CN101108772A - Method for manufacturing xylogen ceramic - Google Patents
Method for manufacturing xylogen ceramic Download PDFInfo
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- CN101108772A CN101108772A CNA2006100103037A CN200610010303A CN101108772A CN 101108772 A CN101108772 A CN 101108772A CN A2006100103037 A CNA2006100103037 A CN A2006100103037A CN 200610010303 A CN200610010303 A CN 200610010303A CN 101108772 A CN101108772 A CN 101108772A
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Abstract
A production method of the lignin ceramics is provided, which relates to the production process of the wooden ceramics. The objective of the invention is to provide a wooden ceramics production method with the industrial lignin as the raw material and with simple method and higher product intensity. The detailed process is that: (I) resin soakage: the lignin is completely soaked via the phenolic resin soakage process and is dried until the water content is below 15 per cent; (II) compression molding: the lignin powder after soaked by phenolic resin and dried is laid in the mould to compress into molding; (III) vacuum or nitrogen protective sintering to gain the lignin ceramics with higher intensity. The invention has low raw material cost, product with excellent mechanical strength and simple production process.
Description
Technical field
The present invention relates to a kind of manufacturing process of wood pottery, particularly relating to a kind of is raw material with the industrial lignin, the simple and higher wooden ceramic process of product strength of method.
Background technology
Along with the attention of people to environment, the novel ecological environmentally conscious materials becomes the focus that common people pay close attention to.Utilize discarded reproducible Biological resources to prepare high performance novel material, gradually reduce the consumption of Nonrenewable resources, environment is significant for preserving our planet.The wood pottery just is based on the thought of " utilizing discarded recyclable materials, creation high-performance novel material " and a kind of novel charcoal material of developing.The wood pottery is that Japanese scholar Gang portion quick great (Toshihiro Okabe) equals the nineteen ninety proposition, with the wood materials novel porous raw material of wood-charcoal material that high temperature sintering forms under vacuum (or nitrogen protection) behind resin impregnating processing, dry solidification.The prices of raw and semifnished materials are cheap, wide material sources, waste paper, waste wood etc. all can be used as its raw material, there is not environmental pollution in the processing and manufacturing process, and ratio of strength to weight height has excellent characteristic at aspects such as mechanics, calorifics, electromagnetism and tribology, can be widely used as electrode, heating element, motor carbon, brake lining, corrosion resistant material, thermal insulation material, filtering material etc. after processing, be the ideal substitute of some non-renewable material of 21 century, have broad application prospects.
Just because of wooden pottery is a kind of novel material that possesses multiple excellent properties that efficiently utilizes timber " three surplus things " to make, caused in recent years that the scientific research personnel more and more paid attention to, as: it is raw material with five-ply board that the Ma Rong of Xi'an Communications University etc. once adopted kahikatea, birch, Qinggang wood, the impregnated phenolic resin ethanolic soln, behind resin solidification, put into vacuum oven, at N
2Speed with 5 ℃/min in the protective atmosphere is warming up to preset temperature respectively, and furnace cooling makes the wood pottery behind the insulation 4h.According to its result of study, the wooden ceramic performance of different seeds exists than big-difference.The various performances of sample generally occur about 400 ℃～600 ℃ than large turn, and minimum as density, intensity, hardness, void content is the highest, and from then on the decline of resistivity slow down.Physics, chemical transformation that this and timber and resin cause at this temperature range generation vigorous reaction are corresponding to.After surpassing this temperature, every performance all will tend towards stability.He thinks, dipping can improve the performance of wood pottery effectively, but performances such as flexural strength, Vickers' hardness have abnormal phenomena, and illustrate after resin adds has two-way influence, that is: resin is to filling and the sealing of pore and deposit, strengthen to fix and limitation impairs and depositing.Be embodied in: because of producing, eliminating sealed porosity, influenced density, thereby weakened sample intensity, increased generation of defects.The Wu Wentao of HeFei University of Technology etc. are raw material with bagasse, adopt and mix the prepared wood pottery that back hot pressing is reburned and tied, and performances such as its density, void