CN110606744A - Special graphite heat exchanger material and preparation method thereof - Google Patents
Special graphite heat exchanger material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of graphite materials, in particular to a special graphite heat exchanger material and a preparation method thereof, wherein the special graphite heat exchanger material has low requirement on equipment, is simple and convenient to operate, has high density and high strength, and is reasonable in process, the special graphite heat exchanger material comprises a mixture and a binder, the weight ratio of the mixture to the binder is (70 ~ 75) to (25 ~ 30), the mixture comprises aggregates and powder, the aggregates are needle-shaped petroleum coke, the powder is special graphite powder and semi-reinforcing carbon black, and the binder is medium-temperature coal pitch.
Description
Technical Field
The invention relates to the technical field of graphite materials, in particular to a special graphite heat exchanger material and a preparation method thereof.
Background
Graphite heat exchangers have developed very rapidly since the 20 th century and the 30 th era. A large number of graphite heat exchangers with excellent performance are used in the process of treating various media such as hydrochloric acid, sulfuric acid, citric acid, pesticide intermediates and the like except strong alkali and strong oxidizing media, are widely applied to various industrial departments such as chemical industry, food industry, pharmaceutical industry and the like, and are mainly used for chemical unit operations such as heating, cooling, condensation, evaporation and the like. Because graphite has good thermal conductivity, excellent corrosion resistance and no pollution to media, the graphite heat exchanger has largely replaced the heat exchanger made of stainless steel or other noble metals, thus solving the corrosion resistance problem of a plurality of devices in the industries of chemical engineering and the like.
The graphite heat exchanger is divided into a plurality of forms such as a tube type, a block hole type, a spray type, an immersion type and the like according to the structural form. Among them, the most widely used are tube-type and block-hole type graphite heat exchangers. They can be divided into several types, such as evaporator, heater, cooler and condenser, according to their application in the technological process.
The graphite heat exchanger has large specification, and the maximum heat exchange area of the tube type reaches 1670m2. In the round block hole type series, the largest heat exchange area reaches 1950m2Paid for use up to 1200m2. The design temperature of the graphite heat exchanger is 320-500 ℃ of divinylbenzene impregnation except that the phenolic resin impregnation temperature is 170 ℃. Certain types of graphite heat exchangers can be used at temperatures as high as 800 c or even 1200 c in an inert atmosphere. The graphite heat exchanger used at present has certain defects in certain aspects, although graphite belongs to a brittle material, if the graphite heat exchanger is properly designed, manufactured and used, the service life of the graphite heat exchanger is long, and therefore certain improvement on the existing graphite heat exchanger is needed to improve various physical and chemical properties of the graphite heat exchanger.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a special graphite heat exchanger material with low equipment requirement, simple and convenient operation, high density and high strength;
the invention also aims to provide a preparation method of the special graphite heat exchanger material with reasonable process.
The special graphite heat exchanger material comprises a mixture and a binder, wherein the weight ratio of the mixture to the binder is (70 ~ 75): (25 ~ 30), the mixture comprises aggregate and powder, the aggregate is needle petroleum coke, the powder is special graphite powder and semi-reinforcing carbon black, and the binder is medium-temperature coal pitch.
The softening point of the medium-temperature coal pitch of the binder is 83-86 ℃, the coking value is more than or equal to 51 percent, the ash content is less than or equal to 0.25 percent, and the quinoline insoluble substance is less than or equal to 0.30 percent.
The invention relates to a special graphite heat exchanger material, which comprises the following components in percentage by weight:
the grain diameter is more than 0.045 mu m and less than or equal to 0.033 mu m 5 ~ 15 wt%;
the grain diameter is more than 0.033 mu m and less than or equal to 0.010 mu m and 15 ~ 25 wt%;
the grain diameter is more than 0.010 mu m and less than or equal to 0.070 mu m, 25 ~ 30 wt%;
0 < particle size < 0.070 μm 40 ~ 45 wt%.
