Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Wen-Tung CHOU

Patent

Atlas literature

Patent

US 10,190,243

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Wen-Tung CHOU

Method of Preparing of Natural Graphene Cellulose Blended Meltblown | Matter42 Literature

Process steps

Additional fabrication and treatment steps described in the patent.

Chemical Oxidation

Step 1

Temperature

20, 40°C

Duration

30, 120 min

Process details

step a:Combine graphite powder with 1-10 wt% acid (H₂SO4, HCl, HClO4, HI, HF, or HNO₃), stir 30 min in ice bath

step b:Add 1-20 wt% KMnO₄ solution, stir 1-2 hours, add distilled water until no purple smoke

step c:Add 1-10 wt% H₂O₂ until no bubbles and mixture is dark green, filter to cake

step d:Rinse cake with 5 wt% HCl to remove sulfate ions, wash with distilled water

step e:Dry cake at 40°C for 2 hrs to obtain dried solid graphite oxide

Materials:graphite powderH₂SO₄HClHClO₄HIHFHNO₃KMnO₄H₂O₂graphite oxide

Ultrasonic Dispersion

Step 2

Duration

30 min

Process details

step f:Add distilled water to dried solid graphite oxide (200 mL per 0.06-1.0 g graphite oxide), treat by ultrasonic vibration 30 min to obtain graphite oxide solution at 0.03-0.5 wt%

Materials:graphite oxide

Chemical Reduction

Step 3

Duration

30, 60 min

Process details

step g:Add 1-10 wt% reducing agent (NaBH4, KBH4, LiAlH4, or sodium citrate) to graphite oxide solution, treat by ultrasonic vibration 30-60 min; ratio of graphene oxide to reducing agent is 1:1 to 1:5 by weight

step h:Filter, wash filtrate with water 3-5 times, back-filtrate to obtain graphene solution

Materials:graphite oxideNaBH₄

Dissolution And Dope Preparation

Step 4

Temperature

60, 80, 80, 130°C

Duration

5 min

Process details

step i:Add graphene solution (0.11-5.0 wt%) to slurry of pulp (wood, cotton, bamboo, or cotton-bamboo mixture; alpha-cellulose >= 65%, polymerization degree 500-1500) with NMMO (50-78%) and stabilizer in expansion dissolving tank, mix at 60-80°C

Meltblown Spinning

Step 5

Ambient

hot air

Process details

step k:Squeeze spinning dope from spinning orifice by meltblown process; pressurize with metering pump, filter and degas with continuous filter (CPF), transport to spinning tank, blow hot air into orifice; form uniform natural graphene cellulose blended filament strand; pile onto fibrous network on collector

step l:Spray water mist to force filament strand into coagulation liquid (2.0-10.0%); solidify, regenerate, wash; water needle punch, dry, oil, coil to form final nonwoven fabric; residual NMMO after washing < 0.1%

Materials:

Reported properties

Performance values and ranges asserted in the specification or claims.

Property	Value	Material
Temperature	40–60 °C	—
Temperature	60–80 °C	—
Temperature	80–130 °C	—
Duration	1–2 hours	—
Duration	30–60 minutes	—
Duration	24–48 hours	—
Temperature	≤ 40 °C	—

Process steps

Additional fabrication and treatment steps described in the patent.

Chemical Oxidation

Step 1

Temperature

20, 40°C

Duration

30, 120 min

Process details

step a:Combine graphite powder with 1-10 wt% acid (H₂SO4, HCl, HClO4, HI, HF, or HNO₃), stir 30 min in ice bath

step b:Add 1-20 wt% KMnO₄ solution, stir 1-2 hours, add distilled water until no purple smoke

step c:Add 1-10 wt% H₂O₂ until no bubbles and mixture is dark green, filter to cake

step d:Rinse cake with 5 wt% HCl to remove sulfate ions, wash with distilled water

step e:Dry cake at 40°C for 2 hrs to obtain dried solid graphite oxide

Materials:graphite powderH₂SO₄HClHClO₄HIHFHNO₃KMnO₄H₂O₂graphite oxide

Ultrasonic Dispersion

Step 2

Duration

30 min

Process details

step f:Add distilled water to dried solid graphite oxide (200 mL per 0.06-1.0 g graphite oxide), treat by ultrasonic vibration 30 min to obtain graphite oxide solution at 0.03-0.5 wt%

Materials:graphite oxide

Chemical Reduction

Step 3

Duration

30, 60 min

Process details

step h:Filter, wash filtrate with water 3-5 times, back-filtrate to obtain graphene solution

Materials:graphite oxideNaBH₄

Dissolution And Dope Preparation

Step 4

Temperature

60, 80, 80, 130°C

Duration

5 min

Process details

Meltblown Spinning

Step 5

Ambient

hot air

Process details

Materials:

Reported properties

Performance values and ranges asserted in the specification or claims.

