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CN104339730A - Sandwich cured carbon felt - Google Patents

Sandwich cured carbon felt Download PDF

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Publication number
CN104339730A
CN104339730A CN201310329454.9A CN201310329454A CN104339730A CN 104339730 A CN104339730 A CN 104339730A CN 201310329454 A CN201310329454 A CN 201310329454A CN 104339730 A CN104339730 A CN 104339730A
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CN
China
Prior art keywords
carbon felt
sandwich
carbon
caking agent
solidification
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201310329454.9A
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Chinese (zh)
Inventor
柴昌盛
杨子元
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Gansu Haoshi Carbon Fiber Co Ltd
Original Assignee
Gansu Haoshi Carbon Fiber Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Gansu Haoshi Carbon Fiber Co Ltd filed Critical Gansu Haoshi Carbon Fiber Co Ltd
Priority to CN201310329454.9A priority Critical patent/CN104339730A/en
Publication of CN104339730A publication Critical patent/CN104339730A/en
Pending legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B32B9/007Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04Interconnection of layers
    • B32B7/12Interconnection of layers using interposed adhesives or interposed materials with bonding properties

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Ceramic Products (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention provides a sandwich cured carbon felt obtained by cross-bonding a layer of substrate carbon felt, a layer of a composite bonding agent, and another layer of substrate carbon felt. The composite bonding agent is a precursor. Through curing, carbonizing and high-temperature purification, a layer of compact heat-flow-resistant layer is obtained. Also, the heat-flow-resistant layer plays a role of bonding the substrate carbon felts on both sides into a whole. With the interaction of the substrate carbon felts and the composite bonding agent, a composite bonding strength is much higher than the peel strength of the carbon felt, such that the bonding strength of the heat-flow-resistant layer and the carbon felts is ensured, and a unified whole which is hard to separate or peel is formed. Also, the hardness and strength of the heat-flow-resistant layer is much better than those of traditional graphite paper. The sandwich cured carbon felt obtained with the preparation method has the capacity of blocking and resisting heat flows, and has supporting performance and overall strength better than those of traditional sandwich cured carbon felts and conventional cured carbon felts.

Description

Sandwich solidification carbon felt
Technical field
The invention belongs to a kind of heat-insulation and heat-preservation solidification carbon felt used in high temperature furnace.
Background technology
At present, solidification carbon felt has low volatility, low operation damage, good support performance compared with the soft felt of graphitization and installs changes the plurality of advantages such as convenient, high-temperature vacuum furnace or inert atmosphere high temperature furnace are widely used in, such as high-pressure gas quenching furnace, vacuum sintering furnace, pressure process sintering furnace, monocrystaline silicon stove, polycrystalline-silicon furnace, carborundum recrystallization stove etc.But in actual production, especially in the body of heater that high-temperature heat flux is more, hot-fluid becomes the main path of heat loss, amount of heat transmits from high-temperature region to low-temperature space (furnace wall) with hot-fluid, for this reason, the Structured cured carbon felt of a kind of sandwich has been invented by foreign study mechanism, namely between carbon felt and carbon felt, adds one deck graphite paper, wherein utilizes between carbon felt-graphite paper-carbon felt that high temperature adhesive is bonding to be formed.Because graphite paper surface porosity factor is very low, effectively prevent heat to collect together loss with hot-fluid, improve energy utilization rate, be thus widely used.
But in actual production and application process, this sandwich solidification carbon felt requires very high to the high temperature adhesive of need of production, mainly because the own inertia of graphite paper added is very strong, be difficult to formed between carbon felt effectively bonding; In addition, though carbon felt with between graphite paper bonding well, because graphite paper itself is a kind of soft graphite, for the bond strength of top layer and paper central layer is very low, be easy to peel off.Therefore, this sandwich structure solidification carbon felt is easy to damage at use procedure carbon felt or graphite paper and comes off, and has a strong impact on its choked flow heat-proof quality and service life.
In sum, break through the intrinsic bottleneck of sandwich solidification carbon felt, research and develop a kind of novel anti-current solidification carbon felt extremely urgent.
  
