CN1807256A - High melt polymeric material manufacturing process - Google Patents
High melt polymeric material manufacturing process Download PDFInfo
- Publication number
- CN1807256A CN1807256A CN 200610012391 CN200610012391A CN1807256A CN 1807256 A CN1807256 A CN 1807256A CN 200610012391 CN200610012391 CN 200610012391 CN 200610012391 A CN200610012391 A CN 200610012391A CN 1807256 A CN1807256 A CN 1807256A
- Authority
- CN
- China
- Prior art keywords
- hours
- temperature
- time
- particle diameter
- ball
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The invention relates to a preparation technique for high-melting-point polymeric material. Wherein, selecting material by weight share as: 2. 5~7 rutile, 5~10 SiO2, 5~15 4MgO.6SiO2.2H2O, 2~6 CaO, 26~40 TiO2, and 38~61 Al2O3; in the first calcination, mixing the Al2O3, SiO2, TiO2 and CaO to grind and dry to let the water content less than 1%, calcinating at 1350~1400Deg and holding for 4~6h; in the second calcination, adding other materials into the first sintered body to grind and dry let the water content less than 1%, heating to 1550~1580Deg and calcinating for 3~7h. This product has well properties.
Description
Technical field
The present invention relates to a kind of production technique of ceramic, be specially a kind of production technique of high melt polymeric material.
Technical background
Make a general survey of the various countries scientific worker has carried out different depths and range to aluminium titanates research, but what carry out emphatically is the research that aluminium titanates itself or interpolation minor amounts of additives improve some performance of sintered compact, the result who obtains mostly is that some performance improves, when improving as intensity, and other useful performance has reduced, and has reduced as low bulk, heat-shock resistance etc.
Aluminium titanates have anti-slag, anti-corrosion, alkaline-resisting and with multiple nonferrous metal melts and the non-wetted advantages of glass melt such as copper, aluminium.Two big shortcomings of aluminium titanates: the one, its crystal is very big at three axial thermal expansion coefficient differences, cause it in process of cooling, easily to produce tiny crack, the sintering difficulty causes physical strength to reduce and destruction in various degree, and its quality is had a greatly reduced quality and the increasing of hidden danger risk; The 2nd, easily decompose at middle low temperature (700～1280 ℃) range content, i.e. its poor heat stability.This drawbacks limit its application in non-ferrous metal and more extensive industry.
Summary of the invention
Technical problem to be solved by this invention provide a kind ofly have high-melting-point, high strength, high stability, low bulk, resistance to wear, the production technique of the low reunion of performance such as anti-thermal shock, high-purity, superfine starting powder-high melt polymeric material.
The present invention adopts following technical scheme:
The present invention adopts following ratio of weight and number component: rutile 2.5～7, quartzy SiO
25～10, sepiolite 4MgO6SiO
22H
2O 5～15, calcium oxide CaO 2～6, titanium dioxide TiO
226～40, aluminium sesquioxide Al
2O
338～61, wherein aluminium sesquioxide divides secondary to add, and adds 33～51 of its weight part for the first time, add for the second time 5～10 of its weight part, wherein the particle diameter of aluminium sesquioxide is 0.5～1 μ m, and the particle diameter of rutile is 0.5～1 μ m, and the particle diameter of sepiolite is 0.5～1 μ m;
Adopt mill three to forge two technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling:
At first carry out the calcining first time: with Al
2O
3, SiO
2, TiO
2, four kinds of raw materials of CaO mix, wherein the aluminium sesquioxide add-on is 25～38 of its weight part, Al
2O
3And TiO
2Mol ratio be 1: 1, with the material that mixes grinding in ball grinder 14～18 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, and cumulative volume is no more than 1/2 of ball mill useful volume, after the grinding, puts into baker and carries out drying, be 10～15 hours time of drying, drying temperature is 80～100 ℃, makes its water content＜1%, with the exsiccant material through 1350～1400 ℃ of high-temperature calcinations and under this temperature, be incubated 4～6 hours;
Calcining for the second time: with particle diameter is the rutile ultra-fine micropowder of 0.5～1 μ m, particle diameter be 0.5～1 μ m be that three kinds of raw materials of sepiolite of 0.5～1 μ m mix with the first sintering body through 4～6 hours aluminium sesquioxide of 1440-1460 ℃ of high-temperature calcination and particle diameter, wherein the aluminium sesquioxide add-on is 5～10 of its weight part, with the material that mixes grinding in ball grinder 14～18 hours, ball wherein, the volume ratio of material and water is 4: 2: 1, ground material is put into baker carry out drying, be 10～15 hours time of drying, drying temperature is 80～100 ℃, makes its water content＜1%;
Material after grinding 20～24 hours internal heating to 1550～1580 ℃, this temperature lower calcination 3～7 hours, is ground to 0.1～0.8 μ m with ball mill with sintered compact at last, thereby obtains low reunite, high-purity, superfine high melt polymeric material.
