CN107540275A - Insulation material and preparation method thereof - Google Patents
Insulation material and preparation method thereof Download PDFInfo
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- CN107540275A CN107540275A CN201710721988.4A CN201710721988A CN107540275A CN 107540275 A CN107540275 A CN 107540275A CN 201710721988 A CN201710721988 A CN 201710721988A CN 107540275 A CN107540275 A CN 107540275A
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Abstract
The invention discloses a kind of insulation material and preparation method thereof, the preparation method includes：Coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, is stirred at 50 70 DEG C, mix asphalt raw material is made；Mix asphalt raw material, pitch viscosity reductant, fibrous material, polyvinyl resin, phenolic resin and methacrylonitrile are mixed to get mixture M；Mixture M is handled through spinning to obtain precursor；Insulation material will be obtained after the heated charing of precursor；The thermal conductivity for solving existing asphalt base carbon fiber is higher so that and its insulating power is weaker, while the problem of its antistatic effect deficiency.
Description
Technical field
The present invention relates to field of heat insulating materials, in particular it relates to a kind of insulation material and preparation method thereof.
Background technology
Asphalt base carbon fiber be one kind using asphalt or coal tar pitch as raw material, refined, spinning, pre-oxidation through pitch,
Carbonization or phosphorus content is more than 92% special fibre prepared by graphitization.It is a kind of new material of excellent in mechanical performance, it
1/4 of proportion less than steel, carbon fiber resin composite material tensile strength is general all in more than 3500Mpa, is 7~9 times of steel, resists
Draw modulus of elasticity be 230~430Gpa be also higher than steel, be indispensable engineering material in aerospace industry, separately traffic,
Also be widely used in terms of machinery, sports and amusement, leisure goods, health care and civil construction, in this meaning predictive of
Broad prospect of application of the carbon fiber in engineering.Asphalt base carbon fiber is also widely used in insulation material, but utilizes traditional work
The thermal conductivity of insulation material prepared by skill is higher so that its insulating power is weaker, while its antistatic effect deficiency.
Therefore it provides one kind on the premise of its mechanical property is ensured, further improves insulating power and antistatic effect
Insulation material and preparation method thereof the problem of being urgent need to resolve of the present invention.
The content of the invention
It is an object of the invention to provide a kind of insulation material and preparation method thereof, solves the thermal conductivity of existing insulation material
It is higher so that its insulating power is weaker, while the problem of its antistatic effect deficiency.
To achieve these goals, the invention provides a kind of preparation method of insulation material, the preparation method to include：
(1) coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, in 50-70
It is stirred at DEG C, mix asphalt raw material is made；
(2) by mix asphalt raw material, pitch viscosity reductant, fibrous material, polyvinyl resin, phenolic resin and methacrylonitrile
It is mixed to get mixture M；
(3) mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10-20
DEG C/min programming rate rises to 150-170 DEG C, then rises to 190-210 DEG C with 5-10 DEG C/min programming rate；
(4) asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, heating the condition of charing includes：Add
The temperature of heat is 1-2h, and the time of heating is 220-240 DEG C；
After (5) mixing asphalt base carbon fiber material, aspen fibers by using silicon, isocyanates, sodium carboxymethylcellulose and acetone
To mixture M, mixture M is obtained into insulation material through hot-forming；Wherein, hot-forming condition includes：The pressure of hot pressing
For 0.4-0.6MPa, the temperature of hot pressing is 150-200 DEG C.
Present invention also offers a kind of insulation material, wherein, the insulation material is made by above-mentioned preparation method.
