CN111253889A - Low-temperature curing high-temperature-resistant carbon graphite material binder and preparation and use methods thereof - Google Patents
Low-temperature curing high-temperature-resistant carbon graphite material binder and preparation and use methods thereof Download PDFInfo
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- CN111253889A CN111253889A CN202010058358.5A CN202010058358A CN111253889A CN 111253889 A CN111253889 A CN 111253889A CN 202010058358 A CN202010058358 A CN 202010058358A CN 111253889 A CN111253889 A CN 111253889A
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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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B37/1284—Application of adhesive
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B2038/0052—Other operations not otherwise provided for
- B32B2038/0076—Curing, vulcanising, cross-linking
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/023—Silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a low-temperature curing high-temperature-resistant carbon graphite material binder and preparation and use methods thereof, and relates to the technical field of refractory materials. The adhesive comprises the following components in percentage by mass: 40-60% of resin, 15-30% of graphite powder, 20-35% of filler and 5-8% of diluent. The preparation method of the adhesive comprises the following steps: preparing resin and filler, and preparing raw materials according to the mass fraction of each raw material; adding a diluent into the resin, stirring, and diluting to 100-150 mPa & s in viscosity for later use; grinding the filler into powder, and uniformly mixing the powder with graphite powder to obtain mixed powder; slowly adding the diluted resin solution into the mixed powder at a constant speed, continuously stirring and dispersing until the solid phase and the liquid phase are uniformly mixed, thus obtaining the binder. When the adhesive is used, the adhesive is coated on the clean connecting surface of the carbon graphite material to be bonded, the carbon graphite material is tightly pressed and bonded, and the carbon graphite material is baked for 1 hour at the temperature of 80-130 ℃ to finish curing. The adhesive has the advantages of high adhesive strength, low cost, convenient use, good high temperature resistance, low-temperature rapid curing and the like.
Description
Technical Field
The invention belongs to the technical field of refractory materials, relates to a refractory material binder, and particularly relates to a low-temperature curing high-temperature-resistant carbon graphite material binder and a preparation method and a use method thereof.
Background
The carbon graphite material has the advantages of light weight, electric conductivity, thermal conductivity, heat resistance, thermal shock resistance, high purity and the like, has high thermal stability in a non-oxidation environment, is widely applied to the electrical engineering and metallurgy industries, and can be made into electrodes, crucibles, molds and the like. However, because the carbon graphite material is brittle, the conventional crucible and mold are generally machined by using an integral carbon graphite blank, a large amount of waste materials are generated in the product manufacturing process, the unit product production cost is high, and the product with a complex shape is difficult to process. Even if the product is combined by adopting a fastening way of homogeneous material fasteners, the defects of stress concentration, short service life, leakage of sealing contact surfaces and the like which are difficult to overcome exist. In the prior art, patent CN109777305A discloses a graphite refractory binder and a preparation method thereof, which can resist high temperature of 900 ℃ and maintain mechanical strength, but the graphite refractory binder has complex components, long curing period and high use cost; the patent CN1428391A discloses a room temperature curing type high-temperature adhesive, which can resist the temperature of 3000 ℃, but uses boron carbide ceramic as a raw material, has high cost, long curing time of 4-24 hours and low bonding use efficiency; patent CN1289813A discloses a heat-resistant carbon material binder, which needs to be cured at low temperature, then heat treated at high temperature of 800-1500 ℃ and put into use, the heat treatment conditions are severe, the process cost is high, and effective application is difficult.
Disclosure of Invention
The invention aims to overcome the defects and provide the low-temperature curing high-temperature-resistant carbon graphite material adhesive which has the advantages of high bonding strength, low cost, convenience in use, good high-temperature resistance, low-temperature rapid curing and the like.
The invention aims to provide a low-temperature curing high-temperature-resistant carbon graphite material binder, which comprises the following components in parts by mass: 40-60% of resin, 15-30% of graphite powder, 20-35% of filler and 5-8% of diluent.
Preferably, the resin is a combination of epoxy resin and phenolic resin, and the mass ratio of the epoxy resin to the phenolic resin is 1-1.5: 2; the epoxy value of the epoxy resin is 0.51, and the high-temperature carbon residue rate of the combined resin is more than 45 percent.
Preferably, the graphite powder is porous graphite powder, and the specific surface area is more than 45m2(iii) a particle size of 5 to 15 μm/g.
