CN107032754A - A kind of method that nonaqueous solvents grouting process prepares the high-grade Longquan celadon of high intensity - Google Patents

A kind of method that nonaqueous solvents grouting process prepares the high-grade Longquan celadon of high intensity Download PDF

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CN107032754A
CN107032754A CN201710260591.XA CN201710260591A CN107032754A CN 107032754 A CN107032754 A CN 107032754A CN 201710260591 A CN201710260591 A CN 201710260591A CN 107032754 A CN107032754 A CN 107032754A
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longquan celadon
slurry
grade
organic solvent
soil
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施群
周灵
方明
李德胜
叶晓平
陈贤生
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Lishui University
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    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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Abstract

The invention discloses a kind of method that nonaqueous solvents grouting process prepares the high-grade Longquan celadon of high intensity, comprise the following steps:Organic solvent is measured first as decentralized medium, then a certain amount of dragon's fountain soil is scattered in solvent, add dispersant, organic solvent slip casting slurry is obtained after stirring, through ball grinding stirring to slurry hybrid reaction it is complete after, slurry is aged, injection forming, biscuiting desolvation are handled, the high-grade Longquan celadon of high intensity can be made through heat treatment after glazing.This invention simplifies traditional Longquan celadon into porcelain process technology scheme, low production cost, reaction time is short, traditional grouting process is broken by adding the thinking that aqueous solvent is molded, the surface tension that overcomes water is excessive, the problem of easily cause particle agglomeration in drying process, form hole, the intensity of Longquan celadon is substantially increased, the key issue of the application of restriction Longquan celadon and development is thoroughly solved, has broad application prospects.

