CN101786286A - Manufacturing method for modified enzymolysis lignin composite board - Google Patents
Manufacturing method for modified enzymolysis lignin composite board Download PDFInfo
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- CN101786286A CN101786286A CN 201010150846 CN201010150846A CN101786286A CN 101786286 A CN101786286 A CN 101786286A CN 201010150846 CN201010150846 CN 201010150846 CN 201010150846 A CN201010150846 A CN 201010150846A CN 101786286 A CN101786286 A CN 101786286A
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Abstract
The invention discloses a manufacturing method for a modified enzymolysis lignin composite board, relating to a manufacturing method for a composite board, and solving the problems of polluting environment and having toxicity to human body caused by taking penolic resin as the adhesive to manufacture composite boards. The method comprises the following steps: 1, stirring enzymolysis lignin and sodium hydroxide water solution for reaction, adding formaldehyde, and lowering the temperature after reaction to obtain modified enzymolysis lignin; 2, evenly stirring and mixing the modified enzymolysis lignin with paper industry lignin or the enzymolysis lignin, drying, paving in a mould, and pressing to obtain a molding green body; and 3, placing the molding green body in a hot press, maintaining pressure and then lowering the temperature to obtain the modified enzymolysis lignin composite board. In the invention, phenolic resin does not need to be used as the adhesive, and phenol from petrochemical industry does not need to be consumed too, thereby lowering the production cost by 40%-50%, having no environmental pollution, avoiding toxicity of the phenol to human body, and having low raw material cost, excellent product performance and simple production process.
Description
Technical field
The present invention relates to a kind of manufacture method of composite plate.
Background technology
With timber is raw material, with phenolic resins is adhesive, through applying glue, technologies such as hot-forming processing are made composite plate, but phenolic resins synthesis material phenol source petrochemical industry, along with the petroleum resources crisis has become the human focus of paying close attention to, oil price rises for one liter again, cause phenol to cost an arm and a leg, phenol meeting simultaneously, bring pollution to environment, and (as: can be inhaled into human body is poisonous, eat or absorb, to skin through skin, mucous membrane has strong corrosiveness, can suppress nervous centralis or infringement liver, renal function sucks the high concentration steam and can cause headache, dizzy, weak, blurred vision, pulmonary edema etc.; Wrongly take and cause that alimentary canal burns, burning pain occurs, exhalation band of gas phenol flavor, vomitus or stool can be with blood, and the possibility of gastric-intestinal perforation is arranged, and shock, pulmonary edema, liver or renal damage can occur, acute renal failure occurs, can die from respiratory failure; The eye contact can cause burns; Can absorb through skin ambustion, after certain incubation period, cause acute renal failure), and synthetic phenolic resins has free phenol to exist, so in the process of making composite plate, can bring injury to human body.
Because fossil resource crises such as oil; with reproducible plant resources is that raw material production alcohol fuel has obtained developing rapidly; yet when cellulose, hemicellulose obtain utilizing, produced a large amount of lignin residue, this part resource is not utilized effectively as yet.Research about the utilization of fuel ethanol production residue lignin at present needs to prepare macromolecular material after the refinement treatment more, trivial operations, and utilization rate is low.
Summary of the invention
The present invention seeks in order to solve with phenolic resins is that adhesive is made composite plate and had contaminated environment, the problem poisonous to human body, and a kind of manufacture method of modified enzymolysis lignin composite board is provided.
The manufacture method of modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 10～200: 1 joins enzymolysis xylogen and sodium hydrate aqueous solution in the reactor, at 30～65 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind reaction 0.5h～5h down at 50～100 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 0.4～4 and mix, to be dried to moisture content then under 20～105 ℃ be below 15% and be paved in the mould, presses down in the condition of 1～10MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 150～250 ℃ conditions and press 5～20min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 2～50: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
The manufacture method of modified enzymolysis lignin composite board of the present invention is different with the manufacture method of common composite plate, common composite plate is that wood materials hot-press solidifying after resin impregnating processing, drying is formed, modified enzymolysis lignin composite board of the present invention is to be base stock with the enzymolysis xylogen powder, need not phenolic resins is adhesive, behind mould molding, drying hot pressing forms again, need not to consume the phenol that derives from petrochemical industry, production cost reduces by 40%～50%, the free from environmental pollution and murder by poisoning of having avoided phenol to bring to human body; Used enzymolysis xylogen powder among the present invention, from the residue lignin in the alcohol fuel fermentation production process (also being called enzymolysis xylogen), it is reserve quality phenols structure originally more, and its basic structural unit is similar to phenol structure; Cost of material of the present invention is low, and product has good performance, and production technology is simple.
