CN114197112A - Preparation method of phenolic aldehyde based activated carbon fiber felt - Google Patents

Preparation method of phenolic aldehyde based activated carbon fiber felt Download PDF

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Publication number
CN114197112A
CN114197112A CN202111612144.9A CN202111612144A CN114197112A CN 114197112 A CN114197112 A CN 114197112A CN 202111612144 A CN202111612144 A CN 202111612144A CN 114197112 A CN114197112 A CN 114197112A
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China
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phenolic
temperature
thermoplastic
fiber felt
carbon fiber
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CN202111612144.9A
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Chinese (zh)
Inventor
陈保磊
赵永谦
陈阳
万月亮
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Qingdao Naboke Environmental Protection Technology Co ltd
Qingdao Huashijie Environment Protection Technology Co ltd
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Qingdao Naboke Environmental Protection Technology Co ltd
Qingdao Huashijie Environment Protection Technology Co ltd
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Priority to CN202111612144.9A priority Critical patent/CN114197112A/en
Publication of CN114197112A publication Critical patent/CN114197112A/en
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326—Condensation or reaction polymers
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/24—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
    • D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C7/00—Heating or cooling textile fabrics
    • D06C7/04—Carbonising or oxidising

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Fibers (AREA)

Abstract

The invention provides a preparation method of an activated carbon fiber felt, in particular to a preparation method of a phenolic aldehyde based activated carbon fiber felt. The preparation method comprises the steps of preparing thermoplastic phenolic fibers from thermoplastic phenolic resin through melt spinning, further preparing thermoplastic phenolic fiber felts, then pre-oxidizing, carbonizing at low temperature and high temperature, and finally activating to obtain the phenolic fiber felts. The obtained phenolic aldehyde based active carbon fiber felt adopts thermoplastic phenolic resin as a raw material, has wide sources and low price, and the increase of the manufacturing cost caused by two-step carbonization procedures is far lower than that of a manufacturing scheme of thermosetting phenolic fiber, thereby having more industrialized advantages.

