CN108033776A - A kind of porous oxidation calcium material and its preparation method and application - Google Patents
A kind of porous oxidation calcium material and its preparation method and application Download PDFInfo
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- CN108033776A CN108033776A CN201711266677.XA CN201711266677A CN108033776A CN 108033776 A CN108033776 A CN 108033776A CN 201711266677 A CN201711266677 A CN 201711266677A CN 108033776 A CN108033776 A CN 108033776A
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/057—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on calcium oxide
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The invention belongs to technical field of inorganic material, is related to a kind of porous oxidation calcium material and its preparation method and application.The preparation method of the porous oxidation calcium material in turn includes the following steps, (1) batch mixing：Calcium hydroxide powder, deionized water, sodium carboxymethylcellulose are mixed in proportion；(2) molding and preliminarily dried：Uniformly mixed batch mixing is pressed into required shape by mould, and carries out preliminarily dried；(3) sinter：Batch mixing after preliminarily dried is added in sintering furnace to heat and is sintered.Utilize the preparation method of the porous oxidation calcium material of the present invention, can simple and convenient, low expense, time-consuming short a large amount of prepare porous oxidation calcium material, and the calcia material loose structure that is prepared with the method is obvious, fusing point is high and steam forces down, the target of nuclear reaction can be used as well.
Description
Technical field
The invention belongs to technical field of inorganic material, is related to a kind of porous oxidation calcium material and its preparation method and application.
Background technology
Required radionuclide can be generated by carrying out nuclear reaction by line and target.The radioactive nucleus of nuclear reaction generation
Element, especially short-life radionuclide need quickly to discharge from target, therefore it is porous generally to require target to have
Structure.In addition, when carrying out nuclear reaction, temperature is very high, therefore it is required that target has higher fusing point and relatively low steam at the same time
Pressure.And since target is disposed in target cylinder when in use, it is not high to the intensity requirement of target, therefore it can be absorbed in
On loose structure.
In conclusion a kind of simple and convenient, low expense, time-consuming short method is needed to be used for a large amount of preparations in practice strongly
The target of nuclear reaction, especially calcium oxide target, and the target loose structure being prepared with the method is obvious, fusing point is high and steams
Vapour pressure is low.
The content of the invention
The primary and foremost purpose of the present invention is to provide a kind of preparation method of porous oxidation calcium material, so as to simple and convenient, low
Expense, it is time-consuming it is short it is a large amount of prepare porous oxidation calcium material, and the calcia material loose structure being prepared with the method is bright
It is aobvious, fusing point is high and steam forces down, the target of nuclear reaction can be used as well.
In order to achieve this, in the embodiment on basis, the present invention provides a kind of preparation side of porous oxidation calcium material
Method, the preparation method in turn include the following steps,
(1) batch mixing：Calcium hydroxide powder, deionized water, sodium carboxymethylcellulose are mixed in proportion；
(2) molding and preliminarily dried：Uniformly mixed batch mixing is pressed into required shape by mould, and is carried out tentatively dry
It is dry；
(3) sinter：Batch mixing after preliminarily dried is added in sintering furnace to heat and is sintered.
The principle of the preparation method of the porous oxidation calcium material of the present invention is as follows：
Calcium hydroxide powder of the purity more than 95% is proportionally uniformly mixed with sodium carboxymethylcellulose, is added afterwards
Suitable deionized water, is extruded by long agitation, eventually becomes a sticky block.Wherein calcium hydroxide, water, carboxylic first
The mixing quality ratio of base sodium cellulosate is (10-20):(8-12):1, preferably 15:10:1.Wherein sodium carboxymethylcellulose dissolves in
Water, has viscosity after dissolving；Sodium carboxymethylcellulose can be decomposed into sodium carbonate, water and dioxy under conditions of high-temperature oxygen-enriched
Change carbon, therefore used in sintering as binding agent and pore creating material.