According to the special graphite heat exchanger material, the crushed particle size range and the content of the acicular petroleum coke are preferably as follows according to the weight percentage content:
the grain diameter is more than 0.045 mu m and less than or equal to 0.033 mu m by weight percent;
the grain diameter is more than 0.033 mu m and less than or equal to 0.010 mu m and 15wt percent;
the grain diameter is more than 0.010 mu m and less than or equal to 0.070 mu m by 30wt percent;
the grain diameter is more than 0 and less than 0.070 mu m, 40wt percent.
The true density of the acicular petroleum coke is more than or equal to 2.13g/cm3Ash content is less than or equal to 0.20 percent, volatile matter is less than or equal to 0.25 percent, and sulfur content is less than or equal to 0.40 percent.
The invention relates to a special graphite heat exchanger material, which comprises the following components in parts by weight:
15 ~ 20% of special graphite powder;
semi-reinforcing carbon black 15 ~ 20%;
60 ~ 70% of needle petroleum coke.
The volume density of the special graphite powder of the powder is 1.85g/cm3The resistivity is less than or equal to 8 mu omega m, the breaking strength is more than or equal to 30Mpa, the compressive strength is more than or equal to 60Mpa, and the grain diameter is-450 meshes.
The particle size of the special graphite powder is preferably 35-40 μm, more preferably 36-39 μm, and most preferably 39 μm;
the semi-reinforcing carbon black has a particle size of 45-50 μm, a resistivity of 0.6-0.9 μ Ω · m, and a pH value of 7.5-9.
The semi-reinforcing carbon black preferably has a particle size of 45 to 50 μm, more preferably 45 to 50 μm, and most preferably 50 μm.
The invention discloses a preparation method of a special graphite heat exchanger material, which comprises the following steps:
(1) crushing and mixing: crushing and screening the aggregate and the powder according to a proportion, and then mixing;
(2) mixing and kneading, namely mixing and kneading into dry mixing and wet mixing, firstly pouring the graded ingredients into a mixing and kneading pot for stirring through dry mixing, wherein the mixing and kneading pot is in a horizontal double-reamer type, the inlet temperature of the mixing and kneading pot is 220 ~ 250 ℃, the dry mixing temperature of aggregate is 130 ~ 140 ℃, the dry mixing time is 45 ~ 50min, then adding a binder for wet mixing, the wet mixing temperature is 140 ~ 150 ℃, and the wet mixing time is 40 ~ 45 min;
(3) preforming: pouring the kneaded paste into a forming container, and performing pre-pressing forming, wherein the pre-pressing pressure is 25MP, and the pre-pressing time is 5 min;
(4) crushing the pre-pressed blank into 25 ~ 30 micron size with crusher;
(5) regrinding: grinding the crushed blank by using a grinder, wherein the granularity of the ground powder is required to be less than 0.80 mu m;
(6) and (4) screening: screening and grading the milled materials, and storing the materials in bins;
(7) and (3) remixing: uniformly mixing the materials stored in a grading way by using a cyclone mixer;
(8) isostatic pressing: the evenly mixed powder is filled into rubberSealing in a rubber mold, keeping the pressure at 150MP for 7min for cold isostatic pressing, and making the molded green body have a volume density of 1.80 ~ 1.90.90 g/cm3；
(9) Primary roasting: placing the molded green body into a graphite crucible, filling metallurgical coke powder into the graphite crucible, compacting the graphite crucible, placing the graphite crucible into a ring type roasting furnace, filling the furnace with coke powder, quartz sand, river sand and the like, gradually heating according to a temperature rise curve under the condition of isolating air, and carrying out primary roasting treatment on the green body;
(10) impregnating, namely preheating the roasted product to 300 ~ 350 ℃, keeping the temperature for 8 hours, putting the roasted product into an impregnating tank, vacuumizing the impregnating tank, pressurizing for 2.5 hours, injecting an impregnant into the impregnating tank, and keeping the pressure for 2 hours to ensure that the impregnant is immersed into pores of the roasted product;
(11) secondary roasting in a tunnel kiln: rapidly sintering asphalt on the impregnated product by a tunnel kiln at the highest temperature of 750 ℃ for 192 hours;
(12) and (3) graphitizing, namely putting the product after secondary roasting into an Acheson graphitizing furnace, heating the roasted product to 2750 ~ 3200 ℃ by current under the condition of air isolation, converting the two-dimensional structure carbon product into a three-dimensional graphite grid structure, and transmitting power for 8 ~ 10 days.
