CN1184076A - Technology process of producing zeolite molecular-sieve with potassium feldspar - Google Patents
Technology process of producing zeolite molecular-sieve with potassium feldspar Download PDFInfo
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- CN1184076A CN1184076A CN 96120734 CN96120734A CN1184076A CN 1184076 A CN1184076 A CN 1184076A CN 96120734 CN96120734 CN 96120734 CN 96120734 A CN96120734 A CN 96120734A CN 1184076 A CN1184076 A CN 1184076A
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- zeolite molecular
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Abstract
In the said technological process, potassium containing rock is crushed and separated to obtain fine ore powder containing potash feldspar; fine ore powder is mixed with sodium carbonate or caustic soda and roasted at 500-850 deg.c; the roasted grog is mixed with caustic soda and water into colloid; after stagnation, ageing, crystallization and filtration, the obtained solid is dried at 105 deg. c to produce the zeolite molecular sieve. The said product after filtration as K2O containing mother liquor may be acidified and separated to produce potash fertilizer. The present invention has reasonable and simple technological process, no environment pollution and low product cost.
Description
The present invention relates to a kind of method of producing zeolite molecular sieve with potassium rich rock.
The insoluble potassium ore resources of China is abundant, and is of a great variety, mainly contains potassium felspar sand, white garnet, alunite, illite, potassium-bearing shale and all kinds of potassium matter volcanics etc.These potassium ore resources almost spread all over the country each province, city autonomous region.According to incompletely statistics, national insoluble potassium resource has nearly 10,000,000,000 tons approximately.According to retrieval, foreign literature does not have the research report of carrying potassium and synthetic zeolite from potassium rich rock.In the document, " the vitriolate of tartar industry of comprehensive utilization potassium felspar sand development China " literary composition is arranged at home, introduced potassium felspar sand and prepared the Chemicals potassium sulfate process; Another piece of writing utilizes approach for " development and use of potassium rock are closed in the Purple Mountain, Lin County " mainly introduces potassium bearing rock, does not relate to concrete technology.Therefore, in the face of abundant insoluble potassium ore resources, be badly in need of that numerous scientific and technical personnel develop, research, reasonable use.
The purpose of this invention is to provide a kind of technology with producing zeolite molecular-sieve with potassium feldspar, be to utilize potassium bearing rock to make zeolite molecular sieve, rationally utilize the resource of China, this zeolite molecular sieve can be done chemical fertilizer carrier and other industrial chemicals usefulness, this technology is simple, no trash discharge, be easy to promote, enforcement.
The present invention realizes by following manner.
This technology with producing zeolite molecular-sieve with potassium feldspar is to be raw material with the fine ore that contains potassium felspar sand, adopts following step to carry out;
(1) calcination steps: with the described fine ore that contains potassium felspar sand and soda ash by 1: the parts by weight of 1.1-1.7 mix, and carry out roasting under 750 ℃ of-850 ℃ of temperature condition, and the time of roasting is 1.5-3 hour.
(2) hydro-thermal synthesis step: with baked grog and caustic soda and water by 1: the parts by weight of 0.3-0.6: 10-20 mix, become colloidal, leave standstill at ambient temperature then, wore out 3-5 hour, it is under 90 ℃-110 ℃ the condition crystallization 4-11 hour in temperature afterwards, adding water again washs, till PH to the solution is 7-11, filter then, the solid after the filtration is drying to obtain the zeolite molecular sieve powder under 105 ℃ of temperature condition.
This technology with producing zeolite molecular-sieve with potassium feldspar is to be raw material with the fine ore that contains potassium felspar sand, also can adopt following step to carry out:
(1) calcination steps: with the described fine ore that contains potassium felspar sand and caustic soda by 1: the parts by weight of 1.1-1.7 mix, and carry out roasting under 500 ℃ of-600 ℃ of temperature condition, and the time of roasting is 1.5-3 hour.
(2) hydro-thermal synthesis step: with baked grog and caustic soda and water by 1: the parts by weight of 0.3-0.6: 10-20 mix, become colloidal, leave standstill at ambient temperature then, wore out 3-5 hour, it is under 90 ℃-110 ℃ the condition crystallization 4-11 hour in temperature afterwards, adding water again washs, till PH to the solution is 7-11, filter then, the solid after the filtration is drying to obtain the zeolite molecular sieve powder under 105 ℃ of temperature condition.