The block is pressed into required shape by mould.Since block is sticky form, required pressure is molded
Power very little, and the material of a large amount of required shapes can be quickly and easily prepared by mould.Compressing batch mixing can be in room
Warm atmospheric pressure, exposed to air drying 2-5 it is small when, preferably 3 it is small when.
Batch mixing after drying is positioned in sintering furnace heating in atmospheric conditions and is sintered heat treatment.The mistake of heat treatment
Journey is divided into four-stage：
A. begin to warm up at room temperature, by 4-6 it is small when, preferably 5 are uniformly heating to 320-380 DEG C, preferably 350 DEG C when small,
Maintain 1.5-2.5 it is small when, preferably 2 it is small when；
B. by 3-5 it is small when, preferably 4 are uniformly heating to 550-650 DEG C, preferably 600 DEG C when small, when maintaining 1.5-2.5 small,
It is preferred that 2 it is small when；
C. by 3-5 it is small when, preferably 4 are uniformly heating to 850-950 DEG C, preferably 900 DEG C when small, when maintaining 1.5-2.5 small,
It is preferred that 2 it is small when；
D. last cooled to room temperature.
Wherein：
The A stages be used to removing it is dry after remaining moisture and sodium carboxymethylcellulose in batch mixing.The carboxylic first at 320-380 DEG C
Base sodium cellulosate is decomposed into sodium carbonate, water and carbon dioxide, while the water and carbon dioxide that generate can be evaporated out matrix.In order to
Matrix is not destroyed, temperature-rise period needs slow.It is in order to which decomposition reaction fully carries out when maintaining 1.5-25 small for 320-380 DEG C.
Different with the ratio of sodium carboxymethylcellulose according to the total amount of batch mixing, the time of maintenance is also different, this point can be with vacuum not
Become the standard of turning to again and judge whether reaction is complete.
B-stage is the catabolic phase of calcium hydroxide.At 550-650 DEG C, calcium hydroxide is decomposed into calcium oxide and water, in order to
Make the reaction was complete will not destroy matrix with moisture slow evaporation, temperature-rise period is slow.
C-stage is used for sintering oxidation calcium particle, strengthens matrix strength, prevents that material is put into nuclear reaction target cylinder afterwards
Material fragmentation when in operation.
Calcia material is taken out after heat treatment process, will since calcium oxide can be with the reaction of moisture in air
Calcia material is put into vacuum bag and is sealed.
In a preferred embodiment, the present invention provides a kind of preparation method of porous oxidation calcium material, wherein walking
Suddenly the calcium hydroxide powder described in (1), deionized water, the mixing quality ratio of sodium carboxymethylcellulose are (10-20):(8-
12):1。
In a preferred embodiment, the present invention provides a kind of preparation method of porous oxidation calcium material, wherein walking
Suddenly the purity of the calcium hydroxide powder described in (1) is more than 95%.
In a preferred embodiment, the present invention provides a kind of preparation method of porous oxidation calcium material, wherein walking
Suddenly the preliminarily dried described in (2) press dry dry for atmosphere at room temperature.
In a kind of more preferred embodiment, the present invention provides a kind of preparation method of porous oxidation calcium material, its
Described in atmosphere at room temperature press dry the dry time for 2-5 it is small when.
In a preferred embodiment, the present invention provides a kind of preparation method of porous oxidation calcium material, wherein walking
Suddenly the process of the sintering described in (3) is：
1) begin to warm up at room temperature, be warming up to 320-380 DEG C, when maintaining 1.5-2.5 small；
2) 550-650 DEG C is continuously heating to, when maintaining 1.5-25 small；
3) 850-950 DEG C is continuously heating to, when maintaining 1.5-25 small；
4) cooled to room temperature.
In a kind of more preferred embodiment, the present invention provides a kind of preparation method of porous oxidation calcium material, its
Middle process 1) in be warming up to 320-380 DEG C of time for 4-6 it is small when.
In a kind of more preferred embodiment, the present invention provides a kind of preparation method of porous oxidation calcium material, its
Middle process 2) in be warming up to 550-650 DEG C of time for 3-5 it is small when.
