CN102030338B - Method for hydrothermally synthesizing kalsilite by using potassium feldspar powder - Google Patents
Method for hydrothermally synthesizing kalsilite by using potassium feldspar powder Download PDFInfo
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- CN102030338B CN102030338B CN 201010543249 CN201010543249A CN102030338B CN 102030338 B CN102030338 B CN 102030338B CN 201010543249 CN201010543249 CN 201010543249 CN 201010543249 A CN201010543249 A CN 201010543249A CN 102030338 B CN102030338 B CN 102030338B
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- kalsilite
- feldspar powder
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- alkali liquor
- potassium
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- 239000000843 powder Substances 0.000 title claims abstract description 47
- 229910001462 kalsilite Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000002194 synthesizing effect Effects 0.000 title abstract description 3
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 title abstract 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000010433 feldspar Substances 0.000 claims description 23
- 239000003513 alkali Substances 0.000 claims description 12
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 8
- 239000011591 potassium Substances 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 abstract description 11
- 239000000126 substance Substances 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000011112 process operation Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000013467 fragmentation Methods 0.000 description 3
- 238000006062 fragmentation reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 235000010469 Glycine max Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000002551 biofuel Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910001387 inorganic aluminate Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- YTCQFLFGFXZUSN-BAQGIRSFSA-N microline Chemical group OC12OC3(C)COC2(O)C(C(/Cl)=C/C)=CC(=O)C21C3C2 YTCQFLFGFXZUSN-BAQGIRSFSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052645 tectosilicate Inorganic materials 0.000 description 1
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Abstract
The invention discloses a process for hydrothermally synthesizing kalsilite by taking potassium feldspar powder as a raw material. The process comprises the following steps of: performing pretreatment such as crushing, grinding and beneficiation on potassium feldspar raw ore to obtain the potassium feldspar powder with certain particle size; and uniformly mixing with potassium hydroxide or mixed solution of sodium hydroxide and the potassium hydroxide, putting into a nickel lined stainless steel kettle, performing hydrothermal reaction at the temperature of between 220 and 280 DEG C for 2 to 8 hours, and filtering, washing and drying to prepare kalsilite powder. Compared with the conventional kalsilite synthesis technology, the process has the advantages of low raw material cost, mild synthesis conditions, easy process operation, high crystallinity of products, uniform crystal chemical compositions and the like.
Description
Technical field
The present invention relates to a kind of take K-feldspar powder as raw material hydro-thermal legal system the method for standby kalsilite.
Background technology
Kalsilite is a kind of tectosilicate, and potassium oxide content is high, and its potassium ion is arranged in lattice, Stability Analysis of Structures at high temperature, potassium ion is difficult for running off, and is a kind of good catalyst adjuvant, is widely used in producing hydrogen from steam conversion of hydrocarbons, ethyl benzene dehydrogenation preparation of styrene and ammonia synthesizing industry.Current research shows, the kalsilite of lithium modification is that soya-bean oil and methanol conversion are a kind of good heterogeneous catalyst of biofuel.At present, the synthetic topmost method of kaliophylite has sol-gel method and coprecipitation method.It is raw material that sol-gel method adopts tetraethoxy and metal alkoxide, it is raw material that coprecipitation method adopts potassium silicate, potassium hydroxide and inorganic aluminate, these two kinds of methods all are the presomas that obtains first kaliophylite, then need to roasting obtain kaliophylite under 800～1200 ℃ condition.
Summary of the invention
The invention provides a kind ofly take the method for K-feldspar powder as raw water thermal synthesis kaliophylite, wherein, potassium felspar sand is the natural silicate mineral, and reserves are abundant, can prepare kaliophylite as silicon source, aluminium source and part potassium source simultaneously; Hydro-thermal synthesis process of the present invention, simple to operate, reaction conditions is gentle, and need not high-temperature roasting, thereby is a kind of economically viable method for preparing kalsilite with development potentiality.
This technique realizes by following steps:
(1) the potassium felspar sand ore is after broken and ore dressing pretreatment, and grinding makes K-feldspar powder;
(2) potassium hydroxide and sodium hydroxide are made into mixed alkali liquor, K-feldspar powder and mixed alkali liquor are placed the stainless steel cauldron of lining nickel, at Water Under thermal response 2～8h of 220～280 ℃, after filtration, washing and dry, make the kalsilite powder.
The granularity of described K-feldspar powder is-200 orders＞95%.