Preferably, the filler component comprises TiO2The filler comprises TiO and Al, Si and kaolin in parts by weight210-13 parts of Al, 20-32 parts of Si, and 20-32 parts of kaolin.
Preferably, the diluent is one or more of acetone, ethanol and glycol.
The invention also aims to provide a preparation method of the low-temperature curing high-temperature-resistant carbon graphite material adhesive, which comprises the following steps:
(1) preparing resin and filler, and preparing raw materials according to 40-60% of resin, 15-30% of graphite powder, 20-35% of filler and 5-8% of diluent;
(2) adding a diluent into the resin, stirring, and diluting to 100-150 mPa & s in viscosity for later use;
(3) grinding the filler into powder, and uniformly mixing the powder with graphite powder to obtain mixed powder;
(4) slowly adding the diluted resin solution into the mixed powder at a constant speed, continuously stirring and dispersing until the solid phase and the liquid phase are uniformly mixed, thus obtaining the binder.
The invention also provides a use method of the low-temperature curing high-temperature-resistant carbon graphite material binder, which comprises the following steps: cleaning the connecting surface of the carbon graphite material to be bonded; coating a binder on the bonding surface of the carbon graphite material, wherein the thickness of the coating is 0.5-1 mm, bonding the carbon graphite material after coating, and properly compressing; baking the bonded carbon graphite material for 1h at 80-130 ℃ in an air environment to finish curing and achieve bonding strength; the bonded carbon graphite material can be directly used in a high-temperature environment.
Compared with the prior art, the adhesive provided by the invention has the following beneficial effects:
(1) the combination of the epoxy resin and the phenolic resin can reduce the brittleness of the phenolic resin and enhance the toughness and bonding strength of the cured adhesive.
(2) The components are added with porous graphite powder, and the porous graphite powder is filled in a secondary carbon network structure generated by the binder at high temperature, and the strong adsorbability of the porous graphite is utilized to form a chimeric effect with the carbon graphite material, so that the adsorption capacity of the binder on the surface of the carbon graphite material is obviously improved, and the binding strength is improved.
(3) Adding Al, Si and TiO2The kaolin is an inorganic filler, so that the oxidation resistance and high temperature resistance of the adhesive are improved, the use temperature of the adhered carbon graphite material exceeds 1800 ℃, and good mechanical properties are still maintained;
(4) the adhesive can be rapidly cured for 1 hour at the low temperature of 80-130 ℃, further high-temperature heat treatment is not needed, the cost of the adhesive brushing and curing process is low, the operation is simple, and the adhesive efficiency is greatly improved.
Detailed Description
The present invention will be further described with reference to the following examples. The described embodiments and their results are only intended to illustrate the invention and should not be taken as limiting the invention described in detail in the claims.
Example 1
The mass fractions of the components of the low-temperature curing high-temperature-resistant carbon graphite material binder in the embodiment are 40% of resin, 25% of graphite powder, 30% of filler and 5% of diluent; wherein the mass ratio of the epoxy resin to the phenolic resin in the resin is that the epoxy resin: phenolic resin is 1:2, epoxy value of epoxy resin is 0.51; the particle diameter of the graphite powder is selected from D508 μm; TiO in the filler210 parts of Al, 18 parts of Si and 20 parts of kaolin; wherein the diluent is ethanol.
(1) Preparing resin and filler, and preparing raw materials according to the raw material components; (2) adding a diluent into the resin, stirring, and diluting to 100-150 mPa & s in viscosity for later use; (3) grinding the filler into powder, and uniformly mixing the powder with graphite powder to obtain mixed powder; (4) slowly adding the diluted resin solution into the mixed powder at a constant speed, and continuously stirring and dispersing for 1h until the solid phase and the liquid phase are uniformly mixed to obtain the binder.
The bonding density of the prepared binder is more than or equal to 1.72t/m3The medium-coarse particle graphite plate has the size of 130 multiplied by 50 multiplied by 10mm, and comprises the following steps: cleaning the connecting surface of the carbon graphite material to be bonded; coating a binder on the bonding surface of the carbon graphite material, wherein the thickness of the coating is 0.5-1 mm, bonding the carbon graphite material after coating, and properly compressing; and (3) baking the bonded carbon graphite material for 1h at 110 ℃ in an air environment to finish curing, so as to achieve the bonding strength.
