CN108947508A - A kind of ceramic element, preparation method and the usage - Google Patents

A kind of ceramic element, preparation method and the usage Download PDF

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CN108947508A
CN108947508A CN201810953658.2A CN201810953658A CN108947508A CN 108947508 A CN108947508 A CN 108947508A CN 201810953658 A CN201810953658 A CN 201810953658A CN 108947508 A CN108947508 A CN 108947508A
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section
temperature
sintering temperature
preparation
heating rate
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CN108947508B (en
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苏发兴
李延涛
苏志波
陈柔羲
苏清龙
叶锦华
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Beyclean Environmental Protection Technology Co Ltd
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    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention discloses a kind of ceramic elements, preparation method and use, the preparation method includes being sintered filter core green compact, sintering temperature is divided into 3-6 sections in the sintering process, ceramic element prepared by the present invention has good high mechanical strength, filter effect, heavy metal free pollution, yields high, at low cost, and technique time-consuming is short, than the time that traditional handicraft reduces 20%-30%, it is suitable for water treatment.

Description

A kind of ceramic element, preparation method and the usage
Technical field
The invention belongs to water purification field, it is related to a kind of ceramic element, preparation method and the usage.
Background technique
Ceramic element has the unique functions such as acid and alkali-resistance, high temperature resistant, anticorrosive, has in water treatment field and widely answers With.It has the following characteristics that lightweight, high porosity, long service life, easy to clean and regeneration;With good state and height Filtering accuracy is a kind of water filtration material of environmental protection.
CN107158805A discloses a kind of multifunctional compound ceramics filter core and preparation method thereof, by ceramic powder, bonding Agent, organic pore-forming agents etc. stir evenly, and slurry liquid is still aging for 24 hours, and then injection forming, demoulding, drying, are finally burnt Knot, it is cooling, obtain ceramic element;CN107089836A disclose a kind of ion activity multi-microporous ceramic filter core composition of raw materials and its Montmorillonite, tripoli, pore creating material, binder etc. are uniformly mixed, first carry out grinding 10-30h with ball mill, then by manufacturing process Two sulfuric acid liquid of catalyst is poured into again and grinds 1~5h in ball milling for the second time again, physical and chemical reaction is synchronous to carry out, shape after grinding At mud;Mud is pumped into stock tank, using pressure mud and after practicing mud, carries out blank forming into assembly room;Finally carry out It is sintered and cooled, obtains ceramic element;CN1299797C discloses a kind of preparation method of porous inorganic microstraining core, by base-material, Composite base-material, repressed molding is made in carrier, curing additive stirring, and green compact are made in normal-temperature reaction solidification;Green compact are dried through demoulding It is dry, ceramic element is made after being sintered and cooled at high temperature.
The shortcomings that above traditional preparation method: (1) adding pore creating material, so that the precision of ceramics is affected;(2) it uses Ball mill is ground, and process flow is increased;(3) composite base-material stirring, time of repose are long, and the green sintering time is long, energy consumption Increase, and the intensity of filter core is inhomogenous, product defect rate is high;(4) final product cannot be removed effectively chromium (sexavalence), aluminium, The heavy metal pollutions such as arsenic, antimony.
Therefore, a kind of high mechanical strength, the ceramics that yields is high, at low cost, technique is time-consuming short and environment friendly and pollution-free are developed Filter core is still the hot spot of this field research.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of ceramic element, preparation method and the usage, The ceramic element has good high mechanical strength, filter effect, heavy metal free pollution, yields high, at low cost, and technique is time-consuming It is short, than the time that traditional handicraft reduces 20%-30%, it is suitable for water treatment.
To achieve this purpose, the present invention adopts the following technical scheme:
One of the objects of the present invention is to provide a kind of preparation method of ceramic element, the preparation method includes by filter core Green compact are sintered, and sintering temperature is divided into 3-6 sections, such as 3 sections, 4 sections, 5 sections or 6 sections in the sintering process.
In the present invention, the sintering temperature is divided into 6 sections, and first segment is the moisture removed in green compact, and second segment is pre-burning Knot, third section are crystallization, and the 4th section is porcelain, and the 5th section is annealing, and the 6th section is cooling.
The present invention controls temperature section in sintering process, by the control more accurate and stringent to temperature, makes entire The sintering process used time is very short, than traditional handicraft reduce about 20%-30% time, and also can be improved ceramic element hardness and Intensity constantly improve the pore structure of ceramic element, and stable dimensions reduce deformation and crackle tendency, to eliminate tissue defects, protects Demonstrate,prove higher yields.
In the present invention, the first segment sintering temperature is warming up to 110 DEG C from 25 DEG C, and heating rate is 1 DEG C/min-15 DEG C/min, such as 1 DEG C/min, 2 DEG C/min, 3 DEG C/min, 4 DEG C/min, 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, 15 DEG C/min etc., preferably 1 DEG C/min.
