WO2017133080A1 - 一种低收缩高强度大规格陶瓷板及其制备方法 - Google Patents
一种低收缩高强度大规格陶瓷板及其制备方法 Download PDFInfo
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- WO2017133080A1 WO2017133080A1 PCT/CN2016/079299 CN2016079299W WO2017133080A1 WO 2017133080 A1 WO2017133080 A1 WO 2017133080A1 CN 2016079299 W CN2016079299 W CN 2016079299W WO 2017133080 A1 WO2017133080 A1 WO 2017133080A1
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- shrinkage
- strength
- preparation
- acicular wollastonite
- ceramic
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- 239000000919 ceramic Substances 0.000 title claims abstract description 90
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 239000010456 wollastonite Substances 0.000 claims abstract description 67
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 67
- 239000002994 raw material Substances 0.000 claims abstract description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 239000008187 granular material Substances 0.000 claims abstract description 3
- 238000010304 firing Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 18
- 238000010521 absorption reaction Methods 0.000 claims description 17
- 239000004576 sand Substances 0.000 claims description 15
- 238000005469 granulation Methods 0.000 claims description 11
- 230000003179 granulation Effects 0.000 claims description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 238000007908 dry granulation Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000000454 talc Substances 0.000 claims description 4
- 229910052623 talc Inorganic materials 0.000 claims description 4
- 229910052572 stoneware Inorganic materials 0.000 claims 2
- 238000005245 sintering Methods 0.000 abstract description 5
- 230000003014 reinforcing effect Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 28
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- 239000006229 carbon black Substances 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
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- 230000000052 comparative effect Effects 0.000 description 2
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- 230000000694 effects Effects 0.000 description 2
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
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- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
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- 210000003298 dental enamel Anatomy 0.000 description 1
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- 239000010433 feldspar Substances 0.000 description 1
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- 229910000077 silane Inorganic materials 0.000 description 1
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- 239000002002 slurry Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Definitions
- the present invention relates to a ceramic board preparation process, and more particularly to a low shrinkage high strength large size ceramic plate and a preparation method thereof.
- ceramic plates greatly save raw materials, energy and transportation costs, they also save space and reduce the weight of building structures, especially in line with the national energy conservation and environmental protection green industry policy.
- industrial production of large-size ceramic plates has two types of dry press forming and wet extrusion molding.
- the extrusion process requires a large moisture content of the billet, and the body is prone to pores and cracks during the drying process, which reduces the quality and yield of the product after firing.
- the dry press forming process is more mature, and the quality and yield of the product are higher.
- CN1191853 A discloses a method for producing a large flat ceramic sintered body. After adding acicular wollastonite and water to a ceramic raw material, it is extruded into a cylindrical shape by a vacuum and a mud machine, and then calendered and formed. High-strength large flat ceramic sintered body. Due to the wet extrusion process, the acicular wollastonite is easily oriented in the direction of extrusion, resulting in an anisotropic strength of the finished product, a high strength in the direction of the vertical extrusion, and a low strength in the direction of the parallel extrusion. .
- Dry pressing requires pulping, is limited to equipment, and is capable of being sprayed by a wet spray granulation process for fibers having a certain aspect ratio, for example, CN102173760A, a method for producing a large-sized silicon oxide ceramic sheet,
- the raw material clay particles were prepared, and acicular wollastonite was added to the raw material, and granulated by spray drying.
- acicular wollastonite has a great influence on the flow rate of the slurry, it is difficult to spray powder, and the aspect ratio is large, and it is difficult to screen and remove iron, which has a great influence on the whiteness of the green body.
- the technical problem to be solved by the present invention is to provide a low-shrinkage, high-strength, large-size ceramic plate and a preparation method thereof.
- the ceramic plate has high strength, good toughness, and small shrinkage.
- the present invention provides a method for preparing a low-shrinkage, high-strength, large-size ceramic plate, comprising the following steps:
- acicular wollastonite is surface-wrapped with a silane coupling agent and pre-dispersed with fumed silica to obtain pretreated acicular wollastonite;
- the present invention fully utilizes the characteristics of acicular wollastonite reinforcement and small firing shrinkage, and introduces acicular wollastonite in the preparation of large-sized ceramic plates, thereby improving the strength of large-size ceramic plates and reducing
- the shrinkage rate of the large-size ceramic plate has been obtained, and a low-shrinkage, high-strength, large-size ceramic plate has been obtained.
