CN116497525A - Preparation method of heat insulation felt - Google Patents
Preparation method of heat insulation felt Download PDFInfo
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- CN116497525A CN116497525A CN202310468929.6A CN202310468929A CN116497525A CN 116497525 A CN116497525 A CN 116497525A CN 202310468929 A CN202310468929 A CN 202310468929A CN 116497525 A CN116497525 A CN 116497525A
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- Prior art keywords
- chopped fiber
- heat insulation
- preparing
- felt
- insulation felt
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- 238000009413 insulation Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000835 fiber Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000000853 adhesive Substances 0.000 claims abstract description 7
- 230000001070 adhesive effect Effects 0.000 claims abstract description 7
- 238000010000 carbonizing Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 11
- 150000001408 amides Chemical class 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000007385 chemical modification Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000003763 carbonization Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- FVJIUQSKXOYFKG-UHFFFAOYSA-N (3,4-dichlorophenyl)methanol Chemical compound OCC1=CC=C(Cl)C(Cl)=C1 FVJIUQSKXOYFKG-UHFFFAOYSA-N 0.000 claims description 5
- TZOYLCXIRKLUQO-UHFFFAOYSA-N 1-(3,5-dichlorophenyl)-5-propylpyrazole-4-carbonyl chloride Chemical compound CCCC1=C(C(Cl)=O)C=NN1C1=CC(Cl)=CC(Cl)=C1 TZOYLCXIRKLUQO-UHFFFAOYSA-N 0.000 claims description 5
- NRHVNPYOTNGECT-UHFFFAOYSA-N 2-(3-chlorophenyl)ethanamine Chemical compound NCCC1=CC=CC(Cl)=C1 NRHVNPYOTNGECT-UHFFFAOYSA-N 0.000 claims description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 238000004440 column chromatography Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012044 organic layer Substances 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 229920002635 polyurethane Polymers 0.000 abstract 1
- 239000004814 polyurethane Substances 0.000 abstract 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229910001510 metal chloride Inorganic materials 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
- D04H1/587—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives characterised by the bonding agents used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4209—Inorganic fibres
- D04H1/4242—Carbon fibres
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/04—Carbonising or oxidising
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/63—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with hydroxylamine or hydrazine
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
- D06M13/148—Polyalcohols, e.g. glycerol or glucose
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/415—Amides of aromatic carboxylic acids; Acylated aromatic amines
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Emergency Medicine (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Polyurethanes Or Polyureas (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention relates to the technical field of chemical industry, in particular to a method for preparing a high-performance polyurethane foamThe preparation method of the heat insulation felt comprises the following steps: s1, crushing and processing the leftover materials of the heat-insulating felt into chopped fiber yarns; s2, chemically modifying the chopped fiber to obtain modified chopped fiber; s3, fully mixing the modified chopped fiber with an adhesive, and heating and pressurizing to form a felt; and S4, carbonizing and graphitizing the felt to obtain the heat-insulating felt. Compared with the prior art, the invention has the beneficial effects that: the heat insulation felt prepared by the invention has excellent performance, the heat conductivity coefficient is only 0.051W/m.K, the tensile strength is up to 0.26Mpa, and the thermal expansion coefficient is only 1.05 x 10 ‑6 And/k, the metal element content is only 19.7ppm.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a preparation method of a heat insulation felt.
Background
The heat preservation furnace comprises a degreasing furnace, a high-temperature carbonization furnace, a low-temperature carbonization furnace, a CVD furnace, a CVI furnace and the like, is widely applied to the fields of chemical industry, energy, aerospace and the like, and the heat insulation layer plays a vital role for the heat preservation furnace. Therefore, the heat insulation felt with excellent high-temperature heat insulation effect can effectively reduce the diffusion of heat in the furnace, reduce the loss of heat, save energy, improve the mechanical strength of the heat insulation felt and prolong the service life of the heat insulation felt.
