CN107778020A - A kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics - Google Patents
A kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics Download PDFInfo
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- CN107778020A CN107778020A CN201711161530.4A CN201711161530A CN107778020A CN 107778020 A CN107778020 A CN 107778020A CN 201711161530 A CN201711161530 A CN 201711161530A CN 107778020 A CN107778020 A CN 107778020A
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- carbon fiber
- epoxy resin
- wood ceramics
- alkali lignin
- reinforced epoxy
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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Abstract
The invention provides a kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics, belong to the technical field in terms of biological material preparation.It is distributed to chopped carbon fiber in resin system, toughness reinforcing is carried out to epoxy resin-matrix industry alkali lignin wood ceramics, by the extraction of fiber, bridging and micro-crack deflecting action, improves the toughness of wood ceramics, its shock resistance as structural ceramics is improved, widens application field.The good combination of chopped carbon fiber and matrix is ensure that using epoxy-resin systems, industrial alkali lignin is introduced and has saved the production cost of wood ceramics, and contribute to the solidification of resin system.
Description
Technical field
The present invention relates to a kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics, belongs to biology
Technical field in terms of material preparation.
Background technology
Wood ceramics are a kind of new carbon-carbon composites proposed by Japanese researchers the nineties in last century, are led to
The timber of high temperature sintering thermosetting resin dipping is crossed, the product with similar ceramic performance can be obtained.By recent two decades
Explore, the research of wood ceramics material has obtained significant progress, and expands out silicon carbide woodceramics, metal wood ceramics etc.
Branch.As a kind of biomass-based new material, wood ceramics show the performance of uniqueness in self-lubricating, electromagnetic shielding etc.,
The extensive concern of domestic and international researcher is attracted, as the substitute of some ceramic materials, wood ceramics have good answer
Use prospect.Traditionally the raw material of wood ceramics is mostly solid wood, wood-based plate, based on wood powder etc., is given birth to by introducing pulping and paper-making
The discarded object industry alkali lignin of production is raw material, can save production cost, acceleration of sintering base substrate curing molding, improve wooden pottery
Porcelain performance.
Although wood ceramics material has certain difference with the fine ceramics material on conventional meaning, inorganic non-metallic is belonged to together
Material, all there is fragility it is big the problem of.In order to improve the impact flexibility of material, application is expanded, can be by adding carbon
The mode of fiber carries out toughness reinforcing to material.Wood ceramics material is when being impacted, extraction, bridging and the wooden pottery of chopped strand
Deflection of the ceramic material internal tiny crack along chopped strand can increase break surface in material, absorb energy, so as to protection materials
Structure is not damaged.
The content of the invention
The purpose of the present invention is intended in view of the shortcomings of the prior art, there is provided a kind of carbon fiber-reinforced epoxy resin-matrix industrial soda
The method of lignin wood ceramics.The preparation method simple process, inexpensive is easily controllable, is chopped using lower-cost
Carbon fiber carries out toughness reinforcing to epoxy resin-matrix industry alkali lignin wood ceramics, effectively improves the big limitation of wood ceramics fragility
Property, application of the wood ceramics as structural ceramics has been widened, has improved the reliability of wood ceramics structural member work.This hair
Technical scheme is used by bright：A kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics, it has
Body step is as follows：
(1) 60~70 parts of E-44 epoxy resin are weighed, heating water bath is standby.
(2) 15~25 parts of industrial alkali lignins, 5~7 parts of curing agent are weighed, 40~50 parts of absolute ethyl alcohols are added, in water-bath
Magnetic agitation is carried out under heating condition, obtains coffee-like solution A.
(3) 1~2 part of PVP K-30 of addition in 30 parts of absolute ethyl alcohols is weighed, then is gradually added 3~10 parts short
Carbon fiber is cut, obtains carbon fiber dispersion liquid B, magnetic agitation is uniform.
(4) first carbon fiber dispersion liquid B is added in coffee-like solution A, keeps heating water bath and magnetic agitation, then delay while hot
Slow injection enters epoxy resin, obtains coffee-like viscous mixture C, continues heating water bath magnetic agitation for a period of time under air-proof condition,
Stop stirring after well mixed, only heated by water-bath, absolute ethyl alcohol is removed as far as possible.
(5) coffee-like viscous mixture C is placed in electric vacunm drying case, vacuum outgas in a heated condition.
(6) in the coffee-like viscous mixture injection metal die while hot finished degassing, 16~18h is displayed.
(7) mould is heated to 200~220 DEG C, is incubated 60~90min, pre-burning base substrate is obtained after cooling.
(8) pre-burning base substrate is coated in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection
Carbon fiber-reinforced wood ceramics.
In steps 1 and 2,4, water bath heating temperature is 65~80 DEG C.