Pass through above-mentioned technical proposal, the invention provides a kind of insulation material and preparation method thereof, the preparation method bag
Include：Coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, is carried out at 50-70 DEG C
Stirring, mix asphalt raw material is made；By mix asphalt raw material, pitch viscosity reductant, fibrous material, polyvinyl resin, phenolic resin
Mixture M is mixed to get with methacrylonitrile；Mixture M is handled through spinning to obtain precursor；Wherein, the heating in spinning processing
Condition includes：150-170 DEG C is risen to 10-20 DEG C/min programming rate, then is risen to 5-10 DEG C/min programming rate
190-210℃；Asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, heating the condition of charing includes：Heating
Temperature be 1-2h, the time of heating is 220-240 DEG C；By asphalt base carbon fiber material, aspen fibers by using silicon, isocyanates and carboxylic first
Mixture M is obtained after base sodium cellulosate and acetone mixing, mixture M is obtained into insulation material through hot-forming；Wherein, it is hot pressed into
The condition of type includes：The pressure of hot pressing is 0.4-0.6MPa, and the temperature of hot pressing is 150-200 DEG C.Pass through the association between each raw material
Same-action so that obtained insulation material not only possesses excellent mechanical property, while also possesses excellent insulating power and resist
Electrostatic capacity, field of heat insulating materials is can be widely applied for, while the method for the insulation material is simple, raw material is easy for preparing
.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The end points of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
The invention provides a kind of preparation method of insulation material, the preparation method includes：
(1) coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, in 50-70
It is stirred at DEG C, mix asphalt raw material is made；
(2) by mix asphalt raw material, pitch viscosity reductant, fibrous material, polyvinyl resin, phenolic resin and methacrylonitrile
It is mixed to get mixture M；
(3) mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10-20
DEG C/min programming rate rises to 150-170 DEG C, then rises to 190-210 DEG C with 5-10 DEG C/min programming rate；
(4) asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, heating the condition of charing includes：Add
The temperature of heat is 1-2h, and the time of heating is 220-240 DEG C；
After (5) mixing asphalt base carbon fiber material, aspen fibers by using silicon, isocyanates and sodium carboxymethylcellulose and acetone
To mixture M, mixture M is obtained into insulation material through hot-forming；Wherein, hot-forming condition includes：The pressure of hot pressing
For 0.4-0.6MPa, the temperature of hot pressing is 150-200 DEG C.
In a kind of preferred embodiment of the present invention, in order to further improve the insulating power of obtained insulation material
And antistatic effect, relative to the mix asphalt raw material of 100 parts by weight, the dosage of pitch viscosity reductant is 5-15 parts by weight, fiber
The dosage of material is 20-40 parts by weight, and the dosage of polyvinyl resin is 10-30 parts by weight, and the dosage of phenolic resin is 25-55 weights
Part is measured, the dosage of methacrylonitrile is 25-60 parts by weight；Relative to the asphalt base carbon fiber material of 100 parts by weight, aspen fibers by using silicon
Dosage be 20-30 parts by weight, the dosage of isocyanates is 10-40 parts by weight, and the dosage of sodium carboxymethylcellulose is 10-20 weights
Part is measured, the dosage of acetone is 50-80 parts by weight.
In a kind of preferred embodiment of the present invention, in order to further improve the insulating power of obtained insulation material
And antistatic effect, relative to the mix asphalt raw material of 100 parts by weight, the dosage of pitch viscosity reductant is 8-12 parts by weight, fiber
The dosage of material is 25-35 parts by weight, and the dosage of polyvinyl resin is 15-25 parts by weight, and the dosage of phenolic resin is 35-45 weights
Part is measured, the dosage of methacrylonitrile is 40-50 parts by weight；Relative to the asphalt base carbon fiber material of 100 parts by weight, aspen fibers by using silicon
Dosage be 24-26 parts by weight, the dosage of isocyanates is 20-30 parts by weight, and the dosage of sodium carboxymethylcellulose is 14-16 weights
Part is measured, the dosage of acetone is 60-70 parts by weight.
In a kind of preferred embodiment of the present invention, in order to further improve the insulating power of obtained insulation material
And antistatic effect, one or more of the inert gas in nitrogen, helium and argon gas.