At present, various heat preservation furnaces in China still adopt traditional felt heat insulation materials, and the traditional felt heat insulation materials have the defects of low strength, poor heat insulation performance, more metal impurities, short service life and the like.
Disclosure of Invention
In order to solve the problems mentioned in the background art, the invention provides a preparation method of a heat insulation felt, which comprises the following steps:
s1, crushing and processing the leftover materials of the heat-insulating felt into chopped fiber yarns;
s2, chemically modifying the chopped fiber to obtain modified chopped fiber;
s3, fully mixing the modified chopped fiber with an adhesive, and heating and pressurizing to form a felt;
and S4, carbonizing and graphitizing the felt to obtain the heat-insulating felt.
Preferably, in the step S1, the average length of the chopped fiber filaments is 1-3cm, and the chopped fiber filaments are polyacrylonitrile-based carbon fibers.
Preferably, in the step S2, the specific method of chemical modification is as follows:
dissolving 1- (3, 5-dichlorophenyl) -5-propyl-1H-pyrazole-4-carbonyl chloride in dimethylbenzene, adding 2- (3-chlorophenyl) ethylamine, heating to 80-90 ℃ and stirring for reaction for 0.5-1.5H, distilling under reduced pressure to remove dimethylbenzene, adding saturated sodium bicarbonate solution and stirring for reaction for 1-3H, extracting with ethyl acetate, combining organic layers, drying with anhydrous magnesium sulfate, concentrating, and performing column chromatography to obtain an amide derivative;
mixing 30-40 parts by weight of chopped fiber, 10-20 parts by weight of amide derivative, 10-20 parts by weight of hydroxylamine hydrochloride and 100-120 parts by weight of ethylene glycol uniformly, stirring and reacting for 1-2 hours at 50-60 ℃, taking out the chopped fiber, and drying to obtain the modified chopped fiber.
Preferably, the molar ratio of the 1- (3, 5-dichlorophenyl) -5-propyl-1H-pyrazole-4-carbonyl chloride to the 2- (3-chlorophenyl) ethylamine is 1:1.
Preferably, in the step S3, the binder is a modified phenolic resin and ethanol mixed according to a mass ratio of 1 (3-5), wherein the preparation method of the modified phenolic resin comprises the following steps: adding 3, 4-dichlorobenzyl alcohol after phenol is melted, regulating the pH to 9 by a sodium hydroxide solution, stirring at 40-50 ℃ for 30-40min, adding formaldehyde for 2 times, adding 70-80% of formaldehyde at the first time, stirring at 60 ℃ for reaction for 30-40min, adding the rest formaldehyde at the second time, stirring at 95 ℃ for reaction for 0.5-1h, cooling to 20-30 ℃, regulating the pH to 7 by hydrochloric acid, and concentrating to obtain the modified phenolic resin.
Preferably, the molar ratio of the phenol, formaldehyde and 3, 4-dichlorobenzyl alcohol is 1:1: (0.1-0.2).
Preferably, the mass ratio of the chopped fiber to the binder is 1: (0.1-0.2).
Preferably, in the step S3, the conditions of heating and pressurizing are as follows: treating at 150-170deg.C and 20-25MPa for 10-20min.
Preferably, in the step S4, the carbonization conditions are as follows: under the protection of nitrogen, the nitrogen passes through 4 different temperature areas in sequence, wherein the first temperature area is 400 ℃, the second temperature area is 500min and 20min, the third temperature area is 800 ℃, the first temperature area is 1h, and the fourth temperature area is 900 ℃ and the second temperature area is 1h.
Preferably, in the step S4, the graphitizing conditions are as follows: and under the protection of nitrogen, treating at 2000-2200 ℃ for 0.5-1h.
