CN102531661B - Method for preparing ceramic material by papermaking waste water sludge - Google Patents
Method for preparing ceramic material by papermaking waste water sludge Download PDFInfo
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- CN102531661B CN102531661B CN 201110442916 CN201110442916A CN102531661B CN 102531661 B CN102531661 B CN 102531661B CN 201110442916 CN201110442916 CN 201110442916 CN 201110442916 A CN201110442916 A CN 201110442916A CN 102531661 B CN102531661 B CN 102531661B
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Abstract
The invention discloses a method for preparing a ceramic material by papermaking waste water sludge, which comprises the following steps: (1) dehydrating papermaking waste water sludge, drying in a baking oven to obtain dry sludge, adding polyvinyl alcohol, well mixing, molding, curing to obtain a sludge blank material; (2) performing carbonization of the sludge blank material in a vacuum sintering furnace to obtain a carbonized sludge blank material; (3) putting the carbonized sludge blank material in a graphite crucible paved with silicon powder, putting the graphite crucible in the vacuum sintering furnace to prepare porous SiC ceramics. The papermaking waste water sludge is dehydrated, dried, and dispersed; then the sludge is molded in a die; the sludge is further dried in the baking oven, and vacuum carbonization is performed; finally the material is silicified, and superfluous free silicon is removed. Therefore, the porous ceramic material which has dense pores and has silicon carbide as a main phase is obtained. The ceramic material is applicable to industries such as industrial and mining enterprises, industrial waste water treatment, tail gas treatment and the like. The porosity of the SiC porous ceramics is above 70%.
Description
Technical field
The present invention relates to the porcelain processing of paper waste mud, the technical field of green ceramic.
Background technology
Along with the progress of society, the raising of economic life level, more and more surging about the cry of global environment problem.At present, people will how to have handled and the waste in fields such as effective recycle industrial production, life, save resource, save energy, and problems such as control blowdown enjoy attention as the important measures of environment protection.In the developing material in the past, people mainly pursue the performance of material, and do not take the carrying capacity of environment that causes in the manufacturing of material and use into account, also reckon without the recycling utilization after the use.Now, along with the raising of people to Environmental awareness, the achievement of scientific and technological progress should preferentially develop towards the direction that alleviates the global environment burden, and advance, comfortableness and the environment compatibility of material combined effectively, makes novel environmentally conscious materials.
Paper waste mud is a kind of rich cellulose, hemicellulose, multiple organic solid matter, and it is effectively handled is the matter of utmost importance that solves paper mill sludge recycling and environment protection.
Paper-making effluent contains a large amount of microfibres, certainly leads to a large amount of mud in wastewater sedimentation, concentration process.The microfibre sludge volume generally accounts for the 1.0%-2.0% of sewage volume.This type of sludge volume is big, easily corrupt, density is little, particle is thin, water content is bigger.
That the processing of existing paper waste mud is mainly is agricultural, landfill, burning.Most of American-European developed countries adopt this way; Still be the main path of paper waste sludge disposal at the agricultural and landfill of developing country.But, but along with the landfill scope reduces gradually, still be main developing direction as agricultural fertilizer.
In addition, because pulping and paper-making mud contains the natural fiber with good tensile property, their filling in the plastic waste with good compressive property, can be obtained having the matrix material of good mechanical properties.This matrix material can be used as Industrial buildings material, industrial container, automobile baffle, casing etc.
The present invention utilizes paper waste mud to contain the characteristics of a large amount of organic celluloses, after its dehydration, drying, carries out carbonization, obtains the micro-pore silicon carbide material by the infiltration prepared in reaction then.This method is simple, gained pyroceramic hole exquisiteness, abundant, intensity is high, can be used for industry and filter industry.
Summary of the invention
The objective of the invention is to utilize the characteristics of wastewater sludge rich cellulose, turn waste into wealth, it is prepared into the high temperature resistant structure ceramics that is rich in micropore, can be widely used in industrial and mining enterprises or off gas treatment.
