CN111423592A - Preparation method of low-viscosity high-carbon-residue-rate binder asphalt for carbon materials - Google Patents
Preparation method of low-viscosity high-carbon-residue-rate binder asphalt for carbon materials Download PDFInfo
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- CN111423592A CN111423592A CN202010281433.4A CN202010281433A CN111423592A CN 111423592 A CN111423592 A CN 111423592A CN 202010281433 A CN202010281433 A CN 202010281433A CN 111423592 A CN111423592 A CN 111423592A
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- asphalt
- raw material
- furfuryl alcohol
- alcohol resin
- binder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J187/00—Adhesives based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C09J187/005—Block or graft polymers not provided for in groups C09J101/00 - C09J185/04
Abstract
A preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials belongs to the technical field of preparation methods of carbon material binders. The technical scheme of the invention is as follows: firstly, heating raw material asphalt to 130-200 ℃ to enable the raw material asphalt to be in a molten state; secondly, adding furfuryl alcohol resin into the molten raw material asphalt, wherein the mass of the added furfuryl alcohol resin is 1-15% of that of the raw material asphalt, and reacting for 20-120 min under the stirring condition; and adjusting the temperature of the heating system to 120-180 ℃, adding a ferric trichloride ethanol solution with the mass of 0.3-1.5% of that of the raw material asphalt, and reacting for 20-80 min under the stirring condition to obtain the binder asphalt with low viscosity and high carbon residue rate. The invention selects the furfuryl alcohol resin as the asphalt modifier, realizes the fundamental change of the asphalt performance, reduces the viscosity of the asphalt, improves the low-temperature wettability of the asphalt, greatly improves the coke precipitation rate of the raw material asphalt by adding the ferric trichloride catalyst, and obviously improves the mechanical property of the carbon product using the modified asphalt as the binder.
Description
Technical Field
The invention belongs to the technical field of preparation methods of carbon material binders, and particularly relates to a preparation method of low-viscosity high-carbon-residue-rate binder asphalt for a carbon material.
Background
The low softening point binder asphalt has good fluidity and wettability due to the material composition and structure of the common binder asphalt, but the residual carbon content is low, so that the binder for preparing carbon materials or graphite materials is difficult to meet the use requirements of high-performance carbon materials, and the binder asphalt needs to be modified to improve the use performance.
The traditional modified asphalt is generally applied to the field of road building materials, natural or synthetic organic or inorganic materials are added into base asphalt, and the material properties of the modifier are utilized to obviously improve the performance of the asphalt. The binder pitch, one of the main raw materials for the preparation of carbon and graphite materials, must be able to wet and penetrate well into the surface and pores of various cokes and form pastes with a good plastic state. The asphalt is gradually decomposed and carbonized during roasting, and simultaneously, coke particles at the periphery are firmly connected together, and when the carbonization rate of the asphalt is higher, the prepared product also has better comprehensive performance. Currently, to improve the performance of binder asphalt, modified asphalt (or modified asphalt) is increasingly receiving attention and being used.
The furfuryl alcohol resin is prepared by condensation polymerization of furfuryl alcohol in the presence of an acidic catalyst (such as phosphoric acid), and is changed into a three-dimensional resin with a cross-linked network structure under the action of an acidic curing agent to be cured, and simultaneously, under the action of the acidic catalyst, the furfuryl alcohol resin can also react with partial components in the asphalt to change the structure and the performance of the asphalt.
Disclosure of Invention
In order to overcome the defects of the prior art and prepare the modified asphalt with good wettability, low viscosity and higher carbon residue value, the invention provides a preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials.
The design concept of the invention is as follows: the furfuryl alcohol resin is used as a modifier, the softening point of the modified asphalt can be obviously reduced by the liquid furfuryl alcohol resin, the wettability of the modified asphalt is improved, and meanwhile, ferric trichloride is added as a catalyst, so that the modified asphalt can be subjected to a crosslinking reaction with the active sites of the raw material asphalt in a carbonization process, the crosslinking degree of macromolecules of the asphalt is improved, and the modified asphalt has a high carbon residue value.
The invention is realized by the following technical scheme.
A preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials comprises the following steps: firstly, heating raw material asphalt to 130-200 ℃ to enable the raw material asphalt to be in a molten state; secondly, adding furfuryl alcohol resin into the molten raw material asphalt, wherein the mass of the added furfuryl alcohol resin is 1-15% of that of the raw material asphalt, and reacting for 20-120 min under the stirring condition; and adjusting the temperature of the heating system to 120-180 ℃, adding a ferric trichloride ethanol solution with the mass of 0.3-1.5% of that of the raw material asphalt, and reacting for 20-80 min under the stirring condition to obtain the binder asphalt with low viscosity and high carbon residue rate.
Further, the softening point of the raw material asphalt is 70-120 ℃, and the raw material asphalt is one or a mixture of more of petroleum asphalt, coal tar asphalt and natural asphalt.
Furthermore, the furfuryl alcohol monomer content in the furfuryl alcohol resin accounts for less than or equal to 5% of the mass percent of the furfuryl alcohol resin, and the viscosity of the furfuryl alcohol resin at normal temperature is less than or equal to 1 Pa.s.
Further, the mass percentage concentration of the iron element in the ferric trichloride ethanol solution is 8-16%.
Compared with the prior art, the invention has the beneficial effects that:
The furfuryl alcohol resin is selected as the asphalt modifier, so that the fundamental change of the asphalt performance is realized, the viscosity of the asphalt is reduced, the low-temperature wettability of the asphalt is improved, the coke precipitation rate of the raw material asphalt is greatly improved by adding the catalyst, and the mechanical property of a carbon product using the modified asphalt as the binder is obviously improved. Therefore, the invention provides a modification method for comprehensively improving the performance of asphalt, and the modified asphalt can be obtained only under mild reaction conditions.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the examples follow conventional experimental conditions. In addition, it will be apparent to those skilled in the art that various modifications or improvements can be made to the material components and amounts in these embodiments without departing from the spirit and scope of the invention as defined in the appended claims.
Example 1
A preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials comprises the following steps: firstly, 1000g of coal tar pitch (the softening point of the coal tar pitch is 70 ℃) is heated to 135 ℃ to ensure that the coal tar pitch is in a molten state; secondly, adding 10g of furfuryl alcohol resin into the coal pitch in the molten state, and reacting for 20min under the condition of mechanical stirring until the furfuryl alcohol resin and the coal pitch are fully mixed; and adjusting the temperature of the heating system to 130 ℃, adding 3g of ferric trichloride ethanol solution with the iron element mass percentage concentration of 15%, and reacting for 20min under the stirring condition to obtain the binder asphalt with low viscosity and high carbon residue rate. The product was tested for properties and the results are shown in Table 1.
Example 2
A preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials comprises the following steps: firstly, 1000g of coal tar pitch (the softening point of the coal tar pitch is 85 ℃) is heated to 159 ℃ so that the coal tar pitch is in a molten state; secondly, adding 50g of furfuryl alcohol resin into the coal pitch in the molten state, and reacting for 30min under the condition of mechanical stirring until the furfuryl alcohol resin and the coal pitch are fully mixed; and adjusting the temperature of the heating system to 150 ℃, adding 5g of ferric trichloride ethanol solution with the iron element mass percentage concentration of 12%, and reacting for 30min under the stirring condition to obtain the binder asphalt with low viscosity and high carbon residue rate. The product was tested for properties and the results are shown in Table 1.
Example 3
A preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials comprises the following steps: firstly, 1000g of coal tar pitch (the softening point of the coal tar pitch is 99 ℃) is heated to 169 ℃ to ensure that the coal tar pitch is in a molten state; secondly, adding 70g of furfuryl alcohol resin into the coal pitch in the molten state, and reacting for 60min under the condition of mechanical stirring until the furfuryl alcohol resin and the coal pitch are fully mixed; and adjusting the temperature of the heating system to 160 ℃, adding 8g of ferric trichloride ethanol solution with the iron element mass percentage concentration of 10%, and reacting for 40min under the stirring condition to obtain the binder asphalt with low viscosity and high carbon residue rate. The product was tested for properties and the results are shown in Table 1.
Example 4
A preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials comprises the following steps: firstly, 1000g of coal tar pitch (the softening point of the coal tar pitch is 109 ℃) is heated to 179 ℃ to ensure that the coal tar pitch is in a molten state; secondly, adding 100g of furfuryl alcohol resin into the coal pitch in the molten state, and reacting for 90min under the condition of mechanical stirring until the furfuryl alcohol resin and the coal pitch are fully mixed; and adjusting the temperature of the heating system to 160 ℃, adding 10g of ferric trichloride ethanol solution with the iron element mass percentage concentration of 10%, and reacting for 40min under the stirring condition to obtain the binder asphalt with low viscosity and high carbon residue rate. The product was tested for properties and the results are shown in Table 1.