Description

Preparation method of phenolic aldehyde based activated carbon fiber felt
Technical Field
The invention relates to a preparation method of an activated carbon fiber felt, in particular to a preparation method of a phenolic aldehyde based activated carbon fiber felt.
Background
The phenolic aldehyde based active carbon fiber, namely the active carbon fiber prepared from the phenolic aldehyde fiber, has the advantages of high yield, developed aperture, high strength, low ash content and the like. The phenolic fiber as the raw material is usually prepared by wet spinning thermosetting phenolic fiber and then heating and curing the thermosetting phenolic fiber to prepare the thermosetting phenolic fiber.
At present, the basic process for preparing the phenolic aldehyde-based active carbon fiber is to prepare thermosetting phenolic aldehyde fiber at first, then carry out needle-punched felt treatment on the thermosetting phenolic aldehyde fiber, and carry out carbonization and activation treatment, and finally finish the preparation. The thermosetting phenolic fiber is generally prepared by using thermosetting phenolic resin through wet spinning forming, and can also be prepared by using thermoplastic phenolic fiber prepared by melt spinning of thermoplastic phenolic resin through crosslinking and curing. The thermosetting phenolic fiber is a good raw material for preparing the activated carbon fiber, and in the carbonization process, the thermosetting phenolic fiber has the characteristics of non-melting and non-combustion, so that the carbonization and activation can be directly carried out without preoxidation, and the preparation process of the activated carbon fiber is very simple. Compared with other organic fibers, the manufacturing difficulty of the activated carbon fiber can be greatly reduced.
However, the phenolic resin monomer used in the process of preparing thermosetting phenolic fibers by wet spinning is special and complex in component, generally needs to be synthesized separately, and meanwhile, the control requirement on each process parameter in the production process is higher. Therefore, the thermosetting phenolic fiber has high manufacturing difficulty and high manufacturing cost, and has high cost performance advantage in the field of flame-retardant and heat-resistant fibers, but the shortage of high cost of the thermosetting phenolic fiber as a raw material for preparing the activated carbon fiber can limit the industrial application of the thermosetting phenolic fiber.
Disclosure of Invention
The invention aims to provide a preparation method of a phenolic aldehyde based activated carbon fiber felt, which adopts thermoplastic phenolic resin as a raw material, has wide sources and low price, and has more industrialized advantages because the increase of the manufacturing cost caused by two-step carbonization procedures is far lower than that of a manufacturing scheme of thermosetting phenolic fibers.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
a preparation method of a phenolic aldehyde based activated carbon fiber felt comprises the following steps:
s1: and melting the thermoplastic phenolic resin, and then carrying out melt spinning to prepare the short thermoplastic phenolic fiber. The thermoplastic phenolic resin preferably has a softening point of 83-100 ℃ and a free phenol content of less than 1.4%. It has been found through experimentation that if the softening point is too low, the pre-oxidation process cannot be performed, and if the softening point is too high, the phenolic resin is difficult to melt. Although a thermoplastic resin, too high a phenol content will increase the time for pre-oxidation.
The melting temperature is preferably 120-150 ℃, and the melting process is preferably carried out under the anaerobic condition of nitrogen and the like, so that the material is prevented from oxidative deterioration.
The titer of the prepared thermoplastic phenolic fiber is preferably 4.0dtex-7.0dtex, so the pore diameter and the stretching ratio of a spinneret plate are selected according to the titer to be prepared. Too low titer of the thermoplastic phenolic fiber can cause the final activated carbon fiber product to have smaller filament diameter and increased wind resistance. The thermoplastic phenolic fiber with too large fineness can form an activated carbon fiber hollow structure due to preoxidation or reduced carbonization uniformity.
The thermoplastic phenolic fibers are preferably chopped fibers cut to a length of 51-76 mm. The short fiber length can obviously reduce the strength of the needled felt, and the overlong fiber length can cause certain difficulty in the opening and carding links before short fiber needling.
S2: and preparing the chopped thermoplastic phenolic fibers obtained in the step S1 into a thermoplastic phenolic fiber felt.
The method for preparing the thermoplastic phenolic fiber felt from the chopped thermoplastic phenolic fibers preferably adopts a needle-punched non-woven processing technology; the gram weight of the thermoplastic phenolic fiber felt is preferably 400-700g/m2The thickness is preferably 3.7-6.2 mm.
S3: and pre-oxidizing the thermoplastic phenolic fiber felt obtained in the S2.
The pre-oxidation temperature is preferably 60-78 ℃; the pre-oxidation time is preferably 14-24 h.
Further, the pre-oxidation is carried out in an air environment, and the pre-oxidation process ensures air circulation.
S4: and (4) carbonizing the preoxidation product obtained in the step (S3) at a low temperature.
The temperature of the low-temperature carbonization is preferably 140-400 ℃, and the time of the low-temperature carbonization is preferably 30-50 min. Thermosetting phenolic fibers can be carbonized at a temperature of 400 ℃ or higher because they are highly crosslinked inside, have a high heat resistance temperature, and have a high thermal decomposition temperature. Compared with thermosetting phenolic fibers, the thermoplastic phenolic fibers are subjected to long-time pre-oxidation treatment but still need to be carbonized at low temperature, and the low-temperature carbonization can enable the phenolic fibers to resist further crosslinking and solidification in an oxidation mode, so that the situation that the fibers are heated and melted to damage the appearance of the fibers due to incomplete solidification is prevented.
