CN104058776A - Preparation method of hard carbon fiber heat preservation material prepared from carbon fiber balls - Google Patents
Preparation method of hard carbon fiber heat preservation material prepared from carbon fiber balls Download PDFInfo
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- CN104058776A CN104058776A CN201410324442.1A CN201410324442A CN104058776A CN 104058776 A CN104058776 A CN 104058776A CN 201410324442 A CN201410324442 A CN 201410324442A CN 104058776 A CN104058776 A CN 104058776A
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Abstract
The invention discloses a preparation method of a hard carbon fiber heat preservation material prepared from carbon fiber balls, and belongs to the technical field of hard carbon fiber heat preservation materials. The hard carbon fiber heat preservation material is prepared by virtue of fiber crushing and mixing, rolling and pelletizing, mold pressing and forming, drying and curing, adhesive layer reinforcement, carbonization treatment, cutting and polishing, surface treatment and high-temperature graphitization. Compared with the prior art, the preparation method disclosed by the invention has the advantages that the preparation method is simple in process, low in cost of prepared felt, good in heat preservation effect and uniform in fiber distribution of the felt, does not have the phenomenon of non-uniform felt fiber distribution caused by fiber agglomerates generated in the forming process using short cutting shreds, and can be used for well using waste materials of carbon fibers and the felt.
Description
Technical field
The invention belongs to a kind of hard carbon fiber heat preservation material technical field, be specifically related to a kind of preparation method of the hard carbon fiber heat preservation material of being made by charcoal fibrous nodules.
Be applied to the high temperature furnace apparatus such as sintering cemented carbide stove, monocrystaline silicon stove, vacuum smelting furnace, vacuum heat treatment furnace, gaseous phase deposition stove.
Background technology
The hard heat-insulated felt of charcoal fiber is a kind of carbon/carbon composite made from special process, density is low, carbon content is high, heat insulation effect is good etc. has active effect to energy-saving and emission-reduction, can under vacuum or inert atmosphere, use temperature reach 2000 DEG C of left and right, be widely used in the aspects such as aviation and wide surface is heat insulation, metallurgical, high-temperature gas.Along with the progress of China's science and technology, its range of application constantly expands, also more and more higher to performance requriements, and demand is also increasing.
The common charcoal felt that the present hard heat-insulated felt of charcoal fiber mainly adopts is prepared hard carbon felt by binding agent layering bonding, the such method of cure process, complex process, production efficiency is low, and heat-insulating property is poor, in bonding binding agent use more, cause density higher.The shortcomings such as under hot environment, binding agent easily lost efficacy, easy layering.In addition, exactly soft felt is flooded with solidifying agent, the hard carbon felt intensity of solidify, compression molding is such is lower, removes and installs inconvenience, easily cracking, and work-ing life is shorter.
Patent CN101628816A discloses a kind of method of preparing hard carbon fiber charcoal felt.Be exactly specifically that short chopping fully mixes with binding agent, dispersion agent, then cast, compression molding, then through not melting and charing processing.When in this moulding process, staple length is very little, the density of the felt of preparation is very high, when staple length is larger, and fiber dispersion difficulty, fiber is easily embraced and is clumped together, and causes the Fiber Distribution of felt inhomogeneous, even has part cavity.
