CN106045516B - A kind of preparation process of environmental protection lignin ceramics - Google Patents
A kind of preparation process of environmental protection lignin ceramics Download PDFInfo
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- CN106045516B CN106045516B CN201610410585.3A CN201610410585A CN106045516B CN 106045516 B CN106045516 B CN 106045516B CN 201610410585 A CN201610410585 A CN 201610410585A CN 106045516 B CN106045516 B CN 106045516B
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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
- C04B35/515—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
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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
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention discloses a kind of preparation processes of environmentally friendly lignin ceramics: (1) enzymatic hydrolysis (EH) lignin modified: according to parts by weight, take 20-25 parts of enzymolysis xylogens, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 50-60min of constant temperature, after treatment is dried with 80-100 DEG C, enzyme deactivation is living, obtains modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；(2) lignin ceramics are prepared: according to weight fraction, taking 20 parts of modified lignin resins, 80-85 parts of enzymolysis xylogens, is thoroughly mixed, are pressed and molded after dry, then vacuum high-temperature sintering both obtains lignin ceramics finished product.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of preparation process of environmental protection lignin ceramics.
Background technique
Lignin is the substance being made of the aromatic alcohol polymerizeing, and is present in lignum, and main function is to pass through
It forms intertexture net and carrys out sclereid wall, be secondary wall main component.Lignin is predominantly located between cellulose fibre, is played resistance to compression and is made
With.In xylophyta, lignin accounts for 25%, is the most abundant organic matter of second in the world (cellulose is first).
The prior art, which is disclosed, is used to substitute the method that phenolic resin prepares lignin ceramics for enzymolysis xylogen, however should
Technology utilization chemical technology is modified, and needs to be unfavorable for environmental protection using chemical substances such as a large amount of sodium hydroxides.
The present invention is intended to provide a kind of preparation process of environmental protection lignin ceramics, using environment-friendly and green technique to enzymatic hydrolysis wood
Element is modified, and is then mixed according to a certain percentage with unmodified enzymolysis xylogen, compression molding, and high temperature sintering is made
The very excellent wood ceramics of performance.
Summary of the invention
Technical problems based on background technology, the present invention background technique there are aiming at the problem that, the invention discloses
A kind of preparation process of environmental protection lignin ceramics, is modified enzymolysis lignin using environment-friendly and green technique, then according to one
The very excellent wood ceramics of performance are made in fixed ratio and the mixing of unmodified enzymolysis xylogen, compression molding, high temperature sintering.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation process of environmental protection lignin ceramics, steps are as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Enzymolysis xylogen is chosen, can be commercially available, it can also voluntarily prepare, wherein content of lignin 70-80%, be crushed to 60
Mesh is spare；
According to parts by weight, 20-25 parts of enzymolysis xylogens are taken, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 50- of constant temperature
60min, after treatment are dried with 80-100 DEG C, and enzyme deactivation is living, obtain modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；
The pretreatment fluid includes: 0.3% phytase, and the phytase is 5000u/g；0.5% laccase, the laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics are prepared:
According to weight fraction, 20 parts of modified lignin resins, 80-85 parts of enzymolysis xylogens are taken, are thoroughly mixed, drying is laggard
Row compression molding, then vacuum high-temperature sintering both obtains lignin ceramics finished product.
The preferred three-step approach of high temperature sintering:
150 DEG C are risen to the temperature of 15 DEG C/min, keeps the temperature 30min；
800 DEG C are risen to the temperature of 8 DEG C/min, keeps the temperature 50min；
150 DEG C or less are down to the temperature of 10 DEG C/min.
The invention has the beneficial effects that:
Enzymolysis lignin is modified using environment-friendly and green technique, it is then wooden with unmodified enzymatic hydrolysis according to a certain percentage
The very excellent wood ceramics of performance are made in quality mixing, compression molding, high temperature sintering.
Specific embodiment
Embodiment 1:
A kind of preparation process of environmental protection lignin ceramics, steps are as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Enzymolysis xylogen is chosen, can be commercially available, it can also voluntarily prepare, wherein content of lignin 70%, be crushed to 60 mesh
It is spare；
According to parts by weight, 25 parts of enzymolysis xylogens are taken, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 50min of constant temperature,
After treatment is dried with 100 DEG C, and enzyme deactivation is living, obtains modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；
The pretreatment fluid includes: 0.3% phytase, and the phytase is 5000u/g；0.5% laccase, the laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics are prepared:
According to weight fraction, 20 parts of modified lignin resins, 80 parts of enzymolysis xylogens are taken, are thoroughly mixed, taken after dry
1.5g20Mpa compression molding, pressure maintaining 20min, then vacuum high-temperature sintering both obtains lignin ceramics finished product；
The high temperature sintering is three-step approach:
150 DEG C are risen to the temperature of 15 DEG C/min, keeps the temperature 30min；
800 DEG C are risen to the temperature of 8 DEG C/min, keeps the temperature 50min；
150 DEG C or less are down to the temperature of 10 DEG C/min.
Embodiment 2:
A kind of preparation process of environmental protection lignin ceramics, steps are as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Enzymolysis xylogen is chosen, can be commercially available, it can also voluntarily prepare, wherein content of lignin 80%, be crushed to 60 mesh
It is spare；
According to parts by weight, 20 parts of enzymolysis xylogens are taken, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 60min of constant temperature,
After treatment is dried with 80 DEG C, and enzyme deactivation is living, obtains modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；
The pretreatment fluid includes: 0.3% phytase, and the phytase is 5000u/g；0.5% laccase, the laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics are prepared:
According to weight fraction, 20 parts of modified lignin resins, 85 parts of enzymolysis xylogens are taken, are thoroughly mixed, taken after dry
1.5g20Mpa compression molding, pressure maintaining 20min, then vacuum high-temperature sintering both obtains lignin ceramics finished product；
The high temperature sintering is three-step approach:
150 DEG C are risen to the temperature of 15 DEG C/min, keeps the temperature 30min；
800 DEG C are risen to the temperature of 8 DEG C/min, keeps the temperature 50min；
150 DEG C or less are down to the temperature of 10 DEG C/min.
Embodiment 3:
A kind of preparation process of environmental protection lignin ceramics, steps are as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Enzymolysis xylogen is chosen, can be commercially available, it can also voluntarily prepare, wherein content of lignin 71%, be crushed to 60 mesh
It is spare；
According to parts by weight, 24 parts of enzymolysis xylogens are taken, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 55min of constant temperature,
After treatment is dried with 95 DEG C, and enzyme deactivation is living, obtains modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；
The pretreatment fluid includes: 0.3% phytase, and the phytase is 5000u/g；0.5% laccase, the laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics are prepared:
According to weight fraction, 20 parts of modified lignin resins, 81 parts of enzymolysis xylogens are taken, are thoroughly mixed, taken after dry
1.5g20Mpa compression molding, pressure maintaining 20min, then vacuum high-temperature sintering both obtains lignin ceramics finished product；
The high temperature sintering is three-step approach:
150 DEG C are risen to the temperature of 15 DEG C/min, keeps the temperature 30min；
800 DEG C are risen to the temperature of 8 DEG C/min, keeps the temperature 50min；
150 DEG C or less are down to the temperature of 10 DEG C/min.
Embodiment 4:
A kind of preparation process of environmental protection lignin ceramics, steps are as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Enzymolysis xylogen is chosen, can be commercially available, it can also voluntarily prepare, wherein content of lignin 79%, be crushed to 60 mesh
It is spare；
According to parts by weight, 21 parts of enzymolysis xylogens are taken, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 53min of constant temperature,
After treatment is dried with 81 DEG C, and enzyme deactivation is living, obtains modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；
The pretreatment fluid includes: 0.3% phytase, and the phytase is 5000u/g；0.5% laccase, the laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics are prepared:
According to weight fraction, 20 parts of modified lignin resins, 84 parts of enzymolysis xylogens are taken, are thoroughly mixed, taken after dry
1.5g20Mpa compression molding, pressure maintaining 20min, then vacuum high-temperature sintering both obtains lignin ceramics finished product；
The high temperature sintering is three-step approach:
150 DEG C are risen to the temperature of 15 DEG C/min, keeps the temperature 30min；
800 DEG C are risen to the temperature of 8 DEG C/min, keeps the temperature 50min；
150 DEG C or less are down to the temperature of 10 DEG C/min.
Embodiment 5:
A kind of preparation process of environmental protection lignin ceramics, steps are as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Enzymolysis xylogen is chosen, can be commercially available, it can also voluntarily prepare, wherein content of lignin 72%, be crushed to 60 mesh
It is spare；
According to parts by weight, 23 parts of enzymolysis xylogens are taken, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 59min of constant temperature,
After treatment is dried with 87 DEG C, and enzyme deactivation is living, obtains modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；
The pretreatment fluid includes: 0.3% phytase, and the phytase is 5000u/g；0.5% laccase, the laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics are prepared:
According to weight fraction, 20 parts of modified lignin resins, 82 parts of enzymolysis xylogens are taken, are thoroughly mixed, taken after dry
1.5g20Mpa compression molding, pressure maintaining 20min, then vacuum high-temperature sintering both obtains lignin ceramics finished product；
The high temperature sintering is three-step approach:
150 DEG C are risen to the temperature of 15 DEG C/min, keeps the temperature 30min；
800 DEG C are risen to the temperature of 8 DEG C/min, keeps the temperature 50min；
150 DEG C or less are down to the temperature of 10 DEG C/min.
6 comparative experiments of embodiment:
The inventors discovered that the formula of pretreatment fluid is critically important, slightly deviation when being modified to enzymolysis xylogen
The composite material that cannot be just satisfied with, following comparative example are only to demonstrate.