Summary of the invention
In view of above-mentioned, the object of the present invention is to provide a kind of sandwich to solidify carbon felt, to reduce or to reduce under hot environment heat with the loss of hot-fluid, and there will not be layering in use procedure, damage the generation of phenomenons such as coming off, and then economize energy and material cost.
For realizing above-mentioned object, the technical scheme that the present invention takes is:
A kind of sandwich solidification carbon felt intersects bonding forming by one deck matrix carbon felt, one deck composite caking agent, again one deck matrix carbon felt.
Above-mentioned composite caking agent is made up of 100 parts of diluents, the inorganic filler of 90-160 part, 2-15 part curing agent and 80-120 part resin.
Above-mentioned diluent is industrial alcohol or is methyl alcohol, or is acetone.
Above-mentioned inorganic filler is the combination of one or more in graphite, white carbon, carbon black, carborundum.
Above-mentioned curing agent is the combination of one or more in boric acid, hexa, p-methyl benzenesulfonic acid, T31, ethyl-sulfate, mahogany acid.
Above-mentioned resin is phenolic resins, or is epoxy resin.
The present invention compared with prior art, has following outstanding advantage and effect:
1. raw material of the present invention is easy to get, and selectable range is wide, and preparation technology is simple, with low cost.
2. the present invention abandons traditional sandwich solidification carbon felt using graphite ply of paper as thermal resistance fluid layer, then utilizes composite caking agent for presoma, through the thermal resistance fluid layer solidifying, carbonize, high temperature purification obtains one deck densification.Meanwhile, this thermal resistance fluid layer serves bonding effect again, by bonding for the matrix carbon felt on both sides one-tenth entirety.Because early stage is in the process of brushing composite caking agent, extend into the fiber in compound sticking oxidant layer, later stage has become the wild phase of thermal resistance fluid layer, and its bond strength is much larger than the peel strength of carbon felt itself, thus ensure that the bond strength of thermal resistance fluid layer and carbon felt, form unified entirety, be difficult to be separated or peel off come off.In addition, the hardness of this thermal resistance fluid layer, intensity are far superior to conventional graphite paper, the sandwich solidification carbon felt prepared so not only has the ability intercepting and resist hot-fluid, and its support performance, bulk strength are better than traditional sandwich solidification carbon felt and conventional solidified carbon felt.
3. the present invention does not restrict by the limitation of graphite paper own, conveniently can prepare various complex-shaped sandwich solidification carbon felt thermal field.
4. the sandwich that the present invention prepares solidifies carbon felt, and interfacial bonding strength is good, and installation, cleaning etc. artificially damage are little, and not easily fall slag or fall block, extend service life, have saved cost.
  