- the dry pressing process can improve the quality and yield of the product.
- the acicular wollastonite is pretreated, specifically, surface-modified with a silane coupling agent and pre-dispersed with a fumed silica, and the surface modification solves the problem that the powder is easily agglomerated and dispersible, and the white carbon black is loose.
- the structure can further improve the powder dispersibility, thereby solving the problem of acicular wollastonite dispersion, and further improving the product quality and the harvest rate.
- the formula of the ceramic raw material is: water washed mud 8 ⁇ 20%, mixed mud 4 ⁇ 16%, potassium sand 12 ⁇ 20 ⁇ 3 ⁇ 4, medium temperature sand 24 ⁇ 30 ⁇ 3 ⁇ 4, 1 # ⁇ 6 ⁇ 12 ⁇ 3 ⁇ 4, 2# Sodium sand 16 ⁇ 22 ⁇ 3 ⁇ 4, black talc 1 ⁇ 2.
- the preparation method of the ceramic raw material powder comprises: pre-pulverizing each ceramic raw material and passing through a 120 mesh sieve, and sieving the raw materials according to the formula, grinding and processing, controlling 250 mesh. Screening ⁇ 2%.
- the granulation by the dry granulation process can be better mixed with the acicular wollastonite.
- the acicular wollastonite has an aspect ratio of 10 to 18.
- acicular wollastonite with an aspect ratio of 10 to 18 it is advantageous for the dispersion of acicular wollastonite and the strength of the ceramic plate.
- the step (2) comprises: the acicular wollastonite is sprayed with a silane coupling agent in the surface modification device.
- the silane coupling agent is at least one of KH550, KH560, and KH570.
- the granulation is carried out by dry granulation.
- the dry granulation can be carried out without limitation to the equipment, and it is easy to obtain a powder containing acicular wollastonite.
- the pressure of the dry press molding is 86000 to 96000 KN, and the molding specification is
- the firing temperature is from 1190 to 1220 °C.
- the present invention provides a low-shrinkage, high-strength, large-size ceramic plate prepared by any of the above methods, the ceramic plate having a specification of (1100 ⁇ 1260) mmx (2200 ⁇ 2500) mmx (3 ⁇ 6) ) mm.
- the ceramic plate comprises a porcelain product and a enamel tile product, wherein the porcelain product has a shrinkage ratio of 5 to 8%, a flexural strength of 55 to 68 MPa (preferably 58 to 68 MPa), and a water absorption rate of less than 0.5%; The rate is 1 ⁇ 5 ⁇ 3 ⁇ 4, the flexural strength is 40 ⁇ 55MPa, and the water absorption rate is 0.5 ⁇ 10 ⁇ 3 ⁇ 4.
- the present invention it is possible to provide a large-sized ceramic plate having high strength, good toughness, and small firing shrinkage. It can not only improve the regularity of product firing, but also reduce consumables and further save energy and reduce consumption.
- FIG. 1 shows a process flow diagram of one embodiment of the present invention.
- Table 2 shows a chemical composition table of ceramic raw materials (Table 1) of one example of the present invention.
- the invention adopts a dry pressing process to prepare a low-shrinkage high-strength large-size ceramic plate. Compared with wet extrusion molding, the dry pressing process is more mature, and the quality and yield of the product are higher.
- the invention is in the original of the ceramic plate
- the needle-shaped wollastonite is added to the material to further improve the strength and toughness of the ceramic plate, and the firing shrinkage rate can be reduced, and the size regularity can be improved.
- the acicular wollastonite is pretreated to solve the problem of acicular wollastonite dispersion.
- Figure 1 shows a process flow diagram of one embodiment of the present invention. Hereinafter, a method of preparing the low shrinkage high strength large-size ceramic plate of the present invention will be described with reference to FIG.
- the ceramic raw material is not particularly limited, and a usual ceramic raw material can be used.
- the ceramic raw material is formulated as follows:
- the ceramic raw materials used are dried. Preferably, it is dried to a moisture content of ⁇ 4%. After drying, the individual ceramic raw materials were pre-pulverized using a pre-comminuted apparatus and passed through a 120 mesh screen. The sieving material is continuously pulverized; the sieving material is pre-mixed according to the formula, and then pulverized together (grinding and milling) to control the remaining 2 mesh of the 250 mesh sieve. The powder is mixed to obtain a ceramic raw material powder.