In a kind of preferred embodiment of the present invention, in order to further improve the insulating power of obtained insulation material
And antistatic effect, the temperature of heating is 500-550 DEG C in step (1), and the time of heating is 0.5-1h.
In a kind of preferred embodiment of the present invention, in order to further improve the insulating power of obtained insulation material
And antistatic effect, coal tar pitch and asphalt are 1 according to mass ratio：1-2 ratio is mixed.
In a kind of preferred embodiment of the present invention, in order to further improve the insulating power of obtained insulation material
And antistatic effect, one or more of the fibrous material in glass fibre, boron fibre and ceramic fibre.
In a kind of preferred embodiment of the present invention, in order to further improve the insulating power of obtained insulation material
And antistatic effect, the weight average molecular weight of polyvinyl resin is 5000-6000, and the weight average molecular weight of phenolic resin is 7000-
8000。
In a kind of preferred embodiment of the present invention, in order to further improve the insulating power of obtained insulation material
And antistatic effect, one or more of the pitch viscosity reductant in phenolic resin, polyacrylamide and ethylene bis stearamide.
Present invention also offers a kind of insulation material, wherein, the insulation material is made by above-mentioned preparation method.
The present invention will be described in detail by way of examples below.In following examples, polyvinyl resin is divided equally again
Son amount is 5000-6000, and the weight average molecular weight of phenolic resin is 7000-8000.
Embodiment 1
100g coal tar pitches and 100g asphalt are mixed, and (temperature of heating is 500 for heating under nitrogen protection
DEG C, the time of heating is 0.5h) to molten condition, it is stirred at 50 DEG C, mix asphalt raw material is made；100g is mixed and dripped
Blue or green raw material, 8g phenolic resin, 25g glass fibres, 15g polyvinyl resins, 35g phenolic resin and 40g methacrylonitriles mix
To mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10 DEG C/
Min programming rate rises to 150 DEG C, then rises to 190 DEG C with 5 DEG C/min programming rate；It will be obtained after the heated charing of precursor
Asphalt base carbon fiber material；Wherein, heating the condition of charing includes：The temperature of heating is 1h, and the time of heating is 220 DEG C；Will
100g asphalt base carbon fibers material, 24g aspen fibers by using silicon, 20g isocyanates and 14g sodium carboxymethylcelluloses and the mixing of 60g acetone
After obtain mixture M, mixture M is obtained into insulation material A1 through hot-forming；Wherein, hot-forming condition includes：Hot pressing
Pressure be 0.4MPa, the temperature of hot pressing is 150 DEG C.
Embodiment 2
100g coal tar pitches and 200g asphalt are mixed, and (temperature of heating is 550 for heating under helium protection
DEG C, the time of heating is 1h) to molten condition, it is stirred at 70 DEG C, mix asphalt raw material is made；By 100g mix asphalts
Raw material, 12g polyacrylamides, 35g boron fibres, 25g polyvinyl resins, 45g phenolic resin and 50g methacrylonitriles are mixed to get
Mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 20 DEG C/min
Programming rate rise to 170 DEG C, then rise to 210 DEG C with 10 DEG C/min programming rate；It will be dripped after the heated charing of precursor
Blue or green base carbon fibre material；Wherein, heating the condition of charing includes：The temperature of heating is 2h, and the time of heating is 240 DEG C；Will
100g asphalt base carbon fibers material, 26g aspen fibers by using silicon, 30g isocyanates and 16g sodium carboxymethylcelluloses and the mixing of 70g acetone
After obtain mixture M, mixture M is obtained into insulation material A2 through hot-forming；Wherein, hot-forming condition includes：Hot pressing
Pressure be 0.6MPa, the temperature of hot pressing is 200 DEG C.