The specific embodiment
The specific embodiment one: the manufacture method of present embodiment modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 10～200: 1 joins enzymolysis xylogen and sodium hydrate aqueous solution in the reactor, at 30～65 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind reaction 0.5h～5h down at 50～100 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 0.4～4 and mix, to be dried to moisture content then under 20～105 ℃ be below 15% and be paved in the mould, presses down in the condition of 1～10MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 150～250 ℃ conditions and press 5～20min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 2～50: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
Enzymolysis xylogen is for the string being the residual lignin after fermenting raw materials is produced alcohol fuel in the present embodiment.
The specific embodiment two: present embodiment and the specific embodiment one are different be in the step 1 by mass ratio 20～180: 1 joins enzymolysis xylogen and sodium hydrate aqueous solution in the reactor, at 35～60 ℃ of following stirring reaction 10min.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: present embodiment and the specific embodiment one are different is by mass ratio 80: 1 enzymolysis xylogen and sodium hydrate aqueous solution to be joined in the reactor in the step 1, at 45 ℃ of following stirring reaction 10min.Other step and parameter are identical with the specific embodiment one.
The specific embodiment four: present embodiment and the specific embodiment one are different is by mass ratio 120: 1 enzymolysis xylogen and sodium hydrate aqueous solution to be joined in the reactor in the step 1, at 55 ℃ of following stirring reaction 10min.Other step and parameter are identical with the specific embodiment one.
The specific embodiment five: present embodiment and the specific embodiment one are different is by mass ratio 10: 1 enzymolysis xylogen and sodium hydrate aqueous solution to be joined in the reactor in the step 1, at 30 ℃ of following stirring reaction 10min.Other step and parameter are identical with the specific embodiment one.
The specific embodiment six: present embodiment and the specific embodiment one are different is by mass ratio 200: 1 enzymolysis xylogen and sodium hydrate aqueous solution to be joined in the reactor in the step 1, at 65 ℃ of following stirring reaction 10min.Other step and parameter are identical with the specific embodiment one.
The specific embodiment seven: what present embodiment was different with one of specific embodiment one to six is to lower the temperature behind reaction 2h～4h down at 70～95 ℃ in the step 1.Other step and parameter are identical with one of specific embodiment one to six.
The specific embodiment eight: what present embodiment was different with one of specific embodiment one to six is to lower the temperature behind the reaction 2h down at 85 ℃ in the step 1.Other step and parameter are identical with one of specific embodiment one to six.
The specific embodiment nine: present embodiment and the specific embodiment eight are different is to join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 0.5～3.5 in the step 2 and mix.Other step and parameter are identical with the specific embodiment eight.
The specific embodiment ten: present embodiment and the specific embodiment eight are different is to join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 1～3 in the step 2 and mix.Other step and parameter are identical with the specific embodiment eight.
The specific embodiment 11: present embodiment and the specific embodiment eight are different is to join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 2 in the step 2 and mix.Other step and parameter are identical with the specific embodiment eight.
The specific embodiment 12: what present embodiment was different with one of specific embodiment nine to 11 is that the paper industry lignin is sulfate lignin, alkali lignin or lignosulfonates in the step 2.Other step and parameter are identical with one of specific embodiment nine to 11.
The specific embodiment 13: what present embodiment and the specific embodiment 12 were different is to mix employing in the step 2 directly to mix under pulverulence; Perhaps adopt and mix after adding entry, water is 1: 0.5～5 amount adding by the volume ratio of lignin in the reactor and water.Other step and parameter are identical with the specific embodiment 12.
Lignin is for pressing mass ratio 1: 0～10 mixing modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the present embodiment reactor.
The specific embodiment 14: present embodiment and the specific embodiment 13 are different is that to be dried to moisture content in the step 2 under 30～90 ℃ be 10%.Other step and parameter are identical with the specific embodiment 13.
The specific embodiment 15: present embodiment and the specific embodiment 13 are different is that to be dried to moisture content in the step 2 under 85 ℃ be 6%.Other step and parameter are identical with the specific embodiment 13.
The specific embodiment 16: present embodiment is different with the specific embodiment 14 or 15 is to press down in the condition of 2～8MPa in the step 2 to make molding blank.Other step and parameter are identical with the specific embodiment 14 or 15.
The specific embodiment 17: present embodiment is different with the specific embodiment 14 or 15 is to press down in the condition of 5MPa in the step 2 to make molding blank.Other step and parameter are identical with the specific embodiment 14 or 15.
The specific embodiment 18: present embodiment and the specific embodiment 17 are different is to press down organizational security 150 ℃ condition in the step 3 to press 20min.Other step and parameter are identical with the specific embodiment 17.
The specific embodiment 19: present embodiment and the specific embodiment 17 are different is to press down organizational security 250 ℃ condition in the step 3 to press 5min.Other step and parameter are identical with the specific embodiment 17.