- the aspect ratio of the acicular wollastonite is preferably from 10 to 18. If the aspect ratio is greater than 18, it will be difficult to disperse; if the aspect ratio is less than 10, the enhancement will be affected.
- the acicular wollastonite may have a diameter of 10 ⁇ m to 60 ⁇ m.
- the acicular wollastonite is subjected to the following pretreatment: surface encapsulation treatment with a silane coupling agent and pre-dispersion with gas phase white carbon black.
- the silane coupling agent can surface-modify the acicular wollastonite to enhance its compatibility with the ceramic raw material.
- the fumed silica can be pre-dispersed with acicular wollastonite. Thereby, the dispersibility of the acicular wollastonite can be remarkably improved, so that the acicular wollastonite can be uniformly dispersed in the ceramic raw material.
- the silane coupling agent but not limited to KH550, KH560, KH570, preferably KH550.
- the specific method of pretreatment is as follows: acicular wollastonite is sprayed with a silane coupling agent (addition amount: 0.1 to 0.8%) to form a coating layer of the modifier in the surface modification equipment, and then with the gas phase White carbon black (addition amount 0.1 to 0.5%) is thoroughly mixed for pre-dispersion treatment.
- the percentage of addition here is for acicular wollastonite.
- the pretreated acicular wollastonite is thoroughly mixed with the above ceramic raw material powder to form a mixed powder.
- the mixing method can be, for example, ball milling mixing.
- the amount of acicular wollastonite added is preferably 10 ⁇ 3 ⁇ 4 ⁇ 30 ⁇ 3 ⁇ 4.
- the addition amount is more than 30%, the firing temperature is low, the sintering range is small, and it is not conducive to firing; if the addition amount is less than 10%, the shrinkage is relatively large, and the increase in size is small, and the effect is not obtained. More preferably, the acicular wollastonite is added in an amount of 15% to 20 ⁇ 3 ⁇ 4.
- the mixed powder is granulated. Since the powdering by the wet spray granulation process cannot be carried out for fibers having a certain aspect ratio, the present invention is preferably dry granulation. Moreover, since the acicular wollastonite has good dispersibility after pretreatment, it is suitable for dry granulation.
- the bismuth micropowder particles spontaneously agglomerate due to surface tension and intermolecular forces.
- the raw material contains about 25% of clay-based raw materials, which further enhances the agglomeration ability of the micropowder.
- the first-formed particles have smaller particle size and lower strength, and then enter the special cyclone.
- the material entering the cyclone barrel is rubbed along the wall of the cylinder and rubbed by friction, and the materials collide with each other, so that the particles are further agglomerated and the sphericity is further improved. Perfect, the strength of the powder is also increased, helping to keep the powder spherical.
- the particles formed by granulation may have a particle diameter of 0.1 to 1 mm.
- the above particles are then dry pressed into shape.
- the particles may be further dried, sieved, aged (e.g., 24 hours) prior to dry pressing to be more suitable for dry pressing.
- the pressure for dry pressing can be from 86,000 KN to 96000 KN.
- the molding specification can be (1150 ⁇ 1300) mmx (2400 ⁇ 2600) mmx (3 ⁇ 6) mm
- the molded green body is fired to obtain a ceramic plate.
- the firing temperature is 11 90 to 1220 ° C.
- the firing time can be 50 to 65 minutes.
- glaze printing can be applied to glaze.
- it can be fired once after glazing printing on the green body.
- the green body may be dried prior to firing. For example, it can be dried at 180 to 210 ° C for 25 to 35 minutes.
- the finished product after firing is a large-sized ceramic plate, and the specification thereof may be (1100 to 1260) mmx (2200 to 2500) mmx (3 to 6) mm.
- the edging can also be cut to obtain the final product.
- the present invention makes full use of the characteristics of small shrinkage of acicular wollastonite, and the firing shrinkage of the porcelain product is 5 to 8%.
- the ceramic sheet of the present invention has a flexural strength as high as 58 to 68 MPa due to the reinforcing effect of the acicular wollastonite. And a water absorption of less than 0. 5 ⁇ 3 ⁇ 4.
- the ceramic plate of the present invention may be a porcelain tile product or a tantalum tile product.
- Porcelain brick product shrinkage rate is 5 ⁇ 8%, flexural strength is 55 ⁇ 68MPa, water absorption is less than 0.5%; ⁇ tile product shrinkage is 1 ⁇ 5 ⁇ 3 ⁇ 4, flexural strength is 40 ⁇ 55MPa, water absorption is 0.5 ⁇ 10 ⁇ 3 ⁇ 4.