The present invention's calcination for the second time is when temperature is from 1550～1300 ℃ after 3～7 hours, and the period is 5～7 hours, and temperature is during from 1280～750 ℃, and the period is 8～12 hours.
Positively effect of the present invention is as follows: the high melt polymeric material that adopts explained hereafter of the present invention, two big shortcomings of aluminium titanates have been overcome, promptly overcome its three axial thermal expansion coefficient difference greatly and the shortcoming of poor heat stability, make it produce qualitative leap, thereby obtain a kind of stable performance, be widely used, technology of the present invention has been selected six kinds of materials, adopts chemical synthesis process, mill three is forged two production technique and is prepared and a kind ofly can substitute and be better than platinum in specified range, alloy, iron and steel, special cermacis, ceramic---the JS high melt polymeric material of most advanced and sophisticated fire-resistant equipment etc.
Adopt the high melt polymeric material fusing point height (2000 ± 10 ℃) of explained hereafter of the present invention, thermal shock resistance good (1650/20 ℃ 38 times do not split), folding strength height (135MPa), thermal expansivity is low by { 0.16～0.6 * 10
-6/ ℃ (RT～1000 ℃) }, adopt the unique high-performance of high melt polymeric material of explained hereafter of the present invention can be widely used in various fields such as industrial thermometric, metallurgy, chemical industry, glass, pottery, automobile making, environmental protection.
The high melt polymeric material physical and chemical index is as shown in the table:
| Void content/% | The close g/cm3 of body | Folding strength MPa | Thermal conductivity w/m.k (600 ℃～800 ℃) | Thermal expansivity/℃ (RT～1000 ℃) |
| 3～6 | 3.0～3.89 | 60～135 | 1～1.5 | 0.16～0.6×10 -6 |
In the castingprocesses of the cobalt Chromium Stainless Steel alloy tooth base of oral cavity tooth section metal ceramic prosthesis, the crucible that the molten alloy ingot is used is a consumable material of introducing the high frequency casting machine, and the sector consumes 150,000 dollars of this kind of import crucibles every year approximately.The crucible working temperature is risen sharply to 1650 ℃ by room temperature, thermal shocking degree height, domestic relevant producer carried out the experiment of mullite, trichroite, fused quartz matter crucible, through once using the damage of thermal shock cracking promptly takes place mostly, and reusable 5 times of external product, the high melting polymerized material crucible that adopts process trial of the present invention is when Shijiazhuang hospital melting cobalt Chromium Stainless Steel alloy casting tooth base, 1650 ℃ of molten steel temperatures, using not generation to ftracture through 38 times damages, far exceeds the requirement that predetermined crucible uses 5 times.
Riser pipe is one of key part on the air injection machine, in the aluminum melt of bottom insertion air injection machine sealed crucible (700～900 ℃ of temperature), the intervalve that the low pressure die-casting machine mold cavity in upper end links to each other joins, apply the dry air of certain pressure to aluminium liquid liquid level every 3～5min air injection machine, aluminium liquid carried in the riser pipe flow in the mold cavity, carry out intermittently, periodically casting.The riser pipe sectional area is all bigger, the aluminum melt flow is big, but flow velocity is not high, so require riser pipe must have heatproof, the liquid of anti-aluminium erosive characteristic, general demestic user requires the online normal work-ing life of ceramic lift tube greater than one month, the riser pipe that adopts technology high melt polymeric material of the present invention to make uses by certain company, and its life-span is all greater than 60 days.
In glass fiber industry, compare with platinum crucible by the glass crucible that adopts technology high melt polymeric material of the present invention to make, the life-span is its 3～5 times, and price be its 1%, and have a power failure and do not scrap, be the production equipment special of glass manufacturer first-selection.