Summary of the invention
Object of the present invention is to solve the complex process existing in above-mentioned prior art, production efficiency is low, and heat-insulating property is poor, in bonding, binding agent uses more, cause density higher, under hot environment, binding agent easily lost efficacy, the easily shortcoming such as layering, provides a kind of preparation method of the hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for the hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules, comprises the steps:
1), fiber is broken mixes: get the short carbon fiber that 70～80 parts of length are 3～10mm, 3～15 parts of toners, 10～30 parts of organic fibres that length is 3～5mm, broken and mix, make the compound that staple length is 1～3mm;
2), round as a ball granulation: in step 1) add after the balling-up liquid-containing binder that 10～20 parts of concentration are 5～30% in the broken compound that makes, carry out round as a ball coated balling-up with granulating disc, and sieve, making diameter is 0.5～10mm, the charcoal fibrous nodules that density is 0.06～0.20g/cm3;
3), compression molding: by step 2) the charcoal fibrous nodules making is placed in the mould of moulding stamper, makes fibrous nodules post-heating to 80～200 DEG C that are evenly distributed in mould, compression molding under the pressure of 0.01～0.1MPa, makes lagging material precast body;
4), baking and curing: the lagging material precast body making is put into baking and curing equipment, dry also settable cementitious at 130 DEG C～180 DEG C;
5), reinforce paste layer: by adhesive preparation, be attached to step 4 with the charcoal fiber composite resin board of carbon fiber sheet, charcoal fibrefelt or 0.1～1mm) make solidify after precast body surface, make charcoal fiber shaped body;
6), charing processing: by step 5) to carry out carbonization temperature be 650 DEG C～900 DEG C again for the charcoal fiber shaped body that makes, the charing processing that carbonization time is 30min～120min;
7), cutting polishing: according to desired size, to step 6) charing formed body after treatment cuts grinding process;
8), surface treatment: flexible graphite paper is attached to the charing formed body surface after grinding process by attach adhesive, or adopts vapour deposition at 5～50 microns of carborundums of charing formed body surface deposition;
9), high temperature graphitization: carry out high temperature graphitization processing to completing surface-treated charing formed body, treatment temp is 1800 DEG C～2500 DEG C, and treatment time 30min～120min, makes graphite formed body, makes hard carbon fiber heat preservation material.
Described organic fibre is polyvinyl alcohol fiber or viscose fiber.
Described toner is one or more mixing of resol powder, epoxy powder, urea-formaldehyde resin powder, asphalt powder.
Described balling-up liquid-containing binder is one or more mixed solution of resol emulsion or solution, furfuryl resin emulsion or solution, epoxy resin latex or solution, polyvinyl alcohol water solution, polyacrylamide solution.
Described adhesive preparation is that softening temperature is 150～300 DEG C of pitches, granularity 50～200 object carbon dusts or carborundum powder, length-to-diameter ratio 5/1～130/1 charcoal fiber, thermosetting resin.
Described thermosetting resin is one or more in resol, furfuryl resin, epoxy resin.
Described charcoal fiber is pitch-based carbon fiber, rayon-based carbon fiber, PAN-based carbon fiber, polyimide based carbon fiber, polyvinyl alcohol based carbon fiber or xylogen based carbon fiber.
Compared with prior art, it is simple that the present invention has technique, and production efficiency is high, and cost is low, high insulating effect, and the Fiber Distribution of felt is even, can be good at utilizing the waste material of charcoal fiber and felt.In bonding, binding agent uses and also can not cause the phenomenon that density is higher more in the situation that.Secondly,, even under hot environment, binding agent is also not easy inefficacy and layering, removes and installs conveniently, not easy to crack, the advantages such as long service life.
Embodiment
Embodiment 1
The present embodiment, a kind of preparation method of the hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules, comprises the steps:
1), fiber is broken mixes: short pitch-based carbon fiber, 3 parts of resol powder, the 10 parts of polyvinyl alcohol fibers that length is 3mm cut that to get 70 parts of length be 3mm, broken and mix, make the compound that staple length is 1mm;
2), round as a ball granulation: in step 1) add after the resol emulsion or solution that 10 parts of concentration are 5% in the broken compound that makes, carry out round as a ball coated balling-up with granulating disc, and sieve, making diameter is 0.5mm, the charcoal fibrous nodules that density is 0.06g/cm3;
3), compression molding: by step 2) the charcoal fibrous nodules making is placed in the mould of moulding stamper, makes the fibrous nodules post-heating to 80 DEG C that is evenly distributed in mould, compression molding under the pressure of 0.01MPa, makes lagging material precast body;
4), baking and curing: the lagging material precast body making is put into baking and curing equipment, dry also settable cementitious at 130 DEG C;
5), reinforce paste layer: be attached to step 4 with the pitch-based carbon fiber that the charcoal fiber composite resin board of carbon fiber sheet, charcoal fibrefelt or 0.1～1mm is 150 DEG C of pitches, granularity 50 object carborundum powders, length-to-diameter ratio 5/1 by softening temperature) make curing after precast body surface, make charcoal fiber shaped body;
6), charing processing: by step 5) the charcoal fiber shaped body that makes carries out charing processing again, carbonization temperature is 650 DEG C, carbonization time is 30min;
7), cutting polishing: according to desired size, to step 6) charing formed body after treatment cuts grinding process;
8), surface treatment: flexible graphite paper is attached to the charing formed body surface after grinding process by attach adhesive, or adopts vapour deposition at 5 microns of carborundums of charing formed body surface deposition;
9), high temperature graphitization: carry out high temperature graphitization processing to completing surface-treated charing formed body, treatment temp is 1800 DEG C, and treatment time 30min makes graphite formed body, makes hard carbon fiber heat preservation material.