Technical scheme of the present invention is: a kind of paper waste mud that utilizes prepares method of ceramic material, and its step is as follows:
(1) paper waste mud is carried out mechanical dehydration 30-60min after, putting into baking oven dried 2-4 hour under 80-120 ℃ condition, obtain dried pug, the dried pug of reuniting is chosen out, disperseed the back to add polyvinyl alcohol, the add-on of polyvinyl alcohol is the 4-10% of dried pug quality, and mix, at 1-2 MPa forming under the pressure, put into baking oven then and under 110-120 ℃ condition, solidified 1-2 hour, obtain the moulded pottery not yet put in a kiln to bake material;
(2) the moulded pottery not yet put in a kiln to bake material is put into vacuum sintering furnace and carry out carbonization, the vacuum tightness of sintering oven is 0.01-0.1Pa, is 1-5 ℃/min at heat-up rate below 900 ℃, heat-up rate is 5-10 ℃/min more than 900 ℃, 1200 ℃ of insulations 3-5 hour, furnace cooling obtained carbonization moulded pottery not yet put in a kiln to bake material;
(3) carbonization moulded pottery not yet put in a kiln to bake material is put into the plumbago crucible that is covered with silica flour, the quality of silica flour is the 4-10% of dried pug quality, put into vacuum sintering furnace, the vacuum tightness of vacuum sintering furnace is 0.01-0.1Pa, and heat-up rate is 10-15 ℃/min, is incubated 30-60min under 1500-1600 ℃ condition, feed Ar gas atmosphere insulation 10-20min then, the row's of vacuumizing silicon is 0.5-3 hour under 1600-1700 ℃ condition, cools to room temperature with the furnace, makes the porous SiC pottery.
The invention has the beneficial effects as follows: paper waste mud disperses by after dehydration, drying; Then with it in die for molding; In baking oven further after the drying, vacuum carburization; At last material is carried out silication, and get rid of unnecessary free silicon.Thereby obtaining having the principal phase of fine and closely woven hole is the porous ceramic film material of silicon carbide.This stupalith can be in sector applications such as industrial and mining enterprises, Industrial Wastewater Treatment, vent gas treatment.The porosity of gained SiC porous ceramics is more than 70%.
Embodiment
Embodiment 1
Paper waste mud 200g carries out mechanical dehydration 30min.Obtain the dried pug of 50g, put into baking oven at 120 ℃ of oven dry 2hr, the dried pug that part is reunited is chosen out, disperse, add the polyvinyl alcohol of 2g then, and mix, at the 1.5MPa forming under the pressure, put into baking oven then and further solidify 1hr at 120 ℃;
Above-mentioned blank moved to carry out carbonization in the vacuum sintering furnace.Vacuum tightness is 10
-2Pa, carbonization temperature is 1200 ℃.Be 2 ℃/min at heat-up rate below 900 ℃, heat-up rate is 5 ℃/min more than 900 ℃, at 1200 ℃ of insulations 2 hours, furnace cooling;
Said sample is put into the plumbago crucible that is covered with the Si powder, put into vacuum sintering furnace.Silica flour is 3g.Heat-up rate is 10 ℃/min, and vacuum tightness is 10
-2Pa is at 1550 ℃ of insulation 30min.Feed Ar gas atmosphere insulation 10min then, through the 1650 ℃ of row's of vacuumizing silicon 1 hr, cool to room temperature with the furnace again, make the porous SiC pottery, the porosity of gained SiC porous ceramics is 75%.
Embodiment 2
Paper waste mud 400g carries out mechanical dehydration 60min.Obtain the dried pug of 90g, put into baking oven at 120 ℃ of oven dry 3hr, the dried pug that part is reunited is chosen out, disperse, add the polyvinyl alcohol of 5g then, and mix, at the 1MPa forming under the pressure, put into baking oven then and further solidify 2hr at 120 ℃;
Above-mentioned blank moved to carry out carbonization in the vacuum sintering furnace.Vacuum tightness is 10
-2Pa, carbonization temperature is 1200 ℃, is 1 ℃/min at heat-up rate below 900 ℃, heat-up rate is 10 ℃/min more than 900 ℃.At 1200 ℃ of insulations 3 hours, furnace cooling;
Said sample is put into the plumbago crucible that is covered with the Si powder, put into vacuum sintering furnace, silica flour is 5g, and heat-up rate is 15 ℃/min, and vacuum tightness is 10
-2Pa is at 1550 ℃ of insulation 60min.Feed Ar gas atmosphere insulation 10min then, through the 1650 ℃ of row's of vacuumizing silicon 0.5 hr, cool to room temperature with the furnace again, make the porous SiC pottery, porosity is 70%.
Embodiment 3
A kind of paper waste mud that utilizes prepares method of ceramic material, and its step is as follows:
(1) paper waste mud is carried out mechanical dehydration 30min after, putting into baking oven dried 2 hours under 80 ℃ condition, obtain dried pug, the dried pug of reuniting is chosen out, disperseed the back to add polyvinyl alcohol, the add-on of polyvinyl alcohol is 4% of dried pug quality, and mix, at 1 MPa forming under the pressure, put into baking oven then and under 110 ℃ condition, solidified 1 hour, obtain the moulded pottery not yet put in a kiln to bake material;
(2) the moulded pottery not yet put in a kiln to bake material is put into vacuum sintering furnace and carry out carbonization, the vacuum tightness of sintering oven is 0.01Pa, is 1 ℃/min at heat-up rate below 900 ℃, heat-up rate is 5 ℃/min more than 900 ℃, 1200 ℃ of insulations 3 hours, furnace cooling obtained carbonization moulded pottery not yet put in a kiln to bake material;
(3) carbonization moulded pottery not yet put in a kiln to bake material is put into the plumbago crucible that is covered with silica flour, the quality of silica flour is the 4-10% of dried pug quality, put into vacuum sintering furnace, the vacuum tightness of vacuum sintering furnace is 0.01Pa, and heat-up rate is 10 ℃/min, under 1500 ℃ condition, be incubated 30min, feed Ar gas atmosphere insulation 10min then, the row's of vacuumizing silicon is 0.5 hour under 1600 ℃ condition, cools to room temperature with the furnace, make the porous SiC pottery, porosity is 72%.
