CN103911664A - Synthesis method of crystal potassium hexatitanate - Google Patents
Synthesis method of crystal potassium hexatitanate Download PDFInfo
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- CN103911664A CN103911664A CN201410180164.7A CN201410180164A CN103911664A CN 103911664 A CN103911664 A CN 103911664A CN 201410180164 A CN201410180164 A CN 201410180164A CN 103911664 A CN103911664 A CN 103911664A
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- 239000013078 crystal Substances 0.000 title claims abstract description 61
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 54
- 239000011591 potassium Substances 0.000 title claims abstract description 54
- 238000001308 synthesis method Methods 0.000 title abstract 3
- 239000000463 material Substances 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000002994 raw material Substances 0.000 claims description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 25
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 23
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 22
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 21
- 238000010189 synthetic method Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 239000012768 molten material Substances 0.000 claims description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 238000010791 quenching Methods 0.000 claims description 11
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 10
- 230000000171 quenching effect Effects 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 7
- 229910001626 barium chloride Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000003337 fertilizer Substances 0.000 claims description 7
- 229940072033 potash Drugs 0.000 claims description 7
- 235000015320 potassium carbonate Nutrition 0.000 claims description 7
- 235000011181 potassium carbonates Nutrition 0.000 claims description 7
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 7
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 7
- 235000011151 potassium sulphates Nutrition 0.000 claims description 7
- 238000001953 recrystallisation Methods 0.000 claims description 7
- 239000001117 sulphuric acid Substances 0.000 claims description 7
- 235000011149 sulphuric acid Nutrition 0.000 claims description 7
- 235000010215 titanium dioxide Nutrition 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 6
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 5
- 239000004323 potassium nitrate Substances 0.000 claims description 5
- 235000010333 potassium nitrate Nutrition 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000002783 friction material Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000012774 insulation material Substances 0.000 abstract 1
- 230000035939 shock Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- Fertilizers (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a synthesis method of crystal potassium hexatitanate. A self-made shock chilling device is adopted to synthesize potassium dititanate crystal beams with uniform length of the synthesized crystal, and the potassium dititanate crystal beams are adopted as a midbody to further synthesize the potassium hexatitanate. The crystal potassium hexatitanate is synthesized by adopting the synthesis method, so that the energy consumption is reduced by 30 percent compared with the traditional kiln, the powder material is reduced, the cost is low, the heat conductivity is small, the infrared reflection rate is high, the high-temperature sound absorption performance is good, and the synthesized potassium hexatitanate can be used as a friction material and an insulation material. The specific surface area of the synthesized crystal potassium hexatitanate is 0.5 to 1.5m<2>/g, the average length is 30 to 50 micrometers, and the yield is more than 96 percent.
Description
Technical field
The present invention relates to the manufacturing technology field of machine salt stupalith, be specifically related to a kind of synthetic method of lenticular six potassium titanates.
Background technology
The Microscopic form of six potassium titanates has crystal whisker-shaped (claiming again fibrous), lenticular, nanotube-shaped, Powdered, sheet is crystalline, flakey etc., the potassium titanate of diverse microcosmic form, be mainly manifested in the difference in physicals, the different special emphasis in corresponding purposes.
Whisker refers to a kind of fiber growing into monocrystalline form under manual control condition, its diameter very tiny (micron order), do not contain the defect (crystal boundary, dislocation, hole etc.) existing in common material, its atomic arrangement high-sequential, thereby its intensity is close to the theoretical value of perfect crystal.The typical characteristics of crystal whisker-shaped six potassium titanates is that tap density is less, is only 0.2～0.4g/cm
3, and have certain toughness, there is comparatively superior enhancing characteristic.The tap density of lenticular six potassium titanates is 0.5～0.9g/cm
3, be defective crystal, diameter is also large than crystal whisker-shaped, has fragility, therefore, often has the powder of some amount in lenticular six potassium titanates, is exactly due to the brittle rupture that causes under external force of crystal.