Accompanying drawing explanation
Fig. 1 is tubular sandwich solidification carbon felt prepared by the present invention.
Fig. 2 is sandwich solidification carbon felt sheet material prepared by the present invention.
Detailed description of the invention
Be described in any further technical scheme of the present invention below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
embodiment 1
The composite caking agent stated is made up of 100 parts of diluents, the inorganic filler of 90-160 part, 2-15 part curing agent and 80-120 part resin.
A kind of A type of I sandwich solidification carbon felt:
A. industrial alcohol thinned oil sulfonic acid is first used, wherein the weight ratio of industrial alcohol and mahogany acid is 100 parts: 2 parts, then stir 20 minutes, then under agitation 80 parts of phenolic resins are added gradually, finally 90 parts, carborundum is added in solution, continue stirring and namely obtain compound binding agent after 30 minutes.
B. on matrix carbon felt gluing of surfaces, evenly brushing a. step obtains composite caking agent, thickness 0.7mm, composite caking agent is pasted matrix carbon felt, then successively stacks compression, pressure 35MPa;
C. by the sample that pressurizes in b step together with mould or pressurized equipment, in atmospheric environment, be elevated to 120 DEG C from room temperature, be incubated after 1.5 hours, then be warming up to 180 DEG C of Post RDBMS and take out Temperature fall after 2.5 hours and obtain solidifying sample;
D. step c being solidified sample is placed with in the retort of argon shield, is warming up to 1000-1500 DEG C of charing lowers the temperature with stove after 2 hours with the heating rate of 40-60 DEG C/h;
E. the sample obtained in Step d is put into high temperature purification stove, 100 DEG C/h is warming up to 2000 DEG C, processes after 1 hour and lowers the temperature with stove, namely prepares sandwich solidification carbon felt sample.
A kind of Type B sandwich solidification of II carbon felt:
A. methanol dilution ethyl-sulfate is first used, wherein the weight ratio of methyl alcohol and ethyl-sulfate is 100 parts: 15 parts, then stirs 20 minutes, is then under agitation added gradually by 120 parts of epoxy resin, finally carbon black 160 parts is added in solution, continue stirring and namely obtain compound binding agent after 30 minutes.
B. on matrix carbon felt gluing of surfaces, evenly brushing a. step obtains composite caking agent, thickness 1.6mm, composite caking agent is pasted matrix carbon felt, then successively stacks compression, pressure 60MPa;
C. by the sample that pressurizes in b step together with mould or pressurized equipment, in atmospheric environment, be elevated to 120 DEG C from room temperature, be incubated after 2 hours, then be warming up to 180 DEG C of Post RDBMS and take out Temperature fall after 4 hours and obtain solidifying sample;
D. step c being solidified sample is placed with in the retort of argon shield, is warming up to 1000-1500 DEG C of charing lowers the temperature with stove after 3 hours with the heating rate of 40-60 DEG C/h;
E. the sample obtained in Step d is put into high temperature purification stove, 100 DEG C/h is warming up to 2500 DEG C of process and lowers the temperature with stove after 2 hours, namely prepares sandwich solidification carbon felt sample.
III common tubular sandwich solidification carbon felt:
A. cut that to prepare carbon felt needed for tubular heat resistanceheat resistant stream thermal field some;
B. composite caking agent is prepared: first dilute 12 parts of p-methyl benzenesulfonic acid with 100 parts of quality industrial alcohols, then stir 20 minutes, then under agitation 100 parts of phenolic resins are added gradually, finally add 90 parts of graphite, 16 parts of white carbons, continue stirring and namely obtain compound binding agent after 30 minutes;
C. one piece, the carbon felt cut is got, by the composite caking agent brushing for preparing at Carbon felt surface, a brushing one side, thickness is 1.6mm;
D. be wrapped on mould by carbon felt in step c, the one side scribbling bonding agent is close to die surface, is then sewed up by interface carbon rope; Then at carbon felt lateral surface (non-coated face) brushing industrial alcohol;
E. c and Step d is repeated, until reach the requirement of the thickness will preparing tubular carbon felt; Note, each mouth of sewing up will stagger; Brush 1mm thickness composite caking agent outside last one deck carbon felt, be then wound around one deck highland barley paper, step up with mould, shape;
F. by above-mentioned sample together with mould, in atmospheric environment, be elevated to 120 DEG C from room temperature, be incubated after 2 hours, then be warming up to 180 DEG C of Post RDBMS Temperature fall after 2 hours, the demoulding obtains solidifying sample;
