CN107759241A - A kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics - Google Patents

A kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics Download PDF

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Publication number
CN107759241A
CN107759241A CN201711161522.XA CN201711161522A CN107759241A CN 107759241 A CN107759241 A CN 107759241A CN 201711161522 A CN201711161522 A CN 201711161522A CN 107759241 A CN107759241 A CN 107759241A
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Prior art keywords
wood ceramics
alkali lignin
phenol formaldehyde
formaldehyde base
industry alkali
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CN201711161522.XA
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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
    • C04B35/71—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
    • 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
    • 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
    • C04B35/64—Burning or sintering processes
    • 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
    • C04B2235/65—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
    • 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
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6587—Influencing the atmosphere by vaporising a solid material, e.g. by using a burying of sacrificial powder

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  • Organic Chemistry (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention provides a kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics.I.e. to pulping and paper-making discarded object --- industrial alkali lignin carries out simple acid treatment, and uniformly mixed with chopped carbon fiber by low speed ball milling, by the way that itself and thermosetting phenolic resin are blended, a kind of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics are obtained after heated solidification, high temperature sintering.Industrial alkali lignin after acid treatment can prepare porous wood ceramics, addition chopped carbon fiber can carry out toughness reinforcing to porous wood ceramics, expand the application of porous wood ceramics with melt foaming in sintering process without pore creating material.

