CN105776253A - Method for preparing potassium nitrate and nanometer kaolinite with kaliophilite powder bodies - Google Patents
Method for preparing potassium nitrate and nanometer kaolinite with kaliophilite powder bodies Download PDFInfo
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- CN105776253A CN105776253A CN201610147724.8A CN201610147724A CN105776253A CN 105776253 A CN105776253 A CN 105776253A CN 201610147724 A CN201610147724 A CN 201610147724A CN 105776253 A CN105776253 A CN 105776253A
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- kaliophilite
- kaolinite
- nitric acid
- potassium nitrate
- powder body
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/04—Preparation with liquid nitric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
The invention relates to a method for synthesizing potassium nitrate as a by-product of nanometer kaolinite with kaliophilite powder bodies, and belongs to the field of preparation of fine chemical materials. The technology comprises the following steps: mixing the kaliophilite powder bodies with a nitric acid solution, performing a hydrothermal reaction under the condition of 210-250 DEG C for 12-36 hours, and performing synthesis so as to obtain a solid phase product, namely the nanometer kaolinite, and a liquid phase product, namely a potassium nitrate solution. According to the method disclosed by the invention, the kaliophilite powder bodies and the nitric acid are used as raw materials, the nanometer kaolinite and the by-product namely the potassium nitrate are synthesized, and components of potassium, aluminum and silicon in kaliophilite are fully utilized, so that the technology of the whole process is simple, modern industrial requirements of 100% resource utilization rate, zero discharge of waste gas, waste water and industrial residues, high efficiency, energy conservation and clean production can be met, and industrialized production is easy to realize.
Description
Technical field
The invention belongs to fine chemistry industry technical field of material, be specifically related to a kind of method utilizing kaliophilite powder body synthesis nano-kaolinite by-product potassium nitrate.
Background technology
Kaolinite belongs to 1: 1 type phyllosilicate, and nano-kaolinite as rubber, the compatibilization filler of plastics and retardant synergist, both can improve the tensile strength of material, can improve again the gas barrier property of material；At ceramic field, nano-kaolinite potting porcelain has high rigidity, high tenacity and good ductility；In coating, nano-kaolinite can make the adsorptivity of coating, stability, stain and fade resistance significantly strengthen, and also can show some special optical effects etc..Constantly expand owing to nano-kaolinite has skin effect, small-size effect, quantum size effect and macro quanta tunnel effect etc., and its new features and application, caused the extensive concern of domestic and international researcher.
The method of Kaolin super-fine processing mainly has: mechanical crushing method, staging, intercalation-stripping process and chemical synthesis.Mechanical crushing method mainly make use of the feature of mineral lamellar structure, under external force, destroys active force between layers, thus reaching super-refinement purpose, but energy consumption is relatively big, and long time treatment is easily destroyed kaolinic crystal formation, and is unable to reach nano-scale dimension.Kaolin is mainly settled according to Stokes rule and obtains ultra-fine kaolin by staging in a liquid, but cost is high, and output capacity is low.Intercalation-stripping process mainly utilizes special adsorption to make Kaolin Minerals interlayer expand, and bonding force greatly weakens, and after removing intercalated object, originally the sheet kaolinite of stacking becomes scutellate kaolinite with regard to natural decomposition, reaches the purpose that nature is peeled off.The method intercalation rate and effect are uneven, and the granularity of gained intercalation product and morphology change are relatively big, and expensive intercalation Organic substance reclaims relatively complicated difficulty, so that the nano-kaolinite prepared of this method is costly.Chemical synthesis generally adopts hydro-thermal method to obtain ultra tiny synthesis kaolinite with aluminium silicate mineral or aluminum Silica hydrogel for raw material, and its product purity is high, suspension stability is good, light scattering good, and it is with low cost simultaneously.
Potassium nitrate is a kind of important inorganic chemical product and nitrogen, potassium binary high-quality compound fertilizer, is mainly used in the high added value crops such as Folium Camelliae sinensis, fruit, Nicotiana tabacum L., vegetable.In nature, natural potassium nitrate resource is few, at present, the potassium nitrate of China is that raw material generates by potassium chloride, sodium nitrate or ammonium nitrate substantially, main method has absorption process, extraction, ion exchange and double decomposition etc., and the problem of being primarily present has that potassium chloride is expensive, complex manufacturing, ammonium nitrate belong to hazardous explosion prone article etc..