In step 2, used curing agent is dicyanodiamine, is needed during use first carefully finely ground with mortar.
In step 3, the chopped carbon fiber length added is 3~5mm.
In step 4, the airtight heating magnetic agitation time is 5~10h, and the time for continuing heating water bath after well mixed is
2~3h.
In steps of 5, drying box temperature is 70~80 DEG C, 0.04~0.05Mpa of vacuum, vacuum outgas time 90min.
In step 8, sintering schedule is：5 DEG C/min of programming rate, 800~1000 DEG C of sintering temperature, soaking time 1h.
Compared with prior art, the present invention has advantages below and effect：
1st, toughness reinforcing is carried out using chopped carbon fiber, toughening material is uniformly dispersed, and without specific orientation, finished product mechanical property does not have
There is anisotropy.
2nd, high temperature latent curing agent is coordinated using epoxy-resin systems, resin and chopped carbon fiber interface cohesion are good,
High-temperature curing agent ensure that even if by high temperature bath improve Resin Flow resin also will not premature cure, introduce industrial soda wood
Quality can save the dosage of curing agent to a certain extent, further reduce cost, and realize the higher value application of lignin.
3rd, the preparation method flow is simple, and simple process, inexpensive is easily controllable, have good development prospect and
Further deeply expand the value of research.
Embodiment
With reference to specific implementation example, the present invention is described in detail：
Embodiment 1
(1) 60 parts of E-44 epoxy resin are weighed, heating water bath is standby.
(2) 15 parts of industrial alkali lignins, 6 parts of curing agent are weighed, 40 parts of absolute ethyl alcohols is added, enters under condition of water bath heating
Row magnetic agitation, obtain coffee-like solution A.
(3) 1 part of PVP K-30 of addition in 30 parts of absolute ethyl alcohols is weighed, then is gradually added 5 parts of chopped carbon fibres
Dimension, obtains carbon fiber dispersion liquid B, magnetic agitation is uniform.
(4) first carbon fiber dispersion liquid B is added in coffee-like solution A, keeps heating water bath and magnetic agitation, then delay while hot
Slow injection enters epoxy resin, obtains coffee-like viscous mixture C, continues heating water bath magnetic agitation for a period of time under air-proof condition,
Stop stirring after well mixed, only heated by water-bath, absolute ethyl alcohol is removed as far as possible.
(5) coffee-like viscous mixture C is placed in electric vacunm drying case, vacuum outgas in a heated condition.
(6) in the coffee-like viscous mixture injection metal die while hot finished degassing, 16h is displayed.
(7) mould is heated to 200 DEG C, is incubated 70min, pre-burning base substrate is obtained after cooling.
(8) pre-burning base substrate is coated in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection
Carbon fiber-reinforced wood ceramics.
In steps 1 and 2,4, water bath heating temperature is 65 DEG C.
In step 2, used curing agent is dicyanodiamine, is needed during use first carefully finely ground with mortar.
In step 3, the chopped carbon fiber length added is 3mm.
In step 4, the airtight heating magnetic agitation time is 8h, and the time for continuing heating water bath after being well mixed is 3h.
In steps of 5, drying box temperature is 80 DEG C, vacuum 0.04Mpa, vacuum outgas time 90min.
In step 8, sintering schedule is：5 DEG C/min of programming rate, 800 DEG C of sintering temperature, soaking time 1h.
Embodiment 2
(1) 65 parts of E-44 epoxy resin are weighed, heating water bath is standby.
(2) 20 parts of industrial alkali lignins, 7 parts of curing agent are weighed, 50 parts of absolute ethyl alcohols is added, enters under condition of water bath heating
Row magnetic agitation, obtain coffee-like solution A.
(3) 1 part of PVP K-30 of addition in 30 parts of absolute ethyl alcohols is weighed, then is gradually added 8 parts of chopped carbon fibres
Dimension, obtains carbon fiber dispersion liquid B, magnetic agitation is uniform.
(4) first carbon fiber dispersion liquid B is added in coffee-like solution A, keeps heating water bath and magnetic agitation, then delay while hot
Slow injection enters epoxy resin, obtains coffee-like viscous mixture C, continues heating water bath magnetic agitation for a period of time under air-proof condition,
Stop stirring after well mixed, only heated by water-bath, absolute ethyl alcohol is removed as far as possible.
(5) coffee-like viscous mixture C is placed in electric vacunm drying case, vacuum outgas in a heated condition.
(6) in the coffee-like viscous mixture injection metal die while hot finished degassing, 18h is displayed.
(7) mould is heated to 200 DEG C, is incubated 90min, pre-burning base substrate is obtained after cooling.
(8) pre-burning base substrate is coated in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection
Carbon fiber-reinforced wood ceramics.
In steps 1 and 2,4, water bath heating temperature is 75 DEG C.