Embodiment 4
A kind of paper waste mud that utilizes prepares method of ceramic material, and its step is as follows:
(1) paper waste mud is carried out mechanical dehydration 60min after, putting into baking oven dried 4 hours under 120 ℃ condition, obtain dried pug, the dried pug of reuniting is chosen out, disperseed the back to add polyvinyl alcohol, the add-on of polyvinyl alcohol is 10% of dried pug quality, and mix, at 2 MPa forming under the pressure, put into baking oven then and under 120 ℃ condition, solidified 2 hours, obtain the moulded pottery not yet put in a kiln to bake material;
(2) the moulded pottery not yet put in a kiln to bake material is put into vacuum sintering furnace and carry out carbonization, the vacuum tightness of sintering oven is 0.1Pa, is 5 ℃/min at heat-up rate below 900 ℃, heat-up rate is 10 ℃/min more than 900 ℃, 1200 ℃ of insulations 5 hours, furnace cooling obtained carbonization moulded pottery not yet put in a kiln to bake material;
(3) carbonization moulded pottery not yet put in a kiln to bake material is put into the plumbago crucible that is covered with silica flour, the quality of silica flour is the 4-10% of dried pug quality, puts into vacuum sintering furnace, and the vacuum tightness of vacuum sintering furnace is 0.1Pa, heat-up rate is 15 ℃/min, be incubated 60min under 1600 ℃ condition, feed Ar gas atmosphere insulation 20min then, the row's of vacuumizing silicon is 3 hours under 1700 ℃ condition, cool to room temperature with the furnace, make the porous SiC pottery,, porosity is 73%.
Embodiment 5
A kind of paper waste mud that utilizes prepares method of ceramic material, and its step is as follows:
(1) paper waste mud is carried out mechanical dehydration 50min after, putting into baking oven dried 3 hours under 100 ℃ condition, obtain dried pug, the dried pug of reuniting is chosen out, disperseed the back to add polyvinyl alcohol, the add-on of polyvinyl alcohol is 5% of dried pug quality, and mix, at 2 MPa forming under the pressure, put into baking oven then and under 115 ℃ condition, solidified 2 hours, obtain the moulded pottery not yet put in a kiln to bake material;
(2) the moulded pottery not yet put in a kiln to bake material is put into vacuum sintering furnace and carry out carbonization, the vacuum tightness of sintering oven is 0.05Pa, is 3 ℃/min at heat-up rate below 900 ℃, heat-up rate is 8 ℃/min more than 900 ℃, 1200 ℃ of insulations 4 hours, furnace cooling obtained carbonization moulded pottery not yet put in a kiln to bake material;
(3) carbonization moulded pottery not yet put in a kiln to bake material is put into the plumbago crucible that is covered with silica flour, the quality of silica flour is the 4-10% of dried pug quality, put into vacuum sintering furnace, the vacuum tightness of vacuum sintering furnace is 0.05Pa, and heat-up rate is 12 ℃/min, under 1550 ℃ condition, be incubated 50min, feed Ar gas atmosphere insulation 15min then, the row's of vacuumizing silicon is 2 hours under 1650 ℃ condition, cools to room temperature with the furnace, make the porous SiC pottery, porosity is 75%.
Embodiment 6
A kind of paper waste mud that utilizes prepares method of ceramic material, and its step is as follows:
(1) paper waste mud is carried out mechanical dehydration 30-60min after, putting into baking oven dried 2-4 hour under 80-120 ℃ condition, obtain dried pug, the dried pug of reuniting is chosen out, disperseed the back to add polyvinyl alcohol, the add-on of polyvinyl alcohol is the 4-10% of dried pug quality, and mix, at 1-2 MPa forming under the pressure, put into baking oven then and under 110-120 ℃ condition, solidified 1-2 hour, obtain the moulded pottery not yet put in a kiln to bake material;
(2) the moulded pottery not yet put in a kiln to bake material is put into vacuum sintering furnace and carry out carbonization, the vacuum tightness of sintering oven is 0.01-0.1Pa, is 1-5 ℃/min at heat-up rate below 900 ℃, heat-up rate is 5-10 ℃/min more than 900 ℃, 1200 ℃ of insulations 3-5 hour, furnace cooling obtained carbonization moulded pottery not yet put in a kiln to bake material;
(3) carbonization moulded pottery not yet put in a kiln to bake material is put into the plumbago crucible that is covered with silica flour, the quality of silica flour is the 4-10% of dried pug quality, put into vacuum sintering furnace, the vacuum tightness of vacuum sintering furnace is 0.01-0.1Pa, and heat-up rate is 10-15 ℃/min, is incubated 30-60min under 1500-1600 ℃ condition, feed Ar gas atmosphere insulation 10-20min then, the row's of vacuumizing silicon is 0.5-3 hour under 1600-1700 ℃ condition, cools to room temperature with the furnace, makes the porous SiC pottery.