Summary of the invention
It is an object of the invention to provide a kind of method utilizing kaliophilite powder body synthesis nano-kaolinite by-product potassium nitrate.The method, with kaliophilite powder body and nitric acid for raw material, adopts water heat transfer nano-kaolinite, by-product potassium nitrate product.The method is simple for process, and resource utilization is high, and three-waste free discharge, added value is higher, has good economic benefit.
To achieve these goals, this technique is realized by following steps:
1) being 1: 6-8: 0.2-0.3 mix homogeneously form slurry in mass ratio by kaliophilite powder body, water and nitric acid, wherein the mass concentration of nitric acid is 65～68wt%；
2) slurry of mix homogeneously in step 1 is placed in, in teflon-lined stainless steel cauldron, reacting at 210～260 DEG C, 12～36 hours response time；
3) being placed in cold water by the reactor of step 2 and quickly cool down, the slurry obtained carries out solid-liquid separation, obtains filtrate and filter cake；
4) filtrate of step 3 is evaporated under 110～120 DEG C of conditions crystallization and prepares potassium nitrate product；
5) being 9-10 by the Cake Wash of step 3 to washing liquid pH value, filter cake dry 6～12h under 95～105 DEG C of conditions prepares nano-kaolinite.
Described kaliophilite powder body is hexagonal structure, and the mass fraction of kaliophilite is more than 90wt%, granularity-200 order > 95%.
Described method step 1 is better control kaliophilite decomposition rate in nitric acid, kaliophilite powder body, water and nitric acid hybrid mode be: first the nitric acid that mass fraction is 65～68wt% being diluted with water to mass fraction is 5～20wt%, again by remaining water and kaliophilite mixing and stirring, finally the nitric acid after dilution is slowly added in the mixed slurry of kaliophilite and water.
In described method, kaliophilite powder body is in hydrothermal reaction process, and potassium oxide dissolution rate is more than 85%.
In described method step 5, after washing, washing liquid can recycle as follow-up washing liquid.
In described method step 5, the nano-kaolinite obtained is flat crystal, and thickness is 15～30nm, and sheet footpath is 400～500nm.
The kaliophilite powder body that the present invention adopts can be that raw material hydrothermal treatment obtains with K-feldspar powder, this technique proposes application for a patent for invention to Patent Office of State Intellectual Property Office: " method utilizing K-feldspar powder Hydrothermal Synthesis kalsilite " (application number: 201010543249.9), and application is artificial: The Chinese Geology Univ. (Beijing).Its potash feldspar raw material sources are extensive, low production cost.Should be with the concrete technical scheme that K-feldspar powder is the method for raw water thermal synthesis kalsilite: by potash feldspar Ore through crushing and after grinding, preparing K-feldspar powder, the granularity of K-feldspar powder is-200 order > 95wt%；The alkali liquor that potassium hydroxide is made into sodium hydroxide is mixed with K-feldspar powder, at the Water Under thermal response 2～8h of 220～280 DEG C, through filtering, wash and being dry, prepares kalsilite powder body；Wherein, the concentration of alkali liquor is 8～12M, and in alkali liquor, the mol ratio of NaOH and KOH is 7/3～0/10；Wherein, when the mol ratio of NaOH and KOH is 0/10, the NaOH in this this alkali liquor is 0；Mass ratio at alkali liquor Yu K-feldspar powder is 2～8, and is stirred in hydrothermal reaction process, and stir speed (S.S.) is 100～200 revs/min.In " a kind of technique utilizing kaliophilite powder body to produce agricultural potassium sulfate ", (application number is obtained kalsilite powder body: directly can use as raw material in 201110064828.X).The content of the potassium oxide in obtained kalsilite powder body is at more than 26.0wt%；The content of sodium oxide is at below 1.2wt%, and (application number is: 201110064828.X) (namely the content of potassium oxide is at more than 26.0wt% in the requirement of the content of the content to potassium oxide in the kaliophilite used and sodium oxide to also comply with " a kind of technique utilizing kaliophilite powder body to produce agricultural potassium sulfate "；The content of sodium oxide is at below 1.2wt%), simultaneously, the granularity of obtained kalsilite powder body is less than 328 orders (namely 48 μm), and (application number is: the 201110064828.X) requirement to granularity in the kaliophilite used to also comply with " a kind of technique utilizing kaliophilite powder body to produce agricultural potassium sulfate ".Therefore, the application for a patent for invention kaliophilite powder body obtained by " method utilizing K-feldspar powder Hydrothermal Synthesis kalsilite " (application for a patent for invention number: 201010543249.9) by name can directly use.