In the present invention, the first segment is in 110 DEG C of heat preservation 1-5h, such as 1h, 2h, 3h, 4h, 5h etc., preferably 2h.
In the present invention, the second segment sintering temperature is warming up to 350 DEG C from 110 DEG C, and heating rate is 1 DEG C/min-15 DEG C/min, such as 1 DEG C/min, 2 DEG C/min, 3 DEG C/min, 4 DEG C/min, 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, 15 DEG C/min etc., preferably 1 DEG C/min.
In the present invention, the second segment is in 350 DEG C of heat preservation 1-5h, such as 1h, 2h, 3h, 4h, 5h etc., preferably 1h.
In the present invention, the third section sintering temperature is warming up to 780 DEG C from 350 DEG C, and heating rate is 1 DEG C/min-15 DEG C/min, such as 1 DEG C/min, 2 DEG C/min, 3 DEG C/min, 4 DEG C/min, 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, 15 DEG C/min etc., preferably 1 DEG C/min.
In the present invention, the third section is in 780 DEG C of heat preservation 1-5h, such as 1h, 2h, 3h, 4h, 5h etc., preferably 2h.
In the present invention, the 4th section of the sintering temperature is warming up to 1100 DEG C from 780 DEG C, and heating rate is 1 DEG C/min- 15 DEG C/min, for example, 1 DEG C/min, 2 DEG C/min, 3 DEG C/min, 4 DEG C/min, 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, 15 DEG C/min etc., preferably 1 DEG C/min.
In the present invention, described 4th section in 1100 DEG C of heat preservation 1-10h, for example, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h etc., preferably 3h.
In the present invention, the 5th section of sintering temperature is cooled to 500 DEG C from 1100 DEG C, and rate of temperature fall is 1 DEG C/min-15 DEG C/min, such as 1 DEG C/min, 2 DEG C/min, 3 DEG C/min, 4 DEG C/min, 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, 15 DEG C/min etc., preferably 1 DEG C/min.
In the present invention, described 5th section in 500 DEG C of heat preservation 1-20h, for example, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h etc., preferably 8h.
In the present invention, the 6th section of sintering temperature is cooled to 80 DEG C from 500 DEG C, and rate of temperature fall is 1 DEG C/min-15 DEG C/min, such as 1 DEG C/min, 2 DEG C/min, 3 DEG C/min, 4 DEG C/min, 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, 15 DEG C/min etc., preferably 1 DEG C/min.
In the present invention, described 6th section in 80 DEG C of heat preservation 10-50h, for example, 10h, 15h, 20h, 25h, 30h, 35h, 40h, 45h, 50h etc., preferably 32h.
In the present invention, the filter core green compact the preparation method comprises the following steps: diatomite, bacteriostatic agent and waterglass are uniformly mixed, Obtain filter core green compact.
In the present invention, the mesh number of the diatomite is 50-1000 mesh, such as 50 mesh, 100 mesh, 200 mesh, 300 mesh, 400 Mesh, 500 mesh, 600 mesh, 700 mesh, 800 mesh, 900 mesh, 1000 mesh etc..
The present invention selects the diatomite of 50-1000 mesh, and the ceramic element pore size being prepared is suitable, is guaranteeing to filter The rate of filtration is ensured that while precision;If the mesh number of diatomite is lower than 50 mesh, the aperture of ceramic element is excessive, influences Filter effect;If being higher than 1000 mesh, the aperture of ceramic element is smaller, filters slower.
It in the present invention, is 50-80 parts by weight (such as 50 parts by weight, 55 parts by weight, 60 weight with the additive amount of diatomite Part, 65 parts by weight, 70 parts by weight, 75 parts by weight, 80 parts by weight etc.) meter, the additive amount of the bacteriostatic agent is 10-30 parts by weight, Such as 10 parts by weight, 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight etc..
In the present invention, the bacteriostatic agent is nano zine oxide, negative ion powder, titanium dioxide, active carbon loading silver, carries silver-colored dioxy Change in titanium or cloves any one or at least two combination, preferably carry the mixing of silver-colored titanium dioxide and titanium dioxide.
In the present invention, it is preferred to the mass ratio for carrying silver-colored titanium dioxide and titanium dioxide is 1:1-2:1, such as 1:1, 1.2:1,1.4:1,1.5:1,1.6:1,1.8:1,2:1 etc..
It in the present invention, is 50-80 parts by weight (such as 50 parts by weight, 55 parts by weight, 60 weight with the additive amount of diatomite Part, 65 parts by weight, 70 parts by weight, 75 parts by weight, 80 parts by weight etc.) meter, the additive amount of the waterglass is 10-15 parts by weight, Such as 10 parts by weight, 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, 15 parts by weight etc..