Example 5
A preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials comprises the following steps: firstly, 1000g of coal tar pitch (the softening point of the coal tar pitch is 120 ℃) is heated to 200 ℃ to ensure that the coal tar pitch is in a molten state; secondly, adding 150g of furfuryl alcohol resin into the coal pitch in the molten state, and reacting for 120min under the condition of mechanical stirring until the furfuryl alcohol resin and the coal pitch are fully mixed; and adjusting the temperature of the heating system to 180 ℃, adding 15g of ferric trichloride ethanol solution with the mass percent concentration of iron element being 8%, and reacting for 80min under the stirring condition to obtain the binder asphalt with low viscosity and high carbon residue rate. The product was tested for properties and the results are shown in Table 1.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (4)
1. A preparation method of binder asphalt with low viscosity and high carbon residue rate for carbon materials is characterized by comprising the following steps: firstly, heating raw material asphalt to 130-200 ℃ to enable the raw material asphalt to be in a molten state; secondly, adding furfuryl alcohol resin into the molten raw material asphalt, wherein the mass of the added furfuryl alcohol resin is 1-15% of that of the raw material asphalt, and reacting for 20-120 min under the stirring condition; and adjusting the temperature of the heating system to 120-180 ℃, adding a ferric trichloride ethanol solution with the mass of 0.3-1.5% of that of the raw material asphalt, and reacting for 20-80 min under the stirring condition to obtain the binder asphalt with low viscosity and high carbon residue rate.
2. The method for preparing the binder pitch with low viscosity and high carbon residue rate for the carbon material according to claim 1, which is characterized in that: the softening point of the raw material asphalt is 70-120 ℃, and the raw material asphalt is one or a mixture of more of petroleum asphalt, coal tar asphalt and natural asphalt.
3. The method for preparing the binder pitch with low viscosity and high carbon residue rate for the carbon material according to claim 1, which is characterized in that: the furfuryl alcohol monomer content in the furfuryl alcohol resin accounts for less than or equal to 5 percent of the mass percent of the furfuryl alcohol resin, and the viscosity of the furfuryl alcohol resin at normal temperature is less than or equal to 1 Pa.s.
4. The method for preparing the binder pitch with low viscosity and high carbon residue rate for the carbon material according to claim 1, which is characterized in that: the mass percentage concentration of the iron element in the ferric trichloride ethanol solution is 8-16%.
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| CN202010281433.4A CN111423592A (en) | 2020-04-10 | 2020-04-10 | Preparation method of low-viscosity high-carbon-residue-rate binder asphalt for carbon materials |
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| CN202010281433.4A CN111423592A (en) | 2020-04-10 | 2020-04-10 | Preparation method of low-viscosity high-carbon-residue-rate binder asphalt for carbon materials |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115785688A (en) * | 2022-12-27 | 2023-03-14 | 新疆晶威新材料有限公司 | Method for modifying binder asphalt |
| CN115785688B (en) * | 2022-12-27 | 2024-05-03 | 新疆晶威新材料有限公司 | Modification method of binder asphalt |
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| CN1304977A (en) * | 2000-09-14 | 2001-07-25 | 中国科学院山西煤炭化学研究所 | Process for preparing asphalt impregnant by co-charring furan resin |
| CN102603336A (en) * | 2012-03-26 | 2012-07-25 | 河南远洋新材料技术有限公司 | High heat conductivity ramming material |
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2020
- 2020-04-10 CN CN202010281433.4A patent/CN111423592A/en active Pending
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| US3491045A (en) * | 1965-11-17 | 1970-01-20 | Amercoat Corp | Crosslinked bitumen-furfuryl alcohol resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115785688A (en) * | 2022-12-27 | 2023-03-14 | 新疆晶威新材料有限公司 | Method for modifying binder asphalt |
| CN115785688B (en) * | 2022-12-27 | 2024-05-03 | 新疆晶威新材料有限公司 | Modification method of binder asphalt |
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Application publication date: 20200717 |
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