content, intensity, resistivity are tested, its performance characteristic, formation mechanism and rule are analyzed, tentatively showed the influence of parameters such as proportioning raw materials, resol concentration, temperature to whole process of preparation and wooden ceramic performance, experimental result has proved by the feasibility of this technology with bagasse preparation wood pottery.The virtuous clear grade of thanking of Shanghai Communications University was once studied wooden ceramic morphological specificity and damping property, and relation between the two, and wooden pottery has bigger damping value, and was bigger when amplitude and vibrational frequency are higher.The applicant had once carried out serial research at manufacturing process, wooden Standpoint of Ceramic Wear-resisting Function and the mechanical strength of wood pottery and the pore texture of wood pottery etc.The resin impregnating wood materials is adopted in research, makes wooden ceramic product through high temperature sintering, and it is bigger that product yield, performance and raw material of wood-charcoal material composition etc. are influenced by resin concentration and sintering temperature.Analyze the ceramic pore texture of wood by low-temperature nitrogen adsorption method, find that common carbide sample adsorptive power is very poor, resol is treated to carbide and introduces more micropore, and adsorptive power improves.Observe by scanning electronic microscope (SEM), resol has swollen, filling effect to wood cell wall, thereby strengthens cell walls, and a lot of resins are filled in the staggered interfibrous space, have strengthened fiber and have combined with interfibrous.
The Japan scholar is after having proved that wooden pottery has characteristic such as excellent wear-resisting, electromagnetic shielding, research begins to turn to wood pottery some relevant natures in application process, as Takahiro Fujino etc. studied 100～800 ℃ and pressure up to the condition of 100MPa under the behavior and the stability of carbonized wood material during hot-water cure, studies show that, because the erosion of high temperature and hot water, wood materials has shown tangible weight loss, and more than 500 ℃, sample corrodes more serious.Yasuko Oishi etc. has also studied the thermal properties of wooden pottery under different oxygen concentrations.In addition, in order to obtain more eco-friendly wood pottery, Takashi Hirose etc. replace resin impregnating waste wood material with liquefaction timber, and have studied the influence to this wood pottery chemical structure of carbonization temperature and charing speed.
Industrial lignin is the byproduct of pulping and paper-making, and recovery utilization rate is not high at present, and most of with discharge of wastewater, both contaminate environment was wasted resource again.The recycling of industrial lignin has great economy, society and environmental benefit.Realize the resource ecology utilization of industrial lignin, technological innovation is most important condition.Though industrial lignin has been obtained certain progress as the research of aspects such as cement water reducing agent, water conditioner, coal water slurry dispersing agent with using after by modification,, according to estimates, 1 ton of paper of every production, the 0.5 ton of xylogen of just having an appointment is discharged.Principal pollutant in China's paper waste are xylogen, and contaminated wastewater accounts for 30% of national amount of industrial wastewater.So the development and use of industrial lignin are extremely urgent.How sufficiently and reasonably to utilize wooden waste, the material and the product of creation high-performance, high added value are that pendulum is in the previous problem demanding prompt solution of China timber scientific worker face.New way has been opened up in the development of lignin ceramics and the efficient utilization that is developed as the industrial lignin waste material, to promoting further developing of composite science, promotes the efficient utilization of timber and realize environment protection all will have positive meaning.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with the industrial lignin, the simple and higher wooden process for preparing ceramic of product strength of method.
The manufacture method of lignin ceramics of the present invention is:
(1) resin impregnation: xylogen is that 5%～50% resin impregnating is handled to soaking into fully through massfraction, and to be dried to water ratio be below 15%;
(2) compression molding: resin impregnating and dried xylogen powder are paved in the mould, at 120 ℃～200 ℃, compression moulding under the condition of 1MPa～20Mpa;
(3) sintering:
A, vacuum sintering: the sample of moulding is put into vacuum sintering furnace, be evacuated to absolute pressure below 104Pa, be heated to more than 600 ℃, keep 0h～3h with the average heating speed that is no more than 10 ℃/min, cooling promptly obtains the higher lignin ceramics of intensity then.