The specific embodiment 20: present embodiment and the specific embodiment 17 are different is to press down organizational security 200 ℃ condition in the step 3 to press 100min.Other step and parameter are identical with the specific embodiment 17.
The specific embodiment 21: the manufacture method of present embodiment modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 200: 1 enzymolysis xylogen and sodium hydrate aqueous solution are joined in the reactor, at 65 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind the reaction 2h down at 80 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 1 and mix, to be dried to moisture content then under 80 ℃ be 4% and be paved in the mould, presses down in the condition of 3MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 180 ℃ conditions and press 8min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 20: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
Need not phenolic resins in the present embodiment is adhesive with phenolic resins, does not consume phenol, and production cost reduces by 50%, the free from environmental pollution and murder by poisoning of having avoided phenol to bring to human body.
The maximum load of gained modified enzymolysis lignin composite board reaches 121N in the present embodiment, and bending strength reaches 23.35MPa, and elastic modelling quantity reaches 3.78GPa; Immersion 24h thickness swelling rate is 10%, and moisture absorption (65%RH) thickness swelling is 0.6854%, and visible gained modified enzymolysis lignin composite board has good performance.
The specific embodiment 22: the manufacture method of present embodiment modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 50: 1 enzymolysis xylogen and sodium hydrate aqueous solution are joined in the reactor, at 55 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind the reaction 0.5h down at 100 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 1.5 and mix, to be dried to moisture content then under 100 ℃ be 3% and be paved in the mould, presses down in the condition of 5MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 175 ℃ conditions and press 10min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 3: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
The maximum load of gained modified enzymolysis lignin composite board reaches 156.8N in the present embodiment, and bending strength reaches 27.62MPa, and elastic modelling quantity reaches 4.48GPa; Immersion 24h thickness swelling rate is 11%, and moisture absorption (65%RH) thickness swelling is 0.6786%, and visible gained modified enzymolysis lignin composite board has good performance.
The specific embodiment 23: the manufacture method of present embodiment modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 30: 1 enzymolysis xylogen and sodium hydrate aqueous solution are joined in the reactor, at 30 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind the reaction 4h down at 70 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 4 and mix, to be dried to moisture content then under 100 ℃ be 8% and be paved in the mould, presses down in the condition of 2MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 170 ℃ conditions and press 8min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 40: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
The maximum load of gained modified enzymolysis lignin composite board reaches 32.6N in the present embodiment, and bending strength reaches 3.455MPa, and elastic modelling quantity reaches 0.57GPa; Immersion 24h thickness swelling rate is 14%, and moisture absorption (65%RH) thickness swelling is 0.4306%, and visible gained modified enzymolysis lignin composite board has good performance.
The specific embodiment 24: the manufacture method of present embodiment modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 20: 1 enzymolysis xylogen and sodium hydrate aqueous solution are joined in the reactor, at 35 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind the reaction 2h down at 85 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 0.5 and mix, to be dried to moisture content then under 40 ℃ be 5% and be paved in the mould, presses down in the condition of 2MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 180 ℃ conditions and press 7min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 12: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
The maximum load of gained modified enzymolysis lignin composite board reaches 108.6N in the present embodiment, and bending strength reaches 22.97MPa, and elastic modelling quantity reaches 3.35GPa; Immersion 24h thickness swelling rate is 6%, and moisture absorption (65%RH) thickness swelling is 0.4258%, and visible gained modified enzymolysis lignin composite board has good performance.
The specific embodiment 25: the manufacture method of present embodiment modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 100: 1 enzymolysis xylogen and sodium hydrate aqueous solution are joined in the reactor, at 65 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind the reaction 2h down at 80 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 3 and mix, to be dried to moisture content then under 80 ℃ be 4% and be paved in the mould, presses down in the condition of 3MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 175 ℃ conditions and press 15min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 30: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
The maximum load of gained modified enzymolysis lignin composite board reaches 23N in the present embodiment, and bending strength reaches 2.482MPa, and elastic modelling quantity reaches 0.68GPa; Immersion 24h thickness swelling rate is 11%, and moisture absorption (65%RH) thickness swelling is 0.5033%, and visible gained modified enzymolysis lignin composite board has good performance.
The specific embodiment 26: the manufacture method of present embodiment modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 15: 1 enzymolysis xylogen and sodium hydrate aqueous solution are joined in the reactor, at 65 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind the reaction 3h down at 90 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 0.5 and mix, to be dried to moisture content then under 80 ℃ be 3% and be paved in the mould, presses down in the condition of 4MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 190 ℃ conditions and press 12min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 6: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
The maximum load of gained modified enzymolysis lignin composite board reaches 24.8N in the present embodiment, and bending strength reaches 2.519MPa, and elastic modelling quantity reaches 0.318GPa; Immersion 24h thickness swelling rate is 8%, and moisture absorption (65%RH) thickness swelling is 0.4825%, and visible gained modified enzymolysis lignin composite board has good performance.
