CN106995216A - The preparation method and device of ice crystal - Google Patents
The preparation method and device of ice crystal Download PDFInfo
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- CN106995216A CN106995216A CN201710242602.1A CN201710242602A CN106995216A CN 106995216 A CN106995216 A CN 106995216A CN 201710242602 A CN201710242602 A CN 201710242602A CN 106995216 A CN106995216 A CN 106995216A
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- ammonia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/50—Fluorides
- C01F7/54—Double compounds containing both aluminium and alkali metals or alkaline-earth metals
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- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention proposes the preparation method and device of a kind of ice crystal, and this method is included after fluosilicic acid and ammonia reaction, isolated ammonium fluoride solution and silica solid；Aluminium chloride, sodium chloride are reacted with the ammonium fluoride solution, and ice crystal and ammonium chloride are obtained after separation；Calcium containing compound reacts with the ammonium chloride, obtains weak aqua ammonia and calcium chloride；The weak aqua ammonia is obtained ammonia or concentrated ammonia liquor, recycled by ammonia still.Equipment includes, first reactor, second reactor, the 3rd reactor, filter, separator, ammonia still and baker.The direct ammonification of fluosilicic acid in the present invention, technique is simple, and flow is short；Various materials can react in higher concentrations, and solid circulating rate is few, energy-conservation；Ammonia recovery is up to more than 99.9%.
Description
Technical field
The present invention relates to a kind of preparation method of ice crystal and device.
Background technology
Ice crystal also known as hexafluoro close sodium aluminate or aluminium sodium fluoride, and molecular formula is Na3AlF6, the tiny crystalline solid of white.Ice
Spar is indispensable fluxing agent in aluminium metallurgy production, and aluminium per ton about consumes 5~10 kilograms of ice crystals.Ice crystal can also make farming
The insecticide of thing, enamel opalizer, opacifier and fluxing agent, the wear-resistant filler of resin rubber of glass and enamel production,
And the dispensing of emery wheel etc..
Chemical industry is that abraum salt produces rich and influential family, and with various various, species of originating, complicated component, environmental hazard is serious, locate
The features such as financial cost is high is managed, manager and public attention is enjoyed, is the most important thing of environment supervision.Although China has established
The management systems such as corresponding laws and regulations, policy criteria, normality condition and treatment technology, but also should be seen that, China's chemical industry
The recycling of abraum salt and the aggregate level of harmlessness disposing and standardization degree are uneven, with advanced country's gap compared with
Greatly, meanwhile, the field environment case of violation of law is multiple (abraum salt flow into dining table etc.), and FUTURE ENVIRONMENT supervision will be stricter, to enterprise
The technical merit of industry processing disposal proposes requirements at the higher level with economic input.
In addition, new《Law on Environmental Protection》、《Prevention and control of environmental pollution by solid wastes method》Implement, environmental management punishment plus tight, enterprise
Industry pressure is suddenly lifted, and is proposed new demand to the processing of the abraum salt of chemical enterprise, is brought new challenge.
Having in existing method uses prodan to prepare ice crystal for raw material.Prodan method is needed prodan
The suspension of low content is configured to, (sodium fluoride is molten in 20 DEG C of -100 DEG C of water so that the sodium fluoride after ammonification does not produce precipitation
Xie Du is 4.06%-5.08%), it is therefore desirable to substantial amounts of water is circulated in technical process；Energy consumption is larger；Because water is big, instead
Weak aqua ammonia concentration after answering is very low, and ammonia recovery is relatively low；Prodan is first made, then goes ammonification desiliconization, technological process is elongated；
The aspect of the above three all causes equipment investment increase.
The content of the invention
The present invention proposes the preparation method and device of a kind of ice crystal, solves technological process length, production in the prior art
The problem of cost is high, equipment investment is big.
This invention also solves the problem of the pollutant produced during production ice crystal.
