CN107903062A - A kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin - Google Patents

A kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin Download PDF

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Publication number
CN107903062A
CN107903062A CN201711161564.3A CN201711161564A CN107903062A CN 107903062 A CN107903062 A CN 107903062A CN 201711161564 A CN201711161564 A CN 201711161564A CN 107903062 A CN107903062 A CN 107903062A
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Prior art keywords
epoxy resin
alkali lignin
industrial alkali
wood ceramics
coffee
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CN201711161564.3A
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王明杰
陈瑶
高建民
刘付
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Beijing Forestry University
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Beijing Forestry University
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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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6022—Injection moulding
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606—Drying
    • 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
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
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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
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
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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
    • C04B2235/658—Atmosphere during thermal treatment

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Epoxy Resins (AREA)

Abstract

The present invention provides a kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin, belong to the technical field in terms of biological material preparation.I.e. using absolute ethyl alcohol as diluent and dispersant, industrial alkali lignin and high temperature latent curing agent are well dispersed in epoxy-resin systems.It is molded by hot setting, calcines and obtain the wood ceramics.Industrial alkali lignin by using low cost is raw material, not only contributes to solve the problem of lignin higher value application, but also can promote epoxy resin cure, saves hardener dose, reduces production cost.It is that resin system has longer room temperature working life by using high temperature latent curing agent, and is adapted to higher whipping temp, further improves processing performance.

Description

A kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin
Technical field
The present invention relates to a kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin, belong to biomass 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.
The aromatic compound most abundant as reserves in nature, lignin are to form wooden three big base of resource material One of this chemical constituent, is to pass through ehter bond and the high carbon content natural reproducible of carbon-to-carbon key connection by construction unit of phenylpropyl alcohol alkane High polymer.The high-valued utilization research of lignin is in the ascendant, but since rapid industrial development, enterprises in pulp and paper industry etc. are produced Supply exceed demand for raw lignin byproduct, and most industrial lignins are not all fully used.Explore lignin high level Change utilizes new way, to promoting sustainable development, realizes that socio-economic development and ecological environmental protection win-win have scientific meaning And economic value.
The content of the invention
The purpose of the present invention is intended in view of the deficiencies of the prior art, there is provided one kind utilizes epoxy resin and industrial alkali lignin The method for preparing wood ceramics.The preparation method simple process, inexpensive is easily controllable, and pulping and paper-making industry is produced Industrial alkali lignin is introduced into the preparation process of wood ceramics, can open up the new way of the high-valued application of lignin, for protection Environment intensive utilization biomass resource contributes, and also can help to further reduce the production cost of wood ceramics material, changes The physicochemical property of kind wood ceramics.The technical solution adopted in the present invention is：One kind utilizes epoxy resin and industrial alkali lignin The method for preparing wood ceramics, it is comprised the following steps that：
(1) 60~80 parts of E-44 epoxy resin are weighed, heating water bath is spare.
(2) 15~30 parts of industrial alkali lignins, 6~8 parts of curing agent are weighed, 50~70 parts of absolute ethyl alcohols are added, in water-bath Magnetic agitation is carried out under heating condition, obtains coffee-like solution A.
(3) epoxy resin is slowly injected in coffee-like solution A while hot, obtains coffee-like viscous mixture B, air-proof condition Lower continuation heating water bath magnetic agitation for a period of time, stops stirring, is only heated by water-bath, by anhydrous second after mixing Alcohol removes as far as possible.
(4) coffee-like viscous mixture B is placed in electric vacunm drying case, vacuum outgas in a heated condition.
(5) in the coffee-like viscous mixture injection metal die while hot finished degassing, 12~18h is displayed.
(6) mould is heated to 180~200 DEG C, keeps the temperature 60~90min, pre-burning base substrate is obtained after cooling.
(7) pre-burning base substrate is coated in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection Wood ceramics.
In steps 1 and 2,3, bath temperature is 65~80 DEG C.
In step 2, used curing agent is dicyanodiamine, and when use needs first carefully finely ground with mortar.
In step 3, the airtight heating magnetic agitation time is 5~10h, after mixing continue heating water bath time be 2~3h.
In step 4, drying box temperature is 70~80 DEG C, 0.04~0.05Mpa of vacuum, vacuum outgas time 90min.
In step 7, 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 the following advantages and effects：
1st, help to improve curing agent and lignin in high viscosity ring as diluent and decentralized medium using absolute ethyl alcohol The dispersiveness of oxygen tree fat, obtains dispersed, density homogeneous mixture system.
2nd, using high temperature latent curing agent, when making resin that there is longer room temperature working life, therefore having sufficient batch mixing Between, while it is also convenient for improving by way of heating the mobility of resin, without worrying resin premature cure.Industrial soda at the same time Lignin has certain facilitation to epoxy resin cure, can save the dosage of curing agent, further reduce the cost.
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) 60~80 parts of E-44 epoxy resin are weighed, heating water bath is spare.
(2) 15~30 parts of industrial alkali lignins, 6~8 parts of curing agent are weighed, 50~70 parts of absolute ethyl alcohols are added, in water-bath Magnetic agitation is carried out under heating condition, obtains coffee-like solution A.
(3) epoxy resin is slowly injected in coffee-like solution A while hot, obtains coffee-like viscous mixture B, air-proof condition Lower continuation heating water bath magnetic agitation for a period of time, stops stirring, is only heated by water-bath, by anhydrous second after mixing Alcohol removes as far as possible.
(4) coffee-like viscous mixture B is placed in electric vacunm drying case, vacuum outgas in a heated condition.
(5) in the coffee-like viscous mixture injection metal die while hot finished degassing, 12~18h is displayed.
(6) mould is heated to 180~200 DEG C, keeps the temperature 60~90min, pre-burning base substrate is obtained after cooling.
(7) pre-burning base substrate is coated in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection Wood ceramics.
In steps 1 and 2,3, bath temperature is 65 DEG C.
In step 2, used curing agent is dicyanodiamine, and when use needs first carefully finely ground with mortar.
In step 3, the airtight heating magnetic agitation time is 10h, and the time for continuing heating water bath after mixing is 2h.
In step 4, drying box temperature is 80 DEG C, vacuum 0.05Mpa, vacuum outgas time 90min.
In step 7, sintering schedule is：5 DEG C/min of programming rate, 800 DEG C of sintering temperature, soaking time 1h.
Embodiment 2
(1) 60~80 parts of E-44 epoxy resin are weighed, heating water bath is spare.
(2) 15~30 parts of industrial alkali lignins, 6~8 parts of curing agent are weighed, 50~70 parts of absolute ethyl alcohols are added, in water-bath Magnetic agitation is carried out under heating condition, obtains coffee-like solution A.
(3) epoxy resin is slowly injected in coffee-like solution A while hot, obtains coffee-like viscous mixture B, air-proof condition Lower continuation heating water bath magnetic agitation for a period of time, stops stirring, is only heated by water-bath, by anhydrous second after mixing Alcohol removes as far as possible.
(4) coffee-like viscous mixture B is placed in electric vacunm drying case, vacuum outgas in a heated condition.
(5) in the coffee-like viscous mixture injection metal die while hot finished degassing, 12~18h is displayed.
(6) mould is heated to 180~200 DEG C, keeps the temperature 60~90min, pre-burning base substrate is obtained after cooling.
(7) pre-burning base substrate is coated in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection Wood ceramics.
In steps 1 and 2,3, bath temperature is 75 DEG C.
In step 2, used curing agent is dicyanodiamine, and when use needs first carefully finely ground with mortar.
In step 3, the airtight heating magnetic agitation time is 8h, and the time for continuing heating water bath after mixing is 3h.
In step 4, drying box temperature is 75 DEG C, vacuum 0.04Mpa, vacuum outgas time 90min.
In step 7, sintering schedule is：5 DEG C/min of programming rate, 850 DEG C of sintering temperature, soaking time 1h.