In the present invention, the number that rubs of the waterglass neutral and alkali metal oxide and silica is 0.3:1-3:1, such as 0.3:1,0.5:1,0.8:1,1:1,1.2:1,1.5:1,1.8:1,2:1,2.3:1,2.5:1,2.8:1,3:1 etc., preferably 3:1.
The number that rubs of waterglass neutral and alkali metal oxide and silica that the present invention selects is 0.3:1-3:1, in the ratio There is waterglass preferable intensity and hardness to be not likely to produce defect to increase the hardness of ceramic element raw embryo in example range, when When the number that rubs of the two is lower than the range, the ceramic element hardness of preparation is lower, and yields is poor, when the number that rubs of the two is higher than the model When enclosing, the hardness of the ceramic element of preparation is too high, be easy to cause internal flaw, and yields is low.
In the present invention, the alkaline metal oxide is sodium oxide molybdena or potassium oxide.
In the present invention, the mixing is to mix under agitation, mixing time 10-60min, such as 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min etc..
In the present invention, the curing molding is solidified by carbon dioxide air hardening method.
In the present invention, the purity of the carbon dioxide be 60%-99%, such as 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 99% etc., preferably 99%
In the present invention, the blow gas pressure of carbon dioxide gas is stated as 0.1MPa-1MPa, such as 0.1MPa, 0.2MPa, 0.3MPa, 0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, 0.8MPa, 0.9MPa, 1MPa etc..
The present invention use carbon dioxide air hardening method curing molding, wherein in waterglass in the presence of column balancing: R2O·mSiO2· nH2O=2ROH+mSiO2·nH2O, wherein R is alkali metal, when being blown into carbon dioxide into mixed material, carbon dioxide conduct The ROH reaction that acidic oxide meeting and reaction obtain, can promote reaction to carry out to the right, then the silicic acid molecule generated increases, silicic acid There is-Si-O-H key in molecule, easily generation polycondensation reaction forms gel, and the hardness of filter core raw embryo depends on the silicic acid generated Gel, moisture resistance depend on the dehydration of unreacted waterglass, and carbon dioxide dew point is -30 DEG C, and very dry, are blowing Cheng Zhong, it is inevitable to be dehydrated induration with physics other than having chemical action, therefore the curing molding of mixed resin can be accelerated.
As a preferred technical solution, the ceramic element preparation method the following steps are included:
(1) 50-80 parts by weight diatomite, 10-30 parts by weight bacteriostatic agent and 10-15 parts by weight waterglass are mixed under stiring Close 10-60min, after in carbon dioxide purity be 99%, it is solid that blow gas pressure carries out carbon dioxide air hardening method under the conditions of being 0.5MPa Chemical conversion type obtains filter core green compact;
(2) the filter core green compact that step (1) obtains are divided into six sections by sintering temperature to be sintered, first segment is by sintering temperature Be warming up to 110 DEG C from 25 DEG C with the heating rate of 1 DEG C/min-15 DEG C/min, keep the temperature 1-5h, second segment by sintering temperature with 1 DEG C/ The heating rate of min-15 DEG C/min is warming up to 350 DEG C from 110 DEG C, keeps the temperature 1-5h, third section is by sintering temperature with 1 DEG C/min- The heating rate of 15 DEG C/min is warming up to 780 DEG C from 350 DEG C, keeps the temperature 1-5h, the 4th section by sintering temperature with 1 DEG C/min-15 DEG C/ The heating rate of min is warming up to 1100 DEG C from 780 DEG C, keeps the temperature 1-10h, the 5th section by sintering temperature with 1 DEG C/min-15 DEG C/min Heating rate be cooled to 500 DEG C from 1100 DEG C, keep the temperature 1-20h, the 6th section by sintering temperature with 1 DEG C/min-15 DEG C/min's Heating rate is cooled to 80 DEG C from 500 DEG C, keeps the temperature 10-50h, obtains ceramic element.
In the present invention, the ceramic element preparation method further includes the ceramic element cooling that will be obtained, removes removing heavy metals And it is dry.
In the present invention, described that removing heavy metals is gone to realize by rinsing or impregnating.
In the present invention, described to rinse or impregnate liquid used for any one in water, alcohol or methanol or at least two The mixing of kind.
In the present invention, the pressure of the flushing be 0.1-0.5MPa, such as 0.1MPa, 0.2MPa, 0.3MPa, 0.4MPa, 0.5MPa etc..
In the present invention, the flow velocity of the flushing is 0.1-10L/min, such as 0.1L/min, 1L/min, 2L/min, 3L/ Min, 4L/min, 5L/min, 6L/min, 7L/min, 8L/min, 9L/min, 10L/min etc..
The present invention selects suitable flushing pressure and rinses speed, both can ensure that remaining metal ion was rinsed completely, It can avoid damaging because of flushing pressure or excessively high generate ceramic element of flushing speed again.
