CN107256724B - The preparation method of tritium proliferation ceramic material metatitanic acid lithium - Google Patents

The preparation method of tritium proliferation ceramic material metatitanic acid lithium Download PDF

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CN107256724B
CN107256724B CN201710434146.0A CN201710434146A CN107256724B CN 107256724 B CN107256724 B CN 107256724B CN 201710434146 A CN201710434146 A CN 201710434146A CN 107256724 B CN107256724 B CN 107256724B
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metatitanic acid
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acid lithium
tritium
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CN107256724A (en
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李化全
孙鹏
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SHANDONG DOGUIDE GROUP CO Ltd
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21B—FUSION REACTORS
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    • G21B1/11—Details
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    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
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    • C01C1/24—Sulfates of ammonium
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    • C01G23/005—Alkali titanates
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The invention belongs to new materials and technical field of function materials, and in particular to a kind of preparation method of tritium proliferation ceramic material metatitanic acid lithium.The method comprises the following steps: the preparation of (1) titanium source presoma；(2) lithium source inlays reaction and iontophoresis adulterates；(3) calcining and micro mist；(4) it post-processes.Process of the present invention is short, simple process, scientific and reasonable, low production cost, production process are easily controllable；The metatitanic acid lithium intensity of preparation is big, partial size is small, impurity is few, open-celled structure is abundant, stable product quality.

Description

The preparation method of tritium proliferation ceramic material metatitanic acid lithium
Technical field
The invention belongs to new materials and technical field of function materials, and in particular to a kind of tritium proliferation ceramic material metatitanic acid The preparation method of lithium.
Background technique
With the high speed development of global economy, the mankind are increasing to energy demand, and the earth leaves the original money of the mankind for Source more use is fewer.The problem of energy shortage and environment worsening becomes the common difficulty of the whole mankind, thus seek more cleaning, Safety, renewable energy are concerned, and become the common recognition of various countries people.
Thermonuclear fusion is one of energy research direction important at present, and the material that Fusion Neutron produces tritium is particularly important.Partially Lithium titanate (Li2TiO3) be used as lithium-based ceramic material as material most promising in tritium-breeding material in thermonuclear reactor it One, because it is with reasonable lithium atom density, activity is low, chemical stability is high, has good compatibility with structural material. Therefore, Li2TiO3Powder preparation method is the focus of attention of lot of domestic and foreign researcher.
Lithium-based ceramic Li2TiO3With its considerable lithium atom density, low reactivity, excellent chemical stability and structural wood Expect good compatibility and good tritium low temperature release performance, is acknowledged as a kind of high comprehensive performance, most future One of solid tritium multiplication agent.The method prepared at present mainly has solid phase method, sol-gel method, combustion synthesis method and hydro-thermal method.Gu Phase reaction multiselect Li2CO3And TiO2For raw material, after being sufficiently mixed, at 700~1000 DEG C, high-temperature calcination 5~24 hours.Powder The parameters such as body particle size, the uniformity, crystallinity, super born of the same parents' structure are all different.Because of TiO2With rutile-type, anatase titanium dioxide, The variforms such as amorphous and mixed type, it is therefore difficult to prepare a kind of metatitanic acid lithium of form.Another defect of solid phase method is exactly The generation for realizing reactant by temperature completely, due to thickness of feed layer, entrainment etc. cause reaction not exclusively, need high temperature Long Time Thermal Processing, obtained Li2TiO3Often uneven components, stoichiometry are difficult to control, size distribution is wide and coarse size for powder, and by Raw material TiO2The limitation of structure and pattern, structure are difficult to regulate and control with pattern.Sol-gel method, combustion synthesis method and hydro-thermal method It is typical wet process reaction, reaction condition and ingredient requirement harshness, the metatitanic acid lithium granule-morphology prepared between different batches, granularity Distribution, structure cell diameter etc. are variant.Aforementioned production method high production cost, is unfavorable for industrialized production.Process conditions simultaneously Harshness causes influence to the quality of tritium proliferation ceramics, seeks a kind of side for preparing metatitanic acid lithium easily controllable, quality is stable Method is even more important to the quality control of tritium proliferation ceramics.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of systems of tritium proliferation ceramic material metatitanic acid lithium Preparation Method, process is short, simple process, scientific and reasonable, low production cost, production process are easily controllable, stable product quality.