Embodiment 2
The present embodiment, a kind of preparation method of the hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules, comprises the steps:
1), fiber is broken mixes: short rayon-based carbon fiber, 15 parts of epoxy powders, 30 parts of polyvinyl alcohol fiber or the viscose fibers that length is 5mm cut that to get 80 parts of length be 10mm, broken and mix, make the compound that staple length is 3mm;
2), round as a ball granulation: in step 1) add after the furfuryl resin emulsion or solution that 20 parts of concentration are 30% in the broken compound that makes, carry out round as a ball coated balling-up with granulating disc, and sieve, making diameter is 10mm, the charcoal fibrous nodules that density is 0.20g/cm3;
3), compression molding: by step 2) the charcoal fibrous nodules making is placed in the mould of moulding stamper, makes the fibrous nodules post-heating to 200 DEG C that is evenly distributed in mould, compression molding under the pressure of 0.1MPa, makes lagging material precast body;
4), baking and curing: the lagging material precast body making is put into baking and curing equipment, dry also settable cementitious at 180 DEG C;
5), reinforce paste layer: with the charcoal fiber composite resin board of carbon fiber sheet, charcoal fibrefelt or 1mm be the resol of 300 DEG C of pitches, granularity 200 object carborundum powders, length-to-diameter ratio 130/1 by softening temperature, be attached to step 4) make solidify after precast body surface, make charcoal fiber shaped body;
6), charing processing: by step 5) the charcoal fiber shaped body that makes carries out charing processing again, carbonization temperature is 900 DEG C, carbonization time is 120mi;
7), cutting polishing: according to desired size, to step 6) charing formed body after treatment cuts grinding process;
8), surface treatment: flexible graphite paper is attached to the charing formed body surface after grinding process by attach adhesive, or adopts vapour deposition at 50 microns of carborundums of charing formed body surface deposition;
9), high temperature graphitization: carry out high temperature graphitization processing to completing surface-treated charing formed body, treatment temp is 2500 DEG C, and treatment time 120min makes graphite formed body, makes hard carbon fiber heat preservation material.
Embodiment 3
The present embodiment, a kind of preparation method of the hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules, comprises the steps:
1), fiber is broken mixes: to get 75 parts of length be 7mm short PAN-based carbon fiber, 10 parts of resol powder, epoxy powder, urea-formaldehyde resin powder, the mixing of asphalt powder, 20 parts of polyvinyl alcohol fibers that length is 4mm cut, broken also mixing, makes the compound that staple length is 2mm;
2), round as a ball granulation: in step 1) add in the broken compound that makes after the mixed solution of resol emulsion that 15 parts of concentration are 20% or solution, furfuryl resin emulsion or solution, epoxy resin latex or solution, polyvinyl alcohol water solution, polyacrylamide solution, carry out round as a ball coated balling-up with granulating disc, and sieve, making diameter is 6mm, the charcoal fibrous nodules that density is 0.10g/cm3;
3), compression molding: by step 2) the charcoal fibrous nodules making is placed in the mould of moulding stamper, makes the fibrous nodules post-heating to 150 DEG C that is evenly distributed in mould, compression molding under the pressure of 0.06MPa, makes lagging material precast body;
4), baking and curing: the lagging material precast body making is put into baking and curing equipment, dry also settable cementitious at 160 DEG C;
5), reinforce paste layer: with the charcoal fiber composite resin board of carbon fiber sheet, charcoal fibrefelt or 0.1～1mm be 250 DEG C of pitches, granularity 150 object carbon dusts, the resol of length-to-diameter ratio 75/1, furfuryl resin, epoxy resin by softening temperature, be attached to step 4) make solidify after precast body surface, make charcoal fiber shaped body;
6), charing processing: by step 5) the charcoal fiber shaped body that makes carries out charing processing again, carbonization temperature is 800 DEG C, carbonization time is 80min;
7), cutting polishing: according to desired size, to step 6) charing formed body after treatment cuts grinding process;
8), surface treatment: flexible graphite paper is attached to the charing formed body surface after grinding process by attach adhesive, or adopts vapour deposition at 30 microns of carborundums of charing formed body surface deposition;
9), high temperature graphitization: carry out high temperature graphitization processing to completing surface-treated charing formed body, treatment temp is 2000 DEG C, and treatment time 80min makes graphite formed body, makes hard carbon fiber heat preservation material.
