阅读说明：本技术 黏胶基碳纤维复合材料石墨毡的制备工艺、制得的石墨毡 (Preparation process of viscose-based carbon fiber composite graphite felt and prepared graphite felt ) 是由 黄猛 吴清贤 马翔翔 卜宇轩 王峰 于 2021-09-17 设计创作，主要内容包括：本发明公开黏胶基碳纤维复合材料石墨毡的制备工艺,涉及石墨毡技术领域,本发明包括以下步骤：步骤一：黏胶基白毡预氧化后制成碳纤维预氧毡,浸泡于1％磷酸氢二胺溶液中,然后烘干,进入预氧炉加热处理,得到预氧毡；步骤二：将预氧毡经连续预处理炉后制成黏胶基碳纤维预处理毡,处理温度为630-650℃,得到预处理毡；步骤三：将预处理毡经连续式碳化石墨化炉处理后制成黏胶基碳纤维石墨毡,处理温度为1900-2400℃。本发明的有益效果在于：通过预处理工艺处理后再进行连续式碳化石墨化炉一体化生产的原料可以得到更高的收率、更高的宽幅,生产效率得到了提高。(The invention discloses a preparation process of an adhesive-based carbon fiber composite graphite felt, which relates to the technical field of graphite felts and comprises the following steps: the method comprises the following steps: pre-oxidizing the viscose-based white felt to prepare a carbon fiber pre-oxidized felt, soaking the carbon fiber pre-oxidized felt in a 1% diammonium hydrogen phosphate solution, drying the carbon fiber pre-oxidized felt, and heating the carbon fiber pre-oxidized felt in a pre-oxidizing furnace to obtain a pre-oxidized felt; step two: preparing the pre-oxidized felt into an adhesive-based carbon fiber pre-treated felt through a continuous pre-treatment furnace at the treatment temperature of 630-650 ℃ to obtain the pre-treated felt; step three: and (3) treating the pretreated felt by a continuous carbonization graphitization furnace to prepare the viscose-based carbon fiber graphite felt at the treatment temperature of 1900-2400 ℃. The invention has the beneficial effects that: the raw material treated by the pretreatment process and then integrally produced by the continuous carbonization graphitization furnace can obtain higher yield and higher breadth, and the production efficiency is improved.)

1. A preparation process of a viscose-based carbon fiber composite graphite felt is characterized by comprising the following steps: the method comprises the following steps:

the method comprises the following steps: pre-oxidizing the viscose-based white felt to prepare a carbon fiber pre-oxidized felt, soaking the carbon fiber pre-oxidized felt in a 1% diammonium hydrogen phosphate solution, drying the carbon fiber pre-oxidized felt, and heating the carbon fiber pre-oxidized felt in a pre-oxidizing furnace to obtain a pre-oxidized felt;

step two: preparing the pre-oxidized felt into an adhesive-based carbon fiber pretreatment felt after passing through a continuous pretreatment furnace, wherein the treatment temperature of the continuous pretreatment furnace is 630-650 ℃, and obtaining the pretreatment felt;

step three: and (3) treating the pretreated felt by a continuous carbonization graphitization furnace to prepare the viscose-based carbon fiber graphite felt, wherein the treatment temperature of the continuous carbonization graphitization furnace is 1900-2400 ℃.

2. The process for preparing the viscose-based carbon fiber composite graphite felt according to claim 1, wherein the process comprises the following steps: in the first step, 85% of diammonium hydrogen phosphate solution is diluted into 1% of diammonium hydrogen phosphate solution.

3. The process for preparing the viscose-based carbon fiber composite graphite felt according to claim 1, wherein the process comprises the following steps: the soaking time in the step one is 2-3 hours.

4. The process for preparing the viscose-based carbon fiber composite graphite felt according to claim 1, wherein the process comprises the following steps: and in the second step, after the pretreatment of the pretreatment felt by the pretreatment furnace, 75-85% of physical size shrinkage is completed.

5. The process for preparing the viscose-based carbon fiber composite graphite felt according to claim 1, wherein the process comprises the following steps: and after the pretreatment in the second step, naturally airing the pretreated felt.

6. The process for preparing the viscose-based carbon fiber composite graphite felt according to claim 1, wherein the process comprises the following steps: and the second step is carried out under the protection of nitrogen.