In the prior art, very many about the patent of crystal whisker-shaped six potassium titanates, as ZL200610031042.7 etc., introduction be the production technique of melting quench method, and be the synthetic method of crystal whisker of hexa potassium titanate, irrelevant with the synthetic method of lenticular six potassium titanates.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of synthetic method of lenticular six potassium titanates, it adopts homemade chilled equipment, the comparatively uniform two potassium titanate crystal bundles of composite crystals length, take this two potassium titanates crystal bundle as intermediate, and then composite crystals shape six potassium titanates, thereby eliminate defect in above-mentioned background technology.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A synthetic method for lenticular six potassium titanates, step is as follows:
By titaniferous materials and containing potassium raw material according to mol ratio TiO
2: K
2the ratio of O=1.5～2.5 weighs, and mixes simply;
(2) pour above-mentioned raw materials into elevated temperature vessel, then enter in the High Temperature Furnaces Heating Apparatus of 900～1300 ℃, stop 30～90 minutes, make raw material miscellany become the molten mass with mobility;
(3) above-mentioned molten mass is taken out, quenching, what now form is the comparatively uniform two potassium titanate crystal bundles of length;
By above-mentioned even two potassium titanate crystal bundles in the ratio of solid-to-liquid ratio 1:15 to 1:10, enter into the lass lining reactor that adds a certain amount of room temperature cold water, soak 12～60 hours, make most crystal bundle in cold water, slowly expand and slowly scatter, in hot water, disperse the too fast crystal that cause in a large number to rupture when rapid expansion to reduce crystal bundle, material to 60～99 ℃ in heating lass lining reactor, adding concentration with liquid meter is the industrial sulphuric acid of 15～25wt%, make the pH value of solution between 10～12, react 90～200 minutes, remaining crystal bundle is further scatter,
(5) the solution in above-mentioned lass lining reactor is entered into microporous filter, carry out solid-liquid separation;
(6) the deionized water directly washing in microporous filter with 20～60 ℃ by above-mentioned solid part, on a small quantity repeatedly, washes most sulfate ion (SO
4 2-), until muddy by 1% barium chloride solution check nothing; Washing water turn back in lass lining reactor and recycle;
(7) by the wet feed drawing off in above-mentioned microporous filter, directly enter in bell-jar electric furnace, at 600～1000 ℃, stop 100～900 minutes, complete recrystallization conversion, be cooled to room temperature, after grading machine classification, be finished product.
Improve as one, the titaniferous materials in described step (1) refers to one or both mixing of various model titanium dioxides, anatase octahedrite, brookite.
Improve as one, in described step (1), refer to one or both mixing of Anhydrous potassium carbonate, Carbon Dioxide hydrogen potassium, saltpetre, Repone K, potassium hydroxide containing potassium raw material.
Improve as one, in described step (3), adopt self-control chilled equipment to realize quenching, described self-control chilled equipment comprises housing, the top of described housing is provided with high-temperature molten material blanking port, and the below of described high-temperature molten material blanking port is provided with accepts funnel, described in accept funnel and be provided with secondary blanking port, the below of described secondary blanking port is provided with at least two strippers of arranging up and down and tilting to install, and the vergence direction of adjacent stripper is contrary; Described high-temperature molten material blanking port with described in accept housing sidewall between funnel and offer the first blast inlet and be connected high pressure positive blower, the air intake of described the first blast inlet blows to the material falling from high-temperature molten material blanking port; The sidewall of described housing also offers the second blast inlet, and the air intake of described the second blast inlet blows to the stripper of bottommost, and the discharge direction contrary of blowing direction and described stripper; The top of described housing is also provided with air outlet.
The advantage of this self-control chilled equipment is: extended the skyborne residence time of high-temperature material, be unlikely to occur that material has little time cooling curing, reunited and pile up the phenomenon adhering to because caking appears in excess Temperature.
Improve as one, in described step (5), the liquid portion that solid-liquid separation obtains is accumulated separately, for pure alkaline potassium sulfate solution, waits until special disposal, is a kind of agricultural high-quality potash fertilizer.
The present invention, as the synthetic method of lenticular six potassium titanates, does not have comparability with the synthetic method of existing crystal whisker of hexa potassium titanate.And the present invention adopt self-control chilled equipment realize quenching, extended the skyborne residence time of high-temperature material, be unlikely to occur that material has little time cooling curing, because of excess Temperature occur caking reunite and pile up adhere to phenomenon.