In the present invention, the drying temperature be 80-500 DEG C, such as 80 DEG C, 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C, 300 DEG C, 350 DEG C, 400 DEG C, 450 DEG C, 500 DEG C etc..
In the present invention, the drying time be 10min-120min, such as 10min, 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min etc..
The second object of the present invention is to provide a kind of ceramic filtering that the preparation method as described in the first purpose is prepared Core.
The third object of the present invention is to provide a kind of application of ceramic element as described above in water filtration.
Compared with the existing technology, the invention has the following advantages:
Temperature section is controlled sintering process by the preparation method of ceramic element provided by the invention, by temperature more For accurate and stringent control, keep the entire sintering process used time very short, than the time that traditional handicraft reduces about 20%-30%;It is logical The number that rubs for crossing control waterglass, to increase the intensity and hardness of ceramic element;The present invention selects the diatomite of suitable mesh number, mistake The filter time is short, and filtering accuracy is high;The ceramic element that the present invention is prepared, high mechanical strength, filter effect are good, heavy metal free is dirty Dye, yields are high, at low cost, and technique time-consuming is short, are suitable for water treatment.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright , the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
In the present embodiment, a kind of preparation method of ceramic element is provided, the ceramic element preparation method includes following Step:
(1) by the silver-colored titanium dioxide of the load of the diatomite of 80 parts by weight, 200 mesh, 5 parts by weight, the titanium dioxide and 10 of 5 parts by weight The Na of parts by weight2O·3SiO2Mix 10min under stiring, after carbon dioxide purity be 99%, blow gas pressure be 0.5MPa item Carbon dioxide air hardening method curing molding is carried out under part, obtains filter core green compact;
(2) the filter core green compact that step (1) obtains are divided into six sections by sintering temperature to be sintered, first segment is by sintering temperature It is warming up to 110 DEG C from 25 DEG C with the heating rate of 1 DEG C/min, keeps the temperature 2h, second segment is by sintering temperature with the heating speed of 1 DEG C/min Rate is warming up to 350 DEG C from 110 DEG C, keeps the temperature 1h, and sintering temperature is warming up to the heating rate of 1 DEG C/min from 350 DEG C by third section 780 DEG C, 2h is kept the temperature, sintering temperature is warming up to 1100 DEG C from 780 DEG C with the heating rate of 1 DEG C/min by the 4th section, 3h is kept the temperature, the Sintering temperature is cooled to 500 DEG C from 1100 DEG C with the heating rate of 1 DEG C/min by five sections, keeps the temperature 8h, and the 6th section by sintering temperature Be cooled to 80 DEG C from 500 DEG C with the heating rate of 1 DEG C/min, keep the temperature 32h, after be cooled to room temperature, rinsed with the flow velocity of 1L/min 10min removes removing heavy metals, 200 DEG C of dry 10min, and polishing removes powder, obtains the ceramic element.
Embodiment 2
(1) by the silver-colored titanium dioxide of the load of the diatomite of 70 parts by weight, 100 mesh, 10 parts by weight, the titanium dioxide and 15 of 5 parts by weight The Na of parts by weight2O·SiO2Mix 10min under stiring, after carbon dioxide purity be 90%, blow gas pressure be 1MPa condition Lower progress carbon dioxide air hardening method curing molding, obtains filter core green compact;
(2) the filter core green compact that step (1) obtains are divided into six sections by sintering temperature to be sintered, first segment is by sintering temperature It is warming up to 110 DEG C from 25 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 2h, second segment is by sintering temperature with the heating speed of 5 DEG C/min Rate is warming up to 350 DEG C from 110 DEG C, keeps the temperature 2h, and sintering temperature is warming up to the heating rate of 5 DEG C/min from 350 DEG C by third section 780 DEG C, 2h is kept the temperature, sintering temperature is warming up to 1100 DEG C from 780 DEG C with the heating rate of 5 DEG C/min by the 4th section, 2h is kept the temperature, the Sintering temperature is cooled to 500 DEG C from 1100 DEG C with the heating rate of 5 DEG C/min by five sections, keeps the temperature 10h, and the 6th section by sintering temperature Be cooled to 80 DEG C from 500 DEG C with the heating rate of 5 DEG C/min, keep the temperature 30h, after be cooled to room temperature, rinsed with the flow velocity of 2L/min 10min removes removing heavy metals, 150 DEG C of dry 10min, and polishing removes powder, obtains the ceramic element.