Further, the low-temperature carbonization process maintains the oxygen content at 4-10%, and the low-temperature carbonization can realize better crosslinking and curing through oxidation under the oxygen content.
S5: and (4) carrying out high-temperature carbonization on the low-temperature carbonization product obtained in the S4.
The temperature of the high-temperature carbonization is preferably 400-1000 ℃, and the time of the high-temperature carbonization is preferably 30-50 min.
Further, the high-temperature carbonization process keeps the oxygen content between 0 and 1 percent less than 1 percent. Under the oxygen content, the crosslinking and curing can be consolidated, and the ablation of the carbon material at high temperature can be prevented.
S6: and (5) activating the high-temperature carbonization product obtained in the step S5 to obtain the catalyst.
The activation temperature is preferably 780-850 ℃, and the activation time is preferably 10-30 min.
The activated activating agent is preferably water vapor.
Compared with the traditional process of firstly preparing the thermosetting phenolic fiber material and then preparing the phenolic-based activated carbon fiber, the process of preparing the activated carbon fiber by using the finished product of the thermoplastic phenolic resin as the raw material for producing the phenolic-based activated carbon fiber felt has the advantages of wide raw material source, low price and thermoplastic phenol although the process of preparing the activated carbon fiber by using the thermoplastic phenolic fiber is relatively complexThe process and equipment of the spinning process of the aldehyde fiber are relatively simple, the cost is reduced, so that the method has more industrial advantages, a novel preparation method of the phenolic activated carbon fiber felt is developed, and the specific surface range of the prepared phenolic activated carbon fiber felt is 1100-2000m2/g。
Drawings
In order to more clearly illustrate the technical solutions of the background and the embodiments of the present invention, the drawings needed to be used in the background and the embodiments will be briefly described below, it should be understood that the following drawings may only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and that for a person skilled in the art, other related drawings may be obtained from these drawings without inventive effort.
FIG. 1 is a schematic flow diagram of a method for preparing a phenolic-based activated carbon fiber mat according to the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "plurality" or "a number" means two or more unless specifically limited otherwise.
Example 1
A preparation method of phenolic aldehyde group activated carbon fiber felt is shown in figure 1, and comprises the steps of melting thermoplastic phenolic resin with a softening point of 85 ℃ and a free phenol content of 1.0% at 130 ℃ in a nitrogen atmosphere, and preparing 6.4dtex and 64mm short fiber felt through melt spinningA fiber. The staple fiber is prepared into the gram weight of 470g/m by needle-punching non-woven processing2And the thickness of the needled felt is 4.3 mm. And oxidizing the needled felt for 24 hours at 75 ℃ in an air atmosphere to finish the pre-oxidation treatment. Under the atmosphere condition of 4 percent of oxygen content, the temperature is slowly increased from 140 ℃ to 400 ℃ by using a carbonization furnace, and the temperature increasing process lasts for 30min, thus completing the low-temperature carbonization. And (3) under the nitrogen atmosphere, slowly heating the mixture from 400 ℃ to 900 ℃ by using a carbonization furnace, and keeping the heating process for 40min to finish high-temperature carbonization. Finally activating with water vapor at 850 deg.C for 25min to obtain 1800m specific surface2Active carbon fiber felt based on phenolic aldehyde/g.
Example 2
A preparation method of phenolic aldehyde group active carbon fiber felt uses thermoplastic phenolic resin with the softening point of 100 ℃ and the free phenol content of 1.4 percent, and the thermoplastic phenolic resin is melted at the temperature of 150 ℃ in nitrogen atmosphere, and short fibers with the length of 4.2dtex and the length of 55mm are prepared through melt spinning. The staple fiber is prepared into the weight of 590g/m by needle-punching non-woven processing26.2mm thick needled felt. And (3) oxidizing the needled felt for 20 hours at 78 ℃ in an air atmosphere to finish the pre-oxidation treatment. Under the atmosphere condition of 6 percent of oxygen content, the temperature is slowly raised from 140 ℃ to 350 ℃ by using a carbonization furnace, and the temperature raising process lasts for 30min, thus completing the low-temperature carbonization. And (3) under the nitrogen atmosphere, slowly heating the mixture from 400 ℃ to 1000 ℃ by using a carbonization furnace, and keeping the heating process for 45min to finish high-temperature carbonization. Activating with water vapor at 800 deg.C for 20min to obtain 1398m specific surface2Active carbon fiber felt based on phenolic aldehyde/g.
Example 3
A preparation method of phenolic aldehyde group activated carbon fiber felt is characterized in that thermoplastic phenolic resin with the softening point of 93 ℃ and the free phenol content of 1.3% is used for melting at 120 ℃ in a nitrogen atmosphere, and 5.6dtex and 76mm short fibers are prepared through melt spinning. The weight of the short fiber is 690g/m by needle punching non-woven processing2And 5.7mm thick needled felt. And oxidizing the needled felt for 24 hours at the temperature of 60 ℃ in the air atmosphere to finish the pre-oxidation treatment. Under the atmosphere condition of 10 percent of oxygen content, the temperature is slowly increased from 140 ℃ to 400 ℃ by using a carbonization furnace, and the temperature increasing process lasts for 30min, thus completing the low-temperature carbonization. Under the atmosphere condition of 1% oxygen content, slowly heating from 400 deg.C to 1000 deg.C with a carbonization furnace, and maintaining the heating process for 50min to complete high-temperature carbonization. Finally activating with water vapor at 780 deg.C for 30min to obtain specific surface 1724m2Active carbon fiber felt based on phenolic aldehyde/g.