The preparation method of the special graphite heat exchanger material comprises the step (9) of heating the material at 150 ~ ℃ for 55h at a heating rate of 2.0 ~.0 ℃/h, keeping the temperature for 40h at 350 ~ ℃, at 400 ~ ℃ for 85h at a heating rate of 1.2 ~.3 ℃/h, at 500 ~ ℃ for 1.7 ~.0 ℃/h and keeping the temperature for 72h at 500 ~ ℃, at 650 ℃ for 650.5 ~ ℃ for 3.5 ~.5 ℃/h and keeping the temperature for 24h at 750 ~ ℃ for 4.0 ~ ℃/h, at 850 ~ ℃ for 1150 ℃, at 6.825.5 h, at 30.0 ℃/h, at 8542 ℃ for 24h, at 1150 ℃ for 24h, at 25, at 30.1250 ℃ for 30.1250 h, at 25 ℃ for 24h, at 25 ℃ for 898.25 ℃/h, and at room temperature for 898.25 ℃ for 24h and cooling at room temperature of 898.25 ℃ for 36 h and room temperature for 898.8 h.
The invention relates to a preparation method of a special graphite heat exchanger material, wherein the impregnant in the step (10) is medium-temperature coal pitch.
The softening point of the medium-temperature coal pitch used as the impregnant is 83-88 ℃, the coking value is more than or equal to 48 percent, and the quinoline insoluble substance is less than or equal to 0.30 percent.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a graphite heat exchanger material with excellent physical and chemical properties and superior quality, which mainly comprises acicular petroleum coke as an aggregate; the powder material is special graphite powder and carbon black; the binder is medium temperature coal pitch; the impregnant is composed of various materials such as medium-temperature coal pitch, and is converted into microcrystal artificial graphite through high-temperature purification treatment at the maximum temperature of 3200 ℃, and the volume density of the microcrystal artificial graphite is more than or equal to 2.0g/cm3The compression strength is more than or equal to 140MPa, the breaking strength is more than or equal to 70MPa, the thermal conductivity is 140 w/(m.K), the resistivity is less than or equal to 7.0 mu omega, m, the Shore hardness is more than or equal to 60, the porosity is less than or equal to 10%, the ash content is less than or equal to 0.5%, and the qualification rate of finished products of the material prepared by the method is more than 90%; wherein, the GB/T245728-; the compressive strength is tested according to GB/T1431-2009 standard; the thermal conductivity is tested according to the GB/T10297-1998 standard; the resistivity is tested according to GB/T1410-2006; shore hardness was tested according to GB/T4341-2001 standard; testing the porosity according to GB/T6155-2008 detection standard; the ash content is according to GB/T9345.1-2008.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The special graphite heat exchanger material comprises a mixture and a binder in a ratio of 70:25, wherein the mixture comprises aggregate and powder, the aggregate is needle petroleum coke, the powder is special graphite powder and semi-reinforcing carbon black, and the binder is medium-temperature coal pitch.
The broken grain size range and the content of the acicular petroleum coke are as follows according to the weight percentage:
the grain diameter is more than 0.045 mu m and less than or equal to 0.033 mu m by weight percent;
the grain diameter is more than 0.033 mu m and less than or equal to 0.010 mu m and 25wt percent;
the grain diameter is more than 0.010 mu m and less than or equal to 0.070 mu m by 25wt percent;
the grain diameter is more than 0 and less than 0.070 mu m and 45wt percent.