Embodiment 3
(1) by the silver-colored titanium dioxide of the load of the diatomite of 70 parts by weight, 200 mesh, 10 parts by weight, the titanium dioxide and 15 of 5 parts by weight The 3Na of parts by weight2O·SiO2Mix 10min under stiring, after carbon dioxide purity be 60%, blow gas pressure be 0.1MPa item Carbon dioxide air hardening method curing molding is carried out under part, obtains filter core green compact;
(2) the filter core green compact that step (1) obtains are divided into six sections by sintering temperature to be sintered, first segment is by sintering temperature It is warming up to 110 DEG C from 25 DEG C with the heating rate of 15 DEG C/min, keeps the temperature 2h, second segment is by sintering temperature with the heating of 15 DEG C/min Rate is warming up to 350 DEG C from 110 DEG C, keeps the temperature 1h, and third section heats up sintering temperature with the heating rate of 15 DEG C/min from 350 DEG C To 780 DEG C, 5h is kept the temperature, sintering temperature is warming up to 1100 DEG C from 780 DEG C with the heating rate of 15 DEG C/min by the 4th section, heat preservation 5h, sintering temperature is cooled to 500 DEG C from 1100 DEG C with the heating rate of 15 DEG C/min by the 5th section, keeps the temperature 8h, and the 6th section will burn Junction temperature is cooled to 80 DEG C from 500 DEG C with the heating rate of 15 DEG C/min, keeps the temperature 27h, after be cooled to room temperature, with the stream of 1L/min Speed rinses 10min and removes removing heavy metals, 200 DEG C of dry 10min, and polishing removes powder, obtains the ceramic element.
Embodiment 4
In the present embodiment, a kind of preparation method of ceramic element is provided, the ceramic element preparation method includes following Step:
(1) by the silver-colored titanium dioxide of the load of the diatomite of 50 parts by weight, 50 mesh, 20 parts by weight, the titanium dioxide and 15 of 15 parts by weight The K of parts by weight2O·3SiO2Mix 10min under stiring, after carbon dioxide purity be 99%, blow gas pressure be 1MPa condition Lower progress carbon dioxide air hardening method curing molding, obtains filter core green compact;
(2) the filter core green compact that step (1) obtains are divided into six sections by sintering temperature to be sintered, first segment is by sintering temperature It is warming up to 110 DEG C from 25 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 5h, second segment is by sintering temperature with the heating of 10 DEG C/min Rate is warming up to 350 DEG C from 110 DEG C, keeps the temperature 5h, and third section heats up sintering temperature with the heating rate of 10 DEG C/min from 350 DEG C To 780 DEG C, 5h is kept the temperature, sintering temperature is warming up to 1100 DEG C from 780 DEG C with the heating rate of 10 DEG C/min by the 4th section, heat preservation 10h, sintering temperature is cooled to 500 DEG C from 1100 DEG C with the heating rate of 10 DEG C/min by the 5th section, keeps the temperature 20h, and the 6th section will Sintering temperature is cooled to 80 DEG C from 500 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 50h, after be cooled to room temperature, with 10L/min Flow velocity rinse 60min and remove removing heavy metals, 500 DEG C of dry 10min polish and remove powder, obtain the ceramic element.
Embodiment 5
In the present embodiment, a kind of preparation method of ceramic element is provided, the ceramic element preparation method includes following Step:
(1) by the silver-colored titanium dioxide of the load of the diatomite of 80 parts by weight, 1000 mesh, 5 parts by weight, the titanium dioxide and 10 of 5 parts by weight The 3K of parts by weight2O·SiO2Mix 60min under stiring, after carbon dioxide purity be 60%, blow gas pressure be 0.1MPa item Carbon dioxide air hardening method curing molding is carried out under part, obtains filter core green compact;
(2) the filter core green compact that step (1) obtains are divided into six sections by sintering temperature to be sintered, first segment is by sintering temperature It is warming up to 110 DEG C from 25 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 1h, second segment is by sintering temperature with the heating speed of 5 DEG C/min Rate is warming up to 350 DEG C from 110 DEG C, keeps the temperature 1h, and sintering temperature is warming up to the heating rate of 5 DEG C/min from 350 DEG C by third section 780 DEG C, 1h is kept the temperature, sintering temperature is warming up to 1100 DEG C from 780 DEG C with the heating rate of 5 DEG C/min by the 4th section, 1h is kept the temperature, the Sintering temperature is cooled to 500 DEG C from 1100 DEG C with the heating rate of 5 DEG C/min by five sections, keeps the temperature 1h, and the 6th section by sintering temperature Be cooled to 80 DEG C from 500 DEG C with the heating rate of 5 DEG C/min, keep the temperature 10h, after be cooled to room temperature, rushed with the flow velocity of 0.1L/min It washes 60min and removes removing heavy metals, 80 DEG C of dry 60min, polishing removes powder, obtains the ceramic element.
Embodiment 6
Difference with embodiment 1 is only that Na in waterglass2O and SiO2Rub number be 5:1, remaining component and component proportion And preparation method is same as Example 1.
Embodiment 7
Difference with embodiment 1 is only that Na in waterglass2O and SiO2Rub number be 1:5, remaining component and component proportion And preparation method is same as Example 1.
Embodiment 8
Difference with embodiment 1 is only that the mesh number of diatomite is 20 mesh, remaining component and component proportion and preparation side Method is same as Example 1.
