CN106045516A - Process for preparing environment-friendly lignin ceramics - Google Patents
Process for preparing environment-friendly lignin ceramics Download PDFInfo
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- CN106045516A CN106045516A CN201610410585.3A CN201610410585A CN106045516A CN 106045516 A CN106045516 A CN 106045516A CN 201610410585 A CN201610410585 A CN 201610410585A CN 106045516 A CN106045516 A CN 106045516A
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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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- 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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Abstract
The invention discloses a process for preparing environment-friendly lignin ceramics. The process comprises a step (1) of performing enzymatic hydrolysis lignin modification: according to the weight parts, taking 20-25 parts of enzymatic hydrolysis lignin and 25 parts of pretreatment solution to perform uniform mixing, performing heat insulation for 50-60 min at a constant temperature of 38 DEG C, performing drying at 80-100 DEG C after the treatment is over, performing enzyme denaturalixation, obtaining modified enzymatic hydrolysis lignin, and grinding the modified enzymatic hydrolysis lignin and sieving the modified enzymatic hydrolysis lignin through a 60-mesh sieve for standby application; a step (2) of preparing the lignin ceramics: according to the weight percentage, taking 20 parts of modified lignin and 80-85 parts of enzymatic hydrolysis lignin, performing stirring fully, performing compression molding after pressing, and then performing vacuum high-temperature sintering to obtain the finished lignin ceramics.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to the preparation technology of a kind of environmental protection lignin ceramics.
Background technology
Lignin is the class material being made up of the aromatic alcohol being polymerized, and is present in lignum, and Main Function is to pass through
Form intertexture net and carry out sclereid wall, for secondary wall main component.Lignin is predominantly located between cellulose fibre, plays resistance to compression and makees
With.In xylophyta, lignin accounts for 25%, is the Organic substance (cellulose is first) that second is the abundantest in the world.
Prior art is disclosed and enzymolysis xylogen is used for substituting the method that lignin ceramics prepared by phenolic resin, but should
Technology utilization chemical technology is modified, and needs to use the chemical substances such as substantial amounts of sodium hydroxide, is unfavorable for environmental protection.
It is desirable to provide the preparation technology of a kind of environmental protection lignin ceramics, it utilizes environment-friendly and green technique to enzymolysis wood
Element is modified, then according to certain ratio and the mixing of unmodified enzymolysis xylogen, compression molding, high temperature sintering, prepares
The wood pottery that performance is the most excellent.
Summary of the invention
The technical problem existed based on background technology, the present invention is directed to the problem that background technology exists, the invention discloses
A kind of preparation technology of environmental protection lignin ceramics, it utilizes environment-friendly and green technique to be modified enzymolysis lignin, then according to one
Fixed ratio and the mixing of unmodified enzymolysis xylogen, compression molding, high temperature sintering, the wood pottery that prepared performance is the most excellent.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation technology of environmental protection lignin ceramics, step is as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Choose enzymolysis xylogen, can be purchased, it is also possible to prepare voluntarily, wherein content of lignin 70-80%, be crushed to 60
Mesh is standby；
According to parts by weight, take 20-25 part enzymolysis xylogen, 25 parts of pretreatment fluid mix homogeneously, constant temperature 38 DEG C insulation 50-
60min, process is lived with 80-100 DEG C of drying, enzyme denaturing, is obtained modified enzymolysis lignin after terminating, crosses 60 mesh sieves standby after grinding；
Described pretreatment fluid comprises: the phytase of 0.3%, and described phytase is 5000u/g；0.5% laccase, described laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics is prepared:
According to weight fraction, take 20 parts of modified lignin resins, 80-85 part enzymolysis xylogen, be thoroughly mixed, be dried laggard
Row compression molding, then vacuum high-temperature sintering had both obtained lignin ceramics finished product.
The preferred three-step approach of described high temperature sintering:
Rise to 150 DEG C with the temperature of 15 DEG C/min, be incubated 30min；
Rise to 800 DEG C with the temperature of 8 DEG C/min, be incubated 50min；
It is down to less than 150 DEG C with the temperature of 10 DEG C/min.