Description of drawings
Accompanying drawing 1 is high melt polymeric material preparation technology schema of the present invention
Accompanying drawing 2 is technology of the present invention calcination temperature control for the second time graphic representation
Embodiment
| Material name | Rutile | Quartzy | Sepiolite | Aluminum oxide | Calcium oxide | Titanium dioxide |
| Content | 2.5～7 | 5～10 | 5～15 | 38～61 | 2～6 | 26～40 |
(1) kind of the material table composed as follows of filling a prescription:
(2) technology:
Calcining for the first time:
With Al
2O
3, TiO
2, quartzy, four kinds of raw materials of CaO mix, Al wherein
2O
3: TiO
2=1: 1 (mol ratio), (ball: material: water=4: 2: 1), and cumulative volume was no more than 1/2 of this equipment useful volume in 14～18 hours in grinding in ball grinder with the material that mixes.After the grinding, put into baker and carry out drying (10～15h, 80～100 ℃), make its water content＜1%.
The exsiccant material through 1350～1400 ℃ of high-temperature calcinations, is incubated 3～6 hours.Al during this period
2O
3With TiO
2Reaction generates Al
2TiO
5, CaO and Al
2TiO
5Form sosoloid and suppressed Al
2TiO
5Decomposition; SiO
2Have dual function: the one, with part A l
2O
3Reaction generates mullite phase (3Al
2O
32SiO
2), Si wherein
4+At high temperature be diffused into and displacement take place in this crystal or add the crack reaction, produce the solid crystal that melts, stablized lattice, and the difference of thermal expansion causes mullite crystal grain to Al
2TiO
5The crystalline stress plays constraint Ti
4+, Al
3+Effect, suppressed the distortion of being heated of lattice, improved its intensity and thermostability; The 2nd, replace Al
2TiO
5Middle part Al
3+Form sosoloid and produce the room, improve its thermostability with this; A spot of Si
4+Replace Ti
4+, form MgTiSiO
5Sosoloid can effectively improve the stability of aluminium titanates.
Calcining for the second time:
With import rutile ultra-fine micropowder, mix with the first sintering body through aluminum oxide and three kinds of raw materials of high-quality sepiolite of 1450 ℃ of high-temperature calcinations.(ball: material: water=4: 2: 1), and cumulative volume was no more than 1/2 of ball mill useful volume in 14～18 hours in grinding in ball grinder with the material that mixes.Ground material is put into baker carry out drying (10～15h, 80～100 ℃), make its water content＜1%.
Through 1550～1580 ℃ of high-temperature calcinations, temperature control sees the temperature control curve table for details with the material after grinding, and the material after being about to grind is 20～24 hours internal heating to 1550～1580 ℃, this temperature lower calcination 3～7 hours, and the Mg in this process in the sepiolite
2+, Si
4+Enter and replace Al in the lattice
3+Ion enters octahedron, and is smaller comparatively speaking at the oscillation space of equilibrium theory of tide because these ionic volume ratios are big, is subjected to ionic constraint on every side stronger.When temperature raises, though ion obtains energy, owing to, played stable Al in conjunction with closely also just being difficult for leaving the equilibrium theory of tide
2TiO
5The effect of lattice.And MgO in the sepiolite and rutile form sosoloid, make that the electric charge in the entire structure reaches balance easily, because
MgO in the sepiolite also can be at Al
2TiO
5Middle solid solution displaces Al
2O
3, reach the self-compensation situation charge balance in the interstitial ion mode, help the balance of structure more, and make its lattice parameter increase; Superfluous magnesium oxide and aluminum oxide reaction generate spinel, and there are the grain growth that hinders aluminium titanates on the crystal boundary in spinel and aluminum oxide, and reduction domain structure reduces the crystal boundary cracking, thereby obtains low intensified-sintered body of reuniting; Fe
3+Replace part A L
3+Form sosoloid, and Fe
3+Radius greater than Al
3+Radius, can suppress its thermolysis, the stability of sosoloid is improved, and adds a certain amount of ferric oxide and can not improve the material coefficient of thermal expansion coefficient.Fe in addition
2O
3Also can be used as sintering aid, improve the amount of liquid phase under the high temperature, solid state reaction is carried out under the effect of liquid phase flow mass transport mechanism, promote high melt polymeric material to generate and densification.Because the reaction of magnesium oxide and aluminum oxide generates spinel in calcination process, more because the existence of spinel and aluminum oxide, make that crystal grain is difficult to grow up, with ball mill sintered compact is ground to 0.1～0.8 μ m at last, thereby obtain low reunite, high-purity, superfine high melt polymeric material.
(3), technology
The present invention adopts unique mill three to forge two Technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling.Make the advantage of each raw material in novel material, find full expression.