Claims (6)

  1. A kind of 1. method for preparing wood ceramics using epoxy resin and industrial alkali lignin, it is characterised in that including following several A step：
    (1) 60~80 parts of E-44 epoxy resin are weighed, heating water bath is spare；
    (2) 15~30 parts of industrial alkali lignins, 6~8 parts of curing agent are weighed, 50~70 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) epoxy resin is slowly injected in coffee-like solution A while hot, obtains coffee-like viscous mixture B, under air-proof condition after Continuous heating water bath magnetic agitation for a period of time, stops stirring, is only heated by water-bath, absolute ethyl alcohol is use up after mixing Amount removes；
    (4) coffee-like viscous mixture B is placed in electric vacunm drying case, vacuum outgas in a heated condition；
    (5) in the coffee-like viscous mixture injection metal die while hot finished degassing, 12~18h is displayed；
    (6) mould is heated to 180~200 DEG C, keeps the temperature 60~90min, pre-burning base substrate is obtained after cooling；
    (7) pre-burning base substrate is coated in quartz sand, sinters, that is, obtain wooden involved by the invention under argon gas atmosphere protection Ceramics.
  2. 2. a kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin according to claim 1, its It is characterized in that, in the step (1), (2), (3), water bath heating temperature is 65~80 DEG C.
  3. 3. a kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin according to claim 1, its It is characterized in that, in the step (2), used curing agent is dicyanodiamine, and when use needs first carefully finely ground with mortar.
  4. 4. a kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin according to claim 1, its It is characterized in that, in the step (3), the airtight heating magnetic agitation time is 5~10h, continues heating water bath after mixing Time is 2~3h.
  5. 5. a kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin according to claim 1, its It is characterized in that, in the step (4), drying box temperature is 70~80 DEG C, 0.04~0.05Mpa of vacuum, the vacuum outgas time 90min。
  6. 6. a kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin according to claim 1, its It is characterized in that, in the step (7), sintering schedule is：5 DEG C/min of programming rate, 800~1000 DEG C of sintering temperature, during insulation Between 1h.
CN201711161564.3A 2017-11-21 2017-11-21 A kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin Withdrawn CN107903062A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113233868A (en) * 2021-05-31 2021-08-10 福建省德化新凯丰陶瓷有限公司 Preparation process of antibacterial blank reinforcing agent for ceramic ornaments

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Publication number Priority date Publication date Assignee Title
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
CN104387107A (en) * 2014-11-14 2015-03-04 广东华科新材料研究院有限公司 Epoxy resin reinforced wood ceramic and preparation method thereof

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
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
CN104387107A (en) * 2014-11-14 2015-03-04 广东华科新材料研究院有限公司 Epoxy resin reinforced wood ceramic and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈祥宝: "《先进复合材料技术导论》", 30 September 2017, 北京航空工业出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113233868A (en) * 2021-05-31 2021-08-10 福建省德化新凯丰陶瓷有限公司 Preparation process of antibacterial blank reinforcing agent for ceramic ornaments

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Application publication date: 20180413