After bonding, the graphite plate is baked in a resistance furnace at room temperature and 950 ℃ for 1 hour and then the bonding strength is respectively tested, the shear strength at room temperature is more than or equal to 11MPa, and the shear strength after high-temperature treatment is more than or equal to 12 MPa.
Example 2
The mass fractions of the components of the low-temperature curing high-temperature-resistant carbon graphite material binder in the embodiment are 48% of resin, 26% of graphite, 20% of filler and 6% of diluent; wherein the mass ratio of the epoxy resin to the phenolic resin in the resin is that the epoxy resin: phenolic resin is 1.5:2, epoxy value of epoxy resin is 0.51; the particle diameter of the graphite powder is selected from D508 μm; TiO in the filler212 parts of Al, 16 parts of Si and 29 parts of kaolin; wherein the diluent is ethanol.
(1) Preparing resin and filler, and preparing raw materials according to the raw material components; (2) adding a diluent into the resin, stirring, and diluting to 100-150 mPa & s in viscosity for later use; (3) grinding the filler into powder, and uniformly mixing the powder with graphite powder to obtain mixed powder; (4) slowly adding the diluted resin solution into the mixed powder at a constant speed, and continuously stirring and dispersing for 1h until the solid phase and the liquid phase are uniformly mixed to obtain the binder.
The bonding density of the prepared binder is more than or equal to 1.8t/m3The fine particle graphite sheet of (1), the size of the graphite sheet is 130X 50X 10mm, according to the following steps: cleaning the connecting surface of the carbon graphite material to be bonded; coating a binder on the bonding surface of the carbon graphite material, wherein the thickness of the coating is 0.5-1 mm, bonding the carbon graphite material after coating, and properly compressing; bonding the carbon graphite materialThe material is baked for 1h at 110 ℃ in the air environment, and the curing is completed, so that the bonding strength is achieved.
After bonding, the graphite plate is baked in a resistance furnace at 1000 ℃ for 0.5h, and then the bonding strength is tested, and the shearing strength of the test result is more than or equal to 13 MPa.
Example 3
The mass fractions of the components of the low-temperature curing high-temperature-resistant carbon graphite material binder in the embodiment are 55% of resin, 15% of graphite, 22% of filler and 8% of diluent; wherein the mass ratio of the epoxy resin to the phenolic resin in the resin is that the epoxy resin: phenolic resin is 1.5:2, epoxy value of epoxy resin is 0.51; the particle diameter of the graphite powder is selected from D5012 μm; TiO in the filler212 parts of Al, 15 parts of Si and 25 parts of kaolin; wherein the diluent is selected from ethanol and acetone and is mixed according to the mass ratio of 1: 1.
(1) Preparing resin and filler, and preparing raw materials according to the raw material components; (2) adding a diluent into the resin, stirring, and diluting to 100-150 mPa & s in viscosity for later use; (3) grinding the filler into powder, and uniformly mixing the powder with graphite powder to obtain mixed powder; (4) slowly adding the diluted resin solution into the mixed powder at a constant speed, and continuously stirring and dispersing for 1h until the solid phase and the liquid phase are uniformly mixed to obtain the binder.
The bonding density of the prepared binder is more than or equal to 1.82t/m3The fine particle graphite sheet of (1), the size of the graphite sheet is 130X 50X 10mm, according to the following steps: cleaning the connecting surface of the carbon graphite material to be bonded; coating a binder on the bonding surface of the carbon graphite material, wherein the thickness of the coating is 0.5-1 mm, bonding the carbon graphite material after coating, and properly compressing; and (3) baking the bonded carbon graphite material for 1h at 130 ℃ in an air environment to finish curing, so as to achieve the bonding strength.
After bonding, the graphite plate is baked in a resistance furnace at 1000 ℃ for 1h, and then the bonding strength is tested, and the shear strength of the test result is more than or equal to 15 MPa.
Claims (7)
1. The low-temperature curing high-temperature-resistant carbon graphite material binder is baked for 1 hour at the temperature of 80-130 ℃, and comprises the following components in parts by mass: 40-60% of resin, 15-30% of graphite powder, 20-35% of filler and 5-8% of diluent.