Description

A kind of method that nonaqueous solvents grouting process prepares the high-grade Longquan celadon of high intensity
Technical field
The present invention relates to technical field of preparation for inorganic material, and in particular to one kind is prepared high using nonaqueous solvents grouting process The method of intensity top grade Longquan celadon.
Background technology
Glaze is a kind of very thin uniform glass matter layer of be melted in ceramic surface one layer, can improve the surface of base substrate Performance, improves the performance and artistic value of product.Longquan celadon is with the gentle moulding such as beautiful glaze colours and smooth grace Receive the favor in market.However, because traditional Longquan celadon preparation technology is complicated and not high into porcelain intensity, causing production cost Improve, so that market share is relatively low, there is larger difference with the ceramic portion of ground production such as Jiangxi Jing Dezhen, Hunan Liling Away from.This is unfavorable for the strategic demand of Longquan celadon industry development, and China sets up resource, urgent being essential of energy conservation type society Ask.Advocated energetically under energy-saving, environmental protection production background in country, urgent need finds a kind of inexpensive, high into porcelain intensity Longquan celadon preparation method.
At present, people more compel to demand of the Longquan celadon moulding process in terms of quick, inexpensive, high-compactness Cut, injection forming is the effective ways that industrial mass prepares the complicated Longquan celadon of reliability height, device shape.Obtain it is low into Originally, the Longquan celadon base substrate of high intensity, it is crucial to prepare low viscosity, the ceramic slurry of high solid volume fraction.Traditional dragon The aqueous slurries of spring celadon add organic liquid and a small amount of electrolyte form metastable suspension using water as solvent, will Sucking moisture in suspension injection gypsum mold solidifies base substrate, reaches the purpose of shaping, therefore gets more and more people's extensive concerning, And be applied successfully in some fields.However, the Longquan celadon base substrate of aqueous slurries injection forming is dehydrating process In necessarily lead to certain shrinkage factor, and the production time is long, and floor space is big, and model consumption is big.In actual production, ceramic water Base-material slurry will form the more difficult regulation and control of condition of good suspension sexual satisfaction injection forming, mainly by Brownian movement, Van der Waals force With the influence of electrostatic dynamic balance, and the formation of hydration shell.When base substrate size is larger, because the moisture of billet surface is waved at first Hair, shrinks result and blocks in the space originally connected from billet surface, causes the moisture inside base substrate to be difficult to smooth removing.
It is above-mentioned to show, still it is difficult to ensure that during for larger-size Longquan celadon base substrate or relatively low solids in pulp amount in base substrate The moisture in portion is fully deviate from, and is damaged so that causing to dry with base substrate spalling in sintering process.This is also water base material traditional in recent years Slurry injection forming technology is difficult to obtain one of major obstacle of high intensity Longquan celadon successful application always.
Propose to prepare Longquan celadon using nonaqueous solvents grouting process for this present invention.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation technology is simple, low production cost, the reaction time The method that short nonaqueous solvents grouting process prepares the high-grade Longquan celadon of high intensity.
To solve above technical problem, the technical scheme is that:A kind of nonaqueous solvents grouting process prepares high intensity The method of high-grade Longquan celadon, comprises the following steps:Organic solvent is measured first as decentralized medium, then by a certain amount of dragon Spring soil is scattered in solvent, adds dispersant, organic solvent slip casting slurry is obtained after stirring, mixed to slurry through ball grinding stirring Close after reaction completely, slurry is aged, injection forming, biscuiting desolvation are handled, can be made high through heat treatment after glazing Intensity top grade Longquan celadon.
The dragon's fountain soil is precious small stream china clay, bamboo township china clay, nasal mucus source china clay, Zijin soil or kaolin.
The organic solvent is the organic solvent of 1~4 carbon atom.
The solid content of the organic solvent and dragon's fountain soil is 15~85%.
Described slurry digestion time is 6~24h.
The heat treatment temperature is 1200~1280 DEG C, and soaking time is 0.5~2.5h, and atmosphere is reducing atmosphere.
The heat treatment includes heating and dries, aoxidizes, being incubated, being reduced into porcelain, five steps of insulation by force.
By comparison, innovation of the invention is to break through using the method for traditional water base injection forming or by addition largely The solid phase methods such as alumina powder, zirconium oxide micro mist improve Longquan celadon into porcelain intensity (rupture strength is about 75~130MPa) Traditional concept, by adding anhydrous organic matter, using solubility in a solvent it is small the characteristics of make forerunner's precursor reactant, it is not only anhydrous The consumption of organic matter is far fewer than the consumption of china clay, and solvent can be with recycling.Each group can be realized using non-aqueous solvent method Divide the uniform mixing in atom level level, be conducive to improving the mobility of slurry;High solid volume fraction slurry is formed, favorably In improving base substrate compactness, reduce cracking when sintering, deform;Reduce the heat treatment temperature of oxide especially composite oxides Degree, but raw material and reaction environment requirement height to preparation.Meanwhile, this invention simplifies traditional Longquan celadon into porcelain technology side Case, Longquan celadon is prepared with nonaqueous solvents grouting process, substantially increases the intensity of Longquan celadon, thoroughly solves restriction dragon's fountain The key issue that celadon is applied and developed.Whole course of reaction environmental protection, is adapted to industrialized production.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment 1
The method that the high-grade Longquan celadon of high intensity is prepared using nonaqueous solvents grouting process, is prepared from by following methods, By following mass percent precise:Precious small stream china clay 13.5%, bamboo township china clay 15.5%, nasal mucus source china clay 14.5%, kaolin 55%, 500mL Glycerol solvents are measured, 0.1gPEG600 dispersants are added, stirring ball-milling is uniform, and slurry is obtained after old 6h; Base substrate is carried out biscuiting by injection forming into being dried after base substrate at 650 DEG C, obtains biscuit;Glazing, glazing are carried out to biscuit 2~3mm of thickness;After biscuit after glazing is dried, it is fitted into kiln, kiln temperature is warming up to 1200 DEG C with 2 DEG C/min speed, Glaze firing is carried out at 1200 DEG C of reducing atmosphere, 1.5h is incubated;It is final to obtain the rupture strength that in the present embodiment prepared by nonaqueous solvents The high-grade Longquan celadon product of 155.5MPa high intensity.
