CN110483011A - Using greasy filth as ceramic material of primary raw material and preparation method thereof - Google Patents

Using greasy filth as ceramic material of primary raw material and preparation method thereof Download PDF

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CN110483011A
CN110483011A CN201910790972.8A CN201910790972A CN110483011A CN 110483011 A CN110483011 A CN 110483011A CN 201910790972 A CN201910790972 A CN 201910790972A CN 110483011 A CN110483011 A CN 110483011A
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raw material
greasy filth
ceramic material
primary raw
ceramic
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李宇
姚长青
马远
刘纯杰
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Shandong Branch Energy Saving Polytron Technologies Inc
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Shandong Branch Energy Saving Polytron Technologies Inc
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    • C04B33/13—Compounding ingredients
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Abstract

The present invention relates to greasy filth to utilize technical field, and in particular to a kind of using greasy filth as ceramic material of primary raw material and preparation method thereof.It is of the present invention using greasy filth as the ceramic material of primary raw material, be made of the greasy filth of 50-80wt% and the calcic non-plastic raw material of 20-50wt%；The preparation method comprises the following steps: adding water for ball milling, sieving, drying after raw material is mixed, raw material powder is obtained；It is granulated, is sieved, base after raw material powder is mixed with water again；It will be sintered after ceramic material body drying, obtain the ceramic material using greasy filth as primary raw material.It is of the invention using greasy filth as the ceramic material of primary raw material, substantially increase the doping of greasy filth in ceramic material, and flexural strength with higher and lower water absorption rate；The present invention also provides preparation methods, compensate for greasy filth and are difficult to the method vacancy that large dosage efficiently utilizes, and have apparent economic benefit and environmental benefit.

Description

Using greasy filth as ceramic material of primary raw material and preparation method thereof
Technical field
The present invention relates to greasy filth to utilize technical field, and in particular to it is a kind of using greasy filth as the ceramic material of primary raw material and its Preparation method.
Background technique
Greasy filth is one of the important pollutant generated in oil field development and storage and transport process, and restricts oilfield environment quality and hold The continuous a great problem improved.China is that the sustained production of ceramic big country, especially Building Ceramics Industry increases, and leads to clay resource Increasingly deficient, many scholars start to carry out ceramic material preparation with non-traditional ceramic raw material.Greasy filth contains high silicon, high alumina as a kind of Siliceous material, ceramics can be prepared.Ceramic post sintering process is not only able to for the silicate solid waste of complicated chemical component being changed into The material of excellent performance, and ceramics have high added value.Ceramic industry has an ability for dissolving large solid waste, and with The limitation of the reduction of quality raw materials and natural resources exploitation, ceramic industry, which is also faced with, utilizes low-grade mineral or Industrial Solid Waste Great demand.Therefore, preparing ceramic material is an effective way for handling greasy filth.
Have a small amount of research that ceramics are prepared using greasy filth at present, but it is less generally there are greasy filth volume the problems such as.
Patent CN106082986A disclose a kind of ceramic tile mixed with biomass combustion lime-ash and oil refining waste oil mud and Preparation method, raw material are oil refining waste oil mud, the 12%- of the biomass combustion lime-ash of 17%-23%, 15%-20% 19% alkaline residue, the serpentine of 23%-31%, the waste mortar of 10%-15%, the cobble of 21%-29%, 14%-22% Manganese tailing, the ball clay of 11%-18%, the barium molybdate of 7%-14%, the red mud of 16%-24%, 24%-32% water quenching phosphorus slag, The feldspathic sandstone of 20%-25%, the stalactite of 18%-26%, 15%-20% antimony ore slag, the anti-folding of the ceramic tile of this method preparation is strong Degree is 35Mpa, good weatherability, can acid-alkali-corrosive-resisting, but the raw material type used is numerous, and preparation process is complicated, and greasy filth is mixed Amount is few.