2. The low-temperature curing high-temperature-resistant carbon graphite material adhesive as claimed in claim 1, wherein: the resin is a combination of epoxy resin and phenolic resin, and the mass ratio is 1-1.5: 2; the epoxy value of the epoxy resin is 0.51, and the high-temperature carbon residue rate of the combined resin is more than 45 percent.
3. The low-temperature curing high-temperature-resistant carbon graphite material adhesive as claimed in claim 1, wherein: the graphite powder is porous graphite powder, and the specific surface area is more than 45m2(iii) a particle size of 5 to 15 μm/g.
4. The low-temperature curing high-temperature-resistant carbon graphite material adhesive as claimed in claim 1, wherein: the filler component comprises TiO2The filler comprises TiO and Al, Si and kaolin in parts by weight210-13 parts of Al, 20-32 parts of Si, and 20-32 parts of kaolin.
5. The low-temperature curing high-temperature-resistant carbon graphite material adhesive as claimed in claim 1, wherein: the diluent is one or a combination of more of acetone, ethanol and glycol.
6. The preparation method of the low-temperature curing high-temperature-resistant carbon graphite material binder as claimed in claims 1-5, which is characterized by comprising the following steps:
(1) preparing resin and filler, and preparing raw materials according to 40-60% of resin, 15-30% of graphite powder, 20-35% of filler and 5-8% of diluent;
(2) adding a diluent into the resin, stirring, and diluting to 100-150 mPa & s in viscosity for later use;
(3) grinding the filler into powder, and uniformly mixing the powder with graphite powder to obtain mixed powder;
(4) slowly adding the diluted resin solution into the mixed powder at a constant speed, continuously stirring and dispersing until the solid phase and the liquid phase are uniformly mixed, thus obtaining the binder.
7. The use method of the low-temperature curing high-temperature resistant carbon graphite material binder as claimed in claims 1-5, is characterized by comprising the following steps: cleaning the connecting surface of the carbon graphite material to be bonded; coating a binder on the bonding surface of the carbon graphite material, wherein the thickness of the coating is 0.5-1 mm, bonding the carbon graphite material after coating, and properly compressing; baking the bonded carbon graphite material for 1h at 80-130 ℃ in an air environment to finish curing and achieve bonding strength; the bonded carbon graphite material can be directly used in a high-temperature environment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010058358.5A CN111253889A (en) | 2020-01-18 | 2020-01-18 | Low-temperature curing high-temperature-resistant carbon graphite material binder and preparation and use methods thereof |
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| CN202010058358.5A CN111253889A (en) | 2020-01-18 | 2020-01-18 | Low-temperature curing high-temperature-resistant carbon graphite material binder and preparation and use methods thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112442328A (en) * | 2020-11-26 | 2021-03-05 | 西安建筑科技大学 | Adhesive, preparation method and application thereof |
| CN114106512A (en) * | 2021-09-09 | 2022-03-01 | 周琬彤 | Preparation method of epoxy resin-based composite material for curved surface and flow channel of hydraulic element |
| CN114410060A (en) * | 2021-12-23 | 2022-04-29 | 厦门泰启力飞科技有限公司 | Face cover of camera device and preparation method thereof |
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| CN104342079A (en) * | 2013-08-01 | 2015-02-11 | 甘肃郝氏炭纤维有限公司 | Preparation method and application method of high-temperature bonding agent used for bonding carbon felts |
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2020
- 2020-01-18 CN CN202010058358.5A patent/CN111253889A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104342079A (en) * | 2013-08-01 | 2015-02-11 | 甘肃郝氏炭纤维有限公司 | Preparation method and application method of high-temperature bonding agent used for bonding carbon felts |
Non-Patent Citations (1)
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| 陈平等: "《环氧树脂及其应用》", 29 February 2004, 化学工业出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112442328A (en) * | 2020-11-26 | 2021-03-05 | 西安建筑科技大学 | Adhesive, preparation method and application thereof |
| CN114106512A (en) * | 2021-09-09 | 2022-03-01 | 周琬彤 | Preparation method of epoxy resin-based composite material for curved surface and flow channel of hydraulic element |
| CN114410060A (en) * | 2021-12-23 | 2022-04-29 | 厦门泰启力飞科技有限公司 | Face cover of camera device and preparation method thereof |
| CN114410060B (en) * | 2021-12-23 | 2023-09-19 | 厦门泰启力飞科技有限公司 | Face cover of camera device and preparation method thereof |
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Application publication date: 20200609 |