The concentration of described mixed alkali liquor is 5～12M, and the mol ratio of NaOH and KOH is 7/3～0/10 in the mixed alkali liquor.
The mass ratio of described mixed alkali liquor and K-feldspar powder is 2～8.
Stir in the described hydrothermal reaction process, stir speed (S.S.) is 100～200 rev/mins.
The used K-feldspar powder cost of material of the present invention is cheap, wide material sources, and technological operation is simple, has economic feasibility and technical feasibility.
Description of drawings
Fig. 1 is the X ray powder crystal diffractogram of raw material K-feldspar powder;
Fig. 2 is the X ray powder crystal diffractogram of embodiment 1 Hydrothermal Synthesis kalsilite powder KAS-01;
Fig. 3 is the stereoscan photograph of embodiment 1 Hydrothermal Synthesis kalsilite powder KAS-01.
Embodiment
Embodiment 1
(1) the potassium felspar sand raw ore is through fragmentation, after the ore dressing pretreatment, grinding to granularity be-200 orders greater than 95%, its chemical composition analysis the results are shown in Table 1, the main phase of this potash feldspar ore is microline, and the X ray powder crystal diffractogram of raw material K-feldspar powder as shown in Figure 1.
Chemical composition analysis result (the w of table 1 K-feldspar powder
B%)
(2) get K-feldspar powder 150g behind the grinding, with 650g concentration be that the KOH solution of 9M mixes, placing volume is the lining nickel and stainless steel reactor of 1L, be heated to 280 ℃ and isothermal reaction 2h, stir speed (S.S.) in the reaction process is 200 rev/mins, and reaction finishes to obtain kalsilite powder KAS-01 by filtration, washing and drying.The X ray powder crystal diffractogram of kalsilite powder KAS-01 as shown in Figure 2, Fig. 2 shows, the diffracted ray of synthetic product and the kalsilite of standard coincide good.The stereoscan photograph of the Hydrothermal Synthesis kalsilite powder KAS-01 of the present embodiment 1 as shown in Figure 3, Fig. 3 shows, synthetic kalsilite crystal grain is that comparatively intact six sides are tabular, size-grade distribution is comparatively even, particle size is 1-3 μ m approximately.The main chemical compositions analytical results of kalsilite powder KAS-01 sees Table 2.X ray diffracting data to synthetic product carries out indexing calculating, and the standard value of kalsilite is near (table 3) in the JCPDS card of its lattice parameter and standard (card 11-0579).
Chemical composition analysis result (the w of table 2 kalsilite powder KAS-01
B%)
The lattice parameter of table 3 kalsilite powder KAS-01 and the contrast of JCPDS card standard value
Embodiment 2
(1) the potassium felspar sand raw ore is through fragmentation, after the ore dressing pretreatment, grinding to granularity be-200 orders greater than 95%, its chemical composition analysis the results are shown in Table 1.
(2) get K-feldspar powder 100g behind the grinding, with 575g concentration be that the mixed alkali liquor (wherein the NaOH/KOH mol ratio is 7/3) of 5M mixes, placing volume is the stainless steel cauldron of the lining nickel of 1L, be heated to 220 ℃ and isothermal reaction 6h, stir speed (S.S.) in the reaction process is 100 rev/mins, and reaction finishes to obtain kalsilite powder KAS-02 by filtration, washing, drying.The main chemical compositions analytical results of kalsilite powder KAS-02 sees Table 4.X ray diffracting data to synthetic product carries out indexing calculating, and the standard value of kalsilite is near (table 5) in the JCPDS card of its lattice parameter and standard (card 11-0579).
Chemical composition analysis result (the w of table 4 kalsilite powder KAS-02
B%)
The lattice parameter of table 5 kalsilite powder KAS-02 and the contrast of JCPDS card standard value
Embodiment 3
(1) the potassium felspar sand raw ore is through fragmentation, after the ore dressing pretreatment, grinding to granularity be-200 orders greater than 95%, its chemical composition analysis the results are shown in Table 1.
(2) get K-feldspar powder 200g behind the grinding, with 700g concentration be that the mixed alkali liquor of 10M mixes (wherein the NaOH/KOH mol ratio is 1/1), placing volume is the stainless steel cauldron of the lining nickel of 1L, be heated to 260 ℃ and be incubated 3h, stir speed (S.S.) in the reaction process is 200 rev/mins, and reaction finishes to obtain kalsilite product K AS-03 by filtration, washing, drying.The main chemical compositions analytical results of kalsilite powder KAS-03 sees Table 6.X ray diffracting data to synthetic product carries out indexing calculating, and the standard value of kalsilite is near (table 7) in the JCPDS card of its lattice parameter and standard (card 11-0579).