Property	Value	Material
Temperature	40–60 °C	—
Temperature	60–80 °C	—
Temperature	80–130 °C	—
Duration	1–2 hours	—
Duration	30–60 minutes	—
Duration	24–48 hours	—
Temperature	≤ 40 °C	—

Process steps

Additional fabrication and treatment steps described in the patent.

Chemical Oxidation

Step 1

Temperature

20, 40°C

Duration

30, 120 min

Process details

step a:Combine graphite powder with 1-10 wt% acid (H₂SO4, HCl, HClO4, HI, HF, or HNO₃), stir 30 min in ice bath

step b:Add 1-20 wt% KMnO₄ solution, stir 1-2 hours, add distilled water until no purple smoke

step c:Add 1-10 wt% H₂O₂ until no bubbles and mixture is dark green, filter to cake

step d:Rinse cake with 5 wt% HCl to remove sulfate ions, wash with distilled water

step e:Dry cake at 40°C for 2 hrs to obtain dried solid graphite oxide

Materials:graphite powderH₂SO₄HClHClO₄HIHFHNO₃KMnO₄H₂O₂graphite oxide

Ultrasonic Dispersion

Step 2

Duration

30 min

Process details

step f:Add distilled water to dried solid graphite oxide (200 mL per 0.06-1.0 g graphite oxide), treat by ultrasonic vibration 30 min to obtain graphite oxide solution at 0.03-0.5 wt%

Materials:graphite oxide

Chemical Reduction

Step 3

Duration

30, 60 min

Process details

step h:Filter, wash filtrate with water 3-5 times, back-filtrate to obtain graphene solution

Materials:graphite oxideNaBH₄

Dissolution And Dope Preparation

Step 4

Temperature

60, 80, 80, 130°C

Duration

5 min

Process details

Meltblown Spinning

Step 5

Ambient

hot air

Process details

Materials:

Reported properties

Performance values and ranges asserted in the specification or claims.

Property	Value	Material
Temperature	40–60 °C	—
Temperature	60–80 °C	—
Temperature	80–130 °C	—
Duration	1–2 hours	—
Duration	30–60 minutes	—
Duration	24–48 hours	—
Temperature	≤ 40 °C	—

Process steps

Additional fabrication and treatment steps described in the patent.

Chemical Oxidation

Step 1

Temperature

20, 40°C

Duration

30, 120 min

Process details

step a:Combine graphite powder with 1-10 wt% acid (H₂SO4, HCl, HClO4, HI, HF, or HNO₃), stir 30 min in ice bath

step b:Add 1-20 wt% KMnO₄ solution, stir 1-2 hours, add distilled water until no purple smoke

step c:Add 1-10 wt% H₂O₂ until no bubbles and mixture is dark green, filter to cake

step d:Rinse cake with 5 wt% HCl to remove sulfate ions, wash with distilled water

step e:Dry cake at 40°C for 2 hrs to obtain dried solid graphite oxide

Materials:graphite powderH₂SO₄HClHClO₄HIHFHNO₃KMnO₄H₂O₂graphite oxide

Ultrasonic Dispersion

Step 2

Duration

30 min

Process details

step f:Add distilled water to dried solid graphite oxide (200 mL per 0.06-1.0 g graphite oxide), treat by ultrasonic vibration 30 min to obtain graphite oxide solution at 0.03-0.5 wt%

Materials:graphite oxide

Chemical Reduction

Step 3

Duration

30, 60 min

Process details

step h:Filter, wash filtrate with water 3-5 times, back-filtrate to obtain graphene solution

Materials:graphite oxideNaBH₄

Dissolution And Dope Preparation

Step 4

Temperature

60, 80, 80, 130°C

Duration

5 min

Process details

Meltblown Spinning

Step 5

Ambient

hot air

Process details

Materials:

Reported properties

Performance values and ranges asserted in the specification or claims.

Property	Value	Material
Temperature	40–60 °C	—
Temperature	60–80 °C	—
Temperature	80–130 °C	—
Duration	1–2 hours	—
Duration	30–60 minutes	—
Duration	24–48 hours	—
Temperature	≤ 40 °C	—

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Method of Preparing of Natural Graphene Cellulose Blended Meltblown

Drawings

Claims

Materials

Process steps

Characterization

Reported properties

Why these are connected

Drawings

Claims

Materials

Process steps

Characterization

Reported properties

Why these are connected

Drawings

Claims

Materials

Process steps

Characterization

Reported properties

Why these are connected

Drawings

Claims

Materials

Process steps

Characterization

Reported properties

Why these are connected