The technical proposal of the invention is realized in this way：
A kind of preparation method of ice crystal, including,
After fluosilicic acid reacts with ammonia, isolated ammonium fluoride solution and silica solid；
Aluminium chloride, sodium chloride are reacted with the ammonium fluoride solution, and ice crystal and ammonium chloride are obtained after separation；
Calcium containing compound reacts with the ammonium chloride, obtains weak aqua ammonia and calcium chloride；
The weak aqua ammonia is obtained ammonia or concentrated ammonia liquor, recycled by ammonia still.
As preferred technical scheme, the calcium containing compound is calcium oxide, calcium hydroxide or calcium carbonate.
As preferred technical scheme, the mol ratio of the fluosilicic acid and ammonia is 1：6-6.3.
As preferred technical scheme, the mol ratio of the aluminium chloride and ammonium fluoride solution is 1-1.05：6.
As preferred technical scheme, the mol ratio of the sodium chloride and ammonium fluoride solution is 3-3.2：6.
As preferred technical scheme, the mol ratio of the calcium oxide and ammonium chloride is 1-1.1：2.
As preferred technical scheme, the reaction temperature of the fluosilicic acid and ammonia is 55 DEG C -130 DEG C.
As preferred technical scheme, the reaction condition of the aluminium chloride, sodium chloride and ammonium fluoride solution is normal pressure, reaction
Temperature is 65 DEG C -120 DEG C.
As preferred technical scheme, the reaction condition of the calcium containing compound and ammonium chloride is normal pressure, and reaction temperature is
75℃-105℃。
As preferred technical scheme, after the ice crystal drying, ice crystal product is obtained；Wherein drying temperature is 220-
550℃。
As preferred technical scheme, the calcium chloride is by being concentrated to give calcium chloride product, and the vapor of generation passes through
Discharge or reuse after condenser cooling.
As preferred technical scheme, the aluminium chloride aluminium hydroxide or aluminum oxide are substituted.
When reactant is aluminium chloride
H2SiF6+6NH3+2H2O→6NH4F+SiO2
6NH4F+Al Cl 3+3NaCl→Na3AlF6+6NH4Cl
2NH4Cl+CaO→Ca Cl2+2NH3·0.5H2O
NH3·H2O→NH3↑+H2O
When reactant is aluminium hydroxide
H2SiF6+6NH3+2H2O→6NH4F+SiO2
6NH4F+Al(OH)3+3NaCl→Na3AlF6+3NH3·H2O+3NH4Cl
2NH4Cl+CaO→Ca Cl2+2NH3·0.5H2O
NH3·H2O→NH3↑+H2O
A kind of device for being used to prepare ice crystal of the present invention, including；
First reactor, second reactor, filter, separator and baker；
The first reactor, filter, second reactor, separator and baker are sequentially connected by pipeline；
The first reactor includes silicofluoric acid charging aperture and ammonia charging aperture；
The second reactor includes aluminium chloride charging aperture and sodium chloride charging aperture；
Also include the 3rd reactor, the 3rd reactor is connected with the ammonium chloride outlet of separator, the described 3rd
There is calcium containing compound charging aperture on reactor；
The discharging opening of 3rd reactor is connected with ammonia still, and the ammonia outlet of the ammonia still passes through pipeline and institute
The ammonia charging aperture for stating first reactor is connected.
As preferred technical scheme, the calcium chloride outlet of the ammonia still is connected with enrichment facility, the concentration dress
The steam put cooled down through subcooler after discharge or or reclaim use.
Beneficial effect
(1) the direct ammonification of fluosilicic acid in the present invention, technique is simple, and flow is short；Various materials can react in higher concentrations, thing
Expect that internal circulating load is few, energy-conservation；Ammonia recovery is up to more than 99.9% (ammonia in water body only less than 10ppm).
(2) F and Si in this preparation method in fluosilicic acid are utilized effectively；Production process is pollution-free；Energy consumption is low；Work
Skill control is simple；The low production cost of ice crystal product；Low equipment investment.
(3) weak aqua ammonia prepared, obtains ammonia or concentrated ammonia liquor, again as raw material and fluosilicic acid by rectification and purification
Reacted, realize recycling for material.