Further, heat treatment includes dry heating, oxidation, is incubated, is reduced into porcelain, five steps of insulation by force in the step Suddenly, table 1 is the glaze firing Technology for Heating Processing temperature rise period.
Table 1
Embodiment 2
The method that the high-grade Longquan celadon of high intensity is prepared using nonaqueous solvents grouting process, is prepared from by following methods, By following mass percent precise:Precious small stream china clay 10.8%, bamboo township china clay 20.2%, nasal mucus source china clay 18%, kaolin 50%, 400mL 1,3-BDO is measured, 0.1gPEG600 dispersants are added, after being well mixed, 50 DEG C, stirring are heated to Slurry is obtained after ball milling, old 24h;Injection forming is into being dried after base substrate;Base substrate is subjected to biscuiting at 750 DEG C, Obtain biscuit;Glazing, 1~2mm of glazing thickness are carried out to biscuit;After biscuit after glazing is dried, it is fitted into kiln, by kiln temperature 1250 DEG C are warming up to 2 DEG C/min speed, glaze firing is carried out at reducing atmosphere, 1250 DEG C, 1.5h is incubated;Finally obtain this reality Apply the high-grade Longquan celadon product of rupture strength 154MPa high intensity that in example prepared by nonaqueous solvents.
Further, heat treatment includes dry heating, oxidation, is incubated, is reduced into porcelain, five steps of insulation by force in the step Suddenly, table 2 is the glaze firing Technology for Heating Processing temperature rise period.
Table 2
Embodiment 3
The method that the high-grade Longquan celadon of high intensity is prepared using nonaqueous solvents grouting process, is prepared from by following methods, By following mass percent precise:Precious small stream china clay 20.5%, bamboo township china clay 19.6%, nasal mucus source china clay 19.5%, bentonite 38.5%, 450mL isopropanol solvents are measured, 0.2gPVB dispersants are added, after being well mixed, 55 DEG C, stirring ball-milling are heated to Uniformly, slurry is obtained after old 12h;Injection forming is into being dried after base substrate;Base substrate is subjected to biscuiting at 650 DEG C, obtained Biscuit;Glazing, 1~2mm of glazing thickness are carried out to biscuit;After biscuit after glazing is dried, it is fitted into kiln, by kiln temperature with 5 DEG C/min speed is warming up to 1270 DEG C, glaze firing is carried out at reducing atmosphere, 1270 DEG C, 2h is incubated;It is final to obtain the present embodiment The high-grade Longquan celadon product of rupture strength 152.5MPa high intensity prepared by middle nonaqueous solvents.
Further, heat treatment includes dry heating, oxidation, is incubated, is reduced into porcelain, five steps of insulation by force in the step Suddenly, table 3 is the glaze firing Technology for Heating Processing temperature rise period.
Table 3
Embodiment 4
The method that the high-grade Longquan celadon of high intensity is prepared using nonaqueous solvents grouting process, is prepared from by following methods, By following mass percent precise:Precious small stream china clay 24%, bamboo township china clay 16.92%, nasal mucus source china clay 36%, kaolin 23%, 550mL glycerine is measured, 0.1g phenolic resin dispersion agent is added, after being well mixed, 50 DEG C are heated to, stirring ball-milling is equal It is even, obtain slurry after old 24h;Injection forming is into being dried after base substrate;Base substrate is subjected to biscuiting at 700 DEG C, element is obtained Base;Glazing, 2~3mm of glazing thickness are carried out to biscuit;By after glazing biscuit dry after, be fitted into kiln, by kiln temperature with 2 DEG C/ Min speed is warming up to 1250 DEG C, and glaze firing is carried out at reducing atmosphere, 1250 DEG C, is incubated 1.5h;It is final to obtain in the present embodiment The high-grade Longquan celadon product of rupture strength 153.8MPa high intensity prepared by nonaqueous solvents.
Further, heat treatment includes dry heating, oxidation, is incubated, is reduced into porcelain, five steps of insulation by force in the step Suddenly, table 4 is the glaze firing Technology for Heating Processing temperature rise period.
Table 4
Embodiment 5
The method that the high-grade Longquan celadon of high intensity is prepared using nonaqueous solvents grouting process, is prepared from by following methods, By following mass percent precise:Precious small stream china clay 18%, bamboo township china clay 20%, nasal mucus source china clay 22%, bentonite 38%, amount 700mL anhydrous normal butyl alcohols are taken, 0.1gPEG600 dispersants are added, stirring ball-milling is uniform, and slurry is obtained after old 24h;Slip casting It is molded into after base substrate and is dried;Base substrate is subjected to biscuiting at 650 DEG C, biscuit is obtained;Glazing, glazing thickness are carried out to biscuit 2~3mm;After biscuit after glazing is dried, it is fitted into kiln, kiln temperature is warming up to 1280 DEG C with 2 DEG C/min speed, also Primordial Qi atmosphere, glaze firing is carried out at 1280 DEG C, be incubated 0.5h;It is final to obtain the rupture strength that in the present embodiment prepared by nonaqueous solvents 154.7MPa high intensity top grade Longquan celadon product.
Further, heat treatment includes dry heating, oxidation, is incubated, is reduced into porcelain, five steps of insulation by force in the step Suddenly, table 5 is the glaze firing Technology for Heating Processing temperature rise period.
Table 5
Embodiment 6
The method that the high-grade Longquan celadon of high intensity is prepared using nonaqueous solvents grouting process, is prepared from by following methods, By following mass percent precise:Precious small stream china clay 22%, bamboo township china clay 18%, nasal mucus source china clay 38%, bentonite 20%, amount Take 650mL without water glycol, add 0.1gPEG400 dispersants, stirring ball-milling is uniform, and slurry is obtained after old 12h;Note Slurry, which is molded into after base substrate, to be dried;Base substrate is subjected to biscuiting at 700 DEG C, biscuit is obtained;Glazing is carried out to biscuit, glazing is thick Spend 2~3mm;After biscuit after glazing is dried, it is fitted into kiln, kiln temperature is warming up to 1260 DEG C with 3 DEG C/min speed, Reducing atmosphere, glaze firing is carried out at 1260 DEG C, be incubated 1.5h;It is final to obtain the rupture strength that in the present embodiment prepared by nonaqueous solvents 154.6MPa high intensity top grade Longquan celadon product.
Further, heat treatment includes dry heating, oxidation, is incubated, is reduced into porcelain, five steps of insulation by force in the step Suddenly, table 6 is the glaze firing Technology for Heating Processing temperature rise period.
Table 6