Embodiment 9
Difference with embodiment 1 is only that the mesh number of diatomite is 1500 mesh, remaining component and component proportion and preparation Method is same as Example 1.
Embodiment 10
Difference with embodiment 1 is only that sintering temperature is divided into 5 sections, i.e., merges first segment and second segment, be as sintered Temperature is directly warming up to 350 DEG C from 25 DEG C with the heating rate of 1 DEG C/min, in 350 DEG C of heat preservation 1h, remaining component and component proportion And preparation method is same as Example 1.
Embodiment 11
Difference with embodiment 1 is only that sintering temperature is divided into 5 sections, i.e., merges third section and the 4th section, be as sintered Temperature is directly warming up to 1100 DEG C from 350 DEG C with the heating rate of 1 DEG C/min, in 1100 DEG C of heat preservation 3h, remaining component and component Proportion and preparation method are same as Example 1.
Embodiment 12
Difference with embodiment 1 is only that sintering temperature is divided into 5 sections, i.e., merges the 5th section and the 6th section, be as sintered Temperature is directly cooled to 80 DEG C from 1100 DEG C with the heating rate of 1 DEG C/min, and in 80 DEG C of heat preservation 32h, remaining component and group are distributed Than and preparation method it is same as Example 1.
Embodiment 13
Difference with embodiment 1 is only that sintering temperature is divided into 4 sections, first segment, second segment and third section is merged, as Sintering temperature is directly warming up to 780 DEG C from 25 DEG C with the heating rate of 1 DEG C/min, in 780 DEG C of heat preservation 2h, remaining component and component Proportion and preparation method are same as Example 1.
Embodiment 14
Difference with embodiment 1 is only that sintering temperature is divided into 3 sections, and first segment and second segment are merged, as sintering temperature Degree is directly warming up to 350 DEG C from 25 DEG C with the heating rate of 1 DEG C/min, and in 350 DEG C of heat preservation 1h, third section and the 4th section are closed And as sintering temperature with the heating rate of 1 DEG C/min is directly warming up to 1100 DEG C from 350 DEG C, in 1100 DEG C of heat preservation 3h, by Five sections and the 6th section merging, as sintering temperature is cooled to 80 DEG C from 1100 DEG C with the rate of temperature fall of 1 DEG C/min, keeps the temperature at 80 DEG C 32h, remaining component and component proportion and preparation method are same as Example 1.
Embodiment 15
Difference with embodiment 1 is only that the mass ratio for carrying silver-colored titanium dioxide and titanium dioxide is 3:7, that is, carries silver-colored titanium dioxide For 3 parts by weight, titanium dioxide is 7 parts by weight, remaining component and component proportion and preparation method are same as Example 1.
Embodiment 16
Difference with embodiment 1 is only that the mass ratio for carrying silver-colored titanium dioxide and titanium dioxide is 4:1, that is, carries silver-colored titanium dioxide For 8 parts by weight, titanium dioxide is 2 parts by weight, remaining component and component proportion and preparation method are same as Example 1.
Embodiment 17
Difference with embodiment 1 is only that the bacteriostatic agent of the present embodiment does not include carrying silver-colored titanium dioxide, and titanium dioxide adds Dosage is that silver-colored the sum of titanium dioxide and the additive amount of titanium dioxide are carried in embodiment 1, i.e. the additive amount of titanium dioxide is 10 parts by weight, Remaining component and component proportion and preparation method are same as Example 1.
Embodiment 18
Difference with embodiment 1 is only that the bacteriostatic agent of the present embodiment does not include titanium dioxide, and carries adding for silver-colored titanium dioxide Dosage is that silver-colored the sum of titanium dioxide and the additive amount of titanium dioxide are carried in embodiment 1, that is, the additive amount for carrying silver-colored titanium dioxide is 10 weights Part is measured, remaining component and component proportion and preparation method are same as Example 1.
Embodiment 19
Difference with embodiment 1 is only that, with the silver-colored titanium dioxide of load in the active carbon loading silver alternate embodiment 1 of equivalent and titanium The sum of additive amount of white powder, the i.e. additive amount of active carbon loading silver are 10 parts by weight.
Embodiment 20
Difference with embodiment 1 is only that, with the silver-colored titanium dioxide of load in the nano zine oxide alternate embodiment 1 of equivalent and titanium The sum of additive amount of white powder, the i.e. additive amount of nano zine oxide are 10 parts by weight.
Comparative example 1
Difference with embodiment 1 is only that sintering process, as sintering temperature are warming up to 1100 DEG C from 25 DEG C, keep the temperature 3h, Remaining component and component proportion and preparation method are same as Example 1.