Temperature Influence: the present invention has carried out controlling (seeing temperature control curve figure for details) to it on temperature, in the different stages different rate temperature changes is arranged, the advantage that so more helps each raw material is embodied more fully and is reduced the appearance that other can avoid shortcoming.Fast cooling during as 1550～1300 ℃ prevents that mullite crystal from becoming coarse-grain; When to 1280～750 ℃, this moment is the transition temperature of solid-liquid just, and slowly cooling.I.e. calcination for the second time is when temperature is from 1550～1300 ℃ after 3～7 hours, and the period is 5～7 hours, and temperature is during from 1280～750 ℃, and the period is 8～12 hours.
The influence of granularity: this invention milling time is elected 16 hours as, that is because of the prolongation along with milling time, its bending strength increases to some extent, the sample bending strength of grinding 16h reaches 135Mpa, and after surpassing 16h, bending strength reduces thereupon, when being ground to 20h, bending strength drops to 78.0Mpa, so adopted this time of 16h in the invention.
Ball milling adopts self-control extra-fine grinding equipment for the third time, and its energy directly acts on grinding medium, but not the big and heavy urceolus of conventional mill.Used grinding medium size is little, and levigate speed is fast.Material and grinding medium are stirred by the vertical center axis that has horizontal agitator, rely on surging force and shearing force that material is levigate, and having little characteristics of particle size distribution range, another characteristics of this grinding machine are to have adopted pottery that a series of no ironys pollute and polymkeric substance as grinding medium.
The contriver is through exploratory development for many years, and comprehensive multiple properties of materials adopts six kinds of purity height, and the material of fine size synthesizes this type material, makes the advantage of used material obtain performance as much as possible; Fully played the advantage of each material especially by three two the technology of forging of grinding at process aspect, by home-built equipment this material is ground to the granularity of 0.1～0.5 μ m at last, this itself is exactly a kind of qualitative leap to a certain extent, and has obtained a kind of material species of novel concept.
Embodiment 1:
The present invention adopts following ratio of weight and number component: rutile 2.5, quartzy SiO
25, sepiolite 4MgO6SiO
22H
2O 15, calcium oxide CaO 2, titanium dioxide TiO
240, aluminium sesquioxide Al
2O
338-61, wherein aluminium sesquioxide divides secondary to add, and adds 33～51 of its weight part for the first time, adds 5～10 of its weight part for the second time, and wherein the particle diameter of aluminium sesquioxide is 0.5 μ m, and the particle diameter of rutile is 0.8 μ m, and the particle diameter of sepiolite is 1 μ m;
Adopt mill three to forge two technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling:
At first carry out the calcining first time: with Al
2O
3, SiO
2, TiO
2, four kinds of raw materials of CaO mix Al
2O
3And TiO
2Mol ratio be 1: 1, with the material that mixes grinding in ball grinder 14 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, and cumulative volume is no more than 1/2 of ball mill useful volume, after the grinding, puts into baker and carries out drying, be 15 hours time of drying, drying temperature is 80 ℃, makes its water content＜1%, and the exsiccant material is incubated 6 hours through 1350 ℃ of high-temperature calcinations and under this temperature;
Calcining for the second time: with particle diameter be rutile ultra-fine micropowder, the particle diameter of 0.8 μ m be 0.5 μ m be that three kinds of raw materials of sepiolite of 0.5 μ m mix with the first sintering body through 5 hours aluminium sesquioxide of 1460 ℃ of high-temperature calcinations and particle diameter, with the material that mixes grinding in ball grinder 16 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, ground material is put into baker carry out drying, be 13 hours time of drying, drying temperature is 90 ℃, makes its water content＜1%;
Material after grinding at 20 hours internal heating to 1550 ℃, this temperature lower calcination 7 hours, is ground to 0.2 μ m with ball mill with sintered compact at last, thereby obtains low reunite, high-purity, superfine high melt polymeric material.
The present invention's calcination for the second time is when temperature is from 1550～1300 ℃ after 7 hours, and the period is 6 hours, and temperature is during from 1280～750 ℃, and the period is 10 hours.