B, nitrogen protective sintering: the work in-process of moulding are put into sintering oven, charge into nitrogen, pressure is normal pressure; Average heating speed with 1 ℃/min～10 ℃/min is heated to 600 ℃～2500 ℃ then, keeps 0h～3h, and cooling promptly obtains the higher lignin ceramics of intensity then.
The manufacture method of the manufacture method of lignin ceramics of the present invention and normal wood pottery is different.The normal wood pottery is with the wood materials novel porous raw material of wood-charcoal material that high temperature sintering forms under vacuum (or nitrogen protection) behind resin impregnating processing, dry solidification.Lignin ceramics of the present invention is a basic raw material with the industrial lignin powder, handles through resin impregnating, uses the mould heat pressure moulding then, forms through high temperature sintering again.Raw materials cost of the present invention is low, and product has excellent mechanical strength, and production technique is simple.
Embodiment
Embodiment one: present embodiment is made lignin ceramics according to following steps:
The first step: resin impregnation.Xylogen is that 5%～50% resin impregnating is handled to soaking into fully through massfraction, and to be dried to water ratio be below 15%, thereby has guaranteed even dipping.
Second step: compression molding.Resin impregnating and dry back powder are paved in the mould, at 120 ℃～200 ℃, compression moulding under the condition of 1MPa～20Mpa.
The 3rd step: modified drying.Slab is through after the hot pressing, still there is moisture gradient in plank inside, plank is bigger with the extraneous temperature difference, so thermal stress distribution inequality of plate, after placing for some time, be very easy to warpage, so need after the hot pressing to be placed under the horizontal wet environment of constant temperature and carry out modifier treatment, and push down with certain weight, to guarantee the smooth of product.Through after the modifier treatment, need be placed in 120 ℃ the constant temperature air dry oven and carry out drying.
The 4th step: vacuum sintering.Earlier the sample of moulding is put into vacuum sintering furnace, be evacuated to absolute pressure 10
4Below the Pa, be heated to more than 600 ℃, keep 0h～3h, then cooling with the average heating speed that is no more than 10 ℃/min.Have a large amount of gases to emit in sintering process, vacuum tightness descends, and needs vacuum pump work to keep vacuum.
Used xylogen can be various industrial lignins in the present embodiment, as vitriol xylogen, alkali lignin (soda processes xylogen, other alkali lignins) or sulfonated lignin.
Embodiment two: what present embodiment and embodiment one were different is that the 4th step was nitrogen protective sintering: the work in-process of moulding are put into sintering oven, charge into nitrogen, pressure is normal pressure; All be heated to 600 ℃～2500 ℃ again, keep 0h～3h with the average heating speed of 1 ℃/min～1 0 ℃/min, cooling then, lignin ceramics is promptly strengthened.
Embodiment three: with the vitriol xylogen is raw material, when according to xylogen: when resol is 4: 1 proportionings, xylogen is carried out resin impregnation handle to soaking into fully, being dried to water ratio is 12%, mat formation hot pressing 20min under 180 ℃, 15.0Mpa.Modified, oven dry are put into vacuum sintering furnace with the sample of moulding, are evacuated to absolute pressure 10
4Below the Pa, starting temperature is 24 ℃, rises to 120 ℃ with the speed of 10 ℃/min, keeps after the 10min, rises to 600 ℃ with the speed of 2 ℃/min, keeps 3h, and cooling naturally then must finished product.The compression shear strength of product reaches 22Mpa, and criticizes powder and resol is raw material with 3: 7 wood, only is 11MPa at the compression shear strengths of 800 ℃ of following sintering gained wood potteries.