In a kind of more preferred embodiment, the present invention provides a kind of preparation method of porous oxidation calcium material, its
Middle process 3) in be warming up to 850-950 DEG C of time for 3-5 it is small when.
Second object of the present invention is to provide the porous oxidation calcium material being prepared using the above method, so as to more
Pore structure is obvious, fusing point is high and steam forces down, and can be used as the target of nuclear reaction well.
In order to achieve this, in the embodiment on basis, the present invention provides a kind of porous oxidation calcium material, it is by above-mentioned
Method is prepared.
Third object of the present invention is to provide anti-as core using the porous oxidation calcium material that the above method is prepared
The purposes of target is answered, so as to the radionuclide that quick release generates after nuclear reaction.
In order to achieve this, in the embodiment on basis, present invention offer is prepared porous using the above method
Calcia material is used as the purposes of nuclear reaction target.
The beneficial effects of the present invention are, can simply just using the preparation method of the porous oxidation calcium material of the present invention
Prompt, low expense, it is time-consuming it is short it is a large amount of prepare porous oxidation calcium material, and the porous knot of calcia material being prepared with the method
Structure is obvious, fusing point is high and steam forces down, and can be used as the target of nuclear reaction well.
Brief description of the drawings
Fig. 1 is the scanning electron microscope testing result figure for No. 5 porous oxidation calcium materials that embodiment 1 is prepared.
Embodiment
The embodiment of the present invention is further illustrated with attached drawing with reference to embodiments.
Embodiment 1：The preparation of porous oxidation calcium material
The preparation of each numbering porous oxidation calcium material is carried out in accordance with the following steps, the preparation of each numbering porous oxidation calcium material
Raw material proportioning (calcium hydroxide powder, deionized water, the mass ratio of sodium carboxymethylcellulose) and specific preparation method condition are as follows
Shown in table 1.
(1) calcium hydroxide powder (purity 95.5%), deionized water, sodium carboxymethylcellulose are mixed in proportion
It is even；
(2) uniformly mixed batch mixing is pressed into circle by mould, and atmosphere at room temperature pressure be exposed in air into
Row preliminarily dried；
(3) batch mixing after preliminarily dried is added in sintering furnace to heat and be sintered.
Wherein, the sintering process of step (3) is：
1) begin to warm up at room temperature, by 4-6 it is small when be uniformly heating to 320-380 DEG C, when maintaining 1.5-2.5 small；
2) by 3-5 it is small when be uniformly heating to 550-650 DEG C, when maintaining 1.5-2.5 small；
3) by 3-5 it is small when be uniformly heating to 850-950 DEG C, when maintaining 1.5-2.5 small；
4) last cooled to room temperature.
The preparing raw material of each numbering porous oxidation calcium material of table 1 is with when specific preparation method condition
Embodiment 2：The detection of each numbering porous oxidation calcium material is prepared in embodiment 1
The porous CaO materials'use gas adsorption method respectively numbered being prepared as described in Example 1 is subjected to hole
The detection of gap rate (referring to：The assay method [J] of Liu Peisheng, aperture of porous material and pore-size distribution, Ti industry progress, 2006,23
(2):29-34.), testing result is as shown in table 2 below.
The porosity testing result of each numbering porous oxidation calcium material of table 2
| Material number | Porosity |
| 1 | 56% |
| 2 | 52% |
| 3 | 42% |
| 4 | 48% |
| 5 | 50% |
In addition, No. 5 porous oxidation calcium materials are scanned with Electronic Speculum detection, the results are shown in Figure 1.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and scope.If in this way, belong to the model of the claims in the present invention and its equivalent technology to these modifications and changes of the present invention
Within enclosing, then the present invention is also intended to comprising including these modification and variations.Above-described embodiment or embodiment are simply to the present invention
For example, the present invention can also be implemented with other ad hoc fashions or other particular form, without departing from the present invention's
Main idea or substantive characteristics.Therefore, it is regarded as from the point of view of the embodiment of description is in terms of any illustrative and non-limiting.This
The scope of invention should be illustrated that any change equivalent with the intention of claim and scope should also be included by appended claims
Within the scope of the invention.