Embodiment 2:
Adopt following ratio of weight and number component: rutile 7, quartzy SiO
210, sepiolite 4MgO6SiO
22H
2O5, calcium oxide CaO 6, titanium dioxide TiO
226, aluminium sesquioxide Al
2O
338～61, wherein aluminium sesquioxide divides secondary to add, and adds 33～51 of its weight part for the first time, adds 5～10 of its weight part for the second time, and wherein the particle diameter of aluminium sesquioxide is 1 μ m, and the particle diameter of rutile is 0.5 μ m, and the particle diameter of sepiolite is 0.5 μ m;
Adopt mill three to forge two technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling:
At first carry out the calcining first time: with Al
2O
3, SiO
2, TiO
2, four kinds of raw materials of CaO mix Al
2O
3And TiO
2Mol ratio be 1: 1, with the material that mixes grinding in ball grinder 18 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, and cumulative volume is no more than 1/2 of ball mill useful volume, after the grinding, puts into baker and carries out drying, be 10 hours time of drying, drying temperature is 100 ℃, makes its water content＜1%, and the exsiccant material is incubated 4 hours through 1400 ℃ of high-temperature calcinations and under this temperature;
Calcining for the second time: with particle diameter be rutile ultra-fine micropowder, the particle diameter of 0.5 μ m be 0.8 μ m be that three kinds of raw materials of sepiolite of 0.8 μ m mix with the first sintering body through 4 hours aluminium sesquioxide of 1440 ℃ of high-temperature calcinations and particle diameter, with the material that mixes grinding in ball grinder 18 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, ground material is put into baker carry out drying, be 10 hours time of drying, drying temperature is 100 ℃, makes its water content＜1%;
Material after grinding at 24 hours internal heating to 1580 ℃, this temperature lower calcination 3 hours, is ground to 0.8 μ m with ball mill with sintered compact at last, thereby obtains low reunite, high-purity, superfine high melt polymeric material.
The present invention's calcination for the second time is when temperature is from 1550～1300 ℃ after 3 hours, and the period is 5 hours, and temperature is during from 1280～750 ℃, and the period is 12 hours.
Embodiment 3:
Adopt following ratio of weight and number component: rutile 5, quartzy SiO
28, sepiolite 4MgO6SiO
22H
2O10, calcium oxide CaO 4, titanium dioxide TiO
235, aluminium sesquioxide Al
2O
338～61, wherein aluminium sesquioxide divides secondary to add, and adds 33～51 of its weight part for the first time, adds 5～10 of its weight part for the second time, and wherein the particle diameter of aluminium sesquioxide is 0.8 μ m, and the particle diameter of rutile is 1 μ m, and the particle diameter of sepiolite is 0.8 μ m;
Adopt mill three to forge two technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling:
At first carry out the calcining first time: with Al
2O
3, SiO
2, TiO
2, four kinds of raw materials of CaO mix Al
2O
3And TiO
2Mol ratio be 1: 1, with the material that mixes grinding in ball grinder 16 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, and cumulative volume is no more than 1/2 of ball mill useful volume, after the grinding, puts into baker and carries out drying, be 13 hours time of drying, drying temperature is 90 ℃, makes its water content＜1%, and the exsiccant material is incubated 5 hours through 1370 ℃ of high-temperature calcinations and under this temperature;
Calcining for the second time: with particle diameter be rutile ultra-fine micropowder, the particle diameter of 1 μ m be 1 μ m be that three kinds of raw materials of sepiolite of 1 μ m mix with the first sintering body through 6 hours aluminium sesquioxide of 1450 ℃ of high-temperature calcinations and particle diameter, with the material that mixes grinding in ball grinder 14 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, ground material is put into baker carry out drying, be 15 hours time of drying, drying temperature is 80 ℃, makes its water content＜1%;
Material after grinding at 22 hours internal heating to 1575 ℃, this temperature lower calcination 5 hours, is ground to 0.6 μ m with ball mill with sintered compact at last, thereby obtains low reunite, high-purity, superfine high melt polymeric material.
The present invention's calcination for the second time is when temperature is from 1550～1300 ℃ after 5 hours, and the period is 7 hours, and temperature is during from 1280～750 ℃, and the period is 8 hours.
Embodiment 4:
The present invention adopts following ratio of weight and number component: rutile 5.94, quartzy SiO
28, sepiolite 4MgO6SiO
22H
2O 15, calcium oxide CaO 6, titanium dioxide TiO
231.4, aluminium sesquioxide Al
2O
348, wherein aluminium sesquioxide divides secondary to add, and adds 40 of its weight part for the first time, adds 8 of its weight part for the second time, and wherein the particle diameter of aluminium sesquioxide is 0.5 μ m, and the particle diameter of rutile is 0.8 μ m, and the particle diameter of sepiolite is 1 μ m;
Adopt mill three to forge two technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling:
At first carry out the calcining first time: with Al
2O
3, SiO
2, TiO
2, four kinds of raw materials of CaO mix Al
2O
3And TiO
2Mol ratio be 1: 1, with the material that mixes grinding in ball grinder 14 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, and cumulative volume is no more than 1/2 of ball mill useful volume, after the grinding, puts into baker and carries out drying, be 15 hours time of drying, drying temperature is 80 ℃, makes its water content＜1%, and the exsiccant material is incubated 6 hours through 1350 ℃ of high-temperature calcinations and under this temperature;
Calcining for the second time: with particle diameter be rutile ultra-fine micropowder, the particle diameter of 0.8 μ m be 0.5 μ m be that three kinds of raw materials of sepiolite of 0.5 μ m mix with the first sintering body through 5 hours aluminium sesquioxide of 1460 ℃ of high-temperature calcinations and particle diameter, with the material that mixes grinding in ball grinder 16 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, ground material is put into baker carry out drying, be 13 hours time of drying, drying temperature is 90 ℃, makes its water content＜1%;
Material after grinding at 20 hours internal heating to 1550 ℃, this temperature lower calcination 7 hours, is ground to 0.2 μ m with ball mill with sintered compact at last, thereby obtains low reunite, high-purity, superfine high melt polymeric material.