Patent CN105967647A discloses a kind of low water absorption high water resistance sintered clay hollow brick and preparation method thereof, former Material is diopside, the 15%-20% of the oil refining waste oil mud of 14%-22%, the calcium hydroxide of 9%-16%, 10%-15% Ceramic waste residue, the loose squama of 7%-13%, the magnesia of 5%-10%, the polyethylene pyrrole network alkanone of 8%-12%, 14%-26% Lithium porcelain stone, the obsidian of 11%-17%, the boron mud of 15%-25%, the hydrophobic type gas phase silica of 5%-10%, 12%- 20% silicon slag, the desulfurized gypsum of 16%-24%, the nacrite of 40%-50%, the odium stearate of 3%-5%, 11%- 19% cobblestone, the aluminosilicate waste residue of 22%-34%, 18%-27% yellow ground, the hollow brick water absorption rate of this method preparation It is 0.62%, compression strength 7.7Mpa, numerous using raw material, preparation process is complicated.
Zhang Qiongjiu, Zhang Xiaodong had once carried out solidification brickmaking test to waste drilling mud, and demonstrate oily sludge brickmaking can Row.But the setting of its test parameters is less, is lacking to the influence factor Research on Regularity of brickmaking.Settling down honor et al. will be different Residue and clay after ratio disposal of oily sludge are made adobe and are sintered, and discovery oily sludge residue is suitable for as fired brick Raw material, clay percentage should be greater than 40% in raw material, and sludge oil content should be less than 4%, the oil-containing for being 2% for oil content Sludge residue brickmaking is more more economically viable than cracking process.But primary raw material is sial component, and greasy filth reaction is insufficient, with same modeling The clay of property raw material cannot mix very well, therefore cannot mix the big greasy filth of oil content.
Gao Hongge et al. has invented a kind of method using greasy filth and gangue production brick.The raw material of this method is 10%- 20% greasy filth, the clay of 40%-65%, the gangue of 10%-30%, the water of 5%-20%.Experiment flow is ingredient, stirring Uniformly, semi-finished product adobe processed, drying, roasting are to 1000-1100 DEG C.Its advantage are as follows: using the method for high temperature sintering, institute in greasy filth Containing combustibles such as oils as fuel；Greasy filth is not necessarily to dehydration；Modified additive solidifies nuisance.This method can be effective Eliminate the influence of hazardous material in greasy filth；But the volume of greasy filth is less, does not make full use of the high sial of greasy filth component and high-ductility The characteristics of.
N.M.Khalil et al. is higher than 1600 in sintering temperature using the greasy filth and natural bauxite of different quality percentage High quality refractory is prepared at DEG C, studies have shown that the greasy filth of 40wt% and the bauxite of 60wt% are to prepare high quality fire resisting The optimum mixture of ceramic body has highest mechanical strength, i.e. 910Mpa at 1500 DEG C.
FRANCA J N et al. utilizes the kaolin of the remaining greasy filth of 1.25-5.00wt.%, 35-38.75wt.%, 47.5wt.% albite and 12.5wt.% quartz, in oxidizing atmosphere 1200-1250 DEG C at a temperature of quickly fire pottery Porcelain plate.
Cao Shuliang prepares ceramic aggregate at 1300 DEG C using the greasy filth of 40wt% and the clay of 60wt%；By oil content 20% Mass fraction be 70% greasy filth and clay be blended in 1180 DEG C and prepare ceramic aggregate.
The greasy filth additive amount of above technical scheme is not high, and needs to can be only achieved preferably by higher sintering temperature Performance.
Non-burning brick research is prepared using greasy filth in addition, also having.Largely use cement or special curing agent cold conditions solidified oil The technique of clay standby cement brick not can solve oil and influence of organic hazardous material to environment in greasy filth, can not effectively consolidate weight Metal, it is therefore desirable to component separation and culture be carried out to greasy filth, what is actually utilized is the silt particle in greasy filth.
