CN104261439A - Method for preparing KNO3 (potassium nitrate) for optical glass - Google Patents

Method for preparing KNO3 (potassium nitrate) for optical glass Download PDF

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Publication number
CN104261439A
CN104261439A CN201410536978.XA CN201410536978A CN104261439A CN 104261439 A CN104261439 A CN 104261439A CN 201410536978 A CN201410536978 A CN 201410536978A CN 104261439 A CN104261439 A CN 104261439A
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China
Prior art keywords
kno3
saltpetre
opticglass
crystallization
solution
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CN201410536978.XA
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CN104261439B (en
Inventor
赵家春
赵晨
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Golden potassium Technology Co.,Ltd.
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赵家春
赵晨
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00Nitrates of sodium, potassium or alkali metals in general
    • C01D9/08Preparation by double decomposition
    • C01D9/10Preparation by double decomposition with ammonium nitrate

Abstract

The invention discloses a method for preparing KNO3 (potassium nitrate) for optical glass. According to the method, potassium chloride and ammonium nitrate are used as raw materials; the method comprises steps as follows: preparation of the raw materials, cooling crystallization for preparation of semi-finished KNO3 crystals, washing of the semi-finished KNO3 crystals, hot melting and secondary crystallization, filtration, finished product dehydration and drying, wherein a crystallization reagent is added during cooling crystallization, and the crystallization reagent is KNO3 crystals and/or a supersaturated KNO3 seed crystal mother solution or a saturated KNO3 seed crystal mother solution. A traditional double decomposition method production technology is adopted, the semi-finished KNO3 crystals are obtained through addition of the crystallization reagent during cooling crystallization, the KNO3 is prepared with a hot melting and secondary crystallization method, the preparation technology is simple, and produced KNO3 products are low in impurity content, high in ionic activity and capable of meeting the requirement of the KNO3 products for the optical glass.