Owing to having adopted technique scheme, the invention has the beneficial effects as follows:
Lenticular six potassium titanates that synthesized by the present invention, can reduce by 30% left and right by loss-rate conventional tunnel kiln, and powder material is less, and cost is low, and thermal conductivity is little, and infrared reflection rate is higher, and high temperature sound absorption qualities is good, can be used as friction materials, lagging material etc.Lenticular six potassium titanates that method is synthesized thus, specific surface area 0.5～1.5m
2/ g, 30～50 microns of mean lengths, its yield is greater than 96%.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention makes chilled equipment by oneself;
Fig. 2 is the SEM figure of the synthetic lenticular of the embodiment of the present invention 3 six potassium titanates;
In figure: 1. housing, 2. high-temperature molten material blanking port, 3. accepts funnel, 4. two blanking ports, 5. stripper, 6. the first blast inlet, 7. the second blast inlet, 8. air outlet.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
A synthetic method for lenticular six potassium titanates, step is as follows:
By titaniferous materials and containing potassium raw material according to mol ratio TiO
2: K
2the ratio of O=1.5 weighs, and mixes simply, and titaniferous materials is titanium dioxide, is Anhydrous potassium carbonate containing potassium raw material;
(2) pour above-mentioned raw materials into elevated temperature vessel, then enter in the High Temperature Furnaces Heating Apparatus of 900 ℃, stop 30 minutes, make raw material miscellany become the molten mass with mobility;
(3) above-mentioned molten mass is taken out, adopt self-control chilled equipment to realize quenching, what now form is the comparatively uniform two potassium titanate crystal bundles of length;
By above-mentioned even two potassium titanate crystal bundles in the ratio of solid-to-liquid ratio 1:15, enter into the lass lining reactor that adds a certain amount of room temperature cold water, soak 12 hours, make most crystal bundle in cold water, slowly expand and slowly scatter, in hot water, disperse the too fast crystal that cause in a large number to rupture when rapid expansion to reduce crystal bundle, material to 60 ℃ in heating lass lining reactor, adding concentration with liquid meter is the industrial sulphuric acid of 15wt%, make the pH value of solution between 10, react 90 minutes, remaining crystal bundle is further scatter;
(5) the solution in above-mentioned lass lining reactor is entered into microporous filter, carry out solid-liquid separation and obtain solid part, the liquid portion that solid-liquid separation obtains is accumulated separately, for pure alkaline potassium sulfate solution, waits until special disposal, is a kind of agricultural high-quality potash fertilizer;
(6) the deionized water directly washing in microporous filter with 20 ℃ by above-mentioned solid part, on a small quantity repeatedly, washes most sulfate ion (SO
4 2-), until muddy by 1% barium chloride solution check nothing; Washing water turn back in lass lining reactor and recycle;
(7) by the wet feed drawing off in above-mentioned microporous filter, directly enter in bell-jar electric furnace, at 600 ℃, stop 100 minutes, complete recrystallization conversion, be cooled to room temperature, after grading machine classification, be finished product.
The lenticular six potassium titanate specific surface area of finished products that the present embodiment obtains are 0.75m
2/ g, 37 microns of mean lengths, yield 97.6%.
Embodiment 2
A synthetic method for lenticular six potassium titanates, step is as follows:
By titaniferous materials and containing potassium raw material according to mol ratio TiO
2: K
2the ratio of O=2.5 weighs, and mixes simply, and titaniferous materials is the mixing of two kinds of various model titanium dioxides, anatase octahedrite, is the mixing of two kinds of Anhydrous potassium carbonates, Carbon Dioxide hydrogen potassium containing potassium raw material;
(2) pour above-mentioned raw materials into elevated temperature vessel, then enter in the High Temperature Furnaces Heating Apparatus of 1300 ℃, stop 90 minutes, make raw material miscellany become the molten mass with mobility;
(3) above-mentioned molten mass is taken out, adopt self-control chilled equipment to realize quenching, what now form is the comparatively uniform two potassium titanate crystal bundles of length;
By above-mentioned even two potassium titanate crystal bundles in the ratio of solid-to-liquid ratio 1:10, enter into the lass lining reactor that adds a certain amount of room temperature cold water, soak 60 hours, make most crystal bundle in cold water, slowly expand and slowly scatter, in hot water, disperse the too fast crystal that cause in a large number to rupture when rapid expansion to reduce crystal bundle, material to 99 ℃ in heating lass lining reactor, adding concentration with liquid meter is the industrial sulphuric acid of 25wt%, make the pH value of solution between 12, react 200 minutes, remaining crystal bundle is further scatter;
(5) the solution in above-mentioned lass lining reactor is entered into microporous filter, carry out solid-liquid separation and obtain solid part, the liquid portion that solid-liquid separation obtains is accumulated separately, for pure alkaline potassium sulfate solution, waits until special disposal, is a kind of agricultural high-quality potash fertilizer;
(6) the deionized water directly washing in microporous filter with 60 ℃ by above-mentioned solid part, on a small quantity repeatedly, washes most sulfate ion (SO
4 2-), until muddy by 1% barium chloride solution check nothing; Washing water turn back in lass lining reactor and recycle;
(7) by the wet feed drawing off in above-mentioned microporous filter, directly enter in bell-jar electric furnace, at 1000 ℃, stop 900 minutes, complete recrystallization conversion, be cooled to room temperature, after grading machine classification, be finished product.