G. above-mentioned solidification sample is placed with in the retort of argon shield, is warming up to 1000 DEG C of charings with the heating rate of 40 DEG C/h and lowers the temperature with stove after 2 hours;
H. the sample carbonized is put into high temperature purification stove, 100 DEG C/h is warming up to 2000 DEG C, processes and lowers the temperature with stove after 2 hours.
Namely tubular sandwich solidification carbon felt thermal field is prepared, as shown in Figure 1.Its bulk density is 0.17g/cm 3, disbonded test result as shown in Figure 2, is all that matrix carbon felt is damaged, shows that bonding force is greater than carbon felt peel strength 0.12-0.16N/mm 2; Tradition tubular sandwich structure solidification carbon felt thermal field bulk density is 0.28g/cm 3, peel strength is less than carbon felt matrix stripping intensity.
embodiment 2
The preparation of super large (diameter is greater than 1.2m) ultra-thin (thickness is less than 0.04m) tubular sandwich solidification carbon felt thermal field:
A. cut that to prepare carbon felt needed for tubular heat resistanceheat resistant stream thermal field some;
B. composite caking agent is prepared: first dilute 12 parts of p-methyl benzenesulfonic acid with 100 parts of quality industrial alcohols, then stir 20 minutes, then under agitation 90 parts of phenolic resins are added gradually, finally add 60 parts of graphite, 30 parts of white carbons, 20 parts of carborundum, continue stirring and namely obtain compound binding agent after 30 minutes;
C. one piece, the carbon felt cut is got, by the composite caking agent brushing for preparing at Carbon felt surface, a brushing one side, thickness is about 1.2mm;
D. be wrapped on mould by carbon felt in step c, the one side scribbling bonding agent is close to die surface, is then sewed up by interface carbon rope; Then at carbon felt lateral surface brushing one deck composite caking agent again, thickness is about 1mm;
E. c and Step d is repeated, until reach the requirement will preparing tubular carbon felt thickness; Note, each mouth of sewing up will stagger; Brush about 1mm thickness composite caking agent outside last one deck carbon felt, be then wound around one deck highland barley paper, step up with mould, shape;
F. sample step e obtained, together with mould, in atmospheric environment, is elevated to 120 DEG C from room temperature, is incubated after 1 hour, then be warming up to 180 DEG C of Post RDBMS Temperature fall after 1 hour, the demoulding obtains solidifying sample;
G. f step solidification sample is placed with in the retort of argon shield, is warming up to 1000 DEG C of charings with the heating rate of 60 DEG C/h and lowers the temperature with stove after 2 hours;
H. the sample that g step carbonizes is put into high temperature purification stove, 100 DEG C/h is warming up to 2500 DEG C, processes and lowers the temperature with stove after 1 hour.
Namely prepare super large ultra-thin tubular sandwich solidification carbon felt thermal field, its bulk density is 0.2g/cm 3.
embodiment 3
The preparation of plates of sandwich solidification carbon felt:
A. cut that to prepare carbon felt needed for tubular heat resistanceheat resistant stream thermal field some;
B. composite caking agent is prepared: first dilute 12 parts of boric acid, 15 parts of T31 with 100 parts of quality industrial alcohols, then stir 20 minutes, then under agitation 90 parts of epoxy resin are added gradually, finally add 90 parts of carbon blacks, 20 parts of white carbons, continue stirring and namely obtain compound binding agent after 30 minutes;
C. one piece, the carbon felt cut is got, by the composite caking agent brushing for preparing at Carbon felt surface, two-sided brushing, thickness is about 1mm;
D. carbon felt in step c is successively stacked, compacting-shaping;
The sample of e. Step d being shaped, together with mould, in atmospheric environment, is elevated to 120 DEG C from room temperature, be incubated after 2 hours, then be warming up to 180 DEG C of Post RDBMS Temperature fall after 3 hours, the demoulding obtains solidification sample;
F. step e being solidified sample is placed with in the retort of argon shield, is warming up to 1000 DEG C of charings lowers the temperature with stove after 3 hours with the heating rate of 60 DEG C/h;
G. the sample that f step carbonizes is put into high temperature purification stove, 100 DEG C/h is warming up to 2000 DEG C or higher temperature, processes and lowers the temperature with stove after 1 hour.
Namely prepare sandwich solidification carbon felt sheet material, its bulk density is 0.16g/cm 3, disbonded test result as shown in Figure 2, is all that matrix carbon felt is damaged, shows that bonding force is greater than carbon felt peel strength 0.12-0.16N/mm 2; Tradition sandwich structure solidification carbon felt sheet material bulk density is 0.26-0.29g/cm 3, peel strength is less than carbon felt matrix stripping intensity.

