阅读说明：本技术 一种由熔喷布为基础碳化制备碳纤维布的方法 (Method for preparing carbon fiber cloth by carbonizing melt-blown cloth ) 是由 马文涯 于 2020-12-30 设计创作，主要内容包括：本发明提供一种由熔喷布为基础碳化制备碳纤维布的方法,涉及碳纤维布制备领域。该由熔喷布为基础碳化制备碳纤维布的方法,包括以下步骤：S1.准备原料；S2.对熔喷布改性；S3.熔喷布上包覆氧化铁膜；S4.干燥处理；S5.对熔喷布进行预氧化和碳化；S6.制成碳纤维布。通过表面改性剂先对熔喷布进行改性,然后加入氧化铁前驱物和氨水,通过化学液相沉淀在熔喷布表面沉淀氧化铁膜,然后再放入气氛炉中进行预氧化和碳化制得碳纤维布,这样可以使聚丙烯纤维在预氧化过程中提供以氧化铁为催化基础的预氧化,使聚丙烯纤维逐渐转变为碳链为主的结构,提高了纤维的抗温变性能,进而能在高温状态下发生高温碳化的时候保持形态,值得大力推广。(The invention provides a method for preparing carbon fiber cloth by carbonizing melt-blown cloth, and relates to the field of carbon fiber cloth preparation. The method for preparing the carbon fiber cloth by carbonizing the melt-blown cloth as the basis comprises the following steps: s1, preparing raw materials; s2, modifying the melt-blown fabric; s3, coating an iron oxide film on the melt-blown fabric; s4, drying; s5, pre-oxidizing and carbonizing the melt-blown fabric; and S6, manufacturing the carbon fiber cloth. The surface modifier is used for modifying the melt-blown fabric firstly, then the ferric oxide precursor and ammonia water are added, a ferric oxide film is precipitated on the surface of the melt-blown fabric through chemical liquid phase precipitation, then the melt-blown fabric is put into an atmosphere furnace for pre-oxidation and carbonization to prepare the carbon fiber fabric, so that the polypropylene fiber is pre-oxidized on the basis of the ferric oxide in the pre-oxidation process, the polypropylene fiber is gradually changed into a structure with a carbon chain as a main part, the temperature resistance of the fiber is improved, and then the form can be kept when high-temperature carbonization is carried out at a high temperature state, and the surface modifier is worthy of being widely popularized.)

1. A method for preparing carbon fiber cloth by taking melt-blown cloth as a base for carbonization is characterized by comprising the following steps: the method comprises the following steps:

s1, preparing

Firstly, preparing the following raw materials in parts by weight: 100 parts of melt-blown fabric, 3-30 parts of ferric oxide precursor and 0.1-1 part of surface modifier;

s2. modification

Filling water into the corrosion-resistant tank, raising the temperature to 90 ℃, soaking the melt-blown fabric in the corrosion-resistant tank, adding the surface modifier into the corrosion-resistant tank, and uniformly stirring;

s3. laminating

Adding an iron oxide precursor into a corrosion-resistant groove, blowing air into the corrosion-resistant groove to change the solution in the corrosion-resistant groove into reddish brown, then slowly dropwise adding ammonia water, precipitating an iron oxide film on the surface of a meltblown fabric fiber through chemical liquid-phase precipitation, observing the coloring condition of the meltblown fabric, supplementing an equal amount of the iron oxide precursor if the meltblown fabric is uniformly reddish brown, continuously blowing air, slowly dropwise adding ammonia water until the pH value of the solution is less than 5, then stopping adding the ammonia water, supplementing an equal amount of a surface modifier if the meltblown fabric is non-uniform, simultaneously continuously blowing air, then slowly dropwise adding ammonia water until the pH value of the solution is less than 5, and then stopping adding the ammonia water;

s4, drying

Fishing out the uniformly colored melt-blown fabric from the corrosion-resistant tank, rinsing the melt-blown fabric with clear water until the rinsing liquid is neutral, then putting the melt-blown fabric into a drying box, and drying the melt-blown fabric at the temperature of 100-110 ℃;

