CN107857286A - A kind of method that ice crystal is produced using fluosilicic acid waste liquid - Google Patents
A kind of method that ice crystal is produced using fluosilicic acid waste liquid Download PDFInfo
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- CN107857286A CN107857286A CN201711311636.8A CN201711311636A CN107857286A CN 107857286 A CN107857286 A CN 107857286A CN 201711311636 A CN201711311636 A CN 201711311636A CN 107857286 A CN107857286 A CN 107857286A
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- Prior art keywords
- ice crystal
- fluosilicic acid
- liquid
- acid waste
- waste liquid
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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
Abstract
The invention discloses a kind of method that ice crystal is produced using fluosilicic acid waste liquid of ice crystal preparing technical field；Comprise the following steps：1st, fluosilicic acid waste liquid is added in reactor with excessive 5% ~ 10% soda ash and is mixed to form feed liquid, stirred feed liquid and be heated to 70 DEG C, until material liquid pH value filters out silica after being 8 ~ 9, filtrate is Fluorinse；2nd, the alundum (Al2O3) of fluosilicic acid waste liquid and reaction ratio is poured into and feed liquid is formed in reactor, stirred feed liquid and be heated to 80 DEG C, up to, without silica is filtered out after particle, filtrate is aluminun fluoride solution in feed liquid；3rd, Fluorinse is put into synthesis reactor and excessive 9% ~ 11% aluminun fluoride solution forms mixed liquor, heating mixed liquor is to 95 DEG C ~ 100 DEG C, until there is no crystal grain generation in synthesis reactor；Mixed liquor is refiltered, ice crystal is filtered out and heats water washing, then dries, dry, obtain ice crystal finished product.This programme can significantly improve the utilization rate of fluosilicic acid waste liquid and the quality of ice crystal and output capacity.
Description
Technical field
The present invention relates to ice crystal preparing technical field, more particularly to a kind of side that ice crystal is produced using fluosilicic acid waste liquid
Method.
Background technology
Fluosilicic acid is typically the byproduct of the production such as phosphoric acid by wet process and general calcium, coarse whiting.Wet phosphoric acid by dihydrate, often produce
One ton of phosphoric acid by wet process (100%P2O5) about 0.06 ton of fluosilicic acid (100%H2SiF6) of by-product, often produce one ton of general calcium (100%
P2O5) about 0.06 ton of fluosilicic acid (100%H2SiF6) of by-product.China is production of phosphate fertilizer and consumes big country, national phosphate fertilizer industry pair
The fluosilicic acid incredible amount of production.Because caused fluosilicic acid is mainly changed into fluosilicic acid by importing pond in phophatic fertilizer production process
Waste liquid, fluosilicic acid waste liquid have highly acid, and by it, directly discharge easily damages to environment, while also result in fluosilicic acid money
The waste in source.And another aspect fluosilicic acid is one of important source material for generating ice crystal.
The use of the main method of fluosilicic acid production ice crystal is at present ammonium fluoride intermediate product and prodan intermediate product
Method, the former is that fluosilicic acid generates with being reacted again with sodium aluminate after ammoniacal liquor ammonification.The latter is by the waste gas containing fluoride in production of phosphate fertilizer
After recovered prodan, then through ammonification synthesis etc. process and be made.Above two method is required to by ammonification, and ammonification
Journey causes the preparation process of ice crystal is cumbersome, conversion ratio is relatively low seriously to add production cost.
The content of the invention
The invention is intended to provide a kind of method that ice crystal is produced using fluosilicic acid waste liquid, to improve the profit of fluosilicic acid waste liquid
With rate and the quality and output capacity of ice crystal.