The present invention's calcination for the second time is when temperature is from 1550～1300 ℃ after 7 hours, and the period is 6 hours, and temperature is during from 1280～750 ℃, and the period is 10 hours.
Embodiment 5:
The present invention adopts following ratio of weight and number component: rutile 2.5, quartzy SiO
210, sepiolite 4MgO6SiO
22H
2O 5, calcium oxide CaO 2, titanium dioxide TiO
226, aluminium sesquioxide Al
2O
338, wherein aluminium sesquioxide divides secondary to add, and adds 33 of its weight part for the first time, adds 5 of its weight part for the second time, and wherein the particle diameter of aluminium sesquioxide is 1 μ m, and the particle diameter of rutile is 0.5 μ m, and the particle diameter of sepiolite is 0.5 μ m;
Adopt mill three to forge two technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling:
At first carry out the calcining first time: with Al
2O
3, SiO
2, TiO
2, four kinds of raw materials of CaO mix Al
2O
3And TiO
2Mol ratio be 1: 1, with the material that mixes grinding in ball grinder 18 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, and cumulative volume is no more than 1/2 of ball mill useful volume, after the grinding, puts into baker and carries out drying, be 10 hours time of drying, drying temperature is 100 ℃, makes its water content＜1%, and the exsiccant material is incubated 4 hours through 1400 ℃ of high-temperature calcinations and under this temperature;
Calcining for the second time: with particle diameter be rutile ultra-fine micropowder, the particle diameter of 0.5 μ m be 0.8 μ m be that three kinds of raw materials of sepiolite of 0.8 μ m mix with the first sintering body through 4 hours aluminium sesquioxide of 1440 ℃ of high-temperature calcinations and particle diameter, with the material that mixes grinding in ball grinder 18 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, ground material is put into baker carry out drying, be 10 hours time of drying, drying temperature is 100 ℃, makes its water content＜1%;
Material after grinding at 24 hours internal heating to 1580 ℃, this temperature lower calcination 3 hours, is ground to 0.8 μ m with ball mill with sintered compact at last, thereby obtains low reunite, high-purity, superfine high melt polymeric material.
The present invention's calcination for the second time is when temperature is from 1550～1300 ℃ after 3 hours, and the period is 5 hours, and temperature is during from 1280～750 ℃, and the period is 12 hours.
Embodiment 6:
The present invention adopts following ratio of weight and number component: rutile 7, quartzy SiO
25, sepiolite 4MgO6SiO
22H
2O 10, calcium oxide CaO 4.42, titanium dioxide TiO
240, aluminium sesquioxide Al
2O
361, wherein aluminium sesquioxide divides secondary to add, and adds 51 of its weight part for the first time, adds 10 of its weight part for the second time, and wherein the particle diameter of aluminium sesquioxide is 0.8 μ m, and the particle diameter of rutile is 1 μ m, and the particle diameter of sepiolite is 0.8 μ m;
Adopt mill three to forge two technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling:
At first carry out the calcining first time: with Al
2O
3, SiO
2, TiO
2, four kinds of raw materials of CaO mix Al
2O
3And TiO
2Mol ratio be 1: 1, with the material that mixes grinding in ball grinder 16 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, and cumulative volume is no more than 1/2 of ball mill useful volume, after the grinding, puts into baker and carries out drying, be 13 hours time of drying, drying temperature is 90 ℃, makes its water content＜1%, and the exsiccant material is incubated 5 hours through 1370 ℃ of high-temperature calcinations and under this temperature;
Calcining for the second time: with particle diameter be rutile ultra-fine micropowder, the particle diameter of 1 μ m be 1 μ m be that three kinds of raw materials of sepiolite of 1 μ m mix with the first sintering body through 6 hours aluminium sesquioxide of 1450 ℃ of high-temperature calcinations and particle diameter, with the material that mixes grinding in ball grinder 14 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, ground material is put into baker carry out drying, be 15 hours time of drying, drying temperature is 80 ℃, makes its water content＜1%;
Material after grinding at 22 hours internal heating to 1575 ℃, this temperature lower calcination 5 hours, is ground to 0.6 μ m with ball mill with sintered compact at last, thereby obtains low reunite, high-purity, superfine high melt polymeric material.