Embodiment four: with the soda processes xylogen is raw material, and when according to xylogen: when resol is 3: 1 proportionings, xylogen is carried out resin impregnation handle to soaking into fully, being dried to water ratio is 5%, mats formation hot pressing 30min under 150 ℃, 10.0Mpa.Modified, oven dry are put into vacuum sintering furnace with the sample of moulding, are evacuated to absolute pressure 10
4Below the Pa, starting temperature is 24 ℃, rises to 120 ℃ with the speed of 15 ℃/min, keeps after the 20min, rises to 800 ℃ with the speed of 1 ℃/min, keeps 1h, and cooling naturally then must finished product.The compression shear strength of product reaches 36Mpa.
Embodiment five: with the vitriol xylogen is raw material, and when according to xylogen: when resol is 2: 1 proportionings, xylogen is carried out resin impregnation handle to soaking into fully, being dried to water ratio is 2%, mats formation hot pressing 50min under 120 ℃, 10.0Mpa.Modified, oven dry are put into vacuum sintering furnace with the sample of moulding, are evacuated to absolute pressure 10
4Below the Pa, starting temperature is a room temperature ℃, rises to 120 ℃ with the speed of 12 ℃/min, keeps after the 10min, rises to 700 ℃ with the speed of 1.5 ℃/min, keeps 2h, and cooling naturally then must finished product.The compression shear strength of product reaches 36Mpa.
Embodiment six: with the industrial soda xylogen is raw material, when according to xylogen: when resol is 1.33: 1 proportionings, xylogen is carried out resin impregnation handle to soaking into fully, being dried to water ratio is 10%, mat formation hot pressing 30min under 150 ℃, 10.0Mpa.Modified, oven dry are put into vacuum sintering furnace with the sample of moulding, are evacuated to absolute pressure 10
4Below the Pa, starting temperature is 24 ℃, rises to 120 ℃ with the speed of 5 ℃/min, keeps after the 30min, rises to 800 ℃ with the speed of 0.5 ℃/min, keeps 1h, and cooling naturally then must finished product.The compression shear strength of product reaches 38Mpa.
Claims (4)
1. the manufacture method of a lignin ceramics is characterized in that described method is:
(1) resin impregnation: xylogen is that 5%～50% resin impregnating is handled to soaking into fully through massfraction, and to be dried to water ratio be below 15%;
(2) compression molding: resin impregnating and dried xylogen powder are paved in the mould, at 120 ℃～200 ℃, compression moulding under the condition of 1MPa～20Mpa;
(3) vacuum sintering: the sample of moulding is put into vacuum sintering furnace, be evacuated to absolute pressure 10
4Below the Pa, be heated to more than 600 ℃ with the average heating speed that is no more than 10 ℃/min, keep 0h～3h, cooling promptly obtains the higher lignin ceramics of intensity then.
2. the manufacture method of a kind of lignin ceramics according to claim 1 is characterized in that described xylogen is vitriol xylogen, alkali lignin or sulfonated lignin.
3. the manufacture method of a lignin ceramics is characterized in that described method is:
(1) resin impregnation: xylogen is that 5%～50% resin impregnating is handled to soaking into fully through massfraction, and to be dried to water ratio be below 15%;
(2) compression molding: resin impregnating and dried xylogen powder are paved in the mould, at 120 ℃～200 ℃, compression moulding under the condition of 1MPa～20Mpa;
(3) nitrogen protective sintering: the work in-process of moulding are put into sintering oven, charge into nitrogen, pressure is normal pressure; Average heating speed with 1 ℃/min～10 ℃/min is heated to 600 ℃～2500 ℃ then, keeps 0h～3h, and cooling promptly obtains the higher lignin ceramics of intensity then.