Claims (7)

1. a sandwich solidification carbon felt, is characterized in that intersecting bonding forming by one deck matrix carbon felt, one deck composite caking agent, again one deck matrix carbon felt.
2. a kind of sandwich solidification carbon felt according to claim 1, is characterized in that above-mentioned matrix carbon felt is one or more combination in PAN based carbon felt, pitch base carbon felt, viscose glue base carbon felt.
3. a kind of sandwich solidifies carbon felt according to claim 1, it is characterized in that above-mentioned composite caking agent is made up of diluent, inorganic filler, curing agent and resin, its weight ratio is diluent 100 parts, inorganic filler 90-160 part, curing agent 2-15 part, resin 80-120 part.
4. a kind of sandwich solidification carbon felt according to claim 1, is characterized in that the diluent of above-mentioned composite caking agent is industrial alcohol or for methyl alcohol or be acetone.
5. a kind of sandwich solidifies carbon felt according to claim 1, it is characterized in that the inorganic filler of above-mentioned composite caking agent is the combination of one or more in graphite, white carbon, carbon black, carborundum.
6. a kind of sandwich solidifies carbon felt according to claim 1, it is characterized in that the curing agent of above-mentioned composite caking agent is the combination of one or more in boric acid, hexa, p-methyl benzenesulfonic acid, T31, ethyl-sulfate, mahogany acid.
7. a kind of sandwich solidifies carbon felt according to claim 1, it is characterized in that the resin of above-mentioned composite caking agent is the combination of one or more in phenol furane resins, urea formaldehyde, epoxy resin.
CN201310329454.9A 2013-08-01 2013-08-01 Sandwich cured carbon felt Pending CN104339730A (en)

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Application Number Priority Date Filing Date Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108625185A (en) * 2018-07-18 2018-10-09 宁晋晶兴电子材料有限公司 Energy-efficient solidification carbon felt of one kind and preparation method thereof
CN110258131A (en) * 2019-07-05 2019-09-20 聊城大学 A kind of solidification carbon felt protective coating
CN111996813A (en) * 2020-08-27 2020-11-27 佛山市石金科技有限公司 Coating of hard felt and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090042009A1 (en) * 2005-04-22 2009-02-12 Kureha Corporation Adhesive for thermal insulator and carbonized-laminated body for thermal insulator using the same
CN101949481A (en) * 2010-09-17 2011-01-19 西安超码科技有限公司 Method for preparing wound heat-insulating drum
CN102575400A (en) * 2009-10-06 2012-07-11 西格里碳素欧洲公司 Composite material comprising soft carbon fiber felt and hard carbon fiber felt
CN102712168A (en) * 2010-01-22 2012-10-03 株式会社吴羽 Carbon fiber laminated molded product, and method for producing same
CN102977824A (en) * 2011-09-06 2013-03-20 甘肃郝氏炭纤维有限公司 High temperature binder used for binding carbon material, and preparation method and application method thereof
CN103193495A (en) * 2013-03-01 2013-07-10 辽阳金谷碳纤维科技有限公司 Production method of insulation materials used for crystal pulling furnace

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090042009A1 (en) * 2005-04-22 2009-02-12 Kureha Corporation Adhesive for thermal insulator and carbonized-laminated body for thermal insulator using the same
CN102575400A (en) * 2009-10-06 2012-07-11 西格里碳素欧洲公司 Composite material comprising soft carbon fiber felt and hard carbon fiber felt
CN102712168A (en) * 2010-01-22 2012-10-03 株式会社吴羽 Carbon fiber laminated molded product, and method for producing same
CN101949481A (en) * 2010-09-17 2011-01-19 西安超码科技有限公司 Method for preparing wound heat-insulating drum
CN102977824A (en) * 2011-09-06 2013-03-20 甘肃郝氏炭纤维有限公司 High temperature binder used for binding carbon material, and preparation method and application method thereof
CN103193495A (en) * 2013-03-01 2013-07-10 辽阳金谷碳纤维科技有限公司 Production method of insulation materials used for crystal pulling furnace

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108625185A (en) * 2018-07-18 2018-10-09 宁晋晶兴电子材料有限公司 Energy-efficient solidification carbon felt of one kind and preparation method thereof
CN110258131A (en) * 2019-07-05 2019-09-20 聊城大学 A kind of solidification carbon felt protective coating
CN111996813A (en) * 2020-08-27 2020-11-27 佛山市石金科技有限公司 Coating of hard felt and preparation method thereof

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Application publication date: 20150211