Example 4
A preparation method of phenolic aldehyde group activated carbon fiber felt is characterized in that thermoplastic phenolic resin with the softening point of 85 ℃ and the free phenol content of 1.0% is used for melting at 130 ℃ in a nitrogen atmosphere, and short fibers of 6.4dtex and 64mm are prepared through melt spinning. The staple fiber is prepared into the gram weight of 470g/m by needle-punching non-woven processing2And the thickness of the needled felt is 4.3 mm. And oxidizing the needled felt for 24 hours at 75 ℃ in an air atmosphere to finish the pre-oxidation treatment. Under the atmosphere condition of 6 percent of oxygen content, the temperature is slowly increased from 140 ℃ to 400 ℃ by using a carbonization furnace, and the temperature increasing process lasts for 30min, thus completing the low-temperature carbonization. Slowly heating from 400 ℃ to 900 ℃ by using a carbonization furnace under the condition that the oxygen content is 0.5%, and continuing the heating process for 40min to finish high-temperature carbonization. Finally activating with water vapor at 850 deg.C for 25min to obtain a specific surface 1978m2Active carbon fiber felt based on phenolic aldehyde/g.
Example 5
A preparation method of phenolic aldehyde group active carbon fiber felt uses thermoplastic phenolic resin with the softening point of 85 ℃ and the free phenol content of 1.0 percent, and the thermoplastic phenolic resin is melted at the temperature of 145 ℃ in nitrogen atmosphere, and 5.2dtex and 64mm short fibers are prepared by melt spinning. The staple fiber is prepared into the gram weight of 420g/m by needle-punching non-woven processing2And 3.7mm thick needled felt. And (3) oxidizing the needled felt for 15h at 75 ℃ in an air atmosphere to finish pre-oxidation treatment. Under the atmosphere condition of 5 percent of oxygen content, the temperature is slowly raised to 380 ℃ from 140 ℃ by using a carbonization furnace, the temperature raising process lasts for 30min, and the low-temperature carbonization is completed. And (3) under the nitrogen atmosphere, slowly heating the mixture from 400 ℃ to 950 ℃ by using a carbonization furnace, and keeping the heating process for 40min to finish high-temperature carbonization. Finally activating with water vapor at 780 deg.C for 25min to obtain specific surface 1183m2Active carbon fiber felt based on phenolic aldehyde/g.
In the description herein, references to the description of the terms "one embodiment," "some embodiments," "preferred embodiments," "specific embodiments," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. A preparation method of a phenolic aldehyde based activated carbon fiber felt comprises the following steps:
s1: after the thermoplastic phenolic resin is melted, the thermoplastic phenolic fiber is prepared through melt spinning;
s2: preparing the thermoplastic phenolic fiber obtained in the step S1 into a thermoplastic phenolic fiber felt;
s3: pre-oxidizing the thermoplastic phenolic fiber felt obtained in the step S2;
s4: carbonizing the preoxidation product obtained in the step S3 at low temperature;
s5: carrying out high-temperature carbonization on the low-temperature carbonization product obtained in the step S4;
s6: and (5) activating the high-temperature carbonization product obtained in the step S5 to obtain the catalyst.
2. The method according to claim 1, wherein the thermoplastic phenol resin has a softening point of 83 to 100 ℃ and a free phenol content of < 1.4% in S1.
3. The method according to claim 1, wherein the S1 further satisfies one or more of the following conditions:
a. the melting temperature is 120-150 ℃;
b. the melting process needs to be carried out under the anaerobic condition;
c. the titer of the prepared thermoplastic phenolic fiber is 4.0dtex-7.0 dtex;
d. the prepared thermoplastic phenolic fiber is cut into short fibers with the length of 51-76 mm.
4. The method of claim 1, wherein in S2, the chopped phenolic thermoplastic fibers are prepared into the phenolic thermoplastic fiber felt by a needle punching non-woven processing technology; the gram weight of the thermoplastic phenolic fiber felt is 400-700g/m2The thickness is 3.7-6.2 mm.
5. The method according to claim 1, wherein the S3 satisfies one or more of the following conditions:
e. the pre-oxidation temperature is 60-78 ℃;
f. the pre-oxidation time is 14-24 h;
g. the pre-oxidation is carried out in an air environment, and the air circulation is ensured in the pre-oxidation process.
6. The method as claimed in claim 1, wherein in S4, the temperature of the low-temperature carbonization is 140-400 ℃, and the time of the low-temperature carbonization is 30-50 min.
7. The method according to claim 1 or 6, wherein the low temperature carbonization process maintains an oxygen content of 4 to 10% in S4.
8. The method as claimed in claim 1, wherein in S5, the temperature of the high temperature carbonization is 400-1000 ℃, and the time of the high temperature carbonization is 30-50 min.
9. The method according to claim 1 or 8, wherein in S5, the high temperature carbonization process maintains an oxygen content of < 1%.
10. The method according to claim 1, wherein the S6 satisfies one or more of the following conditions:
h. the temperature of the activation is 780-850 ℃;
i. the activation time is 10-30 min;
j. the activated activating agent is water vapor.
CN202111612144.9A 2021-12-27 2021-12-27 Preparation method of phenolic aldehyde based activated carbon fiber felt Pending CN114197112A (en)

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