The present invention's calcination for the second time is when temperature is from 1550～1300 ℃ after 5 hours, and the period is 7 hours, and temperature is during from 1280～750 ℃, and the period is 8 hours.
Claims (2)
1, a kind of production technique of high melt polymeric material is characterized in that adopting following ratio of weight and number component: rutile 2.5～7, quartzy SiO
25～10, sepiolite 4MgO6SiO
22H
2O 5～15, calcium oxide CaO 2～6, titanium dioxide TiO
226～40, aluminium sesquioxide Al
2O
338～61, wherein aluminium sesquioxide divides secondary to add, and adds 33～51 of its weight part for the first time, add for the second time 5～10 of its weight part, wherein the particle diameter of aluminium sesquioxide is 0.5～1 μ m, and the particle diameter of rutile is 0.5～1 μ m, and the particle diameter of sepiolite is 0.5～1 μ m;
Adopt mill three to forge two technologies, i.e. ball milling → calcining → ball milling → calcining → ball milling:
At first carry out the calcining first time: with Al
2O
3, SiO
2, TiO
2, four kinds of raw materials of CaO mix, wherein the aluminium sesquioxide add-on is 33～51 of its weight part, Al
2O
3And TiO
2Mol ratio be 1: 1, with the material that mixes grinding in ball grinder 14～18 hours, wherein the volume ratio of ball, material and water is 4: 2: 1, and cumulative volume is no more than 1/2 of ball mill useful volume, after the grinding, puts into baker and carries out drying, be 10～15 hours time of drying, drying temperature is 80～100 ℃, makes its water content＜1%, with the exsiccant material through 1350～1400 ℃ of high-temperature calcinations and under this temperature, be incubated 4～6 hours;
Calcining for the second time: with particle diameter is the rutile ultra-fine micropowder of 0.5～1 μ m, particle diameter be 0.5～1 μ m be that three kinds of raw materials of sepiolite of 0.5～1 μ m mix with the first sintering body through 4～6 hours aluminium sesquioxide of 1440-1460 ℃ of high-temperature calcination and particle diameter, wherein the aluminium sesquioxide add-on is 5～10 of its weight part, with the material that mixes grinding in ball grinder 14～18 hours, ball wherein, the volume ratio of material and water is 4: 2: 1, ground material is put into baker carry out drying, be 10～15 hours time of drying, drying temperature is 80～100 ℃, makes its water content＜1%;
Material after grinding 20～24 hours internal heating to 1550～1580 ℃, this temperature lower calcination 3～7 hours, is ground to 0.1～0.8 μ m with ball mill with sintered compact at last, thereby obtains low reunite, high-purity, superfine high melt polymeric material.