This patent adopts hydro-thermal method, and reaction terminates rear solid-liquid separation, obtains filtrate and can obtain potassium nitrate product through evaporative crystallization, breaches the limitation preparing potassium nitrate with potassium chloride for raw material；The filter cake obtained is scrubbed, dry can obtain nano-kaolinite, has a good application prospect.This patent takes full advantage of the potassium in kaliophilite, aluminum, silicon components, and while synthesis nano-kaolinite, by-product potassium nitrate product, resource utilization is high, three-waste free discharge, and technique is simple, and reaction condition is gentle, with low cost, has good economic benefit.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction figure of the kaliophilite raw material of the present invention.
Fig. 2 is the X-ray powder diffraction figure of the nano-kaolinite made of the present invention.
Fig. 3 is the stereoscan photograph of the nano-kaolinite made of the present invention..
Detailed description of the invention
Embodiment
(1) kaliophilite powder body used by this patent is to obtain with K-feldspar powder for raw material hydrothermal treatment, and chemical composition analysis result such as table 1, being computed kaliophilite weight/mass percentage composition is 91.36wt%, X ray powder diffraction map analysis such as Fig. 1.Raw material X ray powder diffraction data is carried out indexing calculating, the standard value basically identical (table 2) of kalsilite in the JCPDS card (card 85-1413) of its character constant and standard.
Chemical composition analysis result (the W of table 1 kalsilite powder body (S-01)B%)
The lattice paprmeter of table 2 kalsilite powder body (S-01) and the contrast of JCPDS standard card
(2) kaliophilite powder body 7.5g (chemical composition analysis result is in Table 1) is accurately weighed, distilled water 55.4g, nitric acid (mass fraction is 66%) 4.6g, the nitric acid of 4.6g is added 20g and distills dilution with water, by 7.5g kaliophilite powder body and 35.4g distilled water mixing and stirring, again the salpeter solution after dilution is slowly added in the mixed slurry of kaliophilite powder body and distilled water, load after being sufficiently stirred in band teflon-lined stainless steel cauldron, at the Water Under thermal response 24h of 250 DEG C, taking-up reactor is put in cold water and is quickly cooled down immediately, solid-liquid separation is carried out after driving still, filtrate evaporative crystallization at 110～120 DEG C obtains potassium nitrate product.Adopting sodium tetraphenylborate gravimetric method to record potassium oxide dissolution rate is 87.5%.It is 9-10 that filter cake is washed with distilled water to filtrate pH value, and finally at 95～105 DEG C, namely dry 6h obtains nano-kaolinite.The X-ray powder diffraction figure of the nano-kaolinite made by embodiments of the invention is as shown in Figure 2.Adopting the kaolinite that this method synthesizes is flat crystal (see Fig. 3).X ray powder diffraction data is utilized to adopt the kaolinite thickness that Scherrer formula calculates synthesis to be 20nm, by scanning electron microscope (SEM) photograph it can be seen that sheet footpath is 400～500nm.Kaolinic X ray diffracting data is carried out indexing calculating, kaolinic standard value basically identical (see table 3) in the JCPDS card (card 79-1570) of its lattice paprmeter and standard.
Table 3 synthesizes lattice paprmeter and the contrast of JCPDS card standard value of nano-kaolinite
Claims (6)
1. the method utilizing kaliophilite powder body synthesis nano-kaolinite by-product potassium nitrate, it is characterised in that comprise the following steps:
1) being 1: 6～8: 0.2～0.3 mix homogeneously form slurry in mass ratio by kaliophilite powder body, water and nitric acid, wherein the mass concentration of nitric acid is 65～68wt%；
2) slurry of mix homogeneously in step 1 is placed in, in teflon-lined stainless steel cauldron, reacting at 210～260 DEG C, 12～36 hours response time；
3) being placed in cold water by the reactor of step 2 and quickly cool down, the slurry obtained carries out solid-liquid separation, obtains filtrate and filter cake；
4) filtrate of step 3 is evaporated under 110～120 DEG C of conditions crystallization and prepares potassium nitrate product；
5) being 9～10 by the Cake Wash of step 3 to washing liquid pH value, filter cake dry 6～12h under 95～105 DEG C of conditions prepares nano-kaolinite.