s5, carbonizing

Putting the dried modified melt-blown fabric into an atmosphere furnace, introducing nitrogen into the atmosphere furnace for protection, heating to 130 ℃, detecting the moisture content in the tail gas of the atmosphere furnace by using humidity detection equipment, heating to 5 ℃ and preserving heat for 30min when no moisture exists, repeatedly heating to 150 ℃, introducing reducing gas into the atmosphere furnace, adjusting the introduction amount of the nitrogen to be the lowest, preserving heat for 30min, heating to 5 ℃ and 400 ℃ every 5min, and heating to 10 ℃ and 1000 ℃ every 3min, so that the modified melt-blown fabric can be carbonized into carbon fiber fabric;

s6, finished product

And (3) closing the heating of the atmosphere furnace, continuously keeping the lowest introduction amount of nitrogen, slowly reducing the temperature in the atmosphere furnace to room temperature, taking out the carbon fiber cloth, dissolving the iron layer on the surface of the carbon fiber cloth by using dilute hydrochloric acid, washing the carbon fiber cloth by using water until the water solution is neutral, and drying to obtain the finished carbon fiber cloth.

2. The method for preparing the carbon fiber cloth by taking the melt-blown cloth as the base through carbonization as claimed in claim 1, wherein: the surface modifier is one of silane coupling agent, titanate coupling agent and aluminate coupling agent.

3. The method for preparing the carbon fiber cloth by taking the melt-blown cloth as the base through carbonization as claimed in claim 1, wherein: the ferric oxide precursor is one of ferrous chloride, ferric sulfate or ferrous sulfate.

4. The method for preparing the carbon fiber cloth by taking the melt-blown cloth as the base through carbonization as claimed in claim 1, wherein: the temperature in the atmosphere furnace is pre-oxidized when the temperature ranges from 130 ℃ to 150 ℃.

5. The method for preparing the carbon fiber cloth by taking the melt-blown cloth as the base through carbonization as claimed in claim 1, wherein: the reducing gas is hydrogen-carbon oxide or one of ethanol and methanol.

Technical Field

The invention relates to the field of carbon fiber cloth preparation, in particular to a method for preparing carbon fiber cloth by carbonizing melt-blown cloth.

Background

The melt-blown cloth is the most core material of the mask, the melt-blown cloth mainly takes polypropylene as a main raw material, the fiber diameter can reach 1-5 microns, the gaps are large, the structure is fluffy, the anti-wrinkle capacity is good, and the number and the surface area of fibers in unit area are increased by the superfine fibers with unique capillary structures, so that the melt-blown cloth has good filtering property, shielding property, heat insulation property and oil absorption property, and can be used in the fields of air, liquid filtering materials, isolating materials, absorbing materials, mask materials, warm-keeping materials, oil absorbing materials, wiping cloth and the like.

The meltblown fabric is a non-woven fabric formed by spraying polypropylene with a high-speed air stream, and thus has very poor adsorption performance for polar molecules, and polypropylene fibers cannot be directly carbonized into carbon fiber fabrics.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention provides a method for preparing carbon fiber cloth by carbonizing melt-blown cloth as a base, which solves the problem that the melt-blown cloth can not be directly carbonized into the carbon fiber cloth.

(II) technical scheme

In order to achieve the purpose, the invention is realized by the following technical scheme: a method for preparing carbon fiber cloth by carbonizing melt-blown cloth comprises the following steps:

s1, preparing

Firstly, preparing the following raw materials in parts by weight: 100 parts of melt-blown fabric, 3-30 parts of ferric oxide precursor and 0.1-1 part of surface modifier;

s2. modification

Filling water into the corrosion-resistant tank, raising the temperature to 90 ℃, soaking the melt-blown fabric in the corrosion-resistant tank, adding the surface modifier into the corrosion-resistant tank, and uniformly stirring;