Tritium of the present invention is proliferated the ceramic material preparation method of metatitanic acid lithium, and steps are as follows:
(1) preparation of titanium source presoma:
After metatitanic acid after sulfuric acid process is cleaned before salt treatment adds water to be beaten, sal volatile is added, continues to stir after adding It mixes, carries out sheet frame squeezing, obtain filter cake；
(2) lithium source inlays reaction and iontophoresis adulterates:
After adding water mashing to handle filter cake obtained by step (1), Li is added2CO3, continue to stir after adding, then be added lithium from Sub- adsorbent continues to stir, and carries out sheet frame squeezing, obtains filter cake；
(3) calcining and micro mist:
By the calcining drying of filter cake obtained by step (2), it is cooled to room temperature and is crushed, be crushed to 325 meshes and tail over 0.2%, It obtains tritium and is proliferated ceramic material metatitanic acid lithium crude product；
(4) it post-processes:
After the proliferation ceramic material of tritium obtained by step (3) is impregnated in boiling water with metatitanic acid lithium crude product, drying obtains tritium increasing Grow ceramic material metatitanic acid lithium product.
Wherein:
After metatitanic acid described in step (1) adds water to be beaten, TiO2Content be 300~400g/L.
The concentration of sal volatile described in step (1) is 400g/L；Sulfuric acid in the additional amount and metatitanic acid of ammonium carbonate Mass ratio be 1.2~1.4:1.
The mixing speed that sal volatile is added described in step (1) is 10~30 turns/min, continues to stir after adding 30min, the sal volatile are slowly added in 3min.
After filter cake described in step (2) adds water mashing to handle, TiO2Content be 550~600g/L.
Li described in step (2)2CO3With H2TiO3Molar ratio be 1.1~1.3:1.
Addition Li described in step (2)2CO3Speed of agitator be 30~50 turns/min, continue after adding stir 45min.
Lithium ion adsorbent described in step (2) is porous silica or basic zirconium chloride, the use of lithium ion adsorbent Amount is TiO2The 0.8~1.0% of quality.
Calcining drying condition described in step (3) are as follows: it is started to warm up by room temperature, constant temperature 1h after being warming up to 400~500 DEG C, Constant temperature 6h after being continuously heating to 650~700 DEG C.
Soaking time described in step (4) is 6~8h.
The preparation method of tritium proliferation ceramic material metatitanic acid lithium of the present invention, the specific steps are as follows:
(1) preparation of titanium source presoma:
Metatitanic acid after sulfuric acid process is cleaned before salt treatment is beaten, and makes its TiO2Content in 300~400g/L, will The sal volatile of the 400g/L prepared in advance is uniformly added in meta-titanium acid solution, in the additional amount and metatitanic acid of ammonium carbonate The content of sulfuric acid is added according to: sulfuric acid/ammonium carbonate=1:1.2~1.4 mass ratio.The process mixing speed of addition is 10~30 Turn/min, be slowly added to, so that the sulfuric acid for being mingled with metatitanic acid is sufficiently reacted with ammonium carbonate, addition is finished, and continues to stir 30min Afterwards, sheet frame squeezing is carried out, filtrate carries out condensing crystallizing, obtains ammonium sulfate product, filter cake enters next process.
(2) lithium source inlays reaction and iontophoresis adulterates:
Preceding process filter cake is subjected to mashing processing using ionized water, is formulated into TiO2Concentration is 550~600g/L, control Li2CO3/H2TiO3Molar ratio be 1.1~1.3:1 be sufficiently beaten, speed of agitator be 30~50 turns/min, stirring 45min Afterwards, suitable porous silica is added or basic zirconium chloride carries out ion doping, continues after stirring 30min, sheet frame squeezing, filter Liquid is counter to be arrived preceding process and uses as the solution for preparing ammonium carbonate, and filter cake enters subsequent processing.
(3) calcining and micro mist:
The filter cake of previous process is fitted into high purity quartz pallet, calcining drying is carried out, it is desirable that is risen by room temperature, 400 ~500 DEG C after constant temperature 1 hour, after being continuously heating to 650~700 DEG C, after constant temperature 6 hours, stop heating, cool the temperature to room temperature Afterwards, after being crushed using super fine machine, tritium proliferation ceramic material metatitanic acid lithium is obtained.
(4) it post-processes:
In order to reduce the influence of minimal residue lithium, the metatitanic acid lithium being prepared is impregnated 6~8 in the ionized water boiled After hour, drying obtains tritium proliferation ceramic material metatitanic acid lithium final products.
Li2TiO3Purity, granular size, particle diameter distribution of powder etc. all can be to Li2TiO3The preparation of ceramic bead and bead It produces tritium performance to have a huge impact, so to metatitanic acid lithium, more stringent requirements are proposed, to meet the metatitanic acid of subsequent preparation It is superior that lithium is proliferated ceramic performance.