2, the production technique of a kind of high melt polymeric material according to claim 1, when it is characterized in that calcination for the second time temperature be from 1550～1300 ℃ after 3～7 hours, period is 5～7 hours, and temperature is during from 1280～750 ℃, and the period is 8～12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100123914A CN100402436C (en) | 2006-01-27 | 2006-01-27 | High melt polymeric material manufacturing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100123914A CN100402436C (en) | 2006-01-27 | 2006-01-27 | High melt polymeric material manufacturing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1807256A true CN1807256A (en) | 2006-07-26 |
| CN100402436C CN100402436C (en) | 2008-07-16 |
Family
ID=36839382
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100123914A Expired - Fee Related CN100402436C (en) | 2006-01-27 | 2006-01-27 | High melt polymeric material manufacturing process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100402436C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944019B (en) * | 2006-10-20 | 2010-06-09 | 王丕轩 | Method for preparing high melting polymerized material crucible using gypsum mould slip casting method |
| CN1943920B (en) * | 2006-10-20 | 2011-01-05 | 王丕轩 | Method for producing low pressure cast aluminum liquid lift pipe |
| CN101654497B (en) * | 2009-09-27 | 2012-10-17 | 陕西科技大学 | Meerschaum polymer and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4041061A1 (en) * | 1989-12-22 | 1991-06-27 | Siemens Ag | Aluminium titanate ceramic burner plater for flat gas burner - has good resistance to corrosion and thermal shock and low thermal conductivity |
| JP3192700B2 (en) * | 1991-09-30 | 2001-07-30 | 日本碍子株式会社 | Aluminum titanate ceramics and method for producing the same |
| JP3489030B1 (en) * | 2002-04-26 | 2004-01-19 | 勉 福田 | Method for producing aluminum titanate-based sintered body |
| USRE42352E1 (en) * | 2002-11-01 | 2011-05-10 | Ohcera Co., Ltd. | Method for producing aluminum magnesium titanate sintered product |
-
2006
- 2006-01-27 CN CNB2006100123914A patent/CN100402436C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944019B (en) * | 2006-10-20 | 2010-06-09 | 王丕轩 | Method for preparing high melting polymerized material crucible using gypsum mould slip casting method |
| CN1943920B (en) * | 2006-10-20 | 2011-01-05 | 王丕轩 | Method for producing low pressure cast aluminum liquid lift pipe |
| CN101654497B (en) * | 2009-09-27 | 2012-10-17 | 陕西科技大学 | Meerschaum polymer and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100402436C (en) | 2008-07-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108083779B (en) | Rare earth alumina ceramic composite material and preparation method thereof | |
| JP5999715B2 (en) | Method for producing silicon carbide powder | |
| CN108359825B (en) | A kind of preparation method of ceramics-graphene enhancing Cu-base composites | |
| CN103276253B (en) | A kind of Low-cost Al-Ti-B refiner and preparation method thereof | |
| CN103361532B (en) | Sosoloid toughened metal ceramic and preparation method thereof | |
| CN101357843A (en) | Alumina titanate ceramica lift tube preparation method | |
| CN103539467A (en) | Mechanically-pressed carbon-free corundum spinel ladle brick as well as preparation method thereof | |
| CN103641447B (en) | A kind of preparation method of engineering ceramics acid-fast alkali-proof container | |
| CN101687711A (en) | A sintered product based on alumina and chromium oxide | |
| CN102965590B (en) | A kind of brazing and preparation thereof | |
| CN109704774A (en) | A kind of preparation method of the bottom hearth of blast furnace high thermal conductivity castable instead of carbon brick | |
| CN100371246C (en) | High melt polymeric material | |
| CN103172390A (en) | Method for producing hydration-resistant high-purity calcium oxide crucible | |
| CN108911719A (en) | A kind of composite ceramics | |
| CN100582035C (en) | Method for preparing cristobalite by calcining quartz | |
| CN1807256A (en) | High melt polymeric material manufacturing process | |
| CN100494507C (en) | High-density semi-graphite cathode carbon block and method for producing same | |
| CN104451325A (en) | Process for preparing Mo2FeB2-based metal ceramic | |
| CN107244930A (en) | A kind of resistance to molten iron corrodes blast furnace carbon brick and preparation method thereof | |
| CN104495845B (en) | A kind of pure Fe3the preparation technology of C block | |
| CN102557690B (en) | Preparation method for corundum baddeleyite eutectoid composite nonswirl nozzle inner layer | |
| CN102560200A (en) | Aluminum-titanium-iron-carbon-boron intermediate alloy and preparation method thereof | |
| CN201885567U (en) | Graphite melting crucible with built-in ceramic crucible | |
| CN112919470B (en) | Production process of titanium silicon carbide | |
| CN103395752A (en) | Preparation method for boron nitride micron solid ball |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Hebei Yingdu Composite Materials Co., Ltd.? Assignor: Wang Hongzeng Contract fulfillment period: 2008.10.20 to 2024.10.20 contract change Contract record no.: 2008130000178 Denomination of invention: High melt polymeric material manufacturing process Granted publication date: 20080716 License type: Exclusive license Record date: 20081226 |
|
| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.20 TO 2024.10.20; CHANGE OF CONTRACT Name of requester: HEBEI YINGDOU COMPOUND MATERIALS CO., LTD. Effective date: 20081226 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20090320 Address after: No 14 Jie Lu, Hebei, Qinghe County Patentee after: Hebei Yingdu Composite Materials Co., Ltd.? Address before: No 14 Jie Lu, Hebei, Qinghe County Patentee before: Wang Hongzeng |
|
| ASS | Succession or assignment of patent right |
Owner name: HEBEI YINGDOU COMPOUND MATERIALS CO., LTD. Free format text: FORMER OWNER: WANG HONGZENG Effective date: 20090320 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080716 Termination date: 20150127 |
|
| EXPY | Termination of patent right or utility model |