Comparative example 2
Difference with embodiment 1 is only that sintering temperature is divided into 2 sections, by first segment, second segment, third section and the 4th section of conjunction And as sintering temperature with the heating rate of 1 DEG C/min is directly warming up to 1100 DEG C from 25 DEG C, in 1100 DEG C of heat preservation 3h, by Five sections and the 6th section merging, as sintering temperature is directly cooled to 80 DEG C from 1100 DEG C with the heating rate of 1 DEG C/min, at 80 DEG C 32h is kept the temperature, remaining component and component proportion and preparation method are same as Example 1.
The ceramic element for measuring embodiment 1-12 and comparative example 1-2 offer carries out fungistatic effect test, mark-on chlorine residue is tested, Filtering accuracy test, metal ion residue analysis and tensile test, test method are as follows:
Fungistatic effect test: " the anti-of stable state antibacterial agent is measured under the conditions of dynamic Contact according to ASTM E2149-2013a The standard test method of bacterium determination of activity " it is measured;
Mark-on chlorine residue test: it is measured according to GB5750-85 " drinking water standard method of inspection ";
Table 1
Wherein, the chromium remnants are that Cr VI is remaining.
As shown in Table 1, ceramic element prepared by the present invention have preferable mechanical strength, higher degerming rate, Chlorine residue removal rate and filtering accuracy, and heavy metal free pollutes;By the comparison of embodiment 1 and embodiment 6-7 it is found that when in waterglass Sodium oxide molybdena and rubbing for silica count ratio not in the framework of the present definition, then the mechanical performance of ceramic element is poor, and meeting There is micro heavy remaining;It is by the comparison of embodiment 1 and embodiment 8-9 it is found that the mesh number when diatomite is lower than 50 mesh, then ceramic The filtering accuracy of filter core is lower, influences filter effect, when the mesh number of diatomite is higher than 1000 mesh, although not influencing filtering accuracy, But filtering it is slower, need to filtration time it is more long;By the comparison of embodiment 1 and embodiment 10-14 it is found that the machine of ceramic element Tool intensity, degerming rate, chlorine residue removal rate and filtering accuracy are higher, but number of segment is fewer, and the performance of ceramic element can be dropped It is low;By the comparison of embodiment 1 and comparative example 1-2 it is found that temperature is divided into 3-6 sections when ceramic element does not use during the sintering process Control, the performance for the ceramic element being prepared can decline, and will increase the fraction defective of product;By embodiment 1 and embodiment 15-16 Comparison it is found that when carry the mass ratio of silver-colored titanium dioxide and titanium dioxide not present invention provide that in the range of, then the pottery that is prepared The degerming rate of porcelain filter core is poor;By the comparison of embodiment 1 and embodiment 17-20 it is found that when lacking the silver-colored titanium dioxide of load in raw material When replacing with one of titanium dioxide or with other bacteriostatic agents, then the degerming rate of the ceramic element prepared is also poor;Therefore, originally It is high to invent the ceramic element high mechanical strength provided, filtering accuracy, degerming rate and chlorine residue removal rate are high, heavy metal free pollution, and The sintering process used time is shorter, substantially reduces the time of ceramic element preparation process.
The Applicant declares that the foregoing is merely a specific embodiment of the invention, but protection scope of the present invention not office It is limited to this, it should be clear to those skilled in the art, any to belong to those skilled in the art and take off in the present invention In the technical scope of dew, any changes or substitutions that can be easily thought of, and all of which fall within the scope of protection and disclosure of the present invention.

Claims (10)

1. a kind of preparation method of ceramic element, which is characterized in that the preparation method includes being sintered filter core green compact, institute It states in sintering process and sintering temperature is divided into 3-6 sections.
2. preparation method according to claim 1, which is characterized in that the sintering temperature is divided into 6 sections, and first segment is removal Moisture in green compact, second segment are to be pre-sintered, and third section is crystallization, and the 4th section is porcelain, and the 5th section is annealing, and the 6th section is It is cooling.
3. preparation method according to claim 1 or 2, which is characterized in that the first segment sintering temperature heats up from 25 DEG C To 110 DEG C, heating rate is 1 DEG C/min-15 DEG C/min, preferably 1 DEG C/min;
Preferably, the first segment is in 110 DEG C of heat preservations 1-5h, preferably 2h;
Preferably, the second segment sintering temperature is warming up to 350 DEG C from 110 DEG C, and heating rate is 1 DEG C/min-15 DEG C/min, excellent Select 1 DEG C/min;
Preferably, the second segment is in 350 DEG C of heat preservations 1-5h, preferably 1h;
Preferably, the third section sintering temperature is warming up to 780 DEG C from 350 DEG C, and heating rate is 1 DEG C/min-15 DEG C/min, excellent Select 1 DEG C/min;
Preferably, the third section is in 780 DEG C of heat preservations 1-5h, preferably 2h;
Preferably, the 4th section of sintering temperature is warming up to 1100 DEG C from 780 DEG C, and heating rate is 1 DEG C/min-15 DEG C/min, It is preferred that 1 DEG C/min;
Preferably, described 4th section in 1100 DEG C of heat preservations 1-10h, preferably 3h;
Preferably, the 5th section of sintering temperature is cooled to 500 DEG C from 1100 DEG C, and rate of temperature fall is 1 DEG C/min-15 DEG C/min, It is preferred that 1 DEG C/min;
Preferably, described 5th section in 500 DEG C of heat preservations 1-20h, preferably 8h;
Preferably, the 6th section of sintering temperature is cooled to 80 DEG C from 500 DEG C, and rate of temperature fall is 1 DEG C/min-15 DEG C/min, excellent Select 1 DEG C/min;
Preferably, described 6th section in 80 DEG C of heat preservations 10-50h, preferably 32h.