4. the manufacture method of a kind of lignin ceramics according to claim 3 is characterized in that described xylogen is vitriol xylogen, alkali lignin or sulfonated lignin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2006100103037A CN101108772A (en) | 2006-07-20 | 2006-07-20 | Method for manufacturing xylogen ceramic |
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| CNA2006100103037A CN101108772A (en) | 2006-07-20 | 2006-07-20 | Method for manufacturing xylogen ceramic |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941071A (en) * | 2010-09-03 | 2011-01-12 | 江苏大学 | Method for preparing metallized wood ceramics based on bagasse |
| CN102139500A (en) * | 2010-02-01 | 2011-08-03 | 仇峰 | Plasticizing wood and manufacturing method thereof |
| CN102584187A (en) * | 2012-01-16 | 2012-07-18 | 芜湖市天地电子科技有限公司 | High-boron tube and preparation method thereof |
| CN101698604B (en) * | 2009-11-03 | 2013-06-12 | 东北林业大学 | Method for manufacturing enzymatic hydrolysis lignin ceramics |
| CN101838148B (en) * | 2010-02-09 | 2013-11-06 | 西安工程大学 | Method for preparing corn-cob structure morph-genetic ceramic-based composite material |
| CN107778020A (en) * | 2017-11-21 | 2018-03-09 | 北京林业大学 | A kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics |
| CN107778013A (en) * | 2017-11-21 | 2018-03-09 | 北京林业大学 | A kind of preparation method of lignin-base silicon carbide woodceramics base substrate |
| CN107879757A (en) * | 2017-11-21 | 2018-04-06 | 北京林业大学 | A kind of preparation method of toughness reinforcing lignin-base silicon carbide woodceramics base substrate |
| CN107903062A (en) * | 2017-11-21 | 2018-04-13 | 北京林业大学 | A kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin |
| CN107915487A (en) * | 2017-11-21 | 2018-04-17 | 北京林业大学 | A kind of method for preparing porous wood ceramics using phenolic resin and industrial alkali lignin |
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2006
- 2006-07-20 CN CNA2006100103037A patent/CN101108772A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698604B (en) * | 2009-11-03 | 2013-06-12 | 东北林业大学 | Method for manufacturing enzymatic hydrolysis lignin ceramics |
| CN102139500A (en) * | 2010-02-01 | 2011-08-03 | 仇峰 | Plasticizing wood and manufacturing method thereof |
| CN102139500B (en) * | 2010-02-01 | 2013-05-29 | 仇峰 | Manufacturing method of plasticizing wood |
| CN101838148B (en) * | 2010-02-09 | 2013-11-06 | 西安工程大学 | Method for preparing corn-cob structure morph-genetic ceramic-based composite material |
| CN101941071A (en) * | 2010-09-03 | 2011-01-12 | 江苏大学 | Method for preparing metallized wood ceramics based on bagasse |
| CN102584187A (en) * | 2012-01-16 | 2012-07-18 | 芜湖市天地电子科技有限公司 | High-boron tube and preparation method thereof |
| CN102584187B (en) * | 2012-01-16 | 2013-10-16 | 芜湖市天地电子科技有限公司 | High-boron tube and preparation method thereof |
| CN107778020A (en) * | 2017-11-21 | 2018-03-09 | 北京林业大学 | A kind of method of carbon fiber-reinforced epoxy resin-matrix industry alkali lignin wood ceramics |
| CN107778013A (en) * | 2017-11-21 | 2018-03-09 | 北京林业大学 | A kind of preparation method of lignin-base silicon carbide woodceramics base substrate |
| CN107879757A (en) * | 2017-11-21 | 2018-04-06 | 北京林业大学 | A kind of preparation method of toughness reinforcing lignin-base silicon carbide woodceramics base substrate |
| CN107903062A (en) * | 2017-11-21 | 2018-04-13 | 北京林业大学 | A kind of method for preparing wood ceramics using epoxy resin and industrial alkali lignin |
| CN107915487A (en) * | 2017-11-21 | 2018-04-17 | 北京林业大学 | A kind of method for preparing porous wood ceramics using phenolic resin and industrial alkali lignin |
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