For example, Fan Yuqin et al. generates greasy filth using the greasy filth of Gudao area of Shengli Oilfield oil recovery factory as research object, according to it Feature devises the high oily sludge harmless treatment process in oil field.The technique includes two parts, first carries out oil, mud, sand separation- Mention oil, then solidification is contained using mixed crystal by the mud after oil is mentioned.Exterior components test result shows: after the process, greasy filth Crude Oil average removal rate reaches 94.91%；When curing agent and silt particle mixed proportion are 1:4-1:6, intensity be can reach very To be more than light water adobe, and in cured block leachate COD well below integrated wastewater discharge standard (GB8978-1996) Primary standard, and oil immersion output is not detected.
Zhang Junfeng et al. provides a kind of method of oily sludge resource utilization, technical solution are as follows: will first contain greasy dirt Silt particle carries out oil, water, mud, four, sand separation, and the granularmetric composition of oil sludge and sand, the size distribution of oil sludge and sand are gone out with screen analysis technique study It is concentrated mainly on 0.1-0.85mm, yield 90%, average particle size 0.23mm, clay content 1.74% is suitble to production unburned Brick.Sand after separation is added to 15%-50% cement, 10%-30% gravel, 1%-10% curing agent, 20%- in blender 50% clear water is stirred production mortar, be then sent in moulding press with transmission belt be molded be made machine pressure it is non-burning brick. Sampled detection intensity grade reaches MU15, and the indexs such as dimensional discrepancy, appearance, freeze thawing, scum, lime blowing meet national standard The building material products such as the fired brick of index request.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of using greasy filth as the ceramic material of primary raw material, Substantially increase the doping of greasy filth in ceramic material, and flexural strength with higher and lower water absorption rate；The present invention is also Preparation method is provided, greasy filth is compensated for and is difficult to the method vacancy that large dosage efficiently utilizes, there is apparent economic benefit and ring Border benefit.
It is of the present invention using greasy filth as the ceramic material of primary raw material, by the greasy filth and 20-50wt% of 50-80wt% Calcic non-plastic raw material is made.
Calcic non-plastic raw material is one of solid waste raw material or traditional ceramics raw material or a variety of；Solid waste raw material includes bastard coal Stone, flyash, tailing, stone-precessing saw mud, red mud, steel slag, blast furnace slag, gypsum, ferroalloy slag, acetylene slag；Traditional ceramics are former Material includes quartz, feldspar, shale, dolomite, lime stone.
CaO and Al in calcic non-plastic raw material2O3Gross mass content be higher than 30%.
For low calcic non-plastic raw material (i.e. CaO mass content is lower than 10%), Al2O3Mass content need to be higher than 20%, He does not require component；For high calcium-containing non-plastic raw material (i.e. CaO mass content is higher than 30%), other components are not required.In When selecting calcic non-plastic raw material, low calcic non-plastic raw material and high calcium-containing non-plastic raw material can be used in mixed way.
Preferably, CaO mass content is higher than 30%, Al in calcic non-plastic raw material2O3Mass content is higher than 20%.
Greasy filth includes oil exploitation, collects the solid generated during defeated, petroleum refining and oiliness sewage treatment and semisolid Waste material, and the tail mud by the further separation and Extraction of the above waste material after oily.Have the characteristics that good plasticity using greasy filth, can replace For clay as plastic raw material.
By percentage to the quality, 40% < SiO in greasy filth2≤ 80%, 10%≤Al2O3≤ 45%, 0%≤MgO < 5%, 0% < crude oil < 15%.
SiO in greasy filth2、Al2O3, MgO and crude content need to meet the above mass percent, other components do not require. When the oil content of greasy filth or excessively high water content, greasy filth can be calcined, reach after content requirement again with calcic non-plastic raw material It is mixed.
The principal crystalline phase of ceramic material is anorthite phase, and CaO mass content is 10-30% in ceramic material.
Due to containing iron oxide in raw material, ceramic material there is also a small amount of pyroxene phase and red iron in addition to anorthite phase Mine phase.
Ceramic material is sintering ceramsite, Wall or floor tile, fired brick, Antique Imitation Tiles, clear water brick, landscape brick or internal combustion brick.