Claims (10)
1. the manufacture method of a modified enzymolysis lignin composite board, the manufacture method that it is characterized in that modified enzymolysis lignin composite board is carried out according to the following steps: one, by mass ratio 10～200: 1 joins enzymolysis xylogen and sodium hydrate aqueous solution in the reactor, at 30～65 ℃ of following stirring reaction 10min, add mass concentration then and be 37% formaldehyde, lower the temperature behind reaction 0.5h～5h down at 50～100 ℃, get modified enzymolysis lignin; Two, join modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor by mass ratio 1: 0.4～4 and mix, to be dried to moisture content then under 20～105 ℃ be below 15% and be paved in the mould, presses down in the condition of 1～10MPa and make molding blank; Three, molding blank is placed hot press, press down organizational security 150～250 ℃ conditions and press 5～20min, cooling promptly gets modified enzymolysis lignin composite board then; Wherein formaldehyde is that 2～50: 1 amount adds according to the mass ratio of enzymolysis xylogen and formaldehyde in the step 1.
2. the manufacture method of modified enzymolysis lignin composite board according to claim 1 is characterized in that in the step 1 by mass ratio 80: 1 enzymolysis xylogen and sodium hydrate aqueous solution being joined in the reactor, at 45 ℃ of following stirring reaction 10min.
3. the manufacture method of modified enzymolysis lignin composite board according to claim 1 and 2 is characterized in that lowering the temperature behind reaction 2h～4h down at 70～95 ℃ in the step 1.
4. the manufacture method of modified enzymolysis lignin composite board according to claim 3 is characterized in that in the step 2 joining modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor and mixing by mass ratio 1: 0.5～3.5.
5. the manufacture method of modified enzymolysis lignin composite board according to claim 3 is characterized in that in the step 2 joining modified enzymolysis lignin and paper industry lignin or enzymolysis xylogen in the reactor and mixing by mass ratio 1: 1～3.
6. according to the manufacture method of claim 4 or 5 described modified enzymolysis lignin composite boards, it is characterized in that the paper industry lignin is sulfate lignin, alkali lignin or lignosulfonates in the step 2.
7. the manufacture method of modified enzymolysis lignin composite board according to claim 6 is characterized in that mixing in the step 2 employing and directly mixes under pulverulence; Perhaps adopt and mix after adding entry, water is 1: 0.5～5 amount adding by the volume ratio of lignin in the reactor and water.
8. the manufacture method of modified enzymolysis lignin composite board according to claim 7, the condition at 2～8MPa of it is characterized in that in the step 2 presses down and makes molding blank.
9. the manufacture method of modified enzymolysis lignin composite board according to claim 7, the condition at 5MPa of it is characterized in that in the step 2 presses down and makes molding blank.
10. according to Claim 8 or the manufacture method of 9 described modified enzymolysis lignin composite boards, it is characterized in that in the step 3 that pressing down organizational security 200 ℃ condition presses 100min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102051002A (en) * | 2010-12-02 | 2011-05-11 | 东北林业大学 | Zymolytic lignin-wood fiber-polyolefin hybrid composite material and preparation method thereof |
| CN104097247A (en) * | 2014-07-23 | 2014-10-15 | 浙江农林大学 | Self-cleaning environment-friendly bamboo particle board and method for manufacturing same |
| CN104497606A (en) * | 2014-12-03 | 2015-04-08 | 松原光禾能源有限公司 | Preparation method of lignin thermoplastic material |
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| JPH0734396A (en) * | 1993-07-15 | 1995-02-03 | Nippon Paper Ind Co Ltd | Base paper for laminated sheet |
| WO2003047826A1 (en) * | 2001-12-03 | 2003-06-12 | Dynea Chemicals Oy | Method of producing compressed layered structures |
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| CN102051002A (en) * | 2010-12-02 | 2011-05-11 | 东北林业大学 | Zymolytic lignin-wood fiber-polyolefin hybrid composite material and preparation method thereof |
| CN104097247A (en) * | 2014-07-23 | 2014-10-15 | 浙江农林大学 | Self-cleaning environment-friendly bamboo particle board and method for manufacturing same |
| CN104097247B (en) * | 2014-07-23 | 2016-08-17 | 浙江农林大学 | A kind of automatically cleaning Environmental-protection bamboo flakeboard and preparation method thereof |
| CN104497606A (en) * | 2014-12-03 | 2015-04-08 | 松原光禾能源有限公司 | Preparation method of lignin thermoplastic material |
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