The present invention is big to intensity emphatically, partial size is small, impurity is few, open-celled structure is abundant during preparing metatitanic acid lithium Metatitanic acid lithium preparation studied.With the inclined titanium of activity in from a wealth of sources, cheap sulfuric acid method titanium pigment production process Acid is used as titanium source, and after ammonium carbonate is handled, lithium carbonate is added, and realizes that atom or the embedding lithium salts of molecular level are reacted, instead Suitable iontophoresis doping is carried out after answering, again to improve performance of the metatitanic acid lithium in proliferation ceramics.Because of the fusing point of LiOH Compare Li2CO3Fusing point it is low, to promote particle to become larger during reaction, influence the performance of particle, thus lithium salts we select Lithium carbonate is selected, while lithium carbonate provides more micro-channel holes during reaction for metatitanic acid lithium, is subsequent inclined Lithium titanate proliferation ceramics create more open-celled structures, provide more excellent performance.Calcination process strict temperature control In 650~700 DEG C of temperature region, to ensure to be formed the particle of the Large ratio surface of loose shape, specific surface can be in 50m2/ g with The particle of upper anatase titanium dioxide, because the grain graininess of rutile-type is hard and density is high, proliferation ceramic performance is reduced, and has lower The anatase titanium dioxide particle of density is more conducive to the preparation of proliferation ceramics.In order to reduce the influence of the remaining lithium in micropore, will make After standby obtained metatitanic acid lithium crude product is impregnated 6~8 hours in the ionized water boiled, drying obtains tritium proliferation ceramic material and uses Metatitanic acid lithium final products.
Compared with prior art, the beneficial effects of the present invention are:
1, process of the present invention is short, simple process, scientific and reasonable, low production cost, production process are easily controllable, product matter Amount is stablized.
2, metatitanic acid lithium intensity prepared by the present invention is big, partial size is small, impurity is few, open-celled structure is abundant.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but does not limit the present invention.
Embodiment 1
Metatitanic acid 1kg after sulfuric acid process is cleaned before salt treatment carries out mashing metering, makes its TiO2Content be 300g/L, The sal volatile of the 400g/L prepared in advance is uniformly added in meta-titanium acid solution, the additional amount and metatitanic acid of ammonium carbonate The content of middle sulfuric acid is added according to: sulfuric acid/ammonium carbonate=1:1.2 mass ratio.The process mixing speed of addition is 10 turns/min, It is slowly added in 3min, so that the sulfuric acid for being mingled with metatitanic acid is sufficiently reacted with ammonium carbonate, addition is finished, and continues to stir After 30min, sheet frame squeezing is carried out, filtrate carries out condensing crystallizing and obtains ammonium sulfate product.
Filter cake enters lithium source and inlays reaction and iontophoresis doping process: preceding process filter cake is beaten using ionized water Processing, is formulated into TiO2Concentration is 550g/L, controls Li2CO3/H2TiO3Molar ratio be 1.1:1 be sufficiently beaten, stirring turn Speed is 30 turns/min, after stirring 45min, porous silica is added and carries out ion doping, continue after stirring 30min, sheet frame pressure It squeezes, filtrate is counter to arrive preceding process and use as the solution of preparation ammonium carbonate.The additional amount of porous silica is TiO2Quality 0.9%.
Filter cake enters calcining and micro mist process: the filter cake of previous process being fitted into high purity quartz pallet, calcining baking is carried out It is dry, it is desirable that it is risen by room temperature, after constant temperature 1 hour, after being continuously heating to 650 DEG C, after constant temperature 6 hours, stops heating at 400 DEG C, It after cooling the temperature to room temperature, is crushed using super fine machine, is crushed to 325 meshes and tails over 0.2%, obtain tritium proliferation ceramics Material metatitanic acid lithium.In order to reduce the influence of minimal residue lithium, by the metatitanic acid lithium being prepared in the ionized water boiled After impregnating 6 hours, drying obtains tritium proliferation ceramic material metatitanic acid lithium final products.
Embodiment 2
Metatitanic acid 1kg after sulfuric acid process is cleaned before salt treatment carries out mashing metering, makes its TiO2Content be 350g/L, The sal volatile of the 400g/L prepared in advance is uniformly added in meta-titanium acid solution, the additional amount and metatitanic acid of ammonium carbonate The content of middle sulfuric acid is added according to: sulfuric acid/ammonium carbonate=1:1.3 mass ratio.The process mixing speed of addition is 20 turns/min, It is slowly added in 3min, so that the sulfuric acid for being mingled with metatitanic acid is sufficiently reacted with ammonium carbonate, addition is finished, and continues to stir After 30min, sheet frame squeezing is carried out, filtrate carries out condensing crystallizing and obtains ammonium sulfate product.