Description

Prepare the method for opticglass saltpetre
technical field:
The present invention relates to a kind of method preparing saltpetre, particularly relate to a kind of method preparing opticglass saltpetre.
background technology:
Saltpetre is commonly called as nitre, water white transparency rhomboidal crystal or rhomboidan or white powder, odorless, nontoxic, have saline taste, refrigerant sense, water absorbability is little, prevented from caking, soluble in water, be a kind of important inorganization industrial raw material, be widely used in black powder, fireworks, food preservatives, medically makes diuretic(s), sudorific, and be used as to produce potassium salt of penicillin etc.In recent years along with scientific and technological development, the fast development of opticglass Application Areas, and saltpetre improves opticglass, and as the touch-screen etc. of smart mobile phone panel, computer contact screen, watch case and various electronic product, the starting material that intensity is indispensable.
Current domestic opticglass saltpetre market is general or based on import saltpetre for a long time.This is because import potassium nitrate product generally produces acquisition with saltpetre ore for raw material carries out directly purification, not only foreign matter content is low for the potassium nitrate product adopting this method to prepare, and the activity of ion is also high, can meets and produce the requirement of opticglass saltpetre.And the relative comparison of the on the one hand similar saltpetre ore resource of China lacks, the mode that therefore can not directly to take with saltpetre ore be raw material carries out producing the potassium nitrate product of opticglass.And use current conventional raw material particularly as used with Repone K and ammonium nitrate as raw material carries out synthesizing the product of the saltpetre produced, one is that foreign matter content is high, two is that ionic activity is low, is difficult to meet opticglass, the requirement of particularly high-end opticglass saltpetre.
Therefore, how to utilize existing number of chemical raw material as carried out the product of the saltpetre of synthesizing optical glass for raw material with Repone K and ammonium nitrate, to meet the market demand of the potassium nitrate product of growing opticglass production, it is the reality need of current domestic opticglass Production of Potassium Nitrate.
summary of the invention:
A kind of method preparing opticglass saltpetre of the present invention, with Repone K and ammonium nitrate for raw material, adopt traditional double decomposition production technique, add crystalline reagents through crystallisation by cooling and obtain saltpetre work in-process xln, again through the saltpetre that hot melt solution multiple junction mode is produced, production technique is simple, and the potassium nitrate product foreign matter content produced is low, ionic activity is high, can reach the potassium nitrate product requirement of opticglass.
A kind of method preparing opticglass saltpetre of the present invention, with Repone K and ammonium nitrate for raw material, comprises raw material configuration, crystallisation by cooling obtains KNO 3work in-process xln, KNO 3the flushing of work in-process xln, hot melt solution multiple junction, filtration, finished product dehydration, dry, it is in crystallisation by cooling process, adds crystalline reagents, and described crystalline reagents is potassium nitrate crystals and/or supersaturation saltpetre crystal seed mother liquor or saturated saltpetre crystal seed mother liquor.
A kind of method preparing opticglass saltpetre of the present invention, add purification reagent in hot melt solution multiple junction process described in it, described purification reagent is preferably solution of potassium carbonate.
A kind of method preparing opticglass saltpetre of the present invention, is through raw material configuration, after saltpetre reaction soln is made in heating, controls Cl in reaction soln -and NH 4 +mass concentration be respectively 16-22%, 7-12%, and cool to during 0-35 DEG C and add crystalline reagents.
A kind of method preparing opticglass saltpetre of the present invention, described heat of solution multiple junction is to KNO 3work in-process xln after rinsing, carry out heating for dissolving be supersaturated solution and the concentration controlling solution is 45-58Be time add purification reagent.
The present invention prepares the method for opticglass saltpetre, with Repone K and ammonium nitrate for raw material, adopt traditional double decomposition producing and manufacturing technique, again through crystallisation by cooling after raw material makes potassium nitrate solution after reacting by heating, add crystalline reagents when crystallisation by cooling and obtain saltpetre work in-process xln, and then hot melt solution multiple junction is carried out to saltpetre work in-process xln, carrying out adding purification reagent again in hot melt solution multiple junction process, the potassium nitrate product purity of producing purification through above-mentioned two-step process step is high, impurity and impurity ion content few, and production technique is simple, the potassium nitrate product foreign matter content produced is low, ionic activity is high, reach the potassium nitrate product requirement of opticglass.This overcome existing traditional with Repone K and ammonium nitrate and water for raw material, adopt preparing potassium nitrate by means of double decomposition product foreign matter content high, the shortcoming that ionic activity is low, thus prepare the high-quality potassium nitrate product that can be used for opticglass, significantly can reduce the production cost of opticglass saltpetre.
embodiment: below in conjunction with specific embodiment, the present invention is described in further detail.
KCl and NH in the embodiment of the present invention 4nO 3starting material are commercial industrial product;
Cl in file of the present invention -and NH 4 +control numerical value represent in the solution " concentration ", in solid crystal represent " massfraction ".
embodiment 1:
The present embodiment can be undertaken by existing production craft step also can by following processing step, specific as follows:
(1) raw material configuration: by raw material Repone K and ammonium nitrate and water or process recycled water by a certain percentage namely existing production technique proportioning be configured, heating, at the temperature of 80-110 DEG C, saltpetre reaction soln is made in reaction, controls Cl in reaction soln -and NH 4 +concentration is respectively 16-22%, 7-12%, obtains mother liquor;
(2) crystallisation by cooling: above-mentioned mother liquor is cooled to 0-35 DEG C, makes KNO 3crystallization, adding crystalline reagents potassium nitrate crystals or supersaturation saltpetre crystal seed mother liquor, obtaining KNO when starting to be formed and have crystallization 3work in-process xln, cooling fluid is filtered, and filtered liquid reclaims;
(3) KNO 3crystal rinses: by KNO 3on work in-process xln clear water or this post, the water of the low concentration that wheel is discharged after rinsing work in-process rinses, control KNO 3the KNO that work in-process xln obtains after rinsing 3in crystal, in muriate Cl -for 1-4%, in ammonium salt NH 4 +for 1.5-5%, rinse solution is recovered into hold-up vessel;
(4) hot melt solution multiple junction: to (3) step KNO 3the KNO that work in-process xln obtains after rinsing 3in crystal, add water, heating makes it fully to be dissolved as supersaturated solution, and control strength of solution is 45-58Be, and then adds purification reagent solution of potassium carbonate, removes impurity further, obtains the saltpetre supersaturated solution after removal of impurities;
(5) filter: by the saltpetre supersaturated solution after the removal of impurities in (4) step, pump in cooling crystallizer after the foreign material such as desludging after filtration, be cooled to≤30 DEG C after filtration obtain finished product KNO 3, through rinsing control KNO 3in muriate Cl in crystal -be 0.01%, in ammonium salt NH 4 +for being 0.05%, obtain finished product KNO 3;
(6) finished product dehydration, oven dry: by finished product KNO 3after carrying out processed to water content≤3%, drying process is KNO to product water content≤0.1% 3product.
embodiment 2:
Carry out with the production method of embodiment 1 and processing parameter, difference is stated as follows, and it is saturated saltpetre crystal seed mother liquor that (2) step adds crystalline reagents, and (4) hot melt solution multiple junction adds the saturated solution that purificant is salt of wormwood.