Charcoal fiber in above-described embodiment can also be polyimide based carbon fiber, polyvinyl alcohol based carbon fiber or xylogen based carbon fiber.Toner can also be urea-formaldehyde resin powder or asphalt powder.Balling-up liquid-containing binder can also be epoxy resin latex or solution, polyvinyl alcohol water solution, polyacrylamide solution.Thermosetting resin can also be epoxy resin.
Claims (7)
1. a preparation method for the hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules, is characterized in that: comprise the steps:
1), fiber is broken mixes: get the short carbon fiber that 70～80 parts of length are 3～10mm, 3～15 parts of toners, 10～30 parts of organic fibres that length is 3～5mm, broken and mix, make the compound that staple length is 1～3mm;
2), round as a ball granulation: in step 1) add after the balling-up liquid-containing binder that 10～20 parts of concentration are 5～30% in the broken compound that makes; carry out round as a ball coated balling-up with granulating disc; and sieve, making diameter is 0.5～10mm, density is 0.06～0.20g/cm
3charcoal fibrous nodules;
3), compression molding: by step 2) the charcoal fibrous nodules making is placed in the mould of moulding stamper, makes fibrous nodules post-heating to 80～200 DEG C that are evenly distributed in mould, compression molding under the pressure of 0.01～0.1MPa, makes lagging material precast body;
4), baking and curing: the lagging material precast body making is put into baking and curing equipment, dry also settable cementitious at 130 DEG C～180 DEG C;
5), reinforce paste layer: by adhesive preparation, be attached to step 4 with the charcoal fiber composite resin board of carbon fiber sheet, charcoal fibrefelt or 0.1～1mm) make solidify after precast body surface, make charcoal fiber shaped body;
6), charing processing: by step 5) to carry out carbonization temperature be 650 DEG C～900 DEG C again for the charcoal fiber shaped body that makes, the charing processing that carbonization time is 30min～120min;
7), cutting polishing: according to desired size, to step 6) charing formed body after treatment cuts grinding process;
8), surface treatment: flexible graphite paper is attached to the charing formed body surface after grinding process by attach adhesive, or adopts vapour deposition at 5～50 microns of carborundums of charing formed body surface deposition;
9), high temperature graphitization: carry out high temperature graphitization processing to completing surface-treated charing formed body, treatment temp is 1800 DEG C～2500 DEG C, and treatment time 30min～120min, makes graphite formed body, makes hard carbon fiber heat preservation material.
2. the preparation method of a kind of hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules according to claim 1, is characterized in that: described organic fibre is polyvinyl alcohol fiber or viscose fiber.
3. the preparation method of a kind of hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules according to claim 1, is characterized in that: described toner is one or more mixing of resol powder, epoxy powder, urea-formaldehyde resin powder, asphalt powder.
4. the preparation method of a kind of hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules according to claim 1, is characterized in that: described balling-up liquid-containing binder is one or more mixed solution of resol emulsion or solution, furfuryl resin emulsion or solution, epoxy resin latex or solution, polyvinyl alcohol water solution, polyacrylamide solution.
5. the preparation method of a kind of hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules according to claim 1, is characterized in that: described adhesive preparation is that softening temperature is 150～300 DEG C of pitches, granularity 50～200 object carbon dusts or carborundum powder, length-to-diameter ratio 5/1～130/1 charcoal fiber, thermosetting resin.