It is of the present invention using greasy filth as the preparation method of the ceramic material of primary raw material, steps are as follows:
(1) it grinds: being put into after raw material is mixed in planetary ball mill and add water for ball milling 15-30min, the slurry mistake that will be obtained 70-90 mesh is subsequently placed in 8-12h in the drying box of 100-120 DEG C of temperature, obtains raw material powder；
(2) base: being granulated after raw material powder is mixed with water, crosses 15-30 mesh, feed particles is obtained, by feed particles Ceramic material green body is made with mold；
(3) it is sintered: ceramic material green body being first placed in 1-2h in 100-120 DEG C of drying box, then in 1060-1180 DEG C of temperature Under be sintered, obtain the ceramic material using greasy filth as primary raw material.
The mixing mass ratio of material powder and water is 100:8-20 in step (2).
The water content of ceramic material green body is 8-20wt%, preferably 8-10wt% in step (2).
Sintering process in step (3) are as follows: the heating rate of room temperature to 600 DEG C is 250-300 DEG C/h；600-800 DEG C of liter Warm rate is 50-60 DEG C/h；800 DEG C or more of heating rate is 250-300 DEG C/h；Finally it is warming up to 1060-1180 DEG C and protects Warm 1-2h, then room temperature is down to the rate of temperature fall of 500-600 DEG C/h.
The sintering process of ceramic material is divided into three phases: initial adhesion stage, Crystallization stage and blank Densification In the stage, the main process of new Crystallization is earlier than its densification process in green body.Under normal circumstances, it may occur that following reaction:
(1) calcareous material decomposes, and such as calcium carbonate, calcium hydroxide, decomposes and generates calcium oxide；
(2)Al2O3﹒ 2SiO2﹒ 2H2O→Al2O3﹒ 2SiO2+2H2O；
(3)CaO+Al2O3﹒ 2SiO2→ CaO ﹒ Al2O3﹒ 2SiO2。
In order to solve the problems, such as that greasy filth yield is few in ceramic material when the present invention is main, therefore meet national standard preparing Greasy filth ceramic material on the basis of, incorporation greasy filth as much as possible in formula is not easy when greasy filth volume is higher than 80wt% Preparing principal crystalline phase is anorthitic ceramics.
In order to improve greasy filth amount volume, on the one hand need using high-sintering process, it is organic to decompose the nocuousness in greasy filth Component, such as aromatic hydrocarbon；On the other hand, the characteristics of needing to give full play to the high sial of greasy filth and high-ductility, by greasy filth and other originals Material mixes well, while guaranteeing that greasy filth can sufficiently be reacted with other raw materials under high temperature.
During the sintering process, greasy filth is about 14% in 600-800 DEG C of weightlessness, and reaction at this time is mainly organic compound combustion point Solution, is slowly heated up at 600-800 DEG C with slower heating rate, organic matter can be made to decompose complete.Ceramic material green compact exist 1060-1180 DEG C is sintered, and the reaction of calcic non-plastic raw material generates anorthite phase under high temperature, obtains high performance ceramic material.
Compared with other ceramic raw materials (such as clay), it is viscous that liquid phase in sintering process can be greatly lowered in calcic non-plastic raw material Degree promotes object mutually to melt and be homogenized, and to the thermal stability and mechanical strength for improving ceramics, improving whiteness and transparency has one to be set for With.
Compared with prior art, the invention has the following beneficial effects:
(1) calcic non-plastic raw material is added in the present invention in ceramic raw material, for dispersing greasy filth, keeps greasy filth and the lean property of calcic former Material mixes well, while having the characteristics that oil-containing is high, plasticity is strong using greasy filth, avoids the use of one of clay raw materials；
(2) present invention is added calcic non-plastic raw material, keeps silane agent in the greasy filth of large dosage complete in high-temperature sintering process Portion participates in reaction, is formed and enhances the performance of ceramics using anorthite as the ceramics of principal crystalline phase, solves and glues in conventional clay ceramics Soil with problem that is less and causing greasy filth doping low is reacted between greasy filth；
(3) present invention during the sintering process, increases the content of greasy filth, provides heat using the decomposition of organic matter in greasy filth Amount reduces burning energy consumption, and ceramic sintering temperature design ensure that organic in 1000 DEG C or less oils at 1060-1180 DEG C Effective decomposition of object, and the hole after decomposing can densify again in the subsequent sintering process, so that ceramic product is with good Good performance, the flexural strength of the ceramic material of preparation are 70-90Mpa, water absorption rate < 0.2%.