(4) raw material that the present invention is used is the by-product fluorine silicon of the tail gas absorption of hydrogen fluoride production enterprise and production of phosphate fertilizer enterprise
Acid and Nacl or industrial waste salt, can consume a large amount of Nacls and fluosilicic acid during preparing ice crystal, solve present enterprise
The problem of industry industry salt treatment is difficult and the problem of outlet of fluosilicic acid.
(5) one of raw material that the present invention is used is Nacl or industrial waste salt, can so reduce being produced into for ice crystal
This.Aluminium chloride can be aluminium ash and the product of abraum salt acid reaction, it is possible to resolve the problem of abraum salt acid treatment is difficult.Done when using aluminum oxide
During raw material, it is possible to resolve the problem of outlet of waste alumina.Can be all using industrial waste, and produce qualified ice crystal production
Product.
Brief description of the drawings
, below will be to embodiment in order to illustrate more clearly of embodiment of the present invention or technical scheme of the prior art
Or the accompanying drawing used required in description of the prior art is briefly described, it should be apparent that, drawings in the following description are only
It is some embodiments of the present invention, for those of ordinary skill in the art, is not paying the premise of creative labor
Under, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 embodiments 1 are used for the structural representation for preparing the device of ice crystal；
Wherein, first reactor 11, second reactor 12, the 3rd reactor 13, filter 14, separator 15, baker
16th, ammonia still 17, first charging aperture 111, second charging aperture 121, the 3rd charging aperture 122, the 4th charging aperture 131, cooler 18,
Enrichment facility 19.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
F and Si in this preparation method in fluosilicic acid are utilized effectively；Production process is pollution-free.Production procedure is short,
Process conditions are gentle so that low equipment investment.The specific material referred in following examples, in addition to industrial waste, Jun Kecong cities
Field purchase.
Embodiment 1
It is shown in Figure 1, the device for preparing ice crystal, including；First reactor 11, second reactor 12, filtering
Device 14, separator 15 and baker 16.Above-mentioned first reactor 11, filter 14, second reactor 12, separator 15
And baker 16 is sequentially connected by pipeline in sequence.First reactor 11 is provided with first charging aperture 111, silicofluoric acid and liquid
Ammonia enters first reactor 11 by first charging aperture 111.Second reactor 12 is provided with the charging aperture of second charging aperture 121 and the 3rd
122；Aluminium chloride, aluminium hydroxide or aluminum oxide enter second reactor 12 by second charging aperture 121, and sodium chloride enters by the 3rd
Material mouth 122 enters second reactor 12.The device also includes the 3rd reactor 13, the outlet of the 3rd reactor 13 and separator 15
It is connected, the 4th charging aperture 131 is provided with the 3rd reactor 13, calcium containing compound enters the 3rd by the 4th charging aperture 131
Reactor 13.The discharging opening of 3rd reactor 13 is connected with ammonia still 18, and the ammonia outlet of ammonia still 18 passes through pipeline and
The first charging aperture 111 of one reactor 11 is connected, and forms the reuse of raw material, saves raw material, reduces cost, while reducing dirty
Dye.
In order to concentrate calcium chloride product, export the calcium chloride of ammonia still 18 and be connected with enrichment facility 19.Enrichment facility
19 vapor through subcooler 18 cool down after discharge or or reclaim use.
Embodiment 2
Using the equipment shown in embodiment 1, ice crystal is prepared, specific steps include：
Step 1：By fluosilicic acid and liquefied ammonia using mol ratio as 1：6 are passed through in first reactor 11, are 55 DEG C of progress in temperature
Aminating reaction, after reaction completely, is filtered into filter 14；Silica solid is filtered out, ammonium fluoride solution is then passed through
In second reactor 12.
Step 2：Aluminium chloride and sodium chloride are also passed into second reactor 12, wherein aluminium chloride and ammonium fluoride solution rubs
You are than being 1：6, the mol ratio of sodium chloride and ammonium fluoride solution is 1：2, it is 65 DEG C in temperature with above-mentioned ammonium fluoride solution and reacts, instead
After answering completely, pass through the isolated ice crystal of separator 15 and ammonium chloride.