Chemical composition analysis result (the w of table 6 kalsilite powder KAS-03
B%)
The lattice parameter of table 7 kalsilite powder KAS-03 and the contrast of JCPDS card standard value
Claims (4)
1. one kind take the method for K-feldspar powder as raw water thermal synthesis kalsilite, it is characterized in that, may further comprise the steps:
(1) the potassium felspar sand ore is after broken and ore dressing pretreatment, and grinding makes K-feldspar powder;
(2) potassium hydroxide and sodium hydroxide are made into mixed alkali liquor or KOH solution, place the stainless steel cauldron of lining nickel with K-feldspar powder and mixed alkali liquor or with KOH solution, the concentration of described mixed alkali liquor or KOH solution is 8～12M, the mol ratio of NaOH and KOH is 7/3～0/10 in mixed alkali liquor or the KOH solution, Water Under thermal response 2～8h at 220～280 ℃, after filtration, washing and dry, make the kalsilite powder.
2. as claimed in claim 1 a kind ofly it is characterized in that take the method for K-feldspar powder as raw water thermal synthesis kalsilite, grinding potassium felspar sand in described step (1), the granularity requirements of K-feldspar powder is-200 orders＞95%.
3. as claimed in claim 1 or 2 a kind ofly it is characterized in that take the method for K-feldspar powder as raw water thermal synthesis kalsilite, the mass ratio of described mixed alkali liquor or KOH solution and K-feldspar powder is 2～8.
4. as claimed in claim 1 a kind ofly it is characterized in that take the method for K-feldspar powder as raw water thermal synthesis kalsilite, stir in described hydrothermal reaction process, stir speed (S.S.) is 100～200 rev/mins.
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Cited By (1)
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| WO2014182693A1 (en) * | 2013-05-06 | 2014-11-13 | Massachusetts Institute Of Technology | Alkali metal ion source with moderate rate of ion relaease and methods of forming |
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| CN102408256A (en) * | 2011-08-24 | 2012-04-11 | 烟台大学 | Method for quickly extracting soluble potassium at low temperature |
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| CA2909251A1 (en) * | 2013-03-11 | 2014-10-09 | Basf Se | Synthetic megakalsilite via hydrothermal preparation |
| CN103818914B (en) * | 2014-02-26 | 2015-05-27 | 化工部长沙设计研究院 | Method for preparing sodium alumino silicate through decomposing feldspar |
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| WO2020000074A1 (en) * | 2018-06-27 | 2020-01-02 | Numinus Engenharia E Consultoria Ltda | Process for producing kalsilite, potassium sulphate, aluminium silicate and calcium silicate hydrate |
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| CN112028082A (en) * | 2020-08-31 | 2020-12-04 | 江苏康祥实业集团有限公司 | Preparation method of potassium silicate solution based on hydrothermal method |
| CN115806298A (en) * | 2021-09-15 | 2023-03-17 | 中国石油化工股份有限公司 | Method for preparing kaliophilite by solid phase method |
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| US5565394A (en) * | 1994-10-11 | 1996-10-15 | Corning Incorporated | Low expansion molecular sieves and method of making same |
| CN1051056C (en) * | 1996-11-29 | 2000-04-05 | 中国地质大学（北京） | Technology process of producing zeolite molecular-sieve with potassium feldspar |
| CN101781147B (en) * | 2010-01-29 | 2013-04-10 | 中国地质大学（北京） | Process for preparing potassium molecular sieve based slow-release fertilizer carrier from potassium feldspar powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014182693A1 (en) * | 2013-05-06 | 2014-11-13 | Massachusetts Institute Of Technology | Alkali metal ion source with moderate rate of ion relaease and methods of forming |
| US9340465B2 (en) | 2013-05-06 | 2016-05-17 | Massachusetts Institute Of Technology, Inc. | Alkali metal ion source with moderate rate of ion release and methods of forming |
| US10196317B2 (en) | 2013-05-06 | 2019-02-05 | Massachusetts Institute Of Technology | Alkali metal ion source with moderate rate of ion release and methods of forming |
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