Specific embodiment
The present invention will be further described with reference to embodiments, but protection scope of the present invention is not limited only to this.
The chemical composition of each raw material is as shown in table 1 in embodiment, and raw material chemical composition uses AXIOSmax type x-ray fluorescence Spectrometer (XRF) test.
1 raw material chemical composition table of table
Component Greasy filth Tailing It is sintered red mud Dali stone saw mud Gangue Flyash Steel slag
SiO2 67.35 54.33 21.20 9.98 50.50 56.80 19.57
Al2O3 12.61 32.89 7.94 3.48 26.10 28.85 2.92
CaO 6.20 2.22 47.96 80.34 4.21 4.15 42.93
MgO 1.99 0.75 1.50 2.97 1.46 1.06 4.13
Fe2O3 5.04 3.86 12.51 1.83 9.30 5.27 23.08
It is other 6.81 5.95 8.89 1.40 8.43 3.87 7.37
Embodiment 1
(1) it grinds: 240g greasy filth, 45g tailing, the Dali 15g stone saw mud being mixed, is placed in planetary ball mill, adds water polo 20min is ground, gained slurry crosses 80 meshes, and the slurry after sieving is placed in the drying box of 110 DEG C of temperature less than 1% by screen over-size 10h obtains material powder；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:10, crosses 20 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by particle under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 1h of 110 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering, the first heating rate with 300 DEG C/h slowly rise from room temperature to 600 DEG C, then with the heating rate of 60 DEG C/h from 600 DEG C Temperature is warming up to 1120 DEG C to 800 DEG C, in 800 DEG C or more the heating rates with 300 DEG C/h, after keeping the temperature 1h, with the cooling of 600 DEG C/h Rate is down to room temperature, obtains the ceramic material using greasy filth as primary raw material.
Embodiment 2
(1) it grinds: 150g greasy filth, 105g gangue, the Dali 45g stone saw mud being mixed, is placed in planetary ball mill, adds water Ball milling 15min, gained slurry cross 70 meshes, and the slurry after sieving is placed in the drying box of 110 DEG C of temperature less than 1% by screen over-size 8h obtains material powder；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:8, crosses 15 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by grain under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 2h of 110 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering, the first heating rate with 300 DEG C/h slowly rise from room temperature to 600 DEG C, then with the heating rate of 60 DEG C/h from 600 DEG C Temperature is warming up to 1120 DEG C to 800 DEG C, in 800 DEG C or more the heating rates with 300 DEG C/h, after keeping the temperature 1h, with the cooling of 600 DEG C/h Rate is down to room temperature, obtains the ceramic material using greasy filth as primary raw material.
Embodiment 3
(1) it grinds: 150g greasy filth, 90g flyash, the Dali 60g stone saw mud being mixed, is placed in planetary ball mill, adds water Ball milling 30min, gained slurry cross 90 meshes, and the slurry after sieving is placed in the drying box of 120 DEG C of temperature less than 1% by screen over-size 8h obtains material powder；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:10, crosses 30 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by particle under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 1h of 120 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering, the first heating rate with 300 DEG C/h slowly rise from room temperature to 600 DEG C, then with the heating rate of 60 DEG C/h from 600 DEG C Temperature is warming up to 1180 DEG C to 800 DEG C, in 800 DEG C or more the heating rates with 300 DEG C/h, after keeping the temperature 1h, with the cooling of 600 DEG C/h Rate is down to room temperature, obtains the ceramic material using greasy filth as primary raw material.
