CN102942374A - Dehydration and curing processing method of gel casting moulding blank body - Google Patents
Dehydration and curing processing method of gel casting moulding blank body Download PDFInfo
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- CN102942374A CN102942374A CN2012104636873A CN201210463687A CN102942374A CN 102942374 A CN102942374 A CN 102942374A CN 2012104636873 A CN2012104636873 A CN 2012104636873A CN 201210463687 A CN201210463687 A CN 201210463687A CN 102942374 A CN102942374 A CN 102942374A
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Abstract
The invention provides a dehydration and curing processing method of gel casting moulding blank body, belonging to the technical field of gel moulding preparation. The method comprises the following steps of: mixing an organic monomer and a cross-linking agent into a premixed solution of which the mass fraction is 5-10%; then, mixing silicic acid aluminum refractory powder and the premixed solution into slurry of which the volume concentration is 30-70%; performing ball-milling to the slurry, after ball-milling, adding an initiator and a catalyst into the slurry, casting a mould, curing slurry gel, and demoulding to obtain the blank body; and placing the blank body into a dehydrating agent ethanol solution of which the volume concentration is 80% to be dehydrated and cured for 8-10h to complete dehydration and curing of the blank body. According to the invention, during the gel curing process, the organic monomer and the cross-linking agent of the slurry are cross-linked to form the gel to form the slurry; and during the dehydration and curing processes, through replacing the solution, the concentration of the organisms in the blank body rises, so that the organisms which are not cross-linked are cross-linked and cured, and the moisture in the blank body can be removed.
Description
Technical field
The invention belongs to the gel forming preparing technical field, be specifically related to a kind of dehydrating and curing treatment process of gel pouring moulding base substrate.
Background technology
Gel pouring moulding is that early 1990s is by a kind of forming technique of U.S. Oak Ridge National Laboratory researchist invention, for the moulding of pottery and fire resistive material product.This method at first is scattered in slurry in the solution that contains organic monomer, make high solid volume fraction〉50% suspension, then inject definite shape without punch die, under certain catalysis, temperature condition, the organic monomer polymerization, form gel, thereby cause the suspensoid original position to be solidified, can obtain the higher base substrate of intensity finally by super-dry.The object that is fit to the moulding complicated shape.Two kinds of methods of aqueous gel casting and anhydrous gel casting have been developed at present.But, contain more water, organism etc. in the aqueous gel casting base substrate, there are the shortcomings such as drying conditions is harsh, time of drying is long.Thereby, in drying process, ftracture and be out of shape for eliminating the gel pouring moulding base substrate, people have carried out widely and have studied, and have more patent literature.Chinese patent CN200910047501 has announced a kind of method of impelling crack healing in the gelatin casting molding biscuit, the wet biscuit of gel pouring moulding is placed in the constant temperature constant humidity baking oven, at 50～70 ℃, relative humidity is dry 24～96h in 80～95% environment, after the crackle that impels sample to produce effectively heals, adopt again multistep drying method to obtain flawless gelatin casting biscuit.Chinese patent CN101486579A has announced a kind of drying means of gel injection moulding blank, be immersed in base substrate or base substrate in the dry solvent of low-boiling-point organic compound and water preparation together with mould, take out after leaving standstill 1 ~ 48h, again 1～48h complete drying under the state of nature.
The key of gel pouring moulding is to prepare the slurry of low viscosity high solid loading, Chinese patent CN100384783C has announced a kind of method that gel pouring moulding prepares the slurry of ceramic city body of improving, the acrylamide that replaces take N-or Methacrylamide are as organic monomer, N N '-methylene-bisacrylamide is linking agent, the water-soluble azo of salt-independent shape is that initiator and water are mixed with 2～50wt% premixed liquid, adds the slurry that 10～100wt% premixed liquid is mixed with high solid loading to ceramic powder under agitation condition.Chinese patent CN1166588C has announced the preparation method of high solid loading oxide slurry in a kind of gel pouring moulding technique, take a kind of vinylformic acid-acrylate-phosphonic acids-sulfonic acid tetrapolymer as dispersion agent, prepare solid content and be 55% alumina slurry and solid load and reach 50% zirconia slurry.