A kind of method that ice crystal is produced using fluosilicic acid waste liquid in this programme, is comprised the following steps：
Step 1: the preparation of Fluorinse：
1）Fluosilicic acid waste liquid after decontamination is poured into steel lining plastic reactor, then into steel lining plastic reactor excessive addition 5% ~
10% soda ash forms feed liquid, stirs feed liquid and is heated to 70 DEG C, until material liquid pH value is 8 ~ 9；Chemical equation is：H2SiF6+
3Na2CO3→6NaF+SiO2+3CO2+H2O；
2）Filtering：Feed liquid after filtering and heating, filters out silica, and filtrate is Fluorinse；
Step 2: the preparation of aluminun fluoride solution：
1）Fluosilicic acid waste liquid after decontamination is poured into steel lining plastic reactor, then added by reaction ratio into steel lining plastic reactor
Add alundum (Al2O3) to form feed liquid, stir feed liquid and be heated to 80 DEG C, until without particle in feed liquid；Chemical equation is：
H2SiF6+Al2O3→2AlF3+SiO2+H2O；
2）Filtering：Feed liquid after filtering and heating, filters out silica, and filtrate is aluminun fluoride solution；
Step 3：The synthesis of ice crystal：
1）Fluorinse is put into synthesis reactor, then excessive 9% ~ 11% aluminun fluoride solution formation mixing is added into synthesis reactor
Liquid, heating mixed liquor is to 95 DEG C ~ 100 DEG C, until there is no crystal grain generation in synthesis reactor；Chemical equation is：3NaF+AlF3→
Na3AlF6；
2）Filter mixed liquor, filter out ice crystal and heat water washing, then dry, dry, obtain ice crystal finished product.
Beneficial effects of the present invention：Fluorine is made with soda ash and alundum (Al2O3) reaction respectively using fluosilicic acid waste liquid in this programme
Change sodium and aluminum fluoride, recycle the reaction generation ice crystal between sodium fluoride and aluminum fluoride；The whole course of reaction time is short, and makes fluorine
Silicic acid waste liquid is fully reacted, so that the quality of ice crystal and conversion ratio are all greatly improved；Simultaneously in course of reaction
In generate available silica.In Fluorinse preparation process, excessive addition 5% ~ 10% in a kettle
Soda ash fluosilicic acid is fully reacted, and the temperature of feed liquid is brought up to 70 degrees Celsius, further promote soda ash with
Reaction between fluosilicic acid waste liquid, while the reaction time is greatly reduced, improve operating efficiency；PH value is 8 ~ 9 explanation fluosilicic acid
Obtain more sufficiently reacting.In the preparation process of aluminun fluoride solution, due to fluosilicic acid waste liquid concentration typically only 11% ~
12%, it can fully be reacted with fluosilicic acid waste liquid from alundum (Al2O3), be advantageous to improve the utilization rate of fluosilicic acid, simultaneously will
The reaction temperature of feed liquid is controlled at 80 DEG C, is significantly improved reaction speed and is improved the consumption of fluosilicic acid.In ice crystal
In preparation process, due to the concentration typically only 11% ~ 12% of fluosilicic acid waste liquid, so that obtained Fluorinse and aluminum fluoride
The concentration of solution is respectively at 18% ~ 22% and 11% ~ 13% or so, and because both concentration are relatively low, and aluminum fluoride is lazy with respect to sodium fluoride
Property it is stronger, excessive 9% ~ 11% aluminun fluoride solution is added in the mixed liquor formed to Fluorinse and aluminun fluoride solution makes both
Between reactant reach balanced, be advantageous to both and fully react, improve the conversion ratio of ice crystal, reduce the contaminative of filtrate；
And reacted at a temperature of 95 DEG C ~ 100 DEG C, significantly improve reaction speed between the two and improve the conversion of ice crystal
Rate.
Further, in ice crystal preparation process the concentration of fluosilicic acid waste liquid be 12%, soda ash purity be more than 96%, three oxidation
The purity of two aluminium is more than 95%.It is all linked with one another between each reaction due in the preparation process of ice crystal, wherein any one ring occurs
Problem can all cause the quality of ice crystal low with conversion ratio.The concentration of fluosilicic acid is kept to ensure that remaining soda ash and three oxygen 12%
Change the reaction between two aluminium, while cause cost to improve from avoiding the addition fluosilicic acid into fluosilicic acid waste liquid；And soda ash and three oxygen
The purity for changing two aluminium is maintained at high-order and is advantageous to its reaction between fluosilicic acid waste liquid, while ensures that the sodium fluoride after reaction is molten
Liquid has higher purity with aluminun fluoride solution, so as to save the reaction time for the generation of ice crystal, improves the quality of ice crystal
With conversion ratio.
Further, in step 1, the heating to feed liquid is until material liquid pH value is 9.Material liquid pH value is realized substantially after reaching 8
The abundant reaction of fluosilicic acid, but be