The invention have benefit that:
Utilize environment-friendly and green technique that enzymolysis lignin is modified, then according to certain ratio and unmodified enzymolysis wood
Quality mixes, compression molding, high temperature sintering, the wood pottery that prepared performance is the most excellent.
Detailed description of the invention
Embodiment 1:
A kind of preparation technology of environmental protection lignin ceramics, step is as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Choose enzymolysis xylogen, can be purchased, it is also possible to prepare voluntarily, wherein content of lignin 70%, be crushed to 60 mesh
Standby；
According to parts by weight, taking 25 parts of enzymolysis xylogens, 25 parts of pretreatment fluid mix homogeneously, constant temperature 38 DEG C is incubated 50min,
Process is lived with 100 DEG C of drying, enzyme denaturing, is obtained modified enzymolysis lignin after terminating, and crosses 60 mesh sieves standby after grinding；
Described pretreatment fluid comprises: the phytase of 0.3%, and described phytase is 5000u/g；0.5% laccase, described laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics is prepared:
According to weight fraction, take 20 parts of modified lignin resins, 80 parts of enzymolysis xylogens, be thoroughly mixed, take after drying
1.5g20Mpa compression molding, pressurize 20min, then vacuum high-temperature sintering had both obtained lignin ceramics finished product；
Described high temperature sintering is three-step approach:
Rise to 150 DEG C with the temperature of 15 DEG C/min, be incubated 30min；
Rise to 800 DEG C with the temperature of 8 DEG C/min, be incubated 50min；
It is down to less than 150 DEG C with the temperature of 10 DEG C/min.
Embodiment 2:
A kind of preparation technology of environmental protection lignin ceramics, step is as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Choose enzymolysis xylogen, can be purchased, it is also possible to prepare voluntarily, wherein content of lignin 80%, be crushed to 60 mesh
Standby；
According to parts by weight, taking 20 parts of enzymolysis xylogens, 25 parts of pretreatment fluid mix homogeneously, constant temperature 38 DEG C is incubated 60min,
Process is lived with 80 DEG C of drying, enzyme denaturing, is obtained modified enzymolysis lignin after terminating, and crosses 60 mesh sieves standby after grinding；
Described pretreatment fluid comprises: the phytase of 0.3%, and described phytase is 5000u/g；0.5% laccase, described laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics is prepared:
According to weight fraction, take 20 parts of modified lignin resins, 85 parts of enzymolysis xylogens, be thoroughly mixed, take after drying
1.5g20Mpa compression molding, pressurize 20min, then vacuum high-temperature sintering had both obtained lignin ceramics finished product；
Described high temperature sintering is three-step approach:
Rise to 150 DEG C with the temperature of 15 DEG C/min, be incubated 30min；
Rise to 800 DEG C with the temperature of 8 DEG C/min, be incubated 50min；
It is down to less than 150 DEG C with the temperature of 10 DEG C/min.
Embodiment 3:
A kind of preparation technology of environmental protection lignin ceramics, step is as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Choose enzymolysis xylogen, can be purchased, it is also possible to prepare voluntarily, wherein content of lignin 71%, be crushed to 60 mesh
Standby；
According to parts by weight, taking 24 parts of enzymolysis xylogens, 25 parts of pretreatment fluid mix homogeneously, constant temperature 38 DEG C is incubated 55min,
Process is lived with 95 DEG C of drying, enzyme denaturing, is obtained modified enzymolysis lignin after terminating, and crosses 60 mesh sieves standby after grinding；
Described pretreatment fluid comprises: the phytase of 0.3%, and described phytase is 5000u/g；0.5% laccase, described laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics is prepared:
According to weight fraction, take 20 parts of modified lignin resins, 81 parts of enzymolysis xylogens, be thoroughly mixed, take after drying
1.5g20Mpa compression molding, pressurize 20min, then vacuum high-temperature sintering had both obtained lignin ceramics finished product；
Described high temperature sintering is three-step approach:
Rise to 150 DEG C with the temperature of 15 DEG C/min, be incubated 30min；
Rise to 800 DEG C with the temperature of 8 DEG C/min, be incubated 50min；
It is down to less than 150 DEG C with the temperature of 10 DEG C/min.