Claims (9)

1. a kind of method that nonaqueous solvents grouting process prepares the high-grade Longquan celadon of high intensity, it is characterised in that including following step Suddenly:Organic solvent is measured first as decentralized medium, then a certain amount of dragon's fountain soil is scattered in solvent, adds dispersant, Organic solvent slip casting slurry is obtained after stirring, through ball grinding stirring to slurry hybrid reaction it is complete after, slurry is aged, Injection forming, the processing of biscuiting desolvation, the high-grade Longquan celadon of high intensity can be made after glazing through heat treatment.
2. the method as described in claim 1, it is characterised in that the dragon's fountain soil is precious small stream china clay, bamboo township china clay, nasal mucus source porcelain Soil, Zijin soil or kaolin.
3. the method as described in claim 1, it is characterised in that the organic solvent is the organic solvent of 1~4 carbon atom.
4. the method as described in claim 1, it is characterised in that the solid content of the organic solvent and dragon's fountain soil for 15~ 85%.
5. the method as described in claim 1, it is characterised in that described slurry digestion time is 6~24h.
6. the method as described in claim 1, it is characterised in that the heat treatment temperature is 1200~1280 DEG C, soaking time For 0.5~2.5h, atmosphere is reducing atmosphere.
7. method as claimed in claim 6, it is characterised in that the heat treatment is dried including heating up, aoxidized, being incubated, going back by force It is former into porcelain, five steps of insulation.
8. method according to claim 1, it is characterised in that the slurry is respectively precious small stream porcelain including mass percent Soil 13.5%, bamboo township china clay 15.5%, nasal mucus source china clay 14.5% and kaolin 55%, in addition to 500mL Glycerol solvents, 0.1gPEG600 dispersants.
9. method as claimed in claim 7, it is characterised in that the process such as following table that the heating is dried:
CN201710260591.XA 2017-04-20 2017-04-20 A kind of method that nonaqueous solvents grouting process prepares the high-grade Longquan celadon of high intensity Pending CN107032754A (en)

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Cited By (1)

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CN113858391A (en) * 2021-10-27 2021-12-31 龙泉市尚唐瓷艺发展有限公司 Formula and preparation device of double-layer heat-insulation Longquan celadon

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CN101885601A (en) * 2010-06-20 2010-11-17 景德镇陶瓷学院 Method for manufacturing medium-temperature Longquan powder celadon
CN102060539A (en) * 2009-11-13 2011-05-18 中国科学院上海硅酸盐研究所 Method for preparing yttrium aluminum garnet based transparent ceramic by slip casting
CN106478067A (en) * 2016-10-10 2017-03-08 丽水学院 A kind of base the Longquan celadon base substrate of raw ore complete utilization and the preparation method of glaze

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CN101885601A (en) * 2010-06-20 2010-11-17 景德镇陶瓷学院 Method for manufacturing medium-temperature Longquan powder celadon
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113858391A (en) * 2021-10-27 2021-12-31 龙泉市尚唐瓷艺发展有限公司 Formula and preparation device of double-layer heat-insulation Longquan celadon
CN113858391B (en) * 2021-10-27 2022-11-22 龙泉市尚唐瓷艺发展有限公司 Preparation method and preparation device of double-layer heat-insulation Longquan celadon

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Application publication date: 20170811