The lenticular six potassium titanate specific surface area of finished products 0.5m that the present embodiment obtains
2/ g, 32 microns of mean lengths, its yield 96.5%.
Embodiment 3
A synthetic method for lenticular six potassium titanates, step is as follows:
By titaniferous materials and containing potassium raw material according to mol ratio TiO
2: K
2the ratio of O=1.8 weighs, mix simply, titaniferous materials is one or both mixing of various model titanium dioxides, anatase octahedrite, brookite, is one or both mixing of Anhydrous potassium carbonate, Carbon Dioxide hydrogen potassium, saltpetre, Repone K, potassium hydroxide containing potassium raw material;
(2) pour above-mentioned raw materials into elevated temperature vessel, then enter in the High Temperature Furnaces Heating Apparatus of 1100 ℃, stop 50 minutes, make raw material miscellany become the molten mass with mobility;
(3) above-mentioned molten mass is taken out, adopt self-control chilled equipment to realize quenching, what now form is the comparatively uniform two potassium titanate crystal bundles of length;
By above-mentioned even two potassium titanate crystal bundles in the ratio of solid-to-liquid ratio 1:10, enter into the lass lining reactor that adds a certain amount of room temperature cold water, soak 36 hours, make most crystal bundle in cold water, slowly expand and slowly scatter, in hot water, disperse the too fast crystal that cause in a large number to rupture when rapid expansion to reduce crystal bundle, material to 80 ℃ in heating lass lining reactor, adding concentration with liquid meter is the industrial sulphuric acid of 18wt%, make the pH value of solution between 11, react 160 minutes, remaining crystal bundle is further scatter;
(5) the solution in above-mentioned lass lining reactor is entered into microporous filter, carry out solid-liquid separation and obtain solid part, the liquid portion that solid-liquid separation obtains is accumulated separately, for pure alkaline potassium sulfate solution, waits until special disposal, is a kind of agricultural high-quality potash fertilizer;
(6) the deionized water directly washing in microporous filter with 40 ℃ by above-mentioned solid part, on a small quantity repeatedly, washes most sulfate ion (SO
4 2-), until muddy by 1% barium chloride solution check nothing; Washing water turn back in lass lining reactor and recycle;
(7) by the wet feed drawing off in above-mentioned microporous filter, directly enter in bell-jar electric furnace, at 800 ℃, stop 500 minutes, complete recrystallization conversion, be cooled to room temperature, after grading machine classification, be finished product.
The lenticular six potassium titanate finished product SEM that the present embodiment obtains scheme as shown in Figure 2, product specific surface area 1.5m
2/ g, 50 microns of mean lengths, its yield 98%.
Embodiment 4
A synthetic method for lenticular six potassium titanates, step is as follows:
By titaniferous materials and containing potassium raw material according to mol ratio TiO
2: K
2the ratio of O=1.7 weighs, mix simply, titaniferous materials is one or both mixing of various model titanium dioxides, anatase octahedrite, brookite, is one or both mixing of Anhydrous potassium carbonate, Carbon Dioxide hydrogen potassium, saltpetre, Repone K, potassium hydroxide containing potassium raw material;
(2) pour above-mentioned raw materials into elevated temperature vessel, then enter in the High Temperature Furnaces Heating Apparatus of 900 ℃, stop 30～90 minutes, make raw material miscellany become the molten mass with mobility;
(3) above-mentioned molten mass is taken out, adopt self-control chilled equipment to realize quenching, what now form is the comparatively uniform two potassium titanate crystal bundles of length;
By above-mentioned even two potassium titanate crystal bundles in the ratio of solid-to-liquid ratio 1:13, enter into the lass lining reactor that adds a certain amount of room temperature cold water, soak 30 hours, make most crystal bundle in cold water, slowly expand and slowly scatter, in hot water, disperse the too fast crystal that cause in a large number to rupture when rapid expansion to reduce crystal bundle, material to 70 ℃ in heating lass lining reactor, adding concentration with liquid meter is the industrial sulphuric acid of 15wt%, make the pH value of solution between 10, react 200 minutes, remaining crystal bundle is further scatter;
(5) the solution in above-mentioned lass lining reactor is entered into microporous filter, carry out solid-liquid separation and obtain solid part, the liquid portion that solid-liquid separation obtains is accumulated separately, for pure alkaline potassium sulfate solution, waits until special disposal, is a kind of agricultural high-quality potash fertilizer;
(6) the deionized water directly washing in microporous filter with 40 ℃ by above-mentioned solid part, on a small quantity repeatedly, washes most sulfate ion (SO
4 2-), until muddy by 1% barium chloride solution check nothing; Washing water turn back in lass lining reactor and recycle;
(7) by the wet feed drawing off in above-mentioned microporous filter, directly enter in bell-jar electric furnace, at 1000 ℃, stop 300 minutes, complete recrystallization conversion, be cooled to room temperature, after grading machine classification, be finished product.