The weight ratio of each component in the mixture is as follows:
15% of special graphite powder;
15% of semi-reinforcing carbon black;
70 percent of acicular petroleum coke.
The preparation method comprises the following steps:
(1) crushing and mixing: crushing and screening the aggregate and the powder according to a proportion, and then mixing;
(2) mixing and kneading, namely mixing and kneading into dry mixing and wet mixing, firstly pouring the graded ingredients into a mixing and kneading pot for stirring through dry mixing, wherein the mixing and kneading pot is in a horizontal double-reamer type, the inlet temperature of the mixing and kneading pot is 220 ~ 250 ℃, the dry mixing temperature of aggregate is 130 ~ 140 ℃, the dry mixing time is 45 ~ 50min, then adding a binder for wet mixing, the wet mixing temperature is 140 ~ 150 ℃, and the wet mixing time is 40 ~ 45 min;
(3) preforming: pouring the kneaded paste into a forming container, and performing pre-pressing forming, wherein the pre-pressing pressure is 25MP, and the pre-pressing time is 5 min;
(4) crushing the pre-pressed blank into 25 ~ 30 micron size with crusher;
(5) regrinding: grinding the crushed blank by using a grinder, wherein the granularity of the ground powder is required to be less than 0.80 mu m;
(6) and (4) screening: screening and grading the milled materials, and storing the materials in bins;
(7) and (3) remixing: uniformly mixing the materials stored in a grading way by using a cyclone mixer;
(8) isostatic pressing, namely filling the uniformly mixed powder into a rubber mould and sealing, keeping the pressure for 7min at the forming pressure of 150MP for cold isostatic pressing, wherein the volume density of the formed green body is 1.80 ~ 1.90.90 g/cm3；
(9) Primary roasting, namely placing the molded green body into a graphite crucible, filling metallurgical coke powder into the graphite crucible, compacting the graphite crucible, placing the graphite crucible into a ring-type roasting furnace, filling the graphite crucible with the metallurgical coke powder, quartz sand, river sand and the like, gradually heating the green body according to a heating curve under the condition of isolating air, and carrying out primary roasting treatment on the green body, wherein the heating curve comprises the heating rate of 2.0 ~.0 ℃/h and the holding time of 55h at the temperature of 150 ~ ℃, the heating rate of 1.4 ~.7 ℃/h and the holding time of 40h at the temperature of 350 ~ ℃, the heating rate of 1.2 ~ 1.3 ℃/h and the holding time of 85h at the temperature of 400 ~ ℃, the heating rate of 1.7 ~.0 ℃/h and the holding time of 72h at the temperature of 500 ~ ℃, the heating rate of 3.5 5393.5 ℃/h and the holding time of 24h at the temperature of 650 ~ ℃, the heating rate of 3.5, 5, 84, 5, 7, 5, 7, 5, 7, 5;
(10) dipping, namely preheating the roasted product to 300 ~ 350 ℃, keeping the temperature for 8h, putting the roasted product into a dipping tank, vacuumizing the dipping tank, pressurizing for 2.5h, injecting an impregnant into the dipping tank, and keeping the pressure for 2h to ensure that the impregnant is immersed into pores of the roasted product, wherein the impregnant is medium-temperature coal pitch, and the dipping weight gain rate is 17 ~ 19%;
(11) secondary roasting in a tunnel kiln: rapidly sintering asphalt on the impregnated product by a tunnel kiln at the highest temperature of 750 ℃ for 192 hours;
(12) and (3) graphitizing, namely putting the product after secondary roasting into an Acheson graphitizing furnace, heating the roasted product to 2750 ~ 3200 ℃ by current under the condition of air isolation, converting the two-dimensional structure carbon product into a three-dimensional graphite grid structure, and transmitting power for 8 ~ 10 days.