Embodiment 4
(1) it grinds: 180g greasy filth, 60g tailing, 60g sintering red mud being mixed, is placed in planetary ball mill, adds water for ball milling 20min, gained slurry cross 80 meshes, and the slurry after sieving is placed in the drying box 10h of 110 DEG C of temperature less than 1% by screen over-size, Obtain material powder；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:10, crosses 20 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by particle under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 1h of 110 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering, the first heating rate with 300 DEG C/h slowly rise from room temperature to 600 DEG C, then with the heating rate of 60 DEG C/h from 600 DEG C Temperature is warming up to 1090 DEG C to 800 DEG C, in 800 DEG C or more the heating rates with 300 DEG C/h, after keeping the temperature 1h, with the cooling of 600 DEG C/h Rate is down to room temperature, obtains the ceramic material using greasy filth as primary raw material.
Embodiment 5
(1) it grinds: 150g greasy filth, 90g flyash, 60g steel slag being mixed, is placed in planetary ball mill, adds water for ball milling 20min, gained slurry cross 80 meshes, and the slurry after sieving is placed in the drying box 10h of 110 DEG C of temperature less than 1% by screen over-size, Obtain material powder；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:10, crosses 20 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by particle under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 1h of 110 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering, the first heating rate with 300 DEG C/h slowly rise from room temperature to 600 DEG C, then with the heating rate of 50 DEG C/h from 600 DEG C Temperature is warming up to 1120 DEG C to 800 DEG C, in 800 DEG C or more the heating rates with 300 DEG C/h, after keeping the temperature 1h, with the cooling of 500 DEG C/h Rate is down to room temperature, obtains the ceramic material using greasy filth as primary raw material.
Embodiment 6
(1) it grinds: 180g greasy filth, 60g tailing, the Dali 30g stone saw mud, 30g steel slag being mixed, planetary ball mill is placed in In, add water for ball milling 20min, gained slurry crosses 80 meshes, and screen over-size is placed in 110 DEG C of temperature less than 1%, by the slurry after sieving Drying box 10h, obtains material powder；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:20, crosses 20 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by particle under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 1h of 110 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering, first with the heating rate of 2500 DEG C/h from room temperature to 600 DEG C, then it is slow from 600 DEG C with the heating rate of 50 DEG C/h 800 DEG C are warming up to, 1120 DEG C are warming up in 800 DEG C or more the heating rates with 250 DEG C/h, after keeping the temperature 1h, with the drop of 500 DEG C/h Warm rate is down to room temperature, obtains the ceramic material using greasy filth as primary raw material.
Comparative example 1
This comparative example prepares ceramic material using the greasy filth of 30wt% and the calcic non-plastic raw material of 70wt%, and steps are as follows:
(1) it grinds: 90g greasy filth, 150g tailing, the Dali 60g stone saw mud being mixed, is placed in planetary ball mill, adds water polo 20min is ground, gained slurry crosses 80 meshes, and the slurry after sieving is placed in the drying box of 110 DEG C of temperature less than 1% by screen over-size 10h obtains material powder；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:10, crosses 20 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by particle under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 1h of 110 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering, the first heating rate with 300 DEG C/h slowly rise from room temperature to 600 DEG C, then with the heating rate of 50 DEG C/h from 600 DEG C Temperature is warming up to 1180 DEG C to 800 DEG C, in 800 DEG C or more the heating rates with 300 DEG C/h, after keeping the temperature 1h, with the cooling of 500 DEG C/h Rate is down to room temperature, obtains the ceramic material using greasy filth as primary raw material.
Comparative example 2
This comparative example prepares ceramic material using the greasy filth of 50wt% and the clay of 50wt%, and steps are as follows:
(1) it grinds: 150g greasy filth, the Laiyang 150g soil being mixed, is placed in planetary ball mill, adds water for ball milling 20min, gained Slurry crosses 80 meshes, and the slurry after sieving is placed in the drying box 10h of 110 DEG C of temperature, obtains raw material powder by screen over-size less than 1% Body；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:10, crosses 20 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by particle under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 1h of 110 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering after keeping the temperature 1h, is down to room with the heating rate of 300 DEG C/h from room temperature to 1120 DEG C with the rate of temperature fall of 600 DEG C/h Temperature obtains the ceramic material using greasy filth as primary raw material.