Raw material used in the present invention-contain the fine ore of potassium felspar sand makes from potassium bearing rock.Potassium bearing rock is meant the various rocks that are rich in potassium felspar sand, mainly comprises potassium Chang Yan, rich potassium volcanics, syenite, pegmatite etc.Potassium bearing rock adopts ore dressings such as ordinary method such as gravity treatment, flotation, magnetic separation through fragmentation, obtains containing potassium felspar sand>95% fine ore, requires TFeO<1%.The powder of fine ore is 180 orders-220 orders.
Employed soda ash (Na among the present invention
2CO
3) and caustic soda (NaOH) all be technical grade.The water that uses gets final product as ordinary tap water.
In hydro-thermal synthesis step of the present invention, becoming the glue reactant ratio is grog: caustic soda: water=1: 0.3-0.6: 10-20, the basicity in the resultant colloid is 1.1-2.5N.
In the hydro-thermal synthesis step among the present invention, can add a spot of crystal seed in the colloid after becoming glue, crystal seed is zeolite (a general chemical product), and main effect is the crystallization of accelerating coacervation of colloid, aging and zeolite.
In the hydro-thermal synthesis step among the present invention, the resulting after filtration K that contains
2The mother liquor of O can adopt common method and general equipment to produce potash fertilizer.Promptly this mother liquor obtains K after acidification, Crystallization Separation
2CO
3
Be elaborated in conjunction with the accompanying drawings with embodiment below
Fig. 1 is for producing zeolite molecular sieve and byproduct-the contain process flow sheet of potassium mother liquor with potassium bearing rock.
As shown in Figure 1, raw material is potassium bearing rock, obtains the fine ore of K-feldspar after fragmentation is purified. Join Material is caustic soda or soda ash. Fine ore carries out roasting with batching after mixing. Grog after the roasting and water, caustic soda mix Close and carry out the Hydrothermal Synthesis step. The Hydrothermal Synthesis step comprises into glue, crystallization, filtration. In the colloid behind the one-tenth glue Crystal seed be can add, coacervation of colloid, the aging crystallization that reaches zeolite accelerated. The solid that obtains after the filtration carries out drying Make the molecular sieve powder. The mother liquor that obtains after the filtration separates through acidifying makes potash fertilizer. When use soda ash for prepare burden into Row is during roasting, and what produce contains CO2Tail gas can recycle. And use caustic soda for prepare burden into During the row roasting, the tail gas that produces is emptying.
Embodiment 1
As shown in Figure 1, to contain potassium felspar sand>95% fine ore (TFeO<1%) and require to be crushed to 200 orders, mix with the ratio of weight and number of caustic soda by 1: 1.5, in stoving oven, carry out roasting, the temperature of roasting is 550 ℃-600 ℃, roasting 2 hours, obtain white half sintered clinker, and making this grog fragmentation, the grog after the fragmentation and caustic soda and water mix in reactor by 1: 0.3: 13 ratio of weight and number, stir, and in reactor, leave standstill at ambient temperature, aging 4 hours, crystallization 8 hours under 100 ℃ of conditions then will be expected to place in the tank again and be added water washing, and till transferring PH to be 7-11.Filter then.Solid after will filtering again is placed on the moisture eliminator, 105 ℃ of following thorough dryings, promptly obtains 13X type zeolite molecular sieve powder.Obtain byproduct-contain K after filtering
2The mother liquor of O.This mother liquor can make potash fertilizer after acidifying separates.
Embodiment 2
As shown in Figure 1, will contain potassium felspar sand>95% fine ore (TFeO<1%) and require to be crushed to 200 orders, mix with the ratio of weight and number of soda ash by 1: 4, in stoving oven, carry out roasting, the temperature of roasting is 750 ℃-820 ℃, and roasting 2 hours obtains white half sintered clinker.Meanwhile, be located at the gas concentration unit of stoving oven top, with the CO that contains that produces in the roasting process
2Tail gas recycle, and by recycling after the washing tower udst separation.Above-mentioned grog contains through mixing in reactor by 1: 0.4: 11 ratio of weight and number with caustic soda and water after the fragmentation again, stir, and in reactor, leave standstill at ambient temperature, wore out 4 hours, crystallization 8 hours under 100 ℃ of conditions then, to expect again to place in the tank and add water washing, and till transferring PH to be 7-11, filter then.Solid after will filtering again is placed on the moisture eliminator, 105 ℃ of following thorough dryings, promptly obtains 13X type zeolite molecular sieve powder.Obtain byproduct-contain K after filtering
2The mother liquor of O.This mother liquor can make potash fertilizer after acidifying separates.