Be widely used at porous ceramics and fire resisting material field casting, Chinese patent CN101417888A has announced a kind of porous light heat-insulation and heat-preservation material and preparation method thereof, take Wingdale or lime, kyanite, the low clunch of calcining high alumina, commercial alumina, semi-hydrated gypsum as raw material, add organic/inorganic compounding pore-forming material, by half-dried vibrating casting moulding, a step reaction in－situ sintering is prepared principal goods and is mutually mullite phase and lime feldspar heat insulating refractory materials mutually.Chinese patent CN102659398A has announced a kind of method for preparing the lightweight magnesium-aluminum spinel lagging material, take magnesite powder or aluminum oxide powder, aluminum oxide powder as raw material, take Sodium dodecylbenzene sulfonate as whipping agent, by gel pouring moulding, 1500 ℃ ~ 1800 ℃ sintering obtain the lightweight magnesium-aluminum spinel lagging material.And the patent that relates to porous ceramics and the processing of refractory materials gel pouring moulding base substrate dehydrating and curing has no report.
The present invention proposes the dehydrating and curing process of gel pouring base substrate, and cost is low, and technique easily realizes, technological process also is easy to control.Can low-costly prepare high-performance, complicated shape porous refractory and stupalith, be applicable to the block preparation of gel pouring moulding.
Summary of the invention
The present invention is directed to the technical problem that exists in the prior art, a kind of dehydrating and curing treatment process of gel pouring moulding base substrate is provided.The not yielding or cracking of the base substrate of the method preparation and have higher intensity.And base substrate can further be prepared high-intensity porous refractory.
The dehydrating and curing treatment process concrete steps of a kind of gel pouring moulding base substrate provided by the present invention are as follows:
(1) preparation premixed liquid: organic monomer acrylamide and linking agent N N '-methylene-bisacrylamide and water mixed to be mixed with mass concentration be 5～10% premixed liquid, the mass ratio of described organic monomer acrylamide and linking agent N N '-methylene-bisacrylamide is 10:1.
(2) preparation slurry: the pH value of the premixed liquid of described step (1) preparation is adjusted to 7～10, then the aluminosillicate refractory powder is joined in the described premixed liquid and be mixed with slurry, the volumetric concentration of described aluminosillicate refractory in described slurry is 30～70%.
(3) ball milling: the slurry of step (2) preparation is placed ball grinder, and ratio of grinding media to material is (1～3): 1, and ball milling 5～20h, the rotating speed of ball mill are 500～580r/min.
(4) mould is prepared: mould inner surface is coated with the last layer releasing agent, is easy to the demoulding after making blank forming.
(5) gel pouring moulding: add combustiblematerials pore-forming material or whipping agent in the slurry behind the ball milling, and then adding initiator ammonium persulfate and catalyzer Tetramethyl Ethylene Diamine, after stirring slurry is injected mould, 5～8min gelation obtains the base substrate after the gelation under the room temperature, the add-on of described combustiblematerials pore-forming material is 50～80% of described aluminosillicate refractory quality, the add-on of described whipping agent is 0.5～2% of described aluminosillicate refractory quality, the add-on of described initiator ammonium persulfate is 2～5% of described organic monomer acrylamide quality, and described catalyzer Tetramethyl Ethylene Diamine add-on is 0.03～0.05% of described organic monomer acrylamide quality.
(6) demoulding: the base substrate after the gelation that step (5) is obtained places under the room temperature behind 8～10h, or after placing 70 ℃ of lower insulation 3～5 h, separates the base substrate that obtains after the demoulding between described base substrate and the mold wall.
(7) dehydrating and curing of base substrate: the base substrate after described step (6) demoulding is higher because of water content, quality softness and intensity are not high, need to slough part moisture in the base substrate makes uncrosslinked organism continue crosslinking curing, employing is immersed base substrate in the dewatering agent solution, carry out replacement dewatering, described dehydrating and curing concrete steps are as follows:
A: configuration dewatering agent: adopting dehydrated alcohol and water to mix to be mixed with volumetric concentration is 80% dewatering agent ethanolic soln;
B: under the room temperature, the base substrate after step (6) demoulding is placed described dewatering agent ethanolic soln, behind infuse 8～10h, finish the dehydrating and curing of described base substrate.
Described aluminosillicate refractory is any one or more mixture in mullite synthesizing, commercial alumina, silica, the calcium carbonate.
The present invention has the following advantages:
1, the present invention adopts the aqueous-based gel casting to prepare the fire-resistant and stupalith of porous, and the add-on of organic monomer and linking agent is controlled in the less scope, has simplified simultaneously loaded down with trivial details operating procedure.Raw material is mixed reduced the component segregation of material by ball milling; The slurry of certain viscosity behind the ball milling can evenly distribute through stirring at adding pore-forming material and whipping agent, makes pore can be evenly distributed in the material; Organic monomer and linking agent are evenly distributed in slurry, and after the gelation, the each several part stress equilibrium of material has reduced the material stress uneven and cause crackle or cracking, and therefore the base substrate through gel casting forming has higher intensity.