Embodiment 3
100g coal tar pitches and 150g asphalt are mixed, and (temperature of heating is 520 for heating under argon gas protection
DEG C, the time of heating is 0.8h) to molten condition, it is stirred at 60 DEG C, mix asphalt raw material is made；100g is mixed and dripped
Blue or green raw material, 10g ethylene bis stearamides, 30g ceramic fibres, 20g polyvinyl resins, 40g phenolic resin and 45g methacrylonitriles
It is mixed to get mixture M；Mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With
15 DEG C/min programming rate rises to 160 DEG C, then rises to 200 DEG C with 8 DEG C/min programming rate；After the heated charing of precursor
Obtain asphalt base carbon fiber material；Wherein, heating the condition of charing includes：The temperature of heating is 1.5h, and the time of heating is 230
℃；By 100g asphalt base carbon fibers material, 25g aspen fibers by using silicon, 25g isocyanates and 15g sodium carboxymethylcelluloses and 65g acetone
Mixture M is obtained after mixing, mixture M is obtained into insulation material A3 through hot-forming；Wherein, hot-forming condition includes：
The pressure of hot pressing is 0.5MPa, and the temperature of hot pressing is 180 DEG C.
Embodiment 4
Carried out according to the method for embodiment 3, unlike, relative to 100g mix asphalt raw material, pitch viscosity reductant
Dosage is 5g, and the dosage of fibrous material is 20g, and the dosage of polyvinyl resin is 10g, and the dosage of phenolic resin is 25g, methyl-prop
The dosage of alkene nitrile is 25g, and relative to 100g asphalt base carbon fiber material, the dosage of aspen fibers by using silicon is 20g, the use of isocyanates
Measure as 10g, the dosage of sodium carboxymethylcellulose is 10g, and the dosage of acetone is 50g, obtains insulation material A4.
Embodiment 5
Carried out according to the method for embodiment 3, unlike, relative to 100g mix asphalt raw material, pitch viscosity reductant
Dosage is 15g, and the dosage of fibrous material is 40g, and the dosage of polyvinyl resin is 30g, and the dosage of phenolic resin is 55g, methyl
The dosage of acrylonitrile is 60g, and relative to 100g asphalt base carbon fiber material, the dosage of aspen fibers by using silicon is 30g, isocyanates
Dosage is 40g, and the dosage of sodium carboxymethylcellulose is 20g, and the dosage of acetone is 80g, obtains insulation material A5.
Comparative example 1
Carried out according to the method for embodiment 3, unlike, the Elevated Temperature Conditions in spinning processing include：With 5 DEG C/min liter
Warm speed rises to 140 DEG C, then rises to 170 DEG C with 3 DEG C/min programming rate, and heating the condition of charing includes：The temperature of heating
For 0.5h, the time of heating is 200 DEG C, obtains insulation material D1.
Comparative example 2
Carried out according to the method for embodiment 3, unlike, the Elevated Temperature Conditions in spinning processing include：With 25 DEG C/min's
Programming rate rises to 180 DEG C, then rises to 220 DEG C with 12 DEG C/min programming rate, and heating the condition of charing includes：The temperature of heating
Spend for 2.5h, the time of heating is 250 DEG C, obtains insulation material D2.
Comparative example 3
Carried out according to the method for embodiment 3, unlike, methacrylonitrile is not included in raw material, obtains insulation material D3.
Comparative example 4
Carried out according to the method for embodiment 3, unlike, polyvinyl resin is not included in raw material, obtains insulation material D4.
Comparative example 5
Carried out according to the method for embodiment 3, unlike, phenolic resin is not included in raw material, obtains insulation material D5.