- test methods in the following embodiments are as follows:
- TXY digital ceramic water absorption measuring instrument can be used to measure the water absorption rate, apparent porosity and bulk density of building sanitary ceramics (vacuum degree: ⁇ 0.095MPa adjustable; vacuum Daytime: 0 ⁇ 99 minutes 59 seconds continuously adjustable; Soaking daytime: 0 ⁇ 99 small ⁇ 59 points continuously adjustable; Volume: ⁇ 40 0x450mm; Power: ⁇ 220V).
- Ceramic raw material formula water washing mud 15%, mixed mud 10%, potassium sand 16%, medium temperature sand 28 ⁇ 3 ⁇ 4, 1# sodium sand 10%, 2# sodium sand 20%, black talc 1%; The chemical composition is as shown in Table 1 above; [0047] Needle-shaped wollastonite: an aspect ratio of 15, a diameter of 30 micrometers, purchased from Jiangxi Aote Fine Powder Co., Ltd., model AT-acicular powder.
- acicular wollastonite is surface-wrapped with a silane coupling agent and pre-dispersed with 0.4% fumed silica, and the specific steps are as follows: acicular wollastonite is sprayed with silane by a surface modification device.
- the crosslinking agent (addition amount: 0.5%) forms a coating layer of a modifier to reduce agglomeration, and is sufficiently mixed with the gas phase white carbon (addition amount: 0.4%) to carry out a pre-dispersion treatment.
- step 3 The powder obtained in the step 1) is thoroughly mixed with the pretreated acicular wollastonite obtained in the step 2), and the amount of the pretreated acicular wollastonite is 13%. Then, the granulation method is a dry suspension granulation process.
- the product shrinkage is 7.5%
- the flexural strength is 60Mpa
- the water absorption is 0.27 ⁇ 3 ⁇ 4.
- Example 2 Compared with Example 1, the only difference is that the amount of pretreated acicular wollastonite added was 22%.
- the final specification of the finished ceramic plate is 1204mm*2407mm*5.4mm, the shrinkage of the finished product is 5.6%, the flexural strength is 65MPa, and the water absorption is 0.34%.
- Example 2 Compared with Example 1, the only difference is that the amount of pretreated acicular wollastonite added was 28%.
- the final specification of the finished ceramic plate is 1210mm*2420mm*5.6mm, the shrinkage of the finished product is 5.1%, the flexural strength is 66MPa, and the water absorption is 0.45 ⁇ 3 ⁇ 4.
- Example 2 Compared with Example 1, the only difference is that the amount of pretreated acicular wollastonite added was 11%.
- the finished ceramic plate product ( ⁇ ceramic tile product) has a specification of 1223mm*2445mm*5.5mm, and the finished product shrinks. The rate was 4.1%, the flexural strength was 42 MPa, and the water absorption was 9 ⁇ 3 ⁇ 4.
- Example 2 Compared with Example 1, the only difference was that the amount of pretreated acicular wollastonite added was 27%.
- the finished ceramic plate product ( ⁇ ceramic tile product) has a specification of 1250mm*2499mm*5.5mm, a shrinkage rate of 2%, a flexural strength of 47MPa, and a water absorption of 6 ⁇ 3 ⁇ 4.
- Example 1 Compared with Example 1, ceramic sheets were prepared using only the above ceramic raw materials without adding acicular wollastonite.
- the final specification of the finished ceramic plate is 1141mm*2282mm*5.4mm, the shrinkage of the finished product is 10.5%, the flexural strength is 48MPa, and the water absorption is 0.23 ⁇ 3 ⁇ 4.
- Example 2 Compared with Example 1, acicular wollastonite was added, but acicular wollastonite was not pretreated, and the remaining steps were the same as in Example 1. As a result, it was found that the acicular wollastonite dispersion was very uneven, the agglomerate temperature was high, and the local sintering degree was inconsistent, and the finished product was easily broken in a weak place, and the physical and chemical properties were poor.
- the final specification of the finished ceramic plate is 1173mm*2346mm*5.5mm, the shrinkage of the finished product is 8%, the flexural strength is 48MPa, and the water absorption is 0.6 ⁇ 3 ⁇ 4.
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US20200361823A1 (en) | 2020-11-19 |
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