2, in base substrate dehydrating and curing process, liquid desicoant can with the uniform contact of base substrate, base substrate each several part evenly dehydration shrinks, and has reduced base substrate and has caused the distortion fracture because the dehydration of each several part is uneven.Compare with PEG solution dry base substrate technique, the speed of dehydration is obviously accelerated, and the water content of base substrate also obviously reduces behind the body drying, because dehydrated alcohol is cheap, and can widespread use.
3, behind the base substrate complete drying, base substrate has higher intensity, can carry out mechanical workout.Base substrate is after the moisture short period of time soaks, and the lower hardness of base substrate but intensity still keeps higher level can be processed accurately to base substrate, has reduced the loss of energy and material in the base substrate course of processing.
Description of drawings
Fig. 1 is the base substrate for preparing of the present invention in volumetric concentration is dehydration rate curve over time under the differing temps in 80% the dewatering agent.
Embodiment
Embodiment 1: take by weighing 15g acrylamide organic monomer, 1.5g N N '-methylene-bis propionic acid amide linking agent, be mixed with premixed liquid with 300ml water.Measure mullite synthesizing (the pine dress of 105ml, quality is 120g), Mullite Powder mixed with premixed liquid be placed in the ball grinder, ball milling took out slurry after 20 hours, added starch that 72g crosses 400 mesh sieves in the slurry as pore-forming material, after stirring, add again after the ammonium persulphate of 0.3g and 0.005g methyl ethylenediamine mix, inject mould (145mm * 25mm * 27.5mm), leave standstill 10h under the room temperature, the demoulding after separating between base substrate and the mold wall that the surface scribbles suds.Again the base substrate of the demoulding at room temperature being placed volumetric concentration is 80% ethanolic soln, and the base substrate dehydration rate reaches 30% behind the 10h as shown in Figure 1, base substrate is placed 110 ℃ of drying 5～6h, base substrate complete drying again.
Embodiment 2: the premixed liquid such as embodiment 1 preparation mass concentration 5% takes by weighing Wingdale (CaCO
399%) 35.89g, commercial alumina (Al
2O
399%) 18.35g, SiO
2(chemical pure) 25.92g ball milling mixing, measure 100ml mixing raw material (pine dress, quality is 80g) and 100ml mullite synthesizing powder (pine dress, quality is 120g), both and premixed liquid are placed ball grinder, ball milling took out slurry after 10 hours, adding the 4g Sodium dodecylbenzene sulfonate in the slurry stirs as whipping agent, after adding again 0.5g ammonium persulphate and 0.005g Tetramethyl Ethylene Diamine mixing, injection scribbles the mould (145mm * 25mm * 27.5mm) of suds, after placing 70 ℃ of environment to be incubated 4～5 hours, base substrate separates the rear demoulding with mould.It is that the base substrate dehydration rate reached 45% as shown in Figure 1, base substrate is placed 110 ℃ of drying 5～6h, base substrate complete drying again after 70 ℃ of lower seals of 80% ethanolic soln were preserved 5h that base substrate is placed volumetric concentration.
Claims (2)
1. the dehydrating and curing treatment process of a gel pouring moulding base substrate is characterized in that described method concrete steps are as follows:
(1) preparation premixed liquid: organic monomer acrylamide and linking agent N N '-methylene-bisacrylamide and water mixed to be mixed with mass concentration be 5～10% premixed liquid, the mass ratio of described organic monomer acrylamide and linking agent N N '-methylene-bisacrylamide is 10:1;
(2) preparation slurry: the pH value of the premixed liquid of described step (1) preparation is adjusted to 7～10, then the aluminosillicate refractory powder is joined in the described premixed liquid and be mixed with slurry, the volumetric concentration of described aluminosillicate refractory in described slurry is 30～70%;
(3) ball milling: the slurry of step (2) preparation is placed ball grinder, and ratio of grinding media to material is (1～3): 1, and ball milling 5～20h, the rotating speed of ball mill are 500～580r/min;
(4) mould is prepared: mould inner surface is coated with the last layer releasing agent, is easy to the demoulding after making blank forming;
(5) gel pouring moulding: add combustiblematerials pore-forming material or whipping agent in the slurry behind the ball milling, and then adding initiator ammonium persulfate and catalyzer Tetramethyl Ethylene Diamine, after stirring slurry is injected mould, 5～8min gelation obtains the base substrate after the gelation under the room temperature, the add-on of described combustiblematerials pore-forming material is 50～80% of described aluminosillicate refractory quality, the add-on of described whipping agent is 0.5～2% of described aluminosillicate refractory quality, the add-on of described initiator ammonium persulfate is 2～5% of described organic monomer acrylamide quality, and described catalyzer Tetramethyl Ethylene Diamine add-on is 0.03～0.05% of described organic monomer acrylamide quality;
(6) demoulding: the base substrate after the gelation that step (5) is obtained places under the room temperature behind 8～10h, or after placing 70 ℃ of lower insulation 3～5 h, separates the base substrate that obtains after the demoulding between described base substrate and the mold wall;
(7) dehydrating and curing of base substrate: described dehydrating and curing concrete steps are as follows:
A: configuration dewatering agent: adopting dehydrated alcohol and water to mix to be mixed with volumetric concentration is 80% dewatering agent ethanolic soln;
B: under the room temperature, the base substrate after step (6) demoulding is placed described dewatering agent ethanolic soln, behind infuse 8～10h, finish the dehydrating and curing of described base substrate.