Compared with the prior art, the invention has the beneficial effects that:
1. the chopped fiber is subjected to chemical modification, fully mixed with an adhesive, and modified by amide derivatives and hydroxylamine hydrochloride, so that gaps on the surface and the inside of the chopped fiber contain a large number of active atoms, such as N, O, which can be better combined and cured with modified phenolic resin, the interlayer shear strength and friction performance of a blank are improved, and the felt is subjected to carbonization treatment and graphitization treatment, so that the heat insulation felt has a lower heat conductivity coefficient, a thermal expansion coefficient and a higher tensile strength.
2. Amide derivatives, hydroxylamine hydrochloride and modified phenolic resin dispersed in gaps on the surface and in the interior of the felt all contain chlorine elements, active chlorine can be formed when carbonization is carried out at a high temperature above 2000 ℃, the active chlorine can be diffused along voids and defects on the surface of the fiber and react with metal elements stored in the fiber to form metal chlorides, sublimation points of the metal chlorides are relatively low, the metal chlorides can escape in a gas form, and the metal residue of the heat insulation felt can be obviously reduced.
3. The heat insulation felt prepared by the invention has excellent performance, the heat conductivity coefficient is only 0.051W/m.K, the tensile strength is up to 0.26Mpa, and the thermal expansion coefficient is only 1.05 x 10 -6 And/k, the metal element content is only 19.7ppm.
Detailed Description
Unless otherwise indicated, all reagents used in the present invention are commercially available.
Preparation example 1
Process for preparing amide derivatives
1 mol of 1- (3, 5-dichlorophenyl) -5-propyl-1H-pyrazole-4-carbonyl chloride is dissolved in a proper amount of dimethylbenzene, 1 mol of 2- (3-chlorophenyl) ethylamine is added, the mixture is heated to 85 ℃ and stirred for reaction for 1H, the dimethylbenzene is removed by reduced pressure distillation, saturated sodium bicarbonate solution is added for reaction for 2H under stirring, ethyl acetate is used for extraction, the organic layers are combined, dried with anhydrous magnesium sulfate, concentrated and subjected to column chromatography to obtain the amide derivative.
Preparation example 2
Preparation method of modified phenolic resin
Adding 0.1 mol of 3, 4-dichlorobenzyl alcohol after 1 mol of phenol is melted, regulating the pH to 9 by a sodium hydroxide solution, stirring for 30-40min at 45 ℃, adding formaldehyde for 2 times, adding 0.7 mol of formaldehyde for the first time, stirring for reacting for 35 min at 60 ℃, adding 0.3 mol of formaldehyde for the second time, stirring for reacting for 1h at 95 ℃, cooling to 25 ℃, regulating the pH to 7 by hydrochloric acid, and concentrating to obtain the modified phenolic resin.
Example 1
A preparation method of the heat insulation felt comprises the following steps:
s1, crushing and processing the leftover materials of the heat-insulating felt into chopped fiber yarns;
s2, chemically modifying the chopped fiber to obtain modified chopped fiber;
s3, fully mixing the modified chopped fiber with an adhesive, and heating and pressurizing to form a felt;
s4, carbonizing and graphitizing the felt to obtain the heat-insulating felt;
in the step S1, the average length of chopped fiber is 2cm, and the chopped fiber is polyacrylonitrile-based carbon fiber;
in the step S2, the specific method of chemical modification is as follows: uniformly mixing 35 parts by weight of chopped fiber, 15 parts by weight of amide derivative, 15 parts by weight of hydroxylamine hydrochloride and 110 parts by weight of ethylene glycol, stirring at 55 ℃ for reaction for 1.5 hours, taking out the chopped fiber, and drying to obtain modified chopped fiber;
in the step S3, the mass ratio of the chopped fiber to the binder is 1:0.15, the adhesive is formed by mixing modified phenolic resin and ethanol according to a mass ratio of 1:4, and the heating and pressurizing conditions are as follows: treating 15 min at 160deg.C under 22.5 MPa;
in step S4, the conditions for the carbonization treatment are: under the protection of nitrogen, the process sequentially passes through 4 different temperature areas, wherein the first temperature area is 400 ℃, the second temperature area is 500min and 20min, the third temperature area is 800 ℃, the first temperature area is 1h, the fourth temperature area is 900 ℃, the first temperature area is 1h, and the graphitization treatment conditions are as follows: the treatment was carried out at 2100℃for 0.75h under nitrogen.