Step 3：Above-mentioned ice crystal is dried by baker 16 and has just obtained ice crystal product, drying temperature is 220 DEG C；
And ammonium chloride as raw material then into being continuing with the 3rd reactor 13.
Step 4：Calcium containing compound, such as calcium oxide, calcium hydroxide or calcium carbonate, this implementation are added in the 3rd reactor 13
What is added in example is calcium oxide, and the mol ratio of calcium oxide and ammonium chloride is 1.1：2, reaction temperature is 75 DEG C, is obtained after reaction dilute
Ammoniacal liquor and calcium chloride.Weak aqua ammonia obtains ammonia or concentrated ammonia liquor by ammonia still 18, continues to be passed through in first reactor 11 as original
Material is used, and calcium chloride obtains calcium chloride product after then being concentrated by enrichment facility 19, and vapor is carried out by cooler 18
After cooling, it can discharge or reuse, raw material is utilized, energy-conserving and environment-protective.
The yield of obtained ice crystal is 95%, and product quality is up to state standards GBT4291-2007.
Embodiment 3
Using the equipment shown in embodiment 1, ice crystal is prepared, specific steps include：
Step 1：By fluosilicic acid and liquefied ammonia using mol ratio as 1：6.3 are passed through in first reactor 11, and being 130 DEG C in temperature enters
Row aminating reaction, after reaction completely, is filtered into filter 14；Silica solid is filtered out, ammonium fluoride solution then leads to
Enter in second reactor 12.
Step 2：Aluminium hydroxide and sodium chloride are also passed into second reactor 12, wherein aluminium hydroxide and ammonium fluoride solution
Mol ratio be 1.05：6, the mol ratio of sodium chloride and ammonium fluoride solution is 3.2：6, be in temperature with above-mentioned ammonium fluoride solution
120 DEG C of reactions, after reaction completely, pass through the isolated ice crystal of separator 15 and ammonium chloride.
Step 3：Above-mentioned ice crystal is dried by baker 16 and has just obtained ice crystal product, and drying temperature is 550 DEG C；And
Ammonium chloride then enters to be continuing with the 3rd reactor 13 as raw material.
Step 4：Calcium containing compound, such as calcium oxide, calcium hydroxide or calcium carbonate, this implementation are added in the 3rd reactor 13
What is added in example is calcium carbonate, and the mol ratio of calcium carbonate and ammonium chloride is 1：2, reaction temperature is 105 DEG C, and dilute ammonia is obtained after reaction
Water and calcium chloride.Weak aqua ammonia obtains ammonia or concentrated ammonia liquor by ammonia still 18, continues to be passed through in first reactor 11 as raw material
Use, and calcium chloride obtains calcium chloride product after then being concentrated by enrichment facility 19, vapor is carried out cold by cooler 18
But after, it can discharge or reuse, raw material is utilized, energy-conserving and environment-protective.
The yield of obtained ice crystal is 97%, and product quality is up to state standards GBT4291-2007.
The direct ammonification of fluosilicic acid is used in above-described embodiment 2 and embodiment 3, technique is simple, and flow is short；Various materials can
React, solid circulating rate is few, save in higher concentrations；Ammonia recovery is up to more than 99.9% (only less than 10ppm's in water body
Ammonia).F and Si in this method in fluosilicic acid are utilized effectively；Production process is pollution-free；Energy consumption is low；Technology controlling and process is simple；
The low production cost of ice crystal product；Low equipment investment.The weak aqua ammonia prepared, ammonia is obtained or dense by rectification and purification
Ammoniacal liquor, is reacted as raw material with fluosilicic acid again, realizes recycling for material.The raw material used is hydrogen fluoride production
The by-product fluosilicic acid of the tail gas absorption of enterprise and production of phosphate fertilizer enterprise and Nacl or industrial waste salt, during preparing ice crystal
A large amount of Nacls and fluosilicic acid can be consumed, the problem of outlet of the problem of industrial salt treatment of present enterprise is difficult and fluosilicic acid is solved.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (9)
1. a kind of preparation method of ice crystal, it is characterised in that including,
After fluosilicic acid reacts with ammonia, isolated ammonium fluoride solution and silica solid；
Aluminium chloride, sodium chloride are reacted with the ammonium fluoride solution, and ice crystal and ammonium chloride are obtained after separation；
Calcium containing compound reacts with the ammonium chloride, obtains weak aqua ammonia and calcium chloride；
The weak aqua ammonia is obtained ammonia or concentrated ammonia liquor, recycled by ammonia still.
