to form bundle of fibrous tow;
(f) Feed the air cured fibrous tow into coagulation bath for coagulation, regeneration in coagulation liquid therein, and water rinse to form spinning filaments such that the concentration of the coagulation liquid is in range of 4.5-8.0%, and the residual quantity percentage of the N-methylmorpholine N-oxide (NMMO) solvent is less than 0.1% while the residual quantity percentage of the polyvinyl alcohol (PVA) solution is less than 0.3%; and
(g) Treat the spinning filaments with dry, oil and coil in proper order to produce final product of natural cellulose fiber blended with nano silver.

US Pat. No. 10,094,049

FABRICATING METHOD FOR SPUNBOND NONWOVEN FROM NATURAL CELLULOSE FIBER BLENDED WITH NANO SILVER

ACELON CHEMICALS AND FIBE...

1. A fabricating method for spunbond nonwoven from natural cellulose fiber blended with nano silver comprises following steps:(a) Put partially alkalized polyvinyl alcohol (PVA) power together with silver nitrate (AgNO3) solution as precursor thereof into pure water for agitating to form polyvinyl alcohol (PVA) solution in gel state such that the alkalization degree and the molecular weight of partially alkalized polyvinyl alcohol (PVA) power added is 86-89 mole % and 14,700-98,000 respectively while the weight percentage of polyvinyl alcohol (PVA) solution is 5-12 wt %, and the silver nitrate (AgNO3) solution is created by dissolving the silver nitrate (AgNO3) crystal into pure water;
(b) Put sodium borohydride (NaBH4) into the gel state polyvinyl alcohol (PVA) solution for reduction titration by agitating to form nano silver colloidal sol such that the reduction titration is performed by sodium borohydride (NaBH4) with mole ratio in range of 1:4-1:8, titration speed in range of 5-15 ml/min, agitating frequency about 200 rpm, and titration time in range of 10-20 minutes, and the concentration of produced nano silver sol is in range of 500-20,000 ppm while the diameter of the nano silver particle is in range of 10-150 nm;
(c) Put the nano silver colloidal sol into a mixing cellulose serum of wood pulp raw material and N-methylmorpholine N-oxide (NMMO) solvent for blending process to prepare blending mucilage such that the blending process is performed by putting raw material of chipped wood pulp, solvent of N-methylmorpholine N-oxide (NMMO), and stabilizer together into an expansion dissolving tank with constant temperature in range of 60-80 degrees centigrade (° C.) for blending agitation, and in association of dehydration in a vacuum condensing equipment with vacuum about 933 micro-Pa. Wherein, the raw material wood pulp is a mixture of soft wood and hard wood with blending weight ratio thereof in range of 0:100-100:0, and the content of ?-cellulose is over 85% while the polymerization degree for the cellulose of wood pulp thereof is in range of 500-1200, and the weight percentage for the nano silver sol in the prepared blending mucilage is in range of 5-35 wt % while the concentration of the nano silver particle therein is in range of 100-5000 ppm, as well as the chemical structures of the N-methylmorpholine N-oxide (NMMO) and pulp cellulose used here are shown as in FIGS. 3 and 4 respectively;
(d) Evaporate water contained in the blending mucilage of nano silver colloidal sol and natural cellulose of wood pulp to form spinning dope by heating via a Thin Film Evaporator (TFE) under vacuum in range of 939-926 micro-Pa, heating temperature in range of 80-130 degrees centigrade (° C.) to dehydrate water down to range of 9-18% in time range of 5-10 minutes so that the wood cellulose is dissolved into spinning dope such that the percentage of water (H2O) is in range of 9-18%, the percentage of N-methylmorpholine N-oxide (NMMO) is in range of 75-87%, and the percentage of cellulose is in range of 6-11%;
(e) Spin the spinning dope via “spunbond spinning method” by means of firstly conveying the spinning dope via boosted pressure to a continuous polymer filter (CPF) for filtration and defoaming treatment, secondly feeding the spinning dope into a spinning block for heating to melt the spinning dope by means of constantly blowing hot air into the spinning block, and finally spunbond extruding the melted spinning dope out of spinnerets to form into molten filament tow by means of jetting chilly quenching air through conical-frustum shell-shaped air gaps sheathing the spinnerets for quenched stretching process;
(f) By means of coagulation bath, feed the molten filament tow in a coagulation liquid for coagulation, regeneration, and water rinse such that the concentration of the coagulation liquid is in range of 2.5-7.0%, and the residual quantity percentage of the N-methylmorpholine N-oxide (NMMO) solvent is less than 0.1% while the residual quantity percentage of the polyvinyl alcohol (PVA) solution is less than 0.2%, both of which become leftover mixture of residual N-methylmorpholine N-oxide (NMMO) solvent and residual polyvinyl alcohol (PVA) solution; and
(g) By means of airflow draw stretcher, lay and stack the molten filament tow out of coagulation bath onto a collecting net to form a fibrous web of nonwoven substrate for high-speed stretching process under high pressure condition, and after post treatments of hydro-entangled needle punching, drying, winding-up processes have been orderly applied on the fibrous web of nonwoven substrate, then the spunbond nonwoven of natural cellulose fiber blended with nano silver is fabricated completely.