7. The process for preparing the viscose-based carbon fiber composite graphite felt according to claim 1, wherein the process comprises the following steps: and in the second step, the pre-oxidized felt enters the pretreatment furnace through the whole-course mesh belt transmission.

8. The process for preparing the viscose-based carbon fiber composite graphite felt according to claim 1, wherein the process comprises the following steps: and the third step is carried out under the protection of nitrogen.

9. The process for preparing the viscose-based carbon fiber composite graphite felt according to claim 1, wherein the process comprises the following steps: and in the third step, the carbonization section of the continuous carbonization graphitization furnace is driven by a mesh belt, and the graphitization and cooling section is pulled by a material receiving device.

10. A viscose-based carbon fiber composite graphite felt produced by the method of any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of graphite felts, in particular to a preparation process of an adhesive-based carbon fiber composite material graphite felt and the prepared graphite felt.

Background

The viscose-based carbon fiber is a fibrous carbon material, and is an excellent carbon reinforcing material for military and civil use. The viscose-based carbon fiber heat-insulating material is formed by weaving viscose fibers, has the advantages of low density, corrosion resistance, high temperature resistance, fatigue resistance and low thermal expansion coefficient, has good flexibility, can realize the heat-insulating effect through a wrapping mode, can be used in a 2800 ℃ high-temperature environment, and has great market potential in the aspects of use of equipment such as metallurgy and photovoltaic equipment.

The viscose-based carbon fiber can be combined with resin to prepare cured hard felts with different shapes and specifications through compression molding, the cured hard felts have extremely high compression strength and bending strength and can meet the structural requirements of different types of equipment, the compression strength and the bending strength of the cured hard felts are further increased through deposition treatment, and the cured hard felts can be applied to the high-tech fields of aviation, aerospace and the like, for example, a patent with the publication number of CN104058777A discloses a semi-continuous production method of a carbon fiber hard heat-preservation felt, and thermosetting resin powder is scattered on the upper surface of the impregnated carbon fiber felt. In other aspects, the activated felt with ultrahigh specific surface area and proper pore proportion can be prepared by activating and reaming treatment, and the activated felt can be widely applied to the aspects of chemical industry, environmental protection, energy storage and the like, and can also be used as a carrier to be applied to special fields.

At present, great demand is brought to heat insulation materials in industries such as domestic metallurgy and photovoltaic, the traditional viscose base graphite soft felt mostly adopts a process route of carbon felt-vacuum sintering-graphite soft felt, the production cost is high, the production efficiency is low, the phenomena of slag falling and skirt edge of a product are obvious, when the product is applied to the photovoltaic industry, the phenomena of ash falling, slag falling and the like can obviously affect the product quality of monocrystalline silicon, and the requirements of customers cannot be met. In the aspect of performance, the raw material strength of the viscose-based graphite soft felt is low, the ash content is high, the needling and weaving processes are more backward than those of China, and the phosphorus-containing catalyst is adopted at home to increase the carbon yield of viscose to a certain extent, but the production process has great hidden danger.

Disclosure of Invention

The invention aims to provide a preparation process of a viscose-based carbon fiber composite graphite felt and the prepared viscose-based carbon fiber composite graphite felt.

The invention solves the technical problems through the following technical means:

the preparation process of the viscose-based carbon fiber composite graphite felt comprises the following steps:

the method comprises the following steps: pre-oxidizing the viscose-based white felt to prepare a carbon fiber pre-oxidized felt, soaking the carbon fiber pre-oxidized felt in a 1% diammonium hydrogen phosphate solution, drying the carbon fiber pre-oxidized felt, and heating the carbon fiber pre-oxidized felt in a pre-oxidizing furnace to obtain a pre-oxidized felt;

step two: preparing the pre-oxidized felt into an adhesive-based carbon fiber pretreatment felt after passing through a continuous pretreatment furnace, wherein the treatment temperature of the continuous pretreatment furnace is 630-650 ℃, and obtaining the pretreatment felt;

step three: and (3) treating the pretreated felt by a continuous carbonization graphitization furnace to prepare the viscose-based carbon fiber graphite felt, wherein the treatment temperature of the continuous carbonization graphitization furnace is 1900-2400 ℃.