The lenticular six potassium titanate specific surface area of finished products 1.2m that the present embodiment obtains
2/ g, 35 microns of mean lengths, its yield 97%.
Embodiment 5
A synthetic method for lenticular six potassium titanates, step is as follows:
By titaniferous materials and containing potassium raw material according to mol ratio TiO
2: K
2the ratio of O=2.5 weighs, mix simply, titaniferous materials is one or both mixing of various model titanium dioxides, anatase octahedrite, brookite, is one or both mixing of Anhydrous potassium carbonate, Carbon Dioxide hydrogen potassium, saltpetre, Repone K, potassium hydroxide containing potassium raw material;
(2) pour above-mentioned raw materials into elevated temperature vessel, then enter in the High Temperature Furnaces Heating Apparatus of 900 ℃, stop 60 minutes, make raw material miscellany become the molten mass with mobility;
(3) above-mentioned molten mass is taken out, adopt self-control chilled equipment to realize quenching, what now form is the comparatively uniform two potassium titanate crystal bundles of length;
By above-mentioned even two potassium titanate crystal bundles in the ratio of solid-to-liquid ratio 1:14, enter into the lass lining reactor that adds a certain amount of room temperature cold water, soak 60 hours, make most crystal bundle in cold water, slowly expand and slowly scatter, in hot water, disperse the too fast crystal that cause in a large number to rupture when rapid expansion to reduce crystal bundle, material to 80 ℃ in heating lass lining reactor, adding concentration with liquid meter is the industrial sulphuric acid of 25wt%, make the pH value of solution 12, react 100 minutes, remaining crystal bundle is further scatter;
(5) the solution in above-mentioned lass lining reactor is entered into microporous filter, carry out solid-liquid separation and obtain solid part, the liquid portion that solid-liquid separation obtains is accumulated separately, for pure alkaline potassium sulfate solution, waits until special disposal, is a kind of agricultural high-quality potash fertilizer;
(6) the deionized water directly washing in microporous filter with 45 ℃ by above-mentioned solid part, on a small quantity repeatedly, washes most sulfate ion (SO
4 2-), until muddy by 1% barium chloride solution check nothing; Washing water turn back in lass lining reactor and recycle;
(7) by the wet feed drawing off in above-mentioned microporous filter, directly enter in bell-jar electric furnace, at 700 ℃, stop 500 minutes, complete recrystallization conversion, be cooled to room temperature, after grading machine classification, be finished product.
The lenticular six potassium titanate specific surface area of finished products 0.8m that the present embodiment obtains
2/ g, 41 microns of mean lengths, its yield 97%.
In embodiment 1-5, the special chilled equipment structure of self-control adopting as shown in Figure 2, described self-control chilled equipment comprises housing 1, the top of described housing 1 is provided with high-temperature molten material blanking port 2, the below of described high-temperature molten material blanking port 2 is provided with accepts funnel 3, the described funnel 3 of accepting is provided with secondary blanking port 4, and the below of described secondary blanking port 4 is provided with at least two strippers 5 of arranging up and down and tilting to install, and the vergence direction of adjacent stripper 5 is contrary; Described high-temperature molten material blanking port 2 with described in accept housing 1 sidewall between funnel 3 and offer the first blast inlet 6 and be connected high pressure positive blower, the air intake of described the first blast inlet 6 blows to the material falling from high-temperature molten material blanking port 2; The sidewall of described housing 1 also offers the second blast inlet 7, and the air intake of described the second blast inlet 7 blows to the stripper 5 of bottommost, and the discharge direction contrary of blowing direction and described stripper 5; The top of described housing 1 is also provided with air outlet 8.The advantage of this self-control chilled equipment is: extended the skyborne residence time of high-temperature material, be unlikely to occur that material has little time cooling curing, reunited and pile up the phenomenon adhering to because caking appears in excess Temperature.