Embodiment 4:
A kind of preparation technology of environmental protection lignin ceramics, step is as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Choose enzymolysis xylogen, can be purchased, it is also possible to prepare voluntarily, wherein content of lignin 79%, be crushed to 60 mesh
Standby；
According to parts by weight, taking 21 parts of enzymolysis xylogens, 25 parts of pretreatment fluid mix homogeneously, constant temperature 38 DEG C is incubated 53min,
Process is lived with 81 DEG C of drying, enzyme denaturing, is obtained modified enzymolysis lignin after terminating, and crosses 60 mesh sieves standby after grinding；
Described pretreatment fluid comprises: the phytase of 0.3%, and described phytase is 5000u/g；0.5% laccase, described laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics is prepared:
According to weight fraction, take 20 parts of modified lignin resins, 84 parts of enzymolysis xylogens, be thoroughly mixed, take after drying
1.5g20Mpa compression molding, pressurize 20min, then vacuum high-temperature sintering had both obtained lignin ceramics finished product；
Described high temperature sintering is three-step approach:
Rise to 150 DEG C with the temperature of 15 DEG C/min, be incubated 30min；
Rise to 800 DEG C with the temperature of 8 DEG C/min, be incubated 50min；
It is down to less than 150 DEG C with the temperature of 10 DEG C/min.
Embodiment 5:
A kind of preparation technology of environmental protection lignin ceramics, step is as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Choose enzymolysis xylogen, can be purchased, it is also possible to prepare voluntarily, wherein content of lignin 72%, be crushed to 60 mesh
Standby；
According to parts by weight, taking 23 parts of enzymolysis xylogens, 25 parts of pretreatment fluid mix homogeneously, constant temperature 38 DEG C is incubated 59min,
Process is lived with 87 DEG C of drying, enzyme denaturing, is obtained modified enzymolysis lignin after terminating, and crosses 60 mesh sieves standby after grinding；
Described pretreatment fluid comprises: the phytase of 0.3%, and described phytase is 5000u/g；0.5% laccase, described laccase
For 6000u/g；0.2% trehalose；0.3% citric acid, remaining is water；
(2) lignin ceramics is prepared:
According to weight fraction, take 20 parts of modified lignin resins, 82 parts of enzymolysis xylogens, be thoroughly mixed, take after drying
1.5g20Mpa compression molding, pressurize 20min, then vacuum high-temperature sintering had both obtained lignin ceramics finished product；
Described high temperature sintering is three-step approach:
Rise to 150 DEG C with the temperature of 15 DEG C/min, be incubated 30min；
Rise to 800 DEG C with the temperature of 8 DEG C/min, be incubated 50min；
It is down to less than 150 DEG C with the temperature of 10 DEG C/min.
Embodiment 6 contrast experiment:
The inventors discovered that, the when of being modified enzymolysis xylogen, the formula of pretreatment fluid is critically important, slightly deviation
Just can not get satisfied composite, following comparative example is only demonstration.
A kind of preparation technology of environmental protection lignin ceramics, step is as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
Choose enzymolysis xylogen, can be purchased, it is also possible to prepare voluntarily, wherein content of lignin 78%, be crushed to 60 mesh
Standby；
According to parts by weight, taking 22 parts of enzymolysis xylogens, 25 parts of pretreatment fluid mix homogeneously, constant temperature 38 DEG C is incubated 51min,
Process is lived with 99 DEG C of drying, enzyme denaturing, is obtained modified enzymolysis lignin after terminating, and crosses 60 mesh sieves standby after grinding；
Described pretreatment fluid comprises: the phytase of 0.5%, and described phytase is 5000u/g；0.2% trehalose；0.3%
Citric acid, remaining is water；
(2) lignin ceramics is prepared:
According to weight fraction, take 20 parts of modified lignin resins, 83 parts of enzymolysis xylogens, be thoroughly mixed, take after drying
1.5g20Mpa compression molding, pressurize 20min, then vacuum high-temperature sintering had both obtained lignin ceramics finished product；
Described high temperature sintering is three-step approach:
Rise to 150 DEG C with the temperature of 15 DEG C/min, be incubated 30min；
Rise to 800 DEG C with the temperature of 8 DEG C/min, be incubated 50min；
It is down to less than 150 DEG C with the temperature of 10 DEG C/min.