Example 2
This embodiment differs from embodiment 1 in that: in the chemical modification in step S2, 10 parts by weight of the amide derivative was used, and the rest was the same as in example 1.
Example 3
This embodiment differs from embodiment 1 in that: in the chemical modification in step S2, 20 parts by weight of the amide derivative was obtained, and the rest was the same as in example 1.
Example 4
This embodiment differs from embodiment 1 in that: in the chemical modification in step S2, 10 parts by weight of hydroxylamine hydrochloride was used, and the rest was the same as in example 1.
Example 5
This embodiment differs from embodiment 1 in that: in the chemical modification in step S2, 20 parts by weight of hydroxylamine hydrochloride was used, and the rest was the same as in example 1.
Example 6
This embodiment differs from embodiment 1 in that: in the step S3, the mass ratio of the chopped fiber to the binder is 1:0.1, the remainder being exactly the same as in example 1.
Example 7
This embodiment differs from embodiment 1 in that: in the step S3, the mass ratio of the chopped fiber to the binder is 1:0.2, the remainder being exactly the same as in example 1.
Results and detection
1. Coefficient of thermal conductivity
Test standard: GB/T10294-2008 heat insulating material steady state thermal resistance and related characteristic measuring protection hot plate method
The results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the thermal insulation mats prepared by the present invention have thermal conductivity coefficients of less than 0.11, wherein the thermal conductivity coefficient is the lowest in example 1, and the thermal conductivity coefficients are all 0.051.
2. Tensile Strength
Detection standard: GB/T8721-2009 carbon material tensile strength determination method
The results are shown in Table 2.
TABLE 2
| Project | Tensile Strength (Mpa) |
| Example 1 | 0.26 |
| Example 2 | 0.21 |
| Example 3 | 0.18 |
| Example 4 | 0.22 |
| Example 5 | 0.15 |
| Example 6 | 0.17 |
| Example 7 | 0.19 |
As can be seen from Table 2, the thermal insulation mats prepared according to the present invention all had a tensile strength of greater than 0.15, wherein the highest tensile strength was 0.26 for example 1.
3. Coefficient of thermal expansion
Detection standard: determination of thermal expansion coefficient of heat insulation product for GB/T34185-2017 building equipment and industrial device
The results are shown in Table 3.
TABLE 3 Table 3
| Project | Average expansion coefficient (10) -6 /k) |
| Example 1 | 1.05 |
| Example 2 | 1.10 |
| Example 3 | 1.16 |
| Example 4 | 1.21 |
| Example 5 | 1.25 |
| Example 6 | 1.23 |
| Example 7 | 1.19 |
As can be seen from Table 3, the average expansion coefficients of the heat insulation mats prepared according to the present invention were all lower than 1.3, wherein the lowest average expansion coefficient was 1.05 as in example 1.
4. Metallic element
The testing method comprises the following steps: the total content of the metal impurity elements such as Al, K, ca, na, fe, ti, cu, mg, li, cr, V, co, ni was measured by ICP-AES.
The results are shown in Table 4.
TABLE 4 Table 4
As can be seen from Table 4, the metal element content of the heat insulation felt prepared by the invention is lower than 35, wherein the lowest metal element content is in example 4, and the metal element content is only 19.7.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The preparation method of the heat insulation felt is characterized by comprising the following steps:
s1, crushing and processing the leftover materials of the heat-insulating felt into chopped fiber yarns;
s2, chemically modifying the chopped fiber to obtain modified chopped fiber;
s3, fully mixing the modified chopped fiber with an adhesive, and heating and pressurizing to form a felt;
and S4, carbonizing and graphitizing the felt to obtain the heat-insulating felt.