s3. laminating

Adding an iron oxide precursor into a corrosion-resistant groove, blowing air into the corrosion-resistant groove to change the solution in the corrosion-resistant groove into reddish brown, then slowly dropwise adding ammonia water, precipitating an iron oxide film on the surface of a meltblown fabric fiber through chemical liquid-phase precipitation, observing the coloring condition of the meltblown fabric, supplementing an equal amount of the iron oxide precursor if the meltblown fabric is uniformly reddish brown, continuously blowing air, slowly dropwise adding ammonia water until the pH value of the solution is less than 5, then stopping adding the ammonia water, supplementing an equal amount of a surface modifier if the meltblown fabric is non-uniform, simultaneously continuously blowing air, then slowly dropwise adding ammonia water until the pH value of the solution is less than 5, and then stopping adding the ammonia water;

s4, drying

Fishing out the uniformly colored melt-blown fabric from the corrosion-resistant tank, rinsing the melt-blown fabric with clear water until the rinsing liquid is neutral, then putting the melt-blown fabric into a drying box, and drying the melt-blown fabric at the temperature of 100-110 ℃;

s5, carbonizing

Putting the dried modified melt-blown fabric into an atmosphere furnace, introducing nitrogen into the atmosphere furnace for protection, heating to 130 ℃, detecting the moisture content in the tail gas of the atmosphere furnace by using humidity detection equipment, heating to 5 ℃ and preserving heat for 30min when no moisture exists, repeatedly heating to 150 ℃, introducing reducing gas into the atmosphere furnace, adjusting the introduction amount of the nitrogen to be the lowest, preserving heat for 30min, heating to 5 ℃ and 400 ℃ every 5min, and heating to 10 ℃ and 1000 ℃ every 3min, so that the modified melt-blown fabric can be carbonized into carbon fiber fabric;

s6, finished product

And (3) closing the heating of the atmosphere furnace, continuously keeping the lowest introduction amount of nitrogen, slowly reducing the temperature in the atmosphere furnace to room temperature, taking out the carbon fiber cloth, dissolving the iron layer on the surface of the carbon fiber cloth by using dilute hydrochloric acid, washing the carbon fiber cloth by using water until the water solution is neutral, and drying to obtain the finished carbon fiber cloth.

Preferably, the surface modifier is one of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent.

Preferably, the ferric oxide precursor is one of ferrous chloride, ferric sulfate or ferrous sulfate.

Preferably, the temperature in the atmosphere furnace is pre-oxidized when the temperature ranges from 130 ℃ to 150 ℃.

Preferably, the reducing gas is hydrogen-carbon oxide or one of ethanol and methanol.

(III) advantageous effects

The invention provides a method for preparing carbon fiber cloth by carbonizing melt-blown cloth. The method has the following beneficial effects:

according to the invention, the melt-blown cloth is modified by the surface modifier, then the ferric oxide precursor and ammonia water are added, the ferric oxide film is precipitated on the surface of the melt-blown cloth through chemical liquid phase precipitation, and then the melt-blown cloth is put into an atmosphere furnace for pre-oxidation and carbonization to prepare the carbon fiber cloth, so that the polypropylene fiber is subjected to pre-oxidation based on ferric oxide catalysis in the pre-oxidation process, the polypropylene fiber is gradually converted into a structure mainly comprising a carbon chain, the temperature resistance of the fiber is improved, and the shape of the fiber can be maintained when the fiber is subjected to high-temperature carbonization at a high temperature, so that the melt-blown cloth can be directly carbonized to prepare the carbon fiber cloth, the process is simpler, and the carbon fiber cloth is worthy of great.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The first embodiment is as follows:

the embodiment of the invention provides a method for preparing carbon fiber cloth by carbonizing melt-blown cloth, which comprises the following steps:

s1, preparing

Firstly, preparing the following raw materials in parts by weight: 100 parts of melt-blown cloth, 3 parts of ferric oxide precursor and 0.1 part of surface modifier;