A kind of preparation process of environmental protection lignin ceramics, steps are as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Enzymolysis xylogen is chosen, can be commercially available, it can also voluntarily prepare, wherein content of lignin 78%, be crushed to 60 mesh
It is spare；
According to parts by weight, 22 parts of enzymolysis xylogens are taken, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 51min of constant temperature,
After treatment is dried with 99 DEG C, and enzyme deactivation is living, obtains modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；
The pretreatment fluid includes: 0.5% phytase, and the phytase is 5000u/g；0.2% trehalose；0.3%
Citric acid, remaining is water；
(2) lignin ceramics are prepared:
According to weight fraction, 20 parts of modified lignin resins, 83 parts of enzymolysis xylogens are taken, are thoroughly mixed, taken after dry
1.5g20Mpa compression molding, pressure maintaining 20min, then vacuum high-temperature sintering both obtains lignin ceramics finished product；
The high temperature sintering is three-step approach:
150 DEG C are risen to the temperature of 15 DEG C/min, keeps the temperature 30min；
800 DEG C are risen to the temperature of 8 DEG C/min, keeps the temperature 50min；
150 DEG C or less are down to the temperature of 10 DEG C/min.
7 measure of merit of embodiment:
Method measures the performance of lignin ceramics according to prior art:
As a result as shown in table 1 below:
It can be seen that being modified using environment-friendly and green technique to enzymolysis lignin, then do not change according to a certain percentage and
Property enzymolysis xylogen mixing, compression molding, the very excellent wood ceramics of performance are made in high temperature sintering, and surface hardness is very big.
Furthermore, it was further observed that, the wood ceramics pore-size distribution that the present invention is prepared is highly uniform.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of preparation method of environmental protection lignin ceramics, steps are as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
According to parts by weight, 20-25 parts of enzymolysis xylogens are taken, 25 portions of pretreatment fluids are uniformly mixed, 38 DEG C of heat preservation 50- of constant temperature
60min, after treatment are dried with 80-100 DEG C, and enzyme deactivation is living, obtain modified enzymolysis lignin, and it is spare that 60 meshes are crossed after grinding；
(2) lignin ceramics are prepared:
According to weight fraction, 20 parts of modified enzymolysis lignins, 80-85 parts of enzymolysis xylogens are taken, are thoroughly mixed, drying is laggard
Row compression molding, then vacuum high-temperature sintering both obtains lignin ceramics finished product；
The pretreatment fluid includes: 0.3% phytase, and the phytase is 5000u/g；0.5% laccase, the laccase are
6000u/g ；0.2% trehalose；0.3% citric acid, remaining is water；
Enzymolysis xylogen is chosen, wherein content of lignin 70-80%, it is spare to be crushed to 60 mesh.
2. the preparation method of environmental protection lignin ceramics described in claim 1, it is characterised in that:
The high temperature sintering uses three-step approach:
150 DEG C are risen to the temperature of 15 DEG C/min, keeps the temperature 30min；
800 DEG C are risen to the temperature of 8 DEG C/min, keeps the temperature 50min；
150 DEG C or less are down to the temperature of 10 DEG C/min.
3. the lignin ceramics that preparation method of any of claims 1 or 2 is prepared.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698604A (en) * | 2009-11-03 | 2010-04-28 | 东北林业大学 | Method for manufacturing enzymatic hydrolysis lignin ceramics |
| EP2427549A1 (en) * | 2009-05-08 | 2012-03-14 | BP Corporation North America Inc. | Enzyme recovery sorbent, enzyme recovery unit, lignocellulosic biorefinery, process for recycling enzymes, and renewable material |
| CN104785162A (en) * | 2015-03-17 | 2015-07-22 | 福州大学 | Aminomethylated lignin-based dispersant, and preparation technology and application thereof |
| CN104884615A (en) * | 2012-09-05 | 2015-09-02 | 诺维信公司 | Polypeptides having protease activity |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2427549A1 (en) * | 2009-05-08 | 2012-03-14 | BP Corporation North America Inc. | Enzyme recovery sorbent, enzyme recovery unit, lignocellulosic biorefinery, process for recycling enzymes, and renewable material |
| CN101698604A (en) * | 2009-11-03 | 2010-04-28 | 东北林业大学 | Method for manufacturing enzymatic hydrolysis lignin ceramics |
| CN104884615A (en) * | 2012-09-05 | 2015-09-02 | 诺维信公司 | Polypeptides having protease activity |
| CN104785162A (en) * | 2015-03-17 | 2015-07-22 | 福州大学 | Aminomethylated lignin-based dispersant, and preparation technology and application thereof |
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