2. The method for preparing a heat insulation felt according to claim 1, wherein in the step S1, the average length of the chopped fiber is 1-3cm, and the chopped fiber is polyacrylonitrile-based carbon fiber.
3. The method for preparing the heat insulation felt according to claim 1, wherein in the step S2, the specific method for chemical modification is as follows:
dissolving 1- (3, 5-dichlorophenyl) -5-propyl-1H-pyrazole-4-carbonyl chloride in dimethylbenzene, adding 2- (3-chlorophenyl) ethylamine, heating to 80-90 ℃ and stirring for reaction for 0.5-1.5H, distilling under reduced pressure to remove dimethylbenzene, adding saturated sodium bicarbonate solution and stirring for reaction for 1-3H, extracting with ethyl acetate, combining organic layers, drying with anhydrous magnesium sulfate, concentrating, and performing column chromatography to obtain an amide derivative;
mixing 30-40 parts by weight of chopped fiber, 10-20 parts by weight of amide derivative, 10-20 parts by weight of hydroxylamine hydrochloride and 100-120 parts by weight of ethylene glycol uniformly, stirring and reacting for 1-2 hours at 50-60 ℃, taking out the chopped fiber, and drying to obtain the modified chopped fiber.
4. The method for preparing the heat insulation felt according to claim 3, wherein the molar ratio of the 1- (3, 5-dichlorophenyl) -5-propyl-1H-pyrazole-4-carbonyl chloride to the 2- (3-chlorophenyl) ethylamine is 1:1.
5. The method for preparing the heat insulation felt according to claim 1, wherein in the step S3, the adhesive is formed by mixing modified phenolic resin and ethanol according to the mass ratio of 1 (3-5), wherein the method for preparing the modified phenolic resin is as follows: adding 3, 4-dichlorobenzyl alcohol after phenol is melted, regulating the pH to 9 by a sodium hydroxide solution, stirring for 30-40min at 40-50 ℃, adding formaldehyde for 2 times, adding 70-80% of formaldehyde for the first time, stirring for reaction for 30-40min at 60 ℃, adding the rest formaldehyde for the second time, stirring for reaction for 0.5-1h at 95 ℃, cooling to 20-30 ℃, regulating the pH to 7 by hydrochloric acid, and concentrating to obtain the modified phenolic resin.
6. The method for preparing the heat insulation felt according to claim 7, wherein the molar ratio of phenol, formaldehyde and 3, 4-dichlorobenzyl alcohol is 1:1: (0.1-0.2).
7. The method for preparing the heat insulation felt according to claim 1, wherein the mass ratio of the chopped fiber to the binder is 1: (0.1-0.2).
8. The method for preparing a heat insulation felt according to claim 1, wherein in the step S3, the heating and pressurizing conditions are as follows: treating at 150-170deg.C and 20-25MPa for 10-20min.
9. The method for preparing a heat insulation felt according to claim 1, wherein in the step S4, the carbonization conditions are as follows: under the protection of nitrogen, the nitrogen passes through 4 different temperature areas in sequence, wherein the first temperature area is 400 ℃, the second temperature area is 500min and 20min, the third temperature area is 800 ℃, the first temperature area is 1h, and the fourth temperature area is 900 ℃ and the second temperature area is 1h.
10. The method for preparing a heat insulation felt according to claim 1, wherein in the step S4, the graphitizing treatment conditions are as follows: and under the protection of nitrogen, treating at 2000-2200 ℃ for 0.5-1h.
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| CN114645376A (en) * | 2022-05-13 | 2022-06-21 | 浙江星辉新材料科技有限公司 | Preparation method of low-density carbon fiber hard heat-preservation felt |
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| US5837620A (en) * | 1996-10-10 | 1998-11-17 | Johns Manville International, Inc. | Fiber glass mats and method of making |
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