Example 2
The invention relates to a special graphite heat exchanger material, which comprises a 72:28 mixture and a binder, wherein the mixture comprises aggregate and powder, the aggregate is needle petroleum coke, the powder is special graphite powder and semi-reinforcing carbon black, and the binder is medium-temperature coal pitch.
The broken grain size range and the content of the acicular petroleum coke are as follows according to the weight percentage:
the grain diameter is more than 0.045 mu m and less than or equal to 0.033 mu m by weight;
the grain diameter is more than 0.033 mu m and less than or equal to 0.010 mu m and 20wt percent;
the grain diameter is more than 0.010 mu m and less than or equal to 0.070 mu m by 30wt percent;
the grain diameter is more than 0 and less than 0.070 mu m, 40wt percent.
The weight ratio of each component in the mixture is as follows:
17% of special graphite powder;
18% of semi-reinforcing carbon black;
65 percent of needle petroleum coke.
The preparation method comprises the following steps:
(1) crushing and mixing: crushing and screening the aggregate and the powder according to a proportion, and then mixing;
(2) mixing and kneading, namely mixing and kneading into dry mixing and wet mixing, firstly pouring the graded ingredients into a mixing and kneading pot for stirring through dry mixing, wherein the mixing and kneading pot is in a horizontal double-reamer type, the inlet temperature of the mixing and kneading pot is 220 ~ 250 ℃, the dry mixing temperature of aggregate is 130 ~ 140 ℃, the dry mixing time is 45 ~ 50min, then adding a binder for wet mixing, the wet mixing temperature is 140 ~ 150 ℃, and the wet mixing time is 40 ~ 45 min;
(3) preforming: pouring the kneaded paste into a forming container, and performing pre-pressing forming, wherein the pre-pressing pressure is 25MP, and the pre-pressing time is 5 min;
(4) crushing the pre-pressed blank into 25 ~ 30 micron size with crusher;
(5) regrinding: grinding the crushed blank by using a grinder, wherein the granularity of the ground powder is required to be less than 0.80 mu m;
(6) and (4) screening: screening and grading the milled materials, and storing the materials in bins;
(7) and (3) remixing: uniformly mixing the materials stored in a grading way by using a cyclone mixer;
(8) isostatic pressing, namely filling the uniformly mixed powder into a rubber mould and sealing, keeping the pressure for 7min at the forming pressure of 150MP for cold isostatic pressing, wherein the volume density of the formed green body is 1.80 ~ 1.90.90 g/cm3；
(9) Primary roasting, namely placing the molded green body into a graphite crucible, filling metallurgical coke powder into the graphite crucible, compacting the graphite crucible, placing the graphite crucible into a ring-type roasting furnace, filling the graphite crucible with the metallurgical coke powder, quartz sand, river sand and the like, gradually heating the green body according to a heating curve under the condition of isolating air, and carrying out primary roasting treatment on the green body, wherein the heating curve comprises the heating rate of 2.0 ~.0 ℃/h and the holding time of 55h at the temperature of 150 ~ ℃, the heating rate of 1.4 ~.7 ℃/h and the holding time of 40h at the temperature of 350 ~ ℃, the heating rate of 1.2 ~ 1.3 ℃/h and the holding time of 85h at the temperature of 400 ~ ℃, the heating rate of 1.7 ~.0 ℃/h and the holding time of 72h at the temperature of 500 ~ ℃, the heating rate of 3.5 5393.5 ℃/h and the holding time of 24h at the temperature of 650 ~ ℃, the heating rate of 3.5, 5, 84, 5, 7, 5, 7, 5, 7, 5;
(10) dipping, namely preheating the roasted product to 300 ~ 350 ℃, keeping the temperature for 8h, putting the roasted product into a dipping tank, vacuumizing the dipping tank, pressurizing for 2.5h, injecting an impregnant into the dipping tank, and keeping the pressure for 2h to ensure that the impregnant is immersed into pores of the roasted product, wherein the impregnant is medium-temperature coal pitch, and the dipping weight gain rate is 17 ~ 19%;
(11) secondary roasting in a tunnel kiln: rapidly sintering asphalt on the impregnated product by a tunnel kiln at the highest temperature of 750 ℃ for 192 hours;
(12) and (3) graphitizing, namely putting the product after secondary roasting into an Acheson graphitizing furnace, heating the roasted product to 2750 ~ 3200 ℃ by current under the condition of air isolation, converting the two-dimensional structure carbon product into a three-dimensional graphite grid structure, and transmitting power for 8 ~ 10 days.