Filter cake enters lithium source and inlays reaction and iontophoresis doping process: preceding process filter cake is beaten using ionized water Processing, is formulated into TiO2Concentration is 600g/L, controls Li2CO3/H2TiO3Molar ratio be 1.2:1 be sufficiently beaten, stirring turn Speed is 40 turns/min, after stirring 45min, basic zirconium chloride is added and carries out ion doping, continue after stirring 30min, sheet frame squeezing, filter Liquid is counter to be arrived preceding process and uses as the solution for preparing ammonium carbonate.The additional amount of basic zirconium chloride is TiO2The 0.9% of quality.
Filter cake enters calcining and micro mist process: the filter cake of previous process being fitted into high purity quartz pallet, calcining baking is carried out It is dry, it is desirable that it is risen by room temperature, after constant temperature 1 hour, after being continuously heating to 700 DEG C, after constant temperature 6 hours, stops heating at 500 DEG C, It after cooling the temperature to room temperature, is crushed using super fine machine, is crushed to 325 meshes and tails over 0.2%, obtain tritium proliferation ceramics Material metatitanic acid lithium.In order to reduce the influence of minimal residue lithium, by the metatitanic acid lithium being prepared in the ionized water boiled After impregnating 8 hours, drying obtains tritium proliferation ceramic material metatitanic acid lithium final products.
Embodiment 3
Metatitanic acid 1kg after sulfuric acid process is cleaned before salt treatment carries out mashing metering, makes its TiO2Content be 400g/L, The sal volatile of the 400g/L prepared in advance is uniformly added in meta-titanium acid solution, the additional amount and metatitanic acid of ammonium carbonate The content of middle sulfuric acid is added according to: sulfuric acid/ammonium carbonate=1:1.4 mass ratio.The process mixing speed of addition is 20 turns/min, It is slowly added in 3min, so that the sulfuric acid for being mingled with metatitanic acid is sufficiently reacted with ammonium carbonate, addition is finished, and continues to stir After 30min, sheet frame squeezing is carried out, filtrate carries out condensing crystallizing and obtains ammonium sulfate product.
Filter cake enters lithium source and inlays reaction and iontophoresis doping process: preceding process filter cake is beaten using ionized water Processing, is formulated into TiO2Concentration is 600g/L, controls Li2CO3/H2TiO3Molar ratio be 1.3:1 be sufficiently beaten, stirring turn Speed is 40 turns/min, after stirring 45min, porous silica is added and carries out ion doping, continue after stirring 30min, sheet frame pressure It squeezes, filtrate is counter to arrive preceding process and use as the solution of preparation ammonium carbonate.The additional amount of porous silica is TiO2Quality 0.8%.
Filter cake enters calcining and micro mist process: the filter cake of previous process being fitted into high purity quartz pallet, calcining baking is carried out It is dry, it is desirable that it is risen by room temperature, after constant temperature 1 hour, after being continuously heating to 670 DEG C, after constant temperature 6 hours, stops heating at 400 DEG C, It after cooling the temperature to room temperature, is crushed using super fine machine, is crushed to 325 meshes and tails over 0.2%, obtain tritium proliferation ceramics Material metatitanic acid lithium.In order to reduce the influence of minimal residue lithium, by the metatitanic acid lithium being prepared in the ionized water boiled After impregnating 7 hours, drying obtains tritium proliferation ceramic material metatitanic acid lithium final products.
Embodiment 4
Metatitanic acid 1kg after sulfuric acid process is cleaned before salt treatment carries out mashing metering, makes its TiO2Content be 400g/L, The sal volatile of the 400g/L prepared in advance is uniformly added in meta-titanium acid solution, the additional amount and metatitanic acid of ammonium carbonate The content of middle sulfuric acid is added according to: sulfuric acid/ammonium carbonate=1:1.3 mass ratio.The process mixing speed of addition is 30 turns/min, It is slowly added in 3min, so that the sulfuric acid for being mingled with metatitanic acid is sufficiently reacted with ammonium carbonate, addition is finished, and continues to stir After 30min, sheet frame squeezing is carried out, filtrate carries out condensing crystallizing and obtains ammonium sulfate product.