Has the advantages that: the continuous pretreatment furnace is used for treating the felt to remove most of water and tar in the felt, so that the impurity removal pressure of a subsequent carbonization and graphitization furnace is reduced, the impurity volatilization amount of a subsequent working section is reduced, the production period of subsequent carbonization and graphitization integrated equipment is prolonged, the equipment maintenance frequency is reduced, and the production efficiency is greatly improved.

The raw materials for carrying out integrated production of the continuous carbonization graphitization furnace can obtain higher yield, higher breadth and lower ash value, and the integrated production of the continuous carbonization graphitization furnace can carry out longer production period, thereby improving the production efficiency and the yield.

The invention is improved on the basis of the traditional integrated production process of the continuous carbonization graphitization furnace, the raw materials which are processed by the pretreatment process and then are subjected to integrated production of the continuous carbonization graphitization furnace can obtain higher yield and wider width, the production efficiency is improved, the energy consumption is reduced by more than 40 percent compared with that of a batch furnace, the product quality is greatly improved in the aspects of ash and slag dropping, and the like, and the requirements of the photovoltaic market can be basically met.

Compared with the traditional integrated production process of the continuous carbonization graphitization furnace, the process provided by the invention is additionally provided with a pretreatment process; the weight yield of the final graphite felt can be improved by 1 to 2 percent by carrying out the integrated production of the continuous carbonization graphitization furnace after the pretreatment process treatment.

Compared with the traditional integrated production process of the continuous carbonization graphitization furnace, the process provided by the invention is additionally provided with a pretreatment process; the width of the final graphite felt can be improved by 20 to 25 percent compared with the traditional process by carrying out the integrated production of the continuous carbonization graphitization furnace after the pretreatment process treatment;

compared with the traditional integrated production process of the continuous carbonization graphitization furnace, the process provided by the invention is additionally provided with a pretreatment process; the pretreatment process is adopted for treatment, and then the continuous carbonization graphitization furnace is used for integrated production, so that the production period is prolonged to four weeks, and compared with the production period of two weeks in the traditional process, the production period is doubled, and the yield is improved by 80-100%.

Preferably, in the first step, 85% of the diammonium phosphate solution is diluted to be a 1% diammonium phosphate solution.

Preferably, the soaking time in the step one is 2 to 3 hours.

Preferably, the pre-treated mat after the pre-treatment furnace treatment in step two achieves 75-85% physical size shrinkage.

Preferably, after the pretreatment in the second step, the pretreated felt is naturally aired.

Has the advantages that: to prevent internal temperature build-up and spontaneous ignition.

Preferably, the second step is carried out under the protection of nitrogen.

Has the advantages that: prevent the felt from being oxidized and incapacitated.

Preferably, the pre-oxidized felt in the second step is conveyed into the pretreatment furnace through a whole mesh belt.

Preferably, the step three is performed under the protection of nitrogen.

Has the advantages that: prevent the felt from being oxidized and incapacitated.

Preferably, the carbonization section of the continuous carbonization graphitization furnace in the third step is driven by a mesh belt, and the graphitization and cooling section is pulled by a material receiving device.

The viscose-based carbon fiber composite graphite felt prepared by the method is provided.

The invention has the advantages that: the continuous pretreatment furnace is used for treating the felt to remove most of water and tar in the felt, so that the impurity removal pressure of a subsequent carbonization and graphitization furnace is reduced, the impurity volatilization amount of a subsequent working section is reduced, the production period of subsequent carbonization and graphitization integrated equipment is prolonged, the equipment maintenance frequency is reduced, and the production efficiency is greatly improved.

The raw materials for carrying out integrated production of the continuous carbonization graphitization furnace can obtain higher yield, higher breadth and lower ash value, and the integrated production of the continuous carbonization graphitization furnace can carry out longer production period, thereby improving the production efficiency and the yield.

The invention is improved on the basis of the traditional integrated production process of the continuous carbonization graphitization furnace, the raw materials which are processed by the pretreatment process and then are subjected to integrated production of the continuous carbonization graphitization furnace can obtain higher yield and wider width, the production efficiency is improved, the energy consumption is reduced by more than 40 percent compared with that of a batch furnace, the product quality is greatly improved in the aspects of ash and slag dropping, and the like, and the requirements of the photovoltaic market can be basically met.