Example 3
The special graphite heat exchanger material comprises a 75:30 mixture and a binder, wherein the mixture comprises aggregate and powder, the aggregate is needle petroleum coke, the powder is special graphite powder and semi-reinforcing carbon black, and the binder is medium-temperature coal pitch.
The broken grain size range and the content of the acicular petroleum coke are as follows according to the weight percentage:
the grain diameter is more than 0.045 mu m and less than or equal to 0.033 mu m by weight;
the grain diameter is more than 0.033 mu m and less than or equal to 0.010 mu m and 25wt percent;
the grain diameter is more than 0.010 mu m and less than or equal to 0.070 mu m by 25wt percent;
the grain diameter is more than 0 and less than 0.070 mu m, 40wt percent.
The weight ratio of each component in the mixture is as follows:
20% of special graphite powder;
20% of semi-reinforcing carbon black;
60 percent of acicular petroleum coke.
The preparation method comprises the following steps:
(1) crushing and mixing: crushing and screening the aggregate and the powder according to a proportion, and then mixing;
(2) mixing and kneading, namely mixing and kneading into dry mixing and wet mixing, firstly pouring the graded ingredients into a mixing and kneading pot for stirring through dry mixing, wherein the mixing and kneading pot is in a horizontal double-reamer type, the inlet temperature of the mixing and kneading pot is 220 ~ 250 ℃, the dry mixing temperature of aggregate is 130 ~ 140 ℃, the dry mixing time is 45 ~ 50min, then adding a binder for wet mixing, the wet mixing temperature is 140 ~ 150 ℃, and the wet mixing time is 40 ~ 45 min;
(3) preforming: pouring the kneaded paste into a forming container, and performing pre-pressing forming, wherein the pre-pressing pressure is 25MP, and the pre-pressing time is 5 min;
(4) crushing the pre-pressed blank into 25 ~ 30 micron size with crusher;
(5) regrinding: grinding the crushed blank by using a grinder, wherein the granularity of the ground powder is required to be less than 0.80 mu m;
(6) and (4) screening: screening and grading the milled materials, and storing the materials in bins;
(7) and (3) remixing: uniformly mixing the materials stored in a grading way by using a cyclone mixer;
(8) isostatic pressing, namely filling the uniformly mixed powder into a rubber mould and sealing, keeping the pressure for 7min at the forming pressure of 150MP for cold isostatic pressing, wherein the volume density of the formed green body is 1.80 ~ 1.90.90 g/cm3；
(9) Primary roasting, namely placing the molded green body into a graphite crucible, filling metallurgical coke powder into the graphite crucible, compacting the graphite crucible, placing the graphite crucible into a ring-type roasting furnace, filling the graphite crucible with the metallurgical coke powder, quartz sand, river sand and the like, gradually heating the green body according to a heating curve under the condition of isolating air, and carrying out primary roasting treatment on the green body, wherein the heating curve comprises the heating rate of 2.0 ~.0 ℃/h and the holding time of 55h at the temperature of 150 ~ ℃, the heating rate of 1.4 ~.7 ℃/h and the holding time of 40h at the temperature of 350 ~ ℃, the heating rate of 1.2 ~ 1.3 ℃/h and the holding time of 85h at the temperature of 400 ~ ℃, the heating rate of 1.7 ~.0 ℃/h and the holding time of 72h at the temperature of 500 ~ ℃, the heating rate of 3.5 5393.5 ℃/h and the holding time of 24h at the temperature of 650 ~ ℃, the heating rate of 3.5, 5, 84, 5, 7, 5, 7, 5, 7, 5;