Claims (4)

1. prepare a method for opticglass saltpetre, with Repone K and ammonium nitrate for raw material, comprise raw material configuration, crystallisation by cooling obtains KNO 3work in-process xln, KNO 3the flushing of work in-process xln, hot melt solution multiple junction, filtration, finished product dehydration, oven dry, it is characterized in that in crystallisation by cooling process, add crystalline reagents, described crystalline reagents is potassium nitrate crystals and/or supersaturation saltpetre crystal seed mother liquor or saturated saltpetre crystal seed mother liquor.
2., according to a kind of method preparing opticglass saltpetre according to claim 1, it is characterized in that adding purification reagent in described hot melt solution multiple junction process, described purification reagent is solution of potassium carbonate.
3., according to a kind of method preparing opticglass saltpetre according to claim 1, it is characterized in that, through raw material configuration, after saltpetre reaction soln is made in heating, controlling Cl in reaction soln -and NH 4 +mass concentration be respectively 16-22%, 7-12%, and cool to during 0-35 DEG C and add crystalline reagents.
4., according to a kind of method preparing opticglass saltpetre according to claim 1, it is characterized in that described heat of solution multiple junction is to KNO 3work in-process xln after rinsing, carry out heating for dissolving be supersaturated solution and the concentration controlling solution is 45-58Be time add purification reagent.
CN201410536978.XA 2014-10-13 2014-10-13 Prepare the method for opticglass saltpetre Active CN104261439B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105060317B (en) * 2015-07-30 2016-08-24 湖南丹化农资有限公司 A kind of method being produced high-quality potassium nitrate with ammonium nitrate double decomposition circulation process by potassium chloride
CN107089672A (en) * 2017-05-28 2017-08-25 赵家春 A kind of optical glass Production of Potassium Nitrate method
CN107117634A (en) * 2017-05-28 2017-09-01 赵家春 A kind of Production of Potassium Nitrate method
CN107162022A (en) * 2017-05-28 2017-09-15 赵家春 Production of Potassium Nitrate method
CN108423693A (en) * 2017-05-28 2018-08-21 江西金利达钾业有限责任公司 The high yield preparation method of potassium nitrate

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101659431A (en) * 2009-09-03 2010-03-03 赵家春 Method for preparing potassium nitrate by means of double decomposition
CN101973564A (en) * 2010-11-01 2011-02-16 赵家春 Potassium nitrate for fireworks and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101659431A (en) * 2009-09-03 2010-03-03 赵家春 Method for preparing potassium nitrate by means of double decomposition
CN101973564A (en) * 2010-11-01 2011-02-16 赵家春 Potassium nitrate for fireworks and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105060317B (en) * 2015-07-30 2016-08-24 湖南丹化农资有限公司 A kind of method being produced high-quality potassium nitrate with ammonium nitrate double decomposition circulation process by potassium chloride
CN107089672A (en) * 2017-05-28 2017-08-25 赵家春 A kind of optical glass Production of Potassium Nitrate method
CN107117634A (en) * 2017-05-28 2017-09-01 赵家春 A kind of Production of Potassium Nitrate method
CN107162022A (en) * 2017-05-28 2017-09-15 赵家春 Production of Potassium Nitrate method
CN108423693A (en) * 2017-05-28 2018-08-21 江西金利达钾业有限责任公司 The high yield preparation method of potassium nitrate
CN107089672B (en) * 2017-05-28 2019-06-04 赵家春 A kind of optical glass Production of Potassium Nitrate method

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Application publication date: 20150107

Assignee: Tengda Jiangxi Industrial Co., Ltd.

Assignor: Zhao Jiachun|Zhao Chen

Contract record no.: 2016360000008

Denomination of invention: Method for preparing KNO3 (potassium nitrate) for optical glass

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Patentee after: Tengda Jiangxi Industrial Co., Ltd.

Address before: 336000 Yichun Economic Development Zone, Jiangxi, Yichun

Patentee before: Zhao Jiachun

Patentee before: Zhao Chen

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Effective date of registration: 20220408

Address after: 336000 Yichun economic and Technological Development Zone, Jiangxi

Patentee after: Golden potassium Technology Co.,Ltd.

Address before: 336000 Yichun economic and Technological Development Zone, Jiangxi Province

Patentee before: Tengda Jiangxi Industrial Co.,Ltd.