Embodiment 7 measure of merit:
The performance of the method mensuration lignin ceramics according to prior art:
Result is as shown in table 1 below:
As can be seen here, utilize environment-friendly and green technique that enzymolysis lignin is modified, then according to certain ratio and not changing
Property enzymolysis xylogen mixing, compression molding, high temperature sintering, prepared performance the most excellent wood pottery, its case hardness is the biggest.
Additionally, it was additionally observed that, the wood ceramics pore-size distribution that the present invention prepares is highly uniform.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, according to technical scheme and
Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.
Claims (5)
1. a preparation method for environmental protection lignin ceramics, step is as follows:
(1) enzymatic hydrolysis (EH) lignin modified:
According to parts by weight, take 20-25 part enzymolysis xylogen, 25 parts of pretreatment fluid mix homogeneously, constant temperature 38 DEG C insulation 50-
60min, process is lived with 80-100 DEG C of drying, enzyme denaturing, is obtained modified enzymolysis lignin after terminating, crosses 60 mesh sieves standby after grinding；
(2) lignin ceramics is prepared:
According to weight fraction, take 20 parts of modified lignin resins, 80-85 part enzymolysis xylogen, be thoroughly mixed, carry out mould after drying
Molded, then vacuum high-temperature sintering had both obtained lignin ceramics finished product.
2. the preparation method of the environmental protection lignin ceramics described in claim 1, it is characterised in that:
Choose enzymolysis xylogen, can be purchased, it is also possible to prepare voluntarily, wherein content of lignin 70-80%, be crushed to 60 mesh standby
With.
3. the preparation method of the environmental protection lignin ceramics described in claim 1 or 2, it is characterised in that:
Described pretreatment fluid comprises: the phytase of 0.3%, and described phytase is 5000u/g；0.5% laccase, described laccase is
6000u/g ；0.2% trehalose；0.3% citric acid, remaining is water.
4. the preparation method of the environmental protection lignin ceramics described in claim 1 or 2, it is characterised in that:
Described high temperature sintering use three-step approach:
Rise to 150 DEG C with the temperature of 15 DEG C/min, be incubated 30min；
Rise to 800 DEG C with the temperature of 8 DEG C/min, be incubated 50min；
It is down to less than 150 DEG C with the temperature of 10 DEG C/min.
5. the lignin ceramics that the preparation method described in claim 1-4 prepares.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093572A (en) * | 2019-04-30 | 2019-08-06 | 高玉梅 | A kind of preparation method of bend resistance foamed ceramics |
| 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 |
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 |
-
2016
- 2016-06-12 CN CN201610410585.3A patent/CN106045516B/en active Active
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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093572A (en) * | 2019-04-30 | 2019-08-06 | 高玉梅 | A kind of preparation method of bend resistance foamed ceramics |
| 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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Effective date of registration: 20191203 Address after: 535000 Wenchang industrial community, No.29, Wuma Road, Qinzhou City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi gulongxuan nixing pottery Co.,Ltd. Address before: No. 4-518, building 4, Asia International, Lihai, No. 9, Zhongjian Road, Qingxiu District, Nanning City, Guangxi Zhuang Autonomous Region Patentee before: Guangxi Future Department Enterprise Management Consulting Co.,Ltd. Effective date of registration: 20191203 Address after: No. 4-518, building 4, Asia International, Lihai, No. 9, Zhongjian Road, Qingxiu District, Nanning City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Future Department Enterprise Management Consulting Co.,Ltd. Address before: Room 1,020, Nanxun Science and Technology Pioneering Park, No. 666 Chaoyang Road, Nanxun District, Huzhou City, Zhejiang Province, 313000 Patentee before: Huzhou You Yan Intellectual Property Service Co.,Ltd. |