Comparative example 3
This comparative example uses constant temperature-rising method during the sintering process, and steps are as follows:
(1) it grinds: 180g greasy filth, 60g tailing, 60g sintering red mud being mixed, is placed in planetary ball mill, adds water for ball milling 20min, gained slurry cross 80 meshes, and the slurry after sieving is placed in the drying box 10h of 110 DEG C of temperature less than 1% by screen over-size, Obtain material powder；
(2) it base: is granulated after material powder and water are mixed according to the mass ratio of 100:10, crosses 20 meshes, obtain raw material Feed particles are pressed into 50mm × 10mm × 5mm ceramic material batten with pressure-like machine by particle under 20Mpa pressure；
(3) it is sintered: after ceramic material batten to be placed in the drying box 1h of 110 DEG C of temperature, being placed in gradient Crystallization Furnace and carry out Sintering after keeping the temperature 1h, is down to room with the heating rate of 300 DEG C/h from room temperature to 1100 DEG C with the rate of temperature fall of 600 DEG C/h Temperature obtains the ceramic material using greasy filth as primary raw material.
The embodiment 1-6 ceramic material prepared is tested for the property, test method is as follows:
(1) flexural strength: maximum load F when folding tester test sample fracture anti-with TZS-6000 type digital display ceramics, The width b of sample, the thickness h of pivot distance L and the sample plane of disruption, according to formula R=(3 × F are measured with electronic digital indicator again ×L)/(2×b×h2), calculate flexural strength R.
(2) water absorption rate: carrying out water absorption rate test to sample with CXX-A type ceramics water absorption rate vacuum plant, and with wet rag The moisture of sample surfaces after absorbing water is drawn, then measures the mass M of sample water suction front and back with precision balance3、M4, according to formula W= (M4-M3)/M3× 100%, calculate water absorption rate W.
(3) the green compact mass M of sample burn tinctuer: is measured using accurate balance1With mass M after sintering2, according to formula S= (M1-M2)/M1× 100, calculate burn tinctuer S；
(4) linear shrinkage ratio: with the green compact length L of electronic digital indicator measurement sample1With length L after sintering2, according to formula I =(L1-L2)/L1× 100, calculate linear shrinkage ratio I.
(5) it CaO content in ceramic material: is measured using AXIOSmax type Xray fluorescence spectrometer (XRF).
(6) it ceramic material principal crystalline phase: is analyzed using SMARTLAB (9) type high temperature X-ray diffraction instrument (XRD), test mode Are as follows: continuous scanning, step-length are 0.02 °, and using Cu target, scanning speed is 10 °/min, and scanning range is 10 ° -90 °.
The ceramic material property test result of embodiment 1-6 preparation is as shown in table 2.
The ceramic material property test result of 2 embodiment 1-6 of table preparation
From table 2 it can be seen that calcic non-plastic raw material is added under conditions of high greasy filth doping in the present invention, and to sintering Technique improves, and the ceramic material flexural strength of preparation is 70-90Mpa, water absorption rate < 0.2%, greatly strengthens greasy filth pottery The consistency of ceramic material；Comparative example 1 reduces the doping of greasy filth, and the degree of sintering of the ceramic material of preparation reduces, consistency It is corresponding to reduce, cause the flexural strength of ceramic material to decline, water absorption rate increases, and comprehensive performance is lower than the ceramic material of embodiment； Calcic non-plastic raw material is replaced with clay by comparative example 2, due to reacting less between clay and greasy filth, leads to the ceramic material of preparation Flexural strength is lower than embodiment, and water absorption rate is also higher；Although comparative example 3 using the greasy filth and calcic non-plastic raw material of highly doped amount, But constant heating rate is used in sintering process, decline the properties of ceramic material also.

Claims (10)

1. a kind of using greasy filth as the ceramic material of primary raw material, it is characterised in that: by the greasy filth and 20-50wt% of 50-80wt% Calcic non-plastic raw material be made.