Claims (10)
- A kind of 1. preparation method of porous oxidation calcium material, it is characterised in that the preparation method in turn includes the following steps,(1) batch mixing：Calcium hydroxide powder, deionized water, sodium carboxymethylcellulose are mixed in proportion；(2) molding and preliminarily dried：Uniformly mixed batch mixing is pressed into required shape by mould, and carries out preliminarily dried；(3) sinter：Batch mixing after preliminarily dried is added in sintering furnace to heat and is sintered.
- 2. preparation method according to claim 1, it is characterised in that：Calcium hydroxide powder described in step (1), go from Sub- water, the mixing quality ratio of sodium carboxymethylcellulose are (10-20):(8-12):1.
- 3. preparation method according to claim 1, it is characterised in that：Calcium hydroxide powder described in step (1) it is pure Degree is more than 95%.
- 4. preparation method according to claim 1, it is characterised in that：Preliminarily dried described in step (2) is big for room temperature Air pressure is dried.
- 5. preparation method according to claim 4, it is characterised in that：It is 2-5 that the atmosphere at room temperature, which press dry the dry time, Hour.
- 6. preparation method according to claim 1, it is characterised in that the process of the sintering described in step (3) is：1) begin to warm up at room temperature, be warming up to 320-380 DEG C, when maintaining 1.5-2.5 small；2) 550-650 DEG C is continuously heating to, when maintaining 1.5-2.5 small；3) 850-950 DEG C is continuously heating to, when maintaining 1.5-2.5 small；4) cooled to room temperature.
- 7. preparation method according to claim 6, it is characterised in that：Process 1) in be warming up to 320-380 DEG C of time and be When 4-6 is small.
- 8. preparation method according to claim 6, it is characterised in that：Process 2) in be warming up to 550-650 DEG C of time and be When 3-5 is small；Process 3) in be warming up to 850-950 DEG C of time for 3-5 it is small when.
- A kind of 9. porous oxidation calcium material, it is characterised in that：The porous oxidation calcium material according in claim 1-8 by appointing Preparation method described in meaning one is prepared.
- 10. porous oxidation calcium material according to claim 9 is used as the purposes of nuclear reaction target.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108905949A (en) * | 2018-07-12 | 2018-11-30 | 杭州家爽包装材料有限公司 | A kind of preparation method and product of calcium oxide desiccant |
| CN109097003A (en) * | 2018-08-27 | 2018-12-28 | 上海交通大学 | With infiltrative heat chemistry heat accumulation shaped granule of optimization and preparation method thereof |
| CN113321493A (en) * | 2021-05-25 | 2021-08-31 | 江苏智林空间装备科技有限公司 | Zero-expansion porous ceramic and application and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108905949A (en) * | 2018-07-12 | 2018-11-30 | 杭州家爽包装材料有限公司 | A kind of preparation method and product of calcium oxide desiccant |
| CN108905949B (en) * | 2018-07-12 | 2021-02-26 | 杭州家爽包装材料有限公司 | Preparation method of calcium oxide drying agent and product |
| CN109097003A (en) * | 2018-08-27 | 2018-12-28 | 上海交通大学 | With infiltrative heat chemistry heat accumulation shaped granule of optimization and preparation method thereof |
| CN109097003B (en) * | 2018-08-27 | 2020-06-09 | 上海交通大学 | Thermochemical heat storage molded particle with optimized permeability and preparation method thereof |
| CN113321493A (en) * | 2021-05-25 | 2021-08-31 | 江苏智林空间装备科技有限公司 | Zero-expansion porous ceramic and application and preparation method thereof |
| CN113321493B (en) * | 2021-05-25 | 2022-11-08 | 江苏智林空间装备科技有限公司 | Zero-expansion porous ceramic and application and preparation method thereof |
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Application publication date: 20180515 |