The present invention utilizes fine ore and the batching contain potassium felspar sand to carry out roasting, and makes zeolite molecular sieve powder and byproduct-contain K by the hydro-thermal synthesis step
2The mother liquor of O.Technological design of the present invention is reasonable, technology is simple, free from environmental pollution, no trash discharge.Product of the present invention-zeolite molecular sieve powder can be done chemical fertilizer carrier and other industrial chemicals usefulness, byproduct-contain K
2The mother liquor of O can obtain K after acidification, Crystallization Separation
2CO
3Potash fertilizer, raw material sources of the present invention are extensive, technical process short, investment is little, product cost is low, economic benefit is high, be convenient to implement popularization.
Claims (2)
1, a kind of technology with producing zeolite molecular-sieve with potassium feldspar is characterized in that: be to be raw material with the fine ore that contains potassium felspar sand, adopt following step to carry out:
(1) calcination steps: with the described fine ore that contains potassium felspar sand and soda ash by 1: the parts by weight of 1.1-1.7 mix, and carry out roasting under 750 ℃ of-850 ℃ of temperature condition, and the time of roasting is 1.5-3 hour,
(2) hydro-thermal synthesis step: with baked grog and caustic soda and water by 1: the parts by weight of 0.3-0.6: 10-20 mix, become colloidal, leave standstill at ambient temperature then, wore out 3-5 hour, it is under 90 ℃-110 ℃ the condition crystallization 4-11 hour in temperature afterwards, adding water again washs, till PH to the solution is 7-11, filter then, the solid after the filtration is drying to obtain the zeolite molecular sieve powder under 105 ℃ of temperature condition.
2, a kind of technology with producing zeolite molecular-sieve with potassium feldspar is characterized in that: be to be raw material with the fine ore that contains potassium felspar sand, adopt following step to carry out:
(1) calcination steps: with the described fine ore that contains potassium felspar sand and caustic soda by 1: the parts by weight of 1.1-1.7 mix, and carry out roasting under 500 ℃ of-600 ℃ of temperature condition, and the time of roasting is 1.5-3 hour,
(2) hydro-thermal synthesis step: with baked grog and caustic soda and water by 1: the parts by weight of 0.3-0.6: 10-20 mix, become colloidal, leave standstill at ambient temperature then, wore out 3-5 hour, it is under 90 ℃-110 ℃ the condition crystallization 4-11 hour in temperature afterwards, adding water again washs, till PH to the solution is 7-11, filter then, the solid after the filtration is drying to obtain the zeolite molecular sieve powder under 105 ℃ of temperature condition.
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102030338A (en) * | 2010-11-11 | 2011-04-27 | 中国地质大学(北京) | Method for hydrothermally synthesizing kalsilite by using potassium feldspar powder |
CN102284351A (en) * | 2011-07-28 | 2011-12-21 | 内蒙古科技大学 | Beneficiation method for separating potassium feldspar concentrates from BayanObo potassium-rich slates |
CN102357402A (en) * | 2011-07-28 | 2012-02-22 | 内蒙古科技大学 | Method for separating potassium feldspar ore concentrate and iron ore concentrate from Baiyunebo potassium rich slate |
CN102557050A (en) * | 2011-12-20 | 2012-07-11 | 昆明冶金研究院 | New process for comprehensively utilizing potassium feldspar |
CN102826567A (en) * | 2012-08-24 | 2012-12-19 | 福建师范大学 | Method for preparing lithium-type X molecular sieve with low silica-alumina by using potassium feldspar |
CN103553067A (en) * | 2013-11-19 | 2014-02-05 | 河北工业大学 | Method for producing total-potassium W-type molecular sieve by utilizing KOH alkali-activated potassium feldspar |
CN104045454A (en) * | 2014-06-13 | 2014-09-17 | 宁德师范学院 | Zeolite slow release compound fertilizer and preparation method thereof |
CN104291350A (en) * | 2014-09-29 | 2015-01-21 | 中国地质大学(北京) | Process for synthesizing analcite from potassium feldspar powder by virtue of hydro-thermal alkaline method |