2. according to claim 1 using greasy filth as the ceramic material of primary raw material, it is characterised in that: calcic non-plastic raw material is One of solid waste raw material or traditional ceramics raw material are a variety of；Solid waste raw material includes gangue, flyash, tailing, processing of stone Saw mud, red mud, steel slag, blast furnace slag, gypsum, ferroalloy slag, acetylene slag；Traditional ceramics raw material includes quartz, feldspar, shale, white Marble, lime stone.
3. using greasy filth as the ceramic material of primary raw material according to right 1 or 2, it is characterised in that: in calcic non-plastic raw material CaO and Al2O3Gross mass content be higher than 30%.
4. according to claim 1 using greasy filth as the ceramic material of primary raw material, it is characterised in that: greasy filth includes that petroleum is opened It adopts, collect the solid and semi-solid waste generated during defeated, petroleum refining and oiliness sewage treatment, and greasy filth is further divided From the tail mud after extract oil.
5. according to claim 1 or 4 using greasy filth as the ceramic material of primary raw material, it is characterised in that: with quality percentage Than counting, 40% < SiO in greasy filth2≤ 80%, 10%≤Al2O3≤ 45%, 0%≤MgO < 5%, 0% < crude oil < 15%.
6. according to claim 1 using greasy filth as the ceramic material of primary raw material, it is characterised in that: the oikocryst of ceramic material It is mutually anorthite phase, CaO mass content is 10-30% in ceramic material.
7. according to claim 1 using greasy filth as the ceramic material of primary raw material, it is characterised in that: ceramic material is sintering Haydite, Wall or floor tile, fired brick, Antique Imitation Tiles, clear water brick, landscape brick or internal combustion brick.
8. a kind of described in claim 1 using greasy filth as the preparation method of the ceramic material of primary raw material, which is characterized in that step It is as follows:
(1) it grinds: being put into after raw material is mixed in planetary ball mill and add water for ball milling 15-30min, obtained slurry is crossed into 70-90 Mesh is subsequently placed in 8-12h in the drying box of 100-120 DEG C of temperature, obtains raw material powder；
(2) base: being granulated after raw material powder is mixed with water, crosses 15-30 mesh, obtains feed particles, and feed particles are pressed Ceramic material green body is made in model machine；
(3) be sintered: ceramic material green body is first placed in 1-2h in 100-120 DEG C of drying box, then at a temperature of 1060-1180 DEG C into Row sintering, obtains the ceramic material using greasy filth as primary raw material.
9. according to claim 8 using greasy filth as the preparation method of the ceramic material of primary raw material, it is characterised in that: step (2) mixing mass ratio of material powder and water is 100:8-20 in.
10. according to claim 8 using greasy filth as the preparation method of the ceramic material of primary raw material, it is characterised in that: step Suddenly sintering process in (3) are as follows: the heating rate of room temperature to 600 DEG C is 250-300 DEG C/h；600-800 DEG C of heating rate is 50- 60℃/h；800 DEG C or more of heating rate is 250-300 DEG C/h；Finally it is warming up to 1060-1180 DEG C and keeps the temperature 1-2h, then with The rate of temperature fall of 500-600 DEG C/h is down to room temperature.
CN201910790972.8A 2019-08-26 2019-08-26 Using greasy filth as ceramic material of primary raw material and preparation method thereof Withdrawn CN110483011A (en)

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CN111233450A (en) * 2020-03-03 2020-06-05 北京科技大学 Method for preparing ceramic and byproduct sulfur oxide-rich gas by using industrial byproduct gypsum
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CN112429924A (en) * 2020-10-22 2021-03-02 大连理工大学 System and method for preparing inorganic porous material and recovering oil by using oily sludge as binder
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CN115215636A (en) * 2022-08-19 2022-10-21 安徽美琛生态科技有限公司 Method for preparing ceramsite by using oily sludge
CN117209252A (en) * 2023-01-10 2023-12-12 福建省德化县冠鸿陶瓷有限公司 High-whiteness ceramic blank and firing method thereof
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