2. the preparation method of a kind of ice crystal according to claim 1, it is characterised in that the calcium containing compound is oxidation
Calcium, calcium hydroxide or calcium carbonate.
3. a kind of preparation method of ice crystal according to claim 1, it is characterised in that mole of the fluosilicic acid and ammonia
Than for 1：6-6.3；The mol ratio of the aluminium chloride and ammonium fluoride solution is 1-1.05：6；The sodium chloride and ammonium fluoride solution
Mol ratio is 3-3.2：6；The mol ratio of the calcium oxide and ammonium chloride is 1-1.1：2.
4. a kind of preparation method of ice crystal according to claim 1, it is characterised in that the reaction of the fluosilicic acid and ammonia
Temperature is 55 DEG C -130 DEG C；The reaction condition of the aluminium chloride, sodium chloride and ammonium fluoride solution is normal pressure, and reaction temperature is 65
℃-120℃；The reaction condition of the calcium containing compound and ammonium chloride is normal pressure, and reaction temperature is 75 DEG C -105 DEG C.
5. the preparation method of a kind of ice crystal according to claim 1, it is characterised in that after the ice crystal drying, obtain
To ice crystal product；Wherein drying temperature is 220-550 DEG C.
6. the preparation method of a kind of ice crystal according to claim 1, it is characterised in that the calcium chloride is by being concentrated to give
To calcium chloride product, discharge or reuse after the vapor of generation is cooled down by condenser.
7. a kind of preparation method of ice crystal according to claim 1, it is characterised in that the aluminium chloride hydroxide
Aluminium or aluminum oxide are substituted.
8. a kind of device for being used to prepare ice crystal, it is characterised in that including,
First reactor, second reactor, filter, separator and baker；
The first reactor, filter, second reactor, separator and baker are sequentially connected by pipeline；
The first reactor includes silicofluoric acid charging aperture and ammonia charging aperture；
The second reactor includes aluminium chloride charging aperture and sodium chloride charging aperture；
Also include the 3rd reactor, the 3rd reactor is connected with the ammonium chloride outlet of separator, in the described 3rd reaction
There is calcium containing compound charging aperture on device；
The discharging opening of 3rd reactor is connected with ammonia still, and the ammonia outlet of the ammonia still passes through pipeline and described the
The ammonia charging aperture of one reactor is connected.
9. a kind of device for being used to prepare ice crystal according to claim 8, it is characterised in that the chlorination of the ammonia still
Calcium outlet is connected with enrichment facility, and discharge or recovery are used after the steam of the enrichment facility is cooled down through subcooler.
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| CN201710242602.1A CN106995216A (en) | 2017-04-14 | 2017-04-14 | The preparation method and device of ice crystal |
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Cited By (2)
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| CN107777716A (en) * | 2017-12-11 | 2018-03-09 | 达州励志环保科技有限公司 | The preparation method and device of ice crystal |
| CN113772630A (en) * | 2021-10-19 | 2021-12-10 | 浙江容跃环保科技有限公司 | Method for preparing hydrogen fluoride from cryolite |
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| CN107777716A (en) * | 2017-12-11 | 2018-03-09 | 达州励志环保科技有限公司 | The preparation method and device of ice crystal |
| CN113772630A (en) * | 2021-10-19 | 2021-12-10 | 浙江容跃环保科技有限公司 | Method for preparing hydrogen fluoride from cryolite |
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Inventor after: Ying Shengrong Inventor after: Jiang Zhan Inventor after: Ying Yue Inventor before: Ying Shengrong |
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Application publication date: 20170801 |