Compared with the traditional integrated production process of the continuous carbonization graphitization furnace, the process provided by the invention is additionally provided with a pretreatment process; the weight yield of the final graphite felt can be improved by 1 to 2 percent by carrying out the integrated production of the continuous carbonization graphitization furnace after the pretreatment process treatment.

Compared with the traditional integrated production process of the continuous carbonization graphitization furnace, the process provided by the invention is additionally provided with a pretreatment process; the width of the final graphite felt can be improved by 20 to 25 percent compared with the traditional process by carrying out the integrated production of the continuous carbonization graphitization furnace after the pretreatment process treatment;

compared with the traditional integrated production process of the continuous carbonization graphitization furnace, the process provided by the invention is additionally provided with a pretreatment process; the pretreatment process is adopted for treatment, and then the continuous carbonization graphitization furnace is used for integrated production, so that the production period is prolonged to four weeks, and compared with the production period of two weeks in the traditional process, the production period is doubled, and the yield is improved by 80-100%.

The method is carried out under the protection of nitrogen to prevent the felt from being oxidized and incapacitated.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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 some embodiments of the present invention, but not all 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.

Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.

The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.

Example 1

The preparation process of the viscose-based carbon fiber composite graphite felt comprises the following steps:

the method comprises the following steps: the preparation of the materials comprises purchasing viscose-based white felt, needling the white felt by viscose fiber through a needling process, wherein the heat preservation effects of the felts with different gram weights (generally gram weight of square meter of fabric) are different, and the gram weight of the viscose-based white felt in the embodiment is 1900g/m²It was purchased from ambient technology (tin-free) limited of budafur.

Step two: preparing the viscose-based white felt into a carbon fiber pre-oxidized felt through a pre-oxidation process; soaking the white felt in a soaking pool (85% of diammonium hydrogen phosphate solution is diluted into 1% of diammonium hydrogen phosphate solution) for 2 hours, then drying the white felt in a dryer to treat water vapor in the non-woven felt, heating the white felt in a pre-oxidation furnace at 242 ℃ for 2 hours to remove most of water and tar in the felt, and obtaining the pre-oxidation felt.

Step three: preparing the viscose-based pre-oxidized felt into a viscose-based carbon fiber pre-treated felt after passing through a low-temperature continuous pre-treatment furnace; the pre-oxidized felt enters a pretreatment furnace through the whole-process mesh belt transmission, and the pretreatment furnace adopts continuous production to ensure the production continuity and felt body smoothness. The treatment temperature of the pretreatment furnace is 630 ℃, the treatment time is 3.2 hours, and the pre-oxidized felt finishes 80-85% of physical size shrinkage and about 80% of impurity elements discharge in the pretreatment process, so that the impurity removal pressure of a subsequent carbonization and graphitization furnace is reduced, the impurity volatilization amount of a subsequent working section is reduced, the production period of subsequent carbonization and graphitization integrated equipment is prolonged, the equipment maintenance frequency is reduced, and the production efficiency is greatly improved.

Step four: processing the pretreated felt by a continuous carbonization graphitization furnace to prepare an adhesive-based carbon fiber graphite felt; the carbonization section of the continuous carbonization graphitization furnace is driven by a mesh belt, the length of the mesh belt is 5.8 meters, the transmission speed is 1.7cm/min, the graphitization and cooling section is pulled by a material receiving device, the pulling speed is 1.8cm/min, the continuous carbonization graphitization treatment temperature is 1900 ℃, the treatment time is 3.2 hours, the final shrinkage and impurity discharge of the felt are completed in the process, and the whole process is carried out under the protection of nitrogen to prevent the felt from being oxidized and incapability losing, so that the graphite felt is finally obtained.

Example 2

The preparation process of the viscose-based carbon fiber composite graphite felt comprises the following steps:

the method comprises the following steps: preparing materials, purchasing a viscose-based white felt externally, needling the white felt by viscose fibers through a needling process to form the felt, wherein the heat preservation effects of the felts with different gram weights (generally, the gram weight of the square meter of the fabric) are different, and the gram weight of the viscose-based white felt in the embodiment is 2100g/m²It is purchased from delong environmental technologies (yangzhou) ltd.

Step two: preparing the viscose-based white felt into a carbon fiber pre-oxidized felt through a pre-oxidation process; soaking the white felt in a soaking pool (85% of diammonium hydrogen phosphate solution is diluted into 1% of diammonium hydrogen phosphate solution) for 2.5 hours, then drying the white felt in a dryer to treat water vapor in the non-woven felt, heating the white felt in a pre-oxidation furnace at the temperature of 240 ℃ for 2 hours, and removing most of water and tar in the felt to obtain the pre-oxidation felt.