s2. modification

The method comprises the following steps of filling water into a corrosion resistant groove, raising the temperature to 90 ℃, soaking a melt-blown fabric into the corrosion resistant groove, adding a surface modifier into the corrosion resistant groove, uniformly stirring, wherein the base material of the melt-blown fabric is a polypropylene material and has poor polar molecule adsorption performance, so that the affinity of the polypropylene fiber to polar molecules is enhanced by adding the surface modifier to modify the surface of the polypropylene fiber, and the melt-blown fabric is produced by drawing under the drive of high-speed airflow, the fiber thickness is different, the specific surface of production batches is completely different, so that the amount of the added surface modifier is required to be kept at 0.1-1% of the amount of the melt-blown fabric;

s3. laminating

Adding an iron oxide precursor into a corrosion-resistant groove, blowing air into the corrosion-resistant groove to change the solution in the corrosion-resistant groove into reddish brown, then slowly dropwise adding ammonia water, precipitating an iron oxide film on the surface of a meltblown fabric fiber through chemical liquid phase precipitation, observing the coloring condition of the meltblown fabric, supplementing the equal amount of the iron oxide precursor if the reddish brown on the meltblown fabric is uniform, continuously blowing air, slowly dropwise adding the ammonia water until the pH value of the solution is less than 5, then stopping adding the ammonia water, supplementing the equal amount of a surface modifier if the reddish brown on the meltblown fabric is not uniform, simultaneously continuously blowing air, then slowly dropwise adding the ammonia water until the pH value of the solution is less than 5, then stopping adding the ammonia water, modifying and laminating to ensure that the polypropylene fiber is subjected to preoxidation based on iron oxide catalysis in the preoxidation process, so that the polypropylene fiber is gradually changed into a structure mainly based on carbon chains, and the temperature resistance of the fiber is improved, the shape can be kept when high-temperature carbonization is carried out at a high temperature, so that the melt-blown cloth can be directly carbonized to prepare carbon fiber cloth;

s4, drying

Fishing out the uniformly colored melt-blown cloth from the corrosion-resistant tank, rinsing the melt-blown cloth with clear water until the rinsing liquid is neutral, then putting the melt-blown cloth into a drying box, and drying the melt-blown cloth at the temperature of 100 ℃;

s5, carbonizing

Putting the dried modified melt-blown fabric into an atmosphere furnace, introducing nitrogen into the atmosphere furnace for protection, heating to 130 ℃, detecting the moisture content in the tail gas of the atmosphere furnace by using humidity detection equipment, heating to 5 ℃ and preserving heat for 30min when no moisture exists, repeatedly heating to 150 ℃, introducing reducing gas into the atmosphere furnace, adjusting the introduction amount of the nitrogen to be the lowest, preserving heat for 30min, heating to 5 ℃ and 400 ℃ every 5min, and heating to 10 ℃ and 1000 ℃ every 3min, so that the modified melt-blown fabric can be carbonized into carbon fiber fabric;

s6, finished product

And (3) closing the heating of the atmosphere furnace, continuously keeping the lowest introduction amount of nitrogen, slowly reducing the temperature in the atmosphere furnace to room temperature, taking out the carbon fiber cloth, dissolving the iron layer on the surface of the carbon fiber cloth by using dilute hydrochloric acid, washing the carbon fiber cloth by using water until the water solution is neutral, and drying to obtain the finished carbon fiber cloth.

The surface modifier is one of silane coupling agent, titanate coupling agent and aluminate coupling agent.

The ferric oxide precursor is one of ferrous chloride, ferric sulfate or ferrous sulfate, wherein the ferrous chloride contains less acid radicals than trivalent, and the material consumption is relatively low, so the ferrous chloride is mainly used.

The temperature in the atmosphere furnace is pre-oxidized when the temperature is in the range of 130-150 ℃.

The reducing gas is hydrogen-carbon oxide or one of ethanol and methanol.