(10) dipping, namely preheating the roasted product to 300 ~ 350 ℃, keeping the temperature for 8h, putting the roasted product into a dipping tank, vacuumizing the dipping tank, pressurizing for 2.5h, injecting an impregnant into the dipping tank, and keeping the pressure for 2h to ensure that the impregnant is immersed into pores of the roasted product, wherein the impregnant is medium-temperature coal pitch, and the dipping weight gain rate is 17 ~ 19%;
(11) secondary roasting in a tunnel kiln: rapidly sintering asphalt on the impregnated product by a tunnel kiln at the highest temperature of 750 ℃ for 192 hours;
(12) and (3) graphitizing, namely putting the product after secondary roasting into an Acheson graphitizing furnace, heating the roasted product to 2750 ~ 3200 ℃ by current under the condition of air isolation, converting the two-dimensional structure carbon product into a three-dimensional graphite grid structure, and transmitting power for 8 ~ 10 days.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The special graphite heat exchanger material is characterized by comprising a mixture and a binder, wherein the weight ratio of the mixture to the binder is (70 ~ 75): (25 ~ 30), the mixture comprises aggregates and powder, the aggregates are needle petroleum coke, the powder is special graphite powder and semi-reinforcing carbon black, and the binder is medium-temperature coal pitch.
2. The special graphite heat exchanger material as claimed in claim 1, wherein the needle petroleum coke has a crushed particle size range and content in weight percent:
the grain diameter is more than 0.045 mu m and less than or equal to 0.033 mu m 5 ~ 15 wt%;
the grain diameter is more than 0.033 mu m and less than or equal to 0.010 mu m and 15 ~ 25 wt%;
the grain diameter is more than 0.010 mu m and less than or equal to 0.070 mu m, 25 ~ 30 wt%;
0 < particle size < 0.070 μm 40 ~ 45 wt%.
3. The special graphite heat exchanger material as claimed in claim 2, wherein the needle petroleum coke has a crushed particle size range and content preferably as follows by weight percentage:
the grain diameter is more than 0.045 mu m and less than or equal to 0.033 mu m by weight percent;
the grain diameter is more than 0.033 mu m and less than or equal to 0.010 mu m and 15wt percent;
the grain diameter is more than 0.010 mu m and less than or equal to 0.070 mu m by 30wt percent;
the grain diameter is more than 0 and less than 0.070 mu m, 40wt percent.
4. The special graphite heat exchanger material as claimed in claim 1, wherein the weight ratio of each component in the mixed material is as follows:
15 ~ 20% of special graphite powder;
semi-reinforcing carbon black 15 ~ 20%;
60 ~ 70% of needle petroleum coke.