Step three: preparing the viscose-based pre-oxidized felt into a viscose-based carbon fiber pre-treated felt after passing through a low-temperature continuous pre-treatment furnace; the pre-oxidized felt enters a pretreatment furnace through the whole-process mesh belt transmission, and the pretreatment furnace adopts continuous production to ensure the production continuity and felt body smoothness. The pretreatment temperature of the pretreatment furnace is 630 ℃, the treatment time is 3 hours, the pre-oxidized felt finishes 80-85% of physical size shrinkage and about 80% of impurity elements are discharged in the pretreatment process, the impurity removal pressure of a subsequent carbonization graphitization furnace is reduced, the impurity volatilization amount of a subsequent working section is reduced, the production period of subsequent carbonization graphitization integrated equipment is prolonged, the equipment maintenance frequency is reduced, and therefore the production efficiency is greatly improved.

Step four: processing the pretreated felt by a continuous carbonization graphitization furnace to prepare an adhesive-based carbon fiber graphite felt; the carbonization section of the continuous carbonization graphitization furnace is driven by a mesh belt, the length of the mesh belt is 5.8 meters, the transmission speed is 1.7cm/min, the graphitization and cooling section is pulled by a material receiving device, the pulling speed is 1.8cm/min, the continuous carbonization graphitization treatment temperature is 2100 ℃, the treatment time is 3.3 hours, the felt finishes final shrinkage and impurity discharge in the process, the whole process is carried out under the protection of nitrogen, so that the felt is prevented from being oxidized and incapability losing, and the graphite felt is finally obtained.

Example 3

The preparation process of the viscose-based carbon fiber composite graphite felt comprises the following steps:

the method comprises the following steps: the preparation of materials, i.e. buying viscose base white felt, needling the white felt by viscose fiber through needling process, the heat preservation effect of the felt with different gram weights (generally gram weight of square meter of fabric) is different, in this embodiment, the gram weight of the viscose base white felt is 2050g/m²It is purchased from the ceremony peak industry trade company, ltd.

Step two: preparing the viscose-based white felt into a carbon fiber pre-oxidized felt through a pre-oxidation process; soaking the white felt in a soaking pool (85% diammonium hydrogen phosphate solution is diluted into 1% diammonium hydrogen phosphate solution) for 3 hours, then drying the white felt in a dryer to treat water vapor in the non-woven felt, heating the white felt in a pre-oxidation furnace at 239 ℃ for 2 hours to remove most of water and tar in the felt, and obtaining the pre-oxidation felt.

Step three: preparing the viscose-based pre-oxidized felt into a viscose-based carbon fiber pre-treated felt after passing through a low-temperature continuous pre-treatment furnace; the pre-oxidized felt enters a pretreatment furnace through the whole-process mesh belt transmission, and the pretreatment furnace adopts continuous production to ensure the production continuity and felt body smoothness. The treatment temperature of the pretreatment furnace is 650 ℃, the treatment time is 3 hours, the pre-oxidized felt finishes 80-85% of physical size shrinkage and about 80% of impurity elements are discharged in the pretreatment process, the impurity removal pressure of a subsequent carbonization graphitization furnace is reduced, the impurity volatilization amount of a subsequent working section is reduced, the production period of subsequent carbonization graphitization integrated equipment is prolonged, the equipment maintenance frequency is reduced, and therefore the production efficiency is greatly improved.

Step four: processing the pretreated felt by a continuous carbonization graphitization furnace to prepare an adhesive-based carbon fiber graphite felt; the carbonization section of the continuous carbonization graphitization furnace is driven by a mesh belt, the length of the mesh belt is 5.8 meters, the transmission speed is 1.7cm/min, the graphitization and cooling section is pulled by a material receiving device, the pulling speed is 1.78cm/min, the continuous carbonization graphitization treatment temperature is 2400 ℃, the treatment time is 3.5 hours, the final shrinkage and impurity discharge of the felt are completed in the process, the whole process is carried out under the protection of nitrogen, the oxidation incapability of the felt is prevented, and the graphite felt is finally obtained.

The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.