4. the preparation method of ceramic element according to claim 1-3, which is characterized in that the filter core green compact The preparation method comprises the following steps: diatomite, bacteriostatic agent and waterglass are uniformly mixed, filter core green compact are obtained.
5. the preparation method according to claim 4, which is characterized in that the mesh number of the diatomite is 50-1000 mesh;
Preferably, in terms of by the additive amount of diatomite for 50-80 parts by weight, the additive amount of the bacteriostatic agent is 10-30 parts by weight;
Preferably, the bacteriostatic agent is nano zine oxide, negative ion powder, titanium dioxide, active carbon loading silver, carries silver-colored titanium dioxide or fourth In perfume (or spice) any one or at least two combination, preferably carry the mixing of silver-colored titanium dioxide and titanium dioxide;
Preferably, the silver-colored titanium dioxide and the mass ratio of titanium dioxide of carrying is 1:1-2:1;
Preferably, in terms of by the additive amount of diatomite for 50-80 parts by weight, the additive amount of the waterglass is 10-15 parts by weight;
Preferably, the number that rubs of the waterglass neutral and alkali metal oxide and silica is 0.3:1-3:1, preferably 3:1;
Preferably, the alkaline metal oxide is sodium oxide molybdena or potassium oxide.
6. preparation method according to claim 4 or 5, which is characterized in that the mixing is to mix under agitation, is stirred Mixing the time is 10-60min;
Preferably, the curing molding is solidified by carbon dioxide air hardening method;
Preferably, the purity of the carbon dioxide be 60%-99%, preferably 99%;
Preferably, the blow gas pressure of the carbon dioxide gas is 0.1MPa-1MPa.
7. according to the described in any item preparation methods of claim 4-6, which is characterized in that the ceramic element preparation method includes Following steps:
(1) 50-80 parts by weight diatomite, 10-30 parts by weight bacteriostatic agent and 10-15 parts by weight waterglass are mixed under stiring 10-60min, after carbon dioxide purity be 99%, blow gas pressure be 0.5MPa under the conditions of by carbon dioxide air hardening method solidify Molding, obtains filter core green compact;
(2) the filter core green compact that step (1) obtains are divided into six sections by sintering temperature to be sintered, first segment is by sintering temperature with 1 DEG C/heating rate of min-15 DEG C/min is warming up to 110 DEG C from 25 DEG C, keep the temperature 1-5h, second segment by sintering temperature with 1 DEG C/ The heating rate of min-15 DEG C/min is warming up to 350 DEG C from 110 DEG C, keeps the temperature 1-5h, third section is by sintering temperature with 1 DEG C/min- The heating rate of 15 DEG C/min is warming up to 780 DEG C from 350 DEG C, keeps the temperature 1-5h, the 4th section by sintering temperature with 1 DEG C/min-15 DEG C/ The heating rate of min is warming up to 1100 DEG C from 780 DEG C, keeps the temperature 1-10h, the 5th section by sintering temperature with 1 DEG C/min-15 DEG C/min Heating rate be cooled to 500 DEG C from 1100 DEG C, keep the temperature 1-20h, the 6th section by sintering temperature with 1 DEG C/min-15 DEG C/min's Heating rate is cooled to 80 DEG C from 500 DEG C, keeps the temperature 10-50h, obtains ceramic element.
8. preparation method according to claim 7, which is characterized in that the ceramic element preparation method further includes that will obtain Ceramic element it is cooling, go removing heavy metals and drying;
Preferably, described that removing heavy metals is gone to realize by rinsing or impregnating;
Preferably, the mixing rinsed or impregnate that liquid used is any one in water, alcohol or methanol or at least two;
Preferably, the pressure of the flushing is 0.1-0.5MPa;
Preferably, the flow velocity of the flushing is 0.1-10L/min;
Preferably, the drying temperature is 80-500 DEG C;
Preferably, the drying time is 10min-120min.
9. a kind of ceramic element being prepared by the described in any item preparation methods of claim 1-8.
10. application of the ceramic element according to claim 9 in water filtration.
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Denomination of invention: A ceramic filter element, its preparation method and use

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