Description

A kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics
Technical field
The present invention relates to a kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics, belong to biological material Technical field in terms of preparation.
Background technology
Porous wood ceramics are presented huge with its distinctive structural behaviour in catalyst load, filtering flow etc. Application potential.It is compound by using acid-treated industrial alkali lignin and phenolic resin progress, it can be obtained by solidifying, sintering To the porous wood ceramics with abundant pore structure, cheap technique is simple, is industrial alkali lignin higher value application New results.But the fragility of this wood ceramics is larger, it is impossible to the bad working environments conditions such as motor-vehicle tail-gas filtering are adapted to, thus Need to take appropriate means to carry out it Strengthening and Toughening processing, improve mechanical property.
Similar to traditional fine ceramics method for toughening, the Strengthening and Toughening for realizing wood ceramics is also disconnected by increasing Inner surface area is split, apparatus with shock absorbing, realizes scattered impact stress protection ceramic structure integrality.Carbon fiber density is low, axle Intensity is high on to direction, modulus of elasticity is big, high temperature resistant, is the toughening material being used widely at present, passes through the carbon that is chopped Fiber reinforced porous wood ceramics, it can effectively contain diffusion of the micro-crack inside wood ceramics, realize Strengthening and Toughening purpose.
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 plasticizing phenol formaldehyde base industry alkali lignin The method of wood ceramics.The preparation method simple process, inexpensive is easily controllable, and by carbon fiber-reinforced ceramic technology with The preparation of porous wood ceramics combines, and realizing to obtain at lower cost has the porous wood ceramics of higher force performance Purpose.
The technical solution adopted in the present invention is：A kind of side of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics Method, it is comprised the following steps that：
(1) 300g industry alkali lignins are placed in 2L beakers, add deionized water and be configured to 25wt% solution, in water-bath Under the conditions of heating and magnetic agitation, sulphur acid for adjusting pH is slowly added to, obtains coffee-like solution A；
(2) coffee-like solution is stood into 30min under condition of water bath heating, abandoning supernatant, it is heavy to be washed with deionized Form sediment, drying precipitation obtains light brown lignin powder B；
(3) 30~40 parts of light brown lignin powder B are added in horizontal ball grinder, adds abrading-ball, add 3~5 parts Chopped carbon fiber, dry ball milling is uniform, obtains compound C；
(4) 50~60 parts of thermosetting phenolic resins are weighed, strong stirring is carried out with electric blender, are added while stirring mixed Close material C, continue stirring until its in resin it is dispersed, obtain compound D；
(4) compound D is slowly injected in flexible die, takes out, obtain after being heating and curing in electric drying oven with forced convection Pre-sintered body E；
(5) pre-sintered body E is embedded in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection Porous wood ceramics.
In step (1), bath temperature is 65~75 DEG C, and sulfuric acid concentration is 35~40wt%, with sulfuric acid regulation solution pH It is worth for 2.
In step (2), when precipitation is washed with deionized, filters when filtrate pH is 6~6.5 and stop washing, keep filter Cake is in faintly acid.
In step (3), chopped carbon fiber length is 3~5mm, ratio of grinding media to material 1:1, it can be carbon to use Material quality of grinding balls SiClx or aluminum oxide, ball grinder 100~120r/min of rotating speed, 4~6h of Ball-milling Time.
In step (4), it is silicon rubber to use flexible die material, and brushing dimethicone is as the demoulding when using Agent, solidification temperature are 140~150 DEG C, 3~4h of hardening time.
In step (5), sintering schedule is：5 DEG C/min of programming rate, 750~900 DEG C of sintering temperature, soaking time 4~ 5h, furnace cooling.
Compared with prior art, the present invention has advantages below and effect：
1st, porous wood ceramics are strengthened by chopped carbon fiber, compared with using the means such as carbon cloth, sintering Finished product is in isotropism, the toughness reinforcing available for the porous wood ceramics of complicated shape.
2nd, disperse chopped carbon fiber by low speed ball milling means, reduce the use of solvent, shorten manufacturing cycle, be advantageous to work Industry metaplasia is produced.
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) 300g industry alkali lignins are placed in 2L beakers, add deionized water and be configured to 25wt% solution, in water-bath Under the conditions of heating and magnetic agitation, sulphur acid for adjusting pH is slowly added to, obtains coffee-like solution A；
(2) coffee-like solution is stood into 30min under condition of water bath heating, abandoning supernatant, it is heavy to be washed with deionized Form sediment, drying precipitation obtains light brown lignin powder B；
(3) 35 parts of light brown lignin powder B are added in horizontal ball grinder, adds abrading-ball, it is fine to add 3 parts of chopped carbon Dimension, dry ball milling is uniform, obtains compound C；
(4) 50 parts of thermosetting phenolic resins are weighed, strong stirring is carried out with electric blender, adds compound while stirring C, continue stirring until its in resin it is dispersed, obtain compound D；
(4) compound D is slowly injected in flexible die, takes out, obtain after being heating and curing in electric drying oven with forced convection Pre-sintered body E；
(5) pre-sintered body E is embedded in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection Porous wood ceramics.
In step 1, bath temperature is 65 DEG C, sulfuric acid concentration 40wt%, is 2 with sulfuric acid regulation solution pH value.
In step 2, when precipitation is washed with deionized, filters when filtrate pH is 6.5 and stop washing, keep filter cake in weak It is acid.
In step 3, chopped carbon fiber length is 3mm, ratio of grinding media to material 1:1, use carborundum abrading-ball, ball grinder rotating speed 100r/min, Ball-milling Time 4h.
In step 4, it is silicon rubber to use flexible die material, when using brushing dimethicone as releasing agent, Solidification temperature is 140 DEG C, hardening time 3h.
In steps of 5, sintering schedule is：5 DEG C/min of programming rate, 800 DEG C of sintering temperature, soaking time 4h are cold with stove But.
Embodiment 2
(1) 300g industry alkali lignins are placed in 2L beakers, add deionized water and be configured to 25wt% solution, in water-bath Under the conditions of heating and magnetic agitation, sulphur acid for adjusting pH is slowly added to, obtains coffee-like solution A；
(2) coffee-like solution is stood into 30min under condition of water bath heating, abandoning supernatant, it is heavy to be washed with deionized Form sediment, drying precipitation obtains light brown lignin powder B；
(3) 40 parts of light brown lignin powder B are added in horizontal ball grinder, adds abrading-ball, it is fine to add 4 parts of chopped carbon Dimension, dry ball milling is uniform, obtains compound C；
(4) 60 parts of thermosetting phenolic resins are weighed, strong stirring is carried out with electric blender, adds compound while stirring C, continue stirring until its in resin it is dispersed, obtain compound D；
(4) compound D is slowly injected in flexible die, takes out, obtain after being heating and curing in electric drying oven with forced convection Pre-sintered body E；
(5) pre-sintered body E is embedded in quartz sand, sinters, that is, obtained involved by the invention under argon gas atmosphere protection Porous wood ceramics.
In step (1), bath temperature is 70 DEG C, sulfuric acid concentration 40wt%, is 2 with sulfuric acid regulation solution pH value.
In step (2), when precipitation is washed with deionized, filters when filtrate pH is 6 and stop washing, keep filter cake in weak It is acid.
In step (3), chopped carbon fiber length is 4mm, ratio of grinding media to material 1:1, use aluminum oxide abrading-ball, ball grinder rotating speed 120r/min, Ball-milling Time 4.5h.
In step (4), it is silicon rubber to use flexible die material, and brushing dimethicone is as the demoulding when using Agent, solidification temperature are 145 DEG C, hardening time 3.5h.
In step (5), sintering schedule is：5 DEG C/min of programming rate, 850 DEG C of sintering temperature, soaking time 4h, with stove Cooling.