The present invention is not limited to above-mentioned embodiment, and all are based on technical conceive of the present invention, and the structural improvement of having done, all falls among protection scope of the present invention.
Claims (5)
1. a synthetic method for lenticular six potassium titanates, is characterized in that: step is as follows:
By titaniferous materials and containing potassium raw material according to mol ratio TiO
2: K
2the ratio of O=1.5～2.5 weighs, and mixes simply;
(2) pour above-mentioned raw materials into elevated temperature vessel, then enter in the High Temperature Furnaces Heating Apparatus of 900～1300 ℃, stop 30～90 minutes, make raw material miscellany become the molten mass with mobility;
(3) above-mentioned molten mass is taken out, quenching, what now form is the comparatively uniform two potassium titanate crystal bundles of length;
By above-mentioned even two potassium titanate crystal bundles in the ratio of solid-to-liquid ratio 1:15 to 1:10, enter into the lass lining reactor that adds a certain amount of room temperature cold water, soak 12～60 hours, make most crystal bundle in cold water, slowly expand and slowly scatter, material to 60～99 ℃ in heating lass lining reactor, adding concentration with liquid meter is the industrial sulphuric acid of 15～25wt%, make the pH value of solution between 10～12, react 90～200 minutes, remaining crystal bundle is further scatter;
(5) the solution in above-mentioned lass lining reactor is entered into microporous filter, carry out solid-liquid separation;
(6) the deionized water directly washing in microporous filter with 20～60 ℃ by above-mentioned solid part, on a small quantity repeatedly, washes most sulfate ion (SO
4 2-), until muddy by 1% barium chloride solution check nothing; Washing water turn back in lass lining reactor and recycle;
(7) by the wet feed drawing off in above-mentioned microporous filter, directly enter in bell-jar electric furnace, at 600～1000 ℃, stop 100～900 minutes, complete recrystallization conversion, be cooled to room temperature, after grading machine classification, be finished product.
2. the synthetic method of a kind of lenticular six potassium titanates as claimed in claim 1, is characterized in that: the titaniferous materials in described step (1) refers to one or both mixing of various model titanium dioxides, anatase octahedrite, brookite.
3. the synthetic method of a kind of lenticular six potassium titanates as claimed in claim 1, is characterized in that: in described step (1), refer to one or both mixing of Anhydrous potassium carbonate, Carbon Dioxide hydrogen potassium, saltpetre, Repone K, potassium hydroxide containing potassium raw material.
4. the synthetic method of a kind of lenticular six potassium titanates as claimed in claim 1, it is characterized in that: in described step (3), adopt self-control chilled equipment to realize quenching, described self-control chilled equipment comprises housing, the top of described housing is provided with high-temperature molten material blanking port, the below of described high-temperature molten material blanking port is provided with accepts funnel, the described funnel of accepting is provided with secondary blanking port, the below of described secondary blanking port is provided with at least two strippers of arranging up and down and tilting to install, and the vergence direction of adjacent stripper is contrary; Described high-temperature molten material blanking port with described in accept housing sidewall between funnel and offer the first blast inlet and be connected high pressure positive blower, the air intake of described the first blast inlet blows to the material falling from high-temperature molten material blanking port; The sidewall of described housing also offers the second blast inlet, and the air intake of described the second blast inlet blows to the stripper of bottommost, and the discharge direction contrary of blowing direction and described stripper; The top of described housing is also provided with air outlet.
5. the synthetic method of a kind of lenticular six potassium titanates as claimed in claim 1, it is characterized in that: state in step (5), the liquid portion that solid-liquid separation obtains is accumulated separately, is pure alkaline potassium sulfate solution, waiting until special disposal, is a kind of agricultural high-quality potash fertilizer.
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| CN109928422A (en) * | 2018-08-14 | 2019-06-25 | 华北理工大学 | A kind of method that fused salt prepares potassium titanate crystal |
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