Filter cake enters lithium source and inlays reaction and iontophoresis doping process: preceding process filter cake is beaten using ionized water Processing, is formulated into TiO2Concentration is 600g/L, controls Li2CO3/H2TiO3Molar ratio be 1.3:1 be sufficiently beaten, stirring turn Speed is 40 turns/min, after stirring 45min, basic zirconium chloride is added and carries out ion doping, continue after stirring 30min, sheet frame squeezing, filter Liquid is counter to be arrived preceding process and uses as the solution for preparing ammonium carbonate.The additional amount of basic zirconium chloride is TiO2The 1.0% of quality.
Filter cake enters calcining and micro mist process: the filter cake of previous process being fitted into high purity quartz pallet, calcining baking is carried out It is dry, it is desirable that it is risen by room temperature, after constant temperature 1 hour, after being continuously heating to 700 DEG C, after constant temperature 6 hours, stops heating at 450 DEG C, It after cooling the temperature to room temperature, is crushed using super fine machine, is crushed to 325 meshes and tails over 0.2%, obtain tritium proliferation ceramics Material metatitanic acid lithium.In order to reduce the influence of minimal residue lithium, by the metatitanic acid lithium being prepared in the ionized water boiled After impregnating 8 hours, drying obtains tritium proliferation ceramic material metatitanic acid lithium final products.
The tritium proliferation ceramic material of embodiment 1-4 preparation is shown in Table 1 with the quality test results of metatitanic acid lithium, producing ammonium sulfate byproduct Quality test results be shown in Table 2.
The quality level of the tritium proliferation ceramic material metatitanic acid lithium of 1 embodiment 1-4 of table preparation
The quality level of 2 embodiment 1-4 producing ammonium sulfate byproduct of table

Claims (10)

1. a kind of preparation method of tritium proliferation ceramic material metatitanic acid lithium, it is characterised in that: steps are as follows:
(1) preparation of titanium source presoma:
After metatitanic acid after sulfuric acid process is cleaned before salt treatment adds water to be beaten, sal volatile is added, continues to stir after adding, into The squeezing of andante frame, obtains filter cake；
(2) lithium source inlays reaction and iontophoresis adulterates:
After adding water mashing to handle filter cake obtained by step (1), Li is added2CO3, continue to stir after adding, lithium ion be then added and inhales Attached dose is continued to stir, and is carried out sheet frame squeezing, is obtained filter cake；
(3) calcining and micro mist:
It by the calcining drying of filter cake obtained by step (2), is cooled to room temperature and is crushed, be crushed to 325 meshes and tail over 0.2%, obtain tritium increasing Grow ceramic material metatitanic acid lithium crude product；
(4) it post-processes:
After the proliferation ceramic material of tritium obtained by step (3) is impregnated in boiling water with metatitanic acid lithium crude product, drying obtains tritium proliferation pottery Ceramic material metatitanic acid lithium product.
2. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: step (1) after the metatitanic acid described in adds water to be beaten, TiO2Content be 300~400g/L.
3. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: step (1) concentration of the sal volatile described in is 400g/L；The mass ratio of sulfuric acid is 1.2 in the additional amount and metatitanic acid of ammonium carbonate ~1.4:1.
4. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: step (1) mixing speed of the addition sal volatile described in is 10~30 turns/min, continues to stir 30min after adding, described Sal volatile is slowly added in 3min.
5. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: step (2) after the filter cake described in adds water mashing to handle, TiO2Content be 550~600g/L.
6. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: described Li2CO3Molar ratio with metatitanic acid is 1.1~1.3:1.
7. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: step (2) the addition Li described in2CO3Speed of agitator be 30~50 turns/min, continue after adding stir 45min.
8. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: step (2) the lithium ion adsorbent described in is porous silica or basic zirconium chloride, and the dosage of lithium ion adsorbent is TiO2Quality 0.8~1.0%.
9. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: step (3) the calcining drying condition described in are as follows: started to warm up by room temperature, constant temperature 1h, is continuously heating to 650 after being warming up to 400~500 DEG C Constant temperature 6h after~700 DEG C.
10. the preparation method of tritium proliferation ceramic material metatitanic acid lithium according to claim 1, it is characterised in that: step (4) soaking time described in is 6~8h.
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CN109859858A (en) * 2019-02-01 2019-06-07 中国工程物理研究院核物理与化学研究所 A kind of foam type tritium multiplication agent and preparation method thereof
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Denomination of invention: Preparation method of lithium metatitanate for tritium breeding ceramic materials

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