In step 2, used curing agent is dicyanodiamine, is needed during use first carefully finely ground with mortar.
In step 3, the chopped carbon fiber length added is 4mm.
In step 4, the airtight heating magnetic agitation time is 10h, and the time for continuing heating water bath after being well mixed is 3h.
In steps of 5, drying box temperature is 80 DEG C, vacuum 0.05Mpa, vacuum outgas time 90min.
In step 8, sintering schedule is：5 DEG C/min of programming rate, 850 DEG C of sintering temperature, soaking time 1h.
Claims (7)
- A kind of 1. method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics, it is characterised in that including as follows Several steps：(1) 60~70 parts of E-44 epoxy resin are weighed, heating water bath is standby；(2) 15~25 parts of industrial alkali lignins, 5~7 parts of curing agent are weighed, 40~50 parts of absolute ethyl alcohols are added, in heating water bath Under the conditions of carry out magnetic agitation, obtain coffee-like solution A；(3) 1~2 part of PVP K-30 of addition in 30 parts of absolute ethyl alcohols is weighed, then is gradually added 3~10 parts of chopped carbon Fiber, obtains carbon fiber dispersion liquid B, and magnetic agitation is uniform；(4) first carbon fiber dispersion liquid B is added in coffee-like solution A, keeps heating water bath and magnetic agitation, then slowly note while hot Enter epoxy resin, obtain coffee-like viscous mixture C, continue heating water bath magnetic agitation for a period of time under air-proof condition, mixing Stop stirring after uniformly, only heated by water-bath, absolute ethyl alcohol is removed as far as possible；(5) coffee-like viscous mixture C is placed in electric vacunm drying case, vacuum outgas in a heated condition；(6) in the coffee-like viscous mixture injection metal die while hot finished degassing, 16~18h is displayed；(7) mould is heated to 200~220 DEG C, is incubated 60~90min, pre-burning base substrate is obtained after cooling；(8) pre-burning base substrate is coated in quartz sand, is sintered under 800~1000 DEG C, argon gas atmosphere protection, that is, obtain the invention Involved carbon fiber-reinforced wood ceramics.
- 2. a kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics according to claim 1, Characterized in that, in the step (1), (2), (4), water bath heating temperature is 65~80 DEG C.
- 3. a kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics according to claim 1, Characterized in that, in the step (2), used curing agent is dicyanodiamine, is needed during use first carefully finely ground with mortar.
- 4. a kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics according to claim 1, Characterized in that, in the step (3), the chopped carbon fiber length added is 3~5mm.
- 5. a kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics according to claim 1, Characterized in that, in the step (4), the airtight heating magnetic agitation time is 5~10h, continues heating water bath after well mixed Time be 2~3h.
- 6. a kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics according to claim 1, Characterized in that, in the step (5), drying box temperature is 70~80 DEG C, 0.04~0.05Mpa of vacuum, during vacuum outgas Between 90min.
- 7. a kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics according to claim 1, Characterized in that, in the step (8), sintering schedule is：5 DEG C/min of programming rate, 800~1000 DEG C of sintering temperature, insulation Time 1h.
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| CN201711161530.4A CN107778020A (en) | 2017-11-21 | 2017-11-21 | A kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics |
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| CN201711161530.4A CN107778020A (en) | 2017-11-21 | 2017-11-21 | A kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114425891A (en) * | 2022-02-25 | 2022-05-03 | 中国船舶重工集团公司第十二研究所 | High-permeability intercalation toughening material and preparation method thereof |
| CN115472441A (en) * | 2022-09-13 | 2022-12-13 | 中南林业科技大学 | CNT (carbon nanotube) -modified short fiber/wood ceramic electrode as well as preparation method and application thereof |
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| CN101108772A (en) * | 2006-07-20 | 2008-01-23 | 东北林业大学 | Method for manufacturing xylogen ceramic |
| CN103694640A (en) * | 2013-12-20 | 2014-04-02 | 北京郁懋科技有限责任公司 | Preparation method of conductive thermo-cured epoxy resin system |
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2017
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| CN101108772A (en) * | 2006-07-20 | 2008-01-23 | 东北林业大学 | Method for manufacturing xylogen ceramic |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114425891A (en) * | 2022-02-25 | 2022-05-03 | 中国船舶重工集团公司第十二研究所 | High-permeability intercalation toughening material and preparation method thereof |
| CN115472441A (en) * | 2022-09-13 | 2022-12-13 | 中南林业科技大学 | CNT (carbon nanotube) -modified short fiber/wood ceramic electrode as well as preparation method and application thereof |
| CN115472441B (en) * | 2022-09-13 | 2024-01-30 | 中南林业科技大学 | CNT-modified short fiber/wood ceramic electrode and preparation method and application thereof |
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