5. The method for preparing a special graphite heat exchanger material as claimed in claim 1, comprising the following steps:
(1) crushing and mixing: crushing and screening the aggregate and the powder according to a proportion, and then mixing;
(2) mixing and kneading, namely mixing and kneading into dry mixing and wet mixing, firstly pouring the graded ingredients into a mixing and kneading pot for stirring through dry mixing, wherein the mixing and kneading pot is in a horizontal double-reamer type, the inlet temperature of the mixing and kneading pot is 220 ~ 250 ℃, the dry mixing temperature of aggregate is 130 ~ 140 ℃, the dry mixing time is 45 ~ 50min, then adding a binder for wet mixing, the wet mixing temperature is 140 ~ 150 ℃, and the wet mixing time is 40 ~ 45 min;
(3) preforming: pouring the kneaded paste into a forming container, and performing pre-pressing forming, wherein the pre-pressing pressure is 25MP, and the pre-pressing time is 5 min;
(4) crushing the pre-pressed blank into 25 ~ 30 micron size with crusher;
(5) regrinding: grinding the crushed blank by using a grinder, wherein the granularity of the ground powder is required to be less than 0.80 mu m;
(6) and (4) screening: screening and grading the milled materials, and storing the materials in bins;
(7) and (3) remixing: uniformly mixing the materials stored in a grading way by using a cyclone mixer;
(8) isostatic pressing, namely filling the uniformly mixed powder into a rubber mould and sealing, keeping the pressure for 7min at the forming pressure of 150MP for cold isostatic pressing, wherein the volume density of the formed green body is 1.80 ~ 1.90.90 g/cm3；
(9) Primary roasting: placing the molded green body into a graphite crucible, filling metallurgical coke powder into the graphite crucible, compacting the graphite crucible, placing the graphite crucible into a ring type roasting furnace, filling the furnace with coke powder, quartz sand, river sand and the like, gradually heating according to a temperature rise curve under the condition of isolating air, and carrying out primary roasting treatment on the green body;
(10) impregnating, namely preheating the roasted product to 300 ~ 350 ℃, keeping the temperature for 8 hours, putting the roasted product into an impregnating tank, vacuumizing the impregnating tank, pressurizing for 2.5 hours, injecting an impregnant into the impregnating tank, and keeping the pressure for 2 hours to ensure that the impregnant is immersed into pores of the roasted product;
(11) secondary roasting in a tunnel kiln: rapidly sintering asphalt on the impregnated product by a tunnel kiln at the highest temperature of 750 ℃ for 192 hours;
(12) and (3) graphitizing, namely putting the product after secondary roasting into an Acheson graphitizing furnace, heating the roasted product to 2750 ~ 3200 ℃ by current under the condition of air isolation, converting the two-dimensional structure carbon product into a three-dimensional graphite grid structure, and transmitting power for 8 ~ 10 days.
6. The method for preparing a special graphite heat exchanger material as claimed in claim 5, wherein the temperature rise curve in step (9) is that the temperature rise rate is 2.0 ~.0 ℃/h and the holding time is 55h at 150 ~ ℃ and 350 ℃, the temperature rise rate is 1.4 ~ 1.7 ℃/h and the holding time is 40h at 350 ~ ℃, the temperature rise rate is 1.2 ~.3 ℃/h and the holding time is 85h at 400 ~ ℃, the temperature rise rate is 1.7 ~.0 ℃/h and the holding time is 72h at 500 ~ ℃, the temperature rise rate is 3.5 ~.5 ℃/h and the holding time is 24h at 650 ~ ℃ and 500 ℃, the temperature rise rate is 4.0 ~.0 ℃/h and the holding time is 24h at 750 ~ ℃, the temperature rise rate is 4.1250 ℃/h and the holding time is 24h at 850 ~ ℃, the temperature rise rate is 6.825, the holding time is 30.1250 ℃/h and the temperature rise rate is 30.8 ℃/h and the temperature rise rate is 1150, the temperature rise rate is 36.8 ℃/h and the holding time is 36.8 h and the temperature rise rate is 36 h and the holding time is 36 h at 850 ℃ and the temperature rise time is 36 h.
7. The method for preparing a special graphite heat exchanger material as claimed in claim 5, wherein the impregnant in the step (10) is medium temperature coal pitch.
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| CN111138207A (en) * | 2020-01-14 | 2020-05-12 | 大同新成新材料股份有限公司 | Preparation method of graphite thermal field material for Czochralski silicon furnace |
| CN111215633A (en) * | 2020-01-14 | 2020-06-02 | 大同新成新材料股份有限公司 | Method for preparing lithium ion negative electrode material by using tin graphene composite material |
| CN113185292A (en) * | 2021-04-27 | 2021-07-30 | 宜宾学院 | Production method of extrusion-molded copper graphite material |
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