CN105668584A (en) * | 2016-03-15 | 2016-06-15 | 中国地质大学(北京) | Technology for preparing KH molecular sieve from potassium feldspar powder |
CN106430233A (en) * | 2016-10-18 | 2017-02-22 | 河北工业大学 | Method for preparing low-silicon X-type molecular sieve by fusing and activating potassium-bearing rocks by Na2CO3-NaOH mixed alkali |
US9643423B2 (en) | 2013-01-24 | 2017-05-09 | Seiko Epson Corporation | Liquid container with optically transparent area and liquid ejection apparatus including liquid container with visual recognition portion |
CN114984867A (en) * | 2022-08-03 | 2022-09-02 | 扬州晨化新材料股份有限公司 | Sectional type fixed bed reactor for catalyst production |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5969418A (en) * | 1982-10-14 | 1984-04-19 | Takamura Suzuki | Method for obtaining citric soluble potash fertilizer as well as white powder, deoxidizer, starting material for ceramic or the like from potash ore and lime, magnesia or the like |
-
1996
- 1996-11-29 CN CN96120734A patent/CN1051056C/en not_active Expired - Fee Related
Cited By (18)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102030338A (en) * | 2010-11-11 | 2011-04-27 | 中国地质大学(北京) | Method for hydrothermally synthesizing kalsilite by using potassium feldspar powder |
CN102284351A (en) * | 2011-07-28 | 2011-12-21 | 内蒙古科技大学 | Beneficiation method for separating potassium feldspar concentrates from BayanObo potassium-rich slates |
CN102357402A (en) * | 2011-07-28 | 2012-02-22 | 内蒙古科技大学 | Method for separating potassium feldspar ore concentrate and iron ore concentrate from Baiyunebo potassium rich slate |
CN102357402B (en) * | 2011-07-28 | 2013-05-08 | 内蒙古科技大学 | Method for separating potassium feldspar ore concentrate and iron ore concentrate from Baiyunebo potassium rich slate |
CN102284351B (en) * | 2011-07-28 | 2013-08-28 | 内蒙古科技大学 | Beneficiation method for separating potassium feldspar concentrates from BayanObo potassium-rich slates |
CN102557050A (en) * | 2011-12-20 | 2012-07-11 | 昆明冶金研究院 | New process for comprehensively utilizing potassium feldspar |
CN102557050B (en) * | 2011-12-20 | 2013-09-04 | 昆明冶金研究院 | New process for comprehensively utilizing potassium feldspar |
CN102826567A (en) * | 2012-08-24 | 2012-12-19 | 福建师范大学 | Method for preparing lithium-type X molecular sieve with low silica-alumina by using potassium feldspar |
US9643423B2 (en) | 2013-01-24 | 2017-05-09 | Seiko Epson Corporation | Liquid container with optically transparent area and liquid ejection apparatus including liquid container with visual recognition portion |
CN103553067A (en) * | 2013-11-19 | 2014-02-05 | 河北工业大学 | Method for producing total-potassium W-type molecular sieve by utilizing KOH alkali-activated potassium feldspar |
CN103553067B (en) * | 2013-11-19 | 2015-08-05 | 河北工业大学 | The method of full potassium W type molecular sieve produced by a kind of KOH alkali fusion activation potassium felspar sand |
CN104045454B (en) * | 2014-06-13 | 2016-06-15 | 宁德师范学院 | A kind of zeolite slow-release compound fertilizer and preparation method thereof |
CN104045454A (en) * | 2014-06-13 | 2014-09-17 | 宁德师范学院 | Zeolite slow release compound fertilizer and preparation method thereof |
CN104291350A (en) * | 2014-09-29 | 2015-01-21 | 中国地质大学(北京) | Process for synthesizing analcite from potassium feldspar powder by virtue of hydro-thermal alkaline method |
CN105668584A (en) * | 2016-03-15 | 2016-06-15 | 中国地质大学(北京) | Technology for preparing KH molecular sieve from potassium feldspar powder |
CN106430233A (en) * | 2016-10-18 | 2017-02-22 | 河北工业大学 | Method for preparing low-silicon X-type molecular sieve by fusing and activating potassium-bearing rocks by Na2CO3-NaOH mixed alkali |
CN106430233B (en) * | 2016-10-18 | 2019-01-25 | 河北工业大学 | A kind of Na2CO3The method that-NaOH mixing alkali fusion activation potassium bearing rock produces low-silicon X-shaped molecular screen |
CN114984867A (en) * | 2022-08-03 | 2022-09-02 | 扬州晨化新材料股份有限公司 | Sectional type fixed bed reactor for catalyst production |
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