6. the preparation method of a kind of hard carbon fiber heat preservation material of being made up of charcoal fibrous nodules according to claim 5, is characterized in that: described thermosetting resin is one or more in resol, furfuryl resin, epoxy resin.
7. according to the preparation method of a kind of hard carbon fiber heat preservation material of being made by charcoal fibrous nodules described in claim 1 and 5, it is characterized in that: described charcoal fiber is pitch-based carbon fiber, rayon-based carbon fiber, PAN-based carbon fiber, polyimide based carbon fiber, polyvinyl alcohol based carbon fiber or xylogen based carbon fiber.
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Cited By (7)
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| CN104891950A (en) * | 2015-05-12 | 2015-09-09 | 湖南搏盛天弘新材料技术有限公司 | Hard carbon fiber heat insulation board and preparation method thereof |
| CN105946251A (en) * | 2016-05-06 | 2016-09-21 | 天津鑫诺通树脂制品技术开发有限公司 | Drainage ditch production process |
| CN106336236A (en) * | 2016-08-30 | 2017-01-18 | 湖南南方搏云新材料股份有限公司 | Preparation method for thermal insulation material wet-molded from short-cut carbon fiber |
| CN106987926A (en) * | 2017-04-14 | 2017-07-28 | 河北民族师范学院 | Pitch based carbon fiber, preparation method and its application in lithium ion battery |
| CN107963896A (en) * | 2017-11-27 | 2018-04-27 | 江西德义半导体科技有限公司 | A kind of semiconductor crystal stove insulating layer reparation high temperature resistant cement |
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| CN113547799A (en) * | 2021-08-12 | 2021-10-26 | 因达孚先进材料(苏州)有限公司 | Method for preparing soft carbon fiber heat-preservation felt by adopting batch-type industrial furnace |
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| CN109095946A (en) * | 2018-08-29 | 2018-12-28 | 佛山朝鸿新材料科技有限公司 | A kind of light-weight insulating brick |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103787686A (en) * | 2014-01-26 | 2014-05-14 | 四川创越炭材料有限公司 | Carbon fiber composite ball and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103787686A (en) * | 2014-01-26 | 2014-05-14 | 四川创越炭材料有限公司 | Carbon fiber composite ball and preparation method thereof |
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| CN104891950A (en) * | 2015-05-12 | 2015-09-09 | 湖南搏盛天弘新材料技术有限公司 | Hard carbon fiber heat insulation board and preparation method thereof |
| CN105946251A (en) * | 2016-05-06 | 2016-09-21 | 天津鑫诺通树脂制品技术开发有限公司 | Drainage ditch production process |
| CN105946251B (en) * | 2016-05-06 | 2018-02-06 | 天津鑫诺通树脂制品技术开发有限公司 | A kind of gutter production technology |
| CN106336236A (en) * | 2016-08-30 | 2017-01-18 | 湖南南方搏云新材料股份有限公司 | Preparation method for thermal insulation material wet-molded from short-cut carbon fiber |
| CN106987926A (en) * | 2017-04-14 | 2017-07-28 | 河北民族师范学院 | Pitch based carbon fiber, preparation method and its application in lithium ion battery |
| CN107963896A (en) * | 2017-11-27 | 2018-04-27 | 江西德义半导体科技有限公司 | A kind of semiconductor crystal stove insulating layer reparation high temperature resistant cement |
| CN112321202A (en) * | 2020-11-03 | 2021-02-05 | 中创科技孵化器泰州有限公司 | Preparation method of novel heat insulation material |
| CN113547799A (en) * | 2021-08-12 | 2021-10-26 | 因达孚先进材料(苏州)有限公司 | Method for preparing soft carbon fiber heat-preservation felt by adopting batch-type industrial furnace |
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Denomination of invention: Preparation method of hard carbon fiber heat preservation material prepared from carbon fiber balls Effective date of registration: 20161104 Granted publication date: 20151118 Pledgee: Ma Jiaolu Pledgor: Sichuan Chuangyue Carbon Material Co., Ltd. Registration number: 2016510000060 |
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