2. dehydrating and curing treatment process according to claim 1 is characterized in that described aluminosillicate refractory is any one or more mixture in mullite synthesizing, commercial alumina, silica, the calcium carbonate.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446291A (en) * | 2014-10-21 | 2015-03-25 | 北京科技大学 | Preparation method for preparing panel by using desulfurization gypsum |
| CN105330320A (en) * | 2015-09-29 | 2016-02-17 | 洛阳暖盈电子技术有限公司 | Gel-casting process of ZrO2 toughened Al2O3 foamed ceramics |
| CN106673598A (en) * | 2017-01-05 | 2017-05-17 | 天津大学 | Preparation method of high temperature-resisting mullite fiber porous heat insulation tile |
| CN108395275A (en) * | 2018-04-04 | 2018-08-14 | 刘凡领 | A kind of preparation method of light porous marble composite brick |
| CN112358291A (en) * | 2020-11-25 | 2021-02-12 | 辽宁科技大学 | Method for synthesizing calcium hexaluminate material by gel casting |
| CN112654592A (en) * | 2018-08-27 | 2021-04-13 | 索里迪亚科技公司 | Multi-step curing of green bodies |
| CN114538898A (en) * | 2020-11-25 | 2022-05-27 | 上海三思电子工程有限公司 | Preparation method of gel-casting ceramic green body |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456535A (en) * | 2003-05-30 | 2003-11-19 | 武汉理工大学 | Process for preparing porous ceramic by water-based gel injection moulding method |
| CN101486579A (en) * | 2009-02-24 | 2009-07-22 | 中南大学 | Method for drying gel injection moulding blank |
| CN102432332A (en) * | 2011-09-26 | 2012-05-02 | 昆明理工大学 | Method for preparing aluminum oxide porous ceramics by gel-foaming method |
-
2012
- 2012-11-18 CN CN2012104636873A patent/CN102942374A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456535A (en) * | 2003-05-30 | 2003-11-19 | 武汉理工大学 | Process for preparing porous ceramic by water-based gel injection moulding method |
| CN101486579A (en) * | 2009-02-24 | 2009-07-22 | 中南大学 | Method for drying gel injection moulding blank |
| CN102432332A (en) * | 2011-09-26 | 2012-05-02 | 昆明理工大学 | Method for preparing aluminum oxide porous ceramics by gel-foaming method |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446291A (en) * | 2014-10-21 | 2015-03-25 | 北京科技大学 | Preparation method for preparing panel by using desulfurization gypsum |
| CN105330320A (en) * | 2015-09-29 | 2016-02-17 | 洛阳暖盈电子技术有限公司 | Gel-casting process of ZrO2 toughened Al2O3 foamed ceramics |
| CN106673598A (en) * | 2017-01-05 | 2017-05-17 | 天津大学 | Preparation method of high temperature-resisting mullite fiber porous heat insulation tile |
| CN108395275A (en) * | 2018-04-04 | 2018-08-14 | 刘凡领 | A kind of preparation method of light porous marble composite brick |
| CN108395275B (en) * | 2018-04-04 | 2020-12-08 | 泰州峰飞机械设备有限公司 | Preparation method of lightweight porous marble composite brick |
| CN112654592A (en) * | 2018-08-27 | 2021-04-13 | 索里迪亚科技公司 | Multi-step curing of green bodies |
| CN112654592B (en) * | 2018-08-27 | 2024-02-20 | 索里迪亚科技公司 | Multistep curing of green bodies |
| CN112358291A (en) * | 2020-11-25 | 2021-02-12 | 辽宁科技大学 | Method for synthesizing calcium hexaluminate material by gel casting |
| CN114538898A (en) * | 2020-11-25 | 2022-05-27 | 上海三思电子工程有限公司 | Preparation method of gel-casting ceramic green body |
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Application publication date: 20130227 |