Claims (1)
1. one kind is utilized paper waste mud to prepare method of ceramic material, it is characterized in that its step is as follows:
(1) paper waste mud is carried out mechanical dehydration 30-60min after, putting into baking oven dried 2-4 hour under 80-120 ℃ condition, obtain dried pug, the dried pug of reuniting is chosen out, disperseed the back to add polyvinyl alcohol, the add-on of polyvinyl alcohol is the 4-10% of dried pug quality, and mix, at 1-2 MPa forming under the pressure, put into baking oven then and under 110-120 ℃ condition, solidified 1-2 hour, obtain the moulded pottery not yet put in a kiln to bake material;
(2) the moulded pottery not yet put in a kiln to bake material is put into vacuum sintering furnace and carry out carbonization, the vacuum tightness of sintering oven is 0.01-0.1Pa, is 1-5 ℃/min at heat-up rate below 900 ℃, heat-up rate is 5-10 ℃/min more than 900 ℃, 1200 ℃ of insulations 3-5 hour, furnace cooling obtained carbonization moulded pottery not yet put in a kiln to bake material;
(3) carbonization moulded pottery not yet put in a kiln to bake material is put into the plumbago crucible that is covered with silica flour, the quality of silica flour is the 4-10% of dried pug quality, put into vacuum sintering furnace, the vacuum tightness of vacuum sintering furnace is 0.01-0.1Pa, and heat-up rate is 10-15 ℃/min, is incubated 30-60min under 1500-1600 ℃ condition, feed Ar gas atmosphere insulation 10-20min then, the row's of vacuumizing silicon is 0.5-3 hour under 1600-1700 ℃ condition, cools to room temperature with the furnace, makes the porous SiC pottery.
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| CN 201110442916 CN102531661B (en) | 2011-12-27 | 2011-12-27 | Method for preparing ceramic material by papermaking waste water sludge |
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| CN 201110442916 CN102531661B (en) | 2011-12-27 | 2011-12-27 | Method for preparing ceramic material by papermaking waste water sludge |
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| CN103771858B (en) * | 2014-01-07 | 2015-05-13 | 中原工学院 | Method for preparing porous silicon carbide ceramic employing activated carbon silicification method |
| CN108046758A (en) * | 2017-12-22 | 2018-05-18 | 中原工学院 | A kind of method that low temperature resintering addition SiC prepares high sludge content sludge ceramics |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5582682A (en) * | 1988-12-28 | 1996-12-10 | Ferretti; Arthur | Process and a composition for making cellulosic composites |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5582682A (en) * | 1988-12-28 | 1996-12-10 | Ferretti; Arthur | Process and a composition for making cellulosic composites |
Non-Patent Citations (6)
| Title |
|---|
| Application of the chemical vapor infiltration and reaction (CVI-R) technique for the preparation of highly porous biomorphic SiC ceramics derived from paper;Daniela Almeida Streitwieser et al.;《Journal of the European Ceramic Society》;20040720;第25卷;第817页左栏第1段-第827页左栏第2段 * |
| Daniela Almeida Streitwieser et al..Application of the chemical vapor infiltration and reaction (CVI-R) technique for the preparation of highly porous biomorphic SiC ceramics derived from paper.《Journal of the European Ceramic Society》.2004,第25卷第817页左栏第1段-第827页左栏第2段. |
| 一种新型多孔SiC的制备与性能研究;王伟 等;《无机材料学报》;20080131(第01期);第110页左栏第2段至左栏第4段 * |
| 王伟 等.一种新型多孔SiC的制备与性能研究.《无机材料学报》.2008,(第01期),第110页左栏第2段至左栏第4段. |
| 造纸废水污泥处理技术及资源化利用研究;郗伟;《精细与专用化学品》;20110331;第19卷(第03期);第14页右栏第3段 * |
| 郗伟.造纸废水污泥处理技术及资源化利用研究.《精细与专用化学品》.2011,第19卷(第03期),第14页右栏第3段. |
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