Table 1
It can be obtained by above table, insulation material A1-A5 produced within the scope of the present invention not only possesses excellent
Mechanical property, while have superior antistatic effect and insulating power, and insulation material D1- produced outside the scope of the present invention
D, its mechanical property, antistatic effect and insulating power are relatively weak.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of preparation method of insulation material, it is characterised in that the preparation method includes：
(1) coal tar pitch and asphalt are mixed, and molten condition is heated under inert gas shielding, at 50-70 DEG C
It is stirred, mix asphalt raw material is made；
(2) mix asphalt raw material, pitch viscosity reductant, fibrous material, polyvinyl resin, phenolic resin and methacrylonitrile are mixed
Obtain mixture M；
(3) mixture M is handled through spinning to obtain precursor；Wherein, the Elevated Temperature Conditions in spinning processing include：With 10-20 DEG C/
Min programming rate rises to 150-170 DEG C, then rises to 190-210 DEG C with 5-10 DEG C/min programming rate；
(4) asphalt base carbon fiber material will be obtained after the heated charing of precursor；Wherein, heating the condition of charing includes：Heating
Temperature is 1-2h, and the time of heating is 220-240 DEG C；
(5) mixed after mixing asphalt base carbon fiber material, aspen fibers by using silicon, isocyanates, sodium carboxymethylcellulose and acetone
Compound M, mixture M is obtained into insulation material through hot-forming；Wherein, hot-forming condition includes：The pressure of hot pressing is
0.4-0.6MPa, the temperature of hot pressing is 150-200 DEG C.
2. preparation method according to claim 1, wherein, relative to the mix asphalt raw material of 100 parts by weight, pitch visbreaking
The dosage of agent is 5-15 parts by weight, and the dosage of fibrous material is 20-40 parts by weight, and the dosage of polyvinyl resin is 10-30 weight
Part, the dosage of phenolic resin is 25-55 parts by weight, and the dosage of methacrylonitrile is 25-60 parts by weight；
Relative to the asphalt base carbon fiber material of 100 parts by weight, the dosage of aspen fibers by using silicon is 20-30 parts by weight, isocyanates
Dosage is 10-40 parts by weight, and the dosage of sodium carboxymethylcellulose is 10-20 parts by weight, and the dosage of acetone is 50-80 parts by weight.
3. preparation method according to claim 2, wherein, relative to the mix asphalt raw material of 100 parts by weight, pitch visbreaking
The dosage of agent is 8-12 parts by weight, and the dosage of fibrous material is 25-35 parts by weight, and the dosage of polyvinyl resin is 15-25 weight
Part, the dosage of phenolic resin is 35-45 parts by weight, and the dosage of methacrylonitrile is 40-50 parts by weight；
Relative to the asphalt base carbon fiber material of 100 parts by weight, the dosage of aspen fibers by using silicon is 24-26 parts by weight, isocyanates
Dosage is 20-30 parts by weight, and the dosage of sodium carboxymethylcellulose is 14-16 parts by weight, and the dosage of acetone is 60-70 parts by weight.
4. according to the preparation method described in any one in claim 1-3, wherein, inert gas is selected from nitrogen, helium and argon
One or more in gas.
5. according to the preparation method described in any one in claim 1-3, wherein, the temperature of heating is in step (1)
500-550 DEG C, the time of heating is 0.5-1h.
6. according to the preparation method described in any one in claim 1-3, wherein, coal tar pitch and asphalt are according to quality
Than for 1：1-2 ratio is mixed.
7. according to the preparation method described in any one in claim 1-3, wherein, it is fine that fibrous material is selected from glass fibre, boron
One or more in peacekeeping ceramic fibre.
8. according to the preparation method described in any one in claim 1-3, wherein, the weight average molecular weight of polyvinyl resin is
5000-6000, the weight average molecular weight of phenolic resin is 7000-8000.
9. according to the preparation method described in any one in claim 1-3, wherein, pitch viscosity reductant is selected from phenolic resin, gathered
One or more in acrylamide and ethylene bis stearamide.
10. a kind of insulation material, it is characterised in that the insulation material is as the preparation described in any one in claim 1-9
Method is made.
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| CN108411407A (en) * | 2018-03-21 | 2018-08-17 | 青岛美卡新型材料有限公司 | A kind of long fine, short fine mixed type carbon carbon insulation quilt processing technology |
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