Example two:

the embodiment of the invention provides a method for preparing carbon fiber cloth by carbonizing melt-blown cloth, which comprises the following steps:

s1, preparing

Firstly, preparing the following raw materials in parts by weight: 100 parts of melt-blown cloth, 30 parts of an iron oxide precursor and 1 part of a surface modifier;

s2. modification

The method comprises the following steps of filling water into a corrosion resistant groove, raising the temperature to 90 ℃, soaking a melt-blown fabric into the corrosion resistant groove, adding a surface modifier into the corrosion resistant groove, uniformly stirring, wherein the base material of the melt-blown fabric is a polypropylene material and has poor polar molecule adsorption performance, so that the affinity of the polypropylene fiber to polar molecules is enhanced by adding the surface modifier to modify the surface of the polypropylene fiber, and the melt-blown fabric is produced by drawing under the drive of high-speed airflow, the fiber thickness is different, the specific surface of production batches is completely different, so that the amount of the added surface modifier is required to be kept at 0.1-1% of the amount of the melt-blown fabric;

s3. laminating

Adding an iron oxide precursor into a corrosion-resistant groove, blowing air into the corrosion-resistant groove to change the solution in the corrosion-resistant groove into reddish brown, then slowly dropwise adding ammonia water, precipitating an iron oxide film on the surface of a meltblown fabric fiber through chemical liquid phase precipitation, observing the coloring condition of the meltblown fabric, supplementing the equal amount of the iron oxide precursor if the reddish brown on the meltblown fabric is uniform, continuously blowing air, slowly dropwise adding the ammonia water until the pH value of the solution is less than 5, then stopping adding the ammonia water, supplementing the equal amount of a surface modifier if the reddish brown on the meltblown fabric is not uniform, simultaneously continuously blowing air, then slowly dropwise adding the ammonia water until the pH value of the solution is less than 5, then stopping adding the ammonia water, modifying and laminating to ensure that the polypropylene fiber is subjected to preoxidation based on iron oxide catalysis in the preoxidation process, so that the polypropylene fiber is gradually changed into a structure mainly based on carbon chains, and the temperature resistance of the fiber is improved, the shape can be kept when high-temperature carbonization is carried out at a high temperature, so that the melt-blown cloth can be directly carbonized to prepare carbon fiber cloth;

s4, drying

Fishing out the uniformly colored melt-blown cloth from the corrosion-resistant tank, rinsing the melt-blown cloth with clear water until the rinsing liquid is neutral, then putting the melt-blown cloth into a drying box, and drying the melt-blown cloth at the temperature of 110 ℃;

s5, carbonizing

Putting the dried modified melt-blown fabric into an atmosphere furnace, introducing nitrogen into the atmosphere furnace for protection, heating to 130 ℃, detecting the moisture content in the tail gas of the atmosphere furnace by using humidity detection equipment, heating to 5 ℃ and preserving heat for 30min when no moisture exists, repeatedly heating to 150 ℃, introducing reducing gas into the atmosphere furnace, adjusting the introduction amount of the nitrogen to be the lowest, preserving heat for 30min, heating to 5 ℃ and 400 ℃ every 5min, and heating to 10 ℃ and 1000 ℃ every 3min, so that the modified melt-blown fabric can be carbonized into carbon fiber fabric;

s6, finished product

And (3) closing the heating of the atmosphere furnace, continuously keeping the lowest introduction amount of nitrogen, slowly reducing the temperature in the atmosphere furnace to room temperature, taking out the carbon fiber cloth, dissolving the iron layer on the surface of the carbon fiber cloth by using dilute hydrochloric acid, washing the carbon fiber cloth by using water until the water solution is neutral, and drying to obtain the finished carbon fiber cloth.

The surface modifier is one of silane coupling agent, titanate coupling agent and aluminate coupling agent.

The ferric oxide precursor is one of ferrous chloride, ferric sulfate or ferrous sulfate, wherein the ferrous chloride contains less acid radicals than trivalent, and the material consumption is relatively low, so the ferrous chloride is mainly used.

The temperature in the atmosphere furnace is pre-oxidized when the temperature is in the range of 130-150 ℃.

The reducing gas is hydrogen-carbon oxide or one of ethanol and methanol.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.