2. method according to claim 1, it is characterised in that: selected kaliophilite powder body is hexagonal structure, the mass fraction > 90wt% of kaliophilite, granularity-200 order > 95%.
3. method according to claim 1, it is characterized in that: in step 1, kaliophilite powder body, water and nitric acid hybrid mode are: first the nitric acid that mass fraction is 65～68wt% being diluted with water to mass fraction is 5～20wt%, again by remaining water and kaliophilite mixing and stirring, finally the nitric acid after dilution is slowly added in the mixed slurry of kaliophilite and water.
4. method according to claim 1, it is characterised in that: kaliophilite powder body is in hydrothermal reaction process, and potassium oxide dissolution rate is more than 85%.
5. method according to claim 1, it is characterised in that: in step 5, after washing, washing liquid can recycle as follow-up washing liquid.
6. method according to claim 1, it is characterised in that: the nano-kaolinite obtained in step 5 is flat crystal, and thickness is 15～30nm, and sheet footpath is 400～500nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610147724.8A CN105776253B (en) | 2016-03-15 | 2016-03-15 | A kind of method that utilization kaliophilite powder prepares potassium nitrate and nano-kaolinite |
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| CN201610147724.8A CN105776253B (en) | 2016-03-15 | 2016-03-15 | A kind of method that utilization kaliophilite powder prepares potassium nitrate and nano-kaolinite |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107522208A (en) * | 2017-09-29 | 2017-12-29 | 昊青薪材（北京）技术有限公司 | A kind of method that nanometer muscovite by-product potassium nitrate is synthesized using kaliophilite powder |
| CN107572542A (en) * | 2017-09-29 | 2018-01-12 | 昊青薪材（北京）技术有限公司 | A kind of method that nano-kaolinite is prepared using white mica powder body |
| CN107585782A (en) * | 2017-08-25 | 2018-01-16 | 陕西科技大学 | A kind of method of potassium feldspar extracting sulfuric acid aluminium potassium |
| CN107720767A (en) * | 2017-11-28 | 2018-02-23 | 中国地质大学（北京） | A kind of kaolinic method of anorthite Hydrothermal Synthesiss |
-
2016
- 2016-03-15 CN CN201610147724.8A patent/CN105776253B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| C. - I . FIALIPS，ET AL.: "Hydrothermal formation of kaolinite from various metakaolins", 《CLAY MINERALS》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107585782A (en) * | 2017-08-25 | 2018-01-16 | 陕西科技大学 | A kind of method of potassium feldspar extracting sulfuric acid aluminium potassium |
| CN107522208A (en) * | 2017-09-29 | 2017-12-29 | 昊青薪材（北京）技术有限公司 | A kind of method that nanometer muscovite by-product potassium nitrate is synthesized using kaliophilite powder |
| CN107572542A (en) * | 2017-09-29 | 2018-01-12 | 昊青薪材（北京）技术有限公司 | A kind of method that nano-kaolinite is prepared using white mica powder body |
| CN107522208B (en) * | 2017-09-29 | 2020-02-11 | 昊青薪材（北京）技术有限公司 | Method for synthesizing nano white mica and byproduct potassium nitrate by using kaliophilite powder |
| CN107572542B (en) * | 2017-09-29 | 2020-10-16 | 昊青薪材（北京）技术有限公司 | Method for preparing nano kaolinite by using muscovite powder |
| CN107720767A (en) * | 2017-11-28 | 2018-02-23 | 中国地质大学（北京） | A kind of kaolinic method of anorthite Hydrothermal Synthesiss |
| CN107720767B (en) * | 2017-11-28 | 2020-05-19 | 中国地质大学（北京） | Method for hydrothermally synthesizing kaolinite from anorthite |
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