Claims (6)

  1. A kind of 1. method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics, it is characterised in that including following several steps Suddenly：
    (1) 300g industry alkali lignins are placed in 2L beakers, add deionized water and be configured to 25wt% solution, in heating water bath And under the conditions of magnetic agitation, sulphur acid for adjusting pH is slowly added to, obtain coffee-like solution A；
    (2) coffee-like solution is stood into 30min under condition of water bath heating, abandoning supernatant, precipitation is washed with deionized, dried Dry precipitation obtains light brown lignin powder B；
    (3) 30~40 parts of light brown lignin powder B are added in horizontal ball grinder, adds abrading-ball, added 3~5 parts and be chopped Carbon fiber, dry ball milling is uniform, obtains compound C；
    (4) 50~60 parts of thermosetting phenolic resins are weighed, strong stirring is carried out with electric blender, adds compound while stirring C, continue stirring until its in resin it is dispersed, obtain compound D；
    (4) compound D is slowly injected in flexible die, is taken out after being heating and curing in electric drying oven with forced convection, obtain pre-burning Knot body E；
    (5) pre-sintered body E is embedded in quartz sand, sinters, that is, obtain more involved by the invention under argon gas atmosphere protection Hole wood ceramics.
  2. 2. a kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics according to claim 1, its feature It is, in the step (1), bath temperature is 65~75 DEG C, and sulfuric acid concentration is 35~40wt%, with sulfuric acid regulation solution pH value For 2.
  3. 3. a kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics according to claim 1, its feature It is, in the step (2), when precipitation is washed with deionized, filters when filtrate pH is 6~6.5 and stop washing, keep filter cake In faintly acid.
  4. 4. a kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics according to claim 1, its feature It is, in the step (3), chopped carbon fiber length is 3~5mm, ratio of grinding media to material 1:1, it can be carbon to use Material quality of grinding balls SiClx or aluminum oxide, ball grinder 100~120r/min of rotating speed, 4~6h of Ball-milling Time.
  5. 5. a kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics according to claim 1, its feature Be, in the step (4), it is silicon rubber to use flexible die material, when using brushing dimethicone as releasing agent, Solidification temperature is 140~150 DEG C, 3~4h of hardening time.
  6. 6. a kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics according to claim 1, its feature It is, in the step (5), sintering schedule is：5 DEG C/min of programming rate, 750~900 DEG C of sintering temperature, soaking time 4~ 5h, furnace cooling.
CN201711161522.XA 2017-11-21 2017-11-21 A kind of method of plasticizing phenol formaldehyde base industry alkali lignin wood ceramics Withdrawn CN107759241A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114043589A (en) * 2021-12-01 2022-02-15 北京林业大学 Method for applying modified industrial alkali lignin to wood heat treatment

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102161762A (en) * 2011-01-19 2011-08-24 华东理工大学 Method for modifying benzoxazine resin
CN106220209A (en) * 2016-07-18 2016-12-14 中国科学院上海应用物理研究所 Prepare method and the silicon carbide woodceramics of silicon carbide woodceramics
CN106478121A (en) * 2016-09-30 2017-03-08 巩义市泛锐熠辉复合材料有限公司 A kind of preparation method of carbon fiber toughened silicon carbide wood ceramics

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102161762A (en) * 2011-01-19 2011-08-24 华东理工大学 Method for modifying benzoxazine resin
CN106220209A (en) * 2016-07-18 2016-12-14 中国科学院上海应用物理研究所 Prepare method and the silicon carbide woodceramics of silicon carbide woodceramics
CN106478121A (en) * 2016-09-30 2017-03-08 巩义市泛锐熠辉复合材料有限公司 A kind of preparation method of carbon fiber toughened silicon carbide wood ceramics

Non-Patent Citations (3)

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Title
JUNMIN QIAN等: ""Structure and basic properties of woodceramics made from phenolic resin–basswood powder composite"", 《MATERIALS SCIENCE AND ENGINEERING》 *
李忠正: "《禾草类纤维制浆造纸 中文版 第2卷》", 31 March 2013, 中国轻工业出版社 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114043589A (en) * 2021-12-01 2022-02-15 北京林业大学 Method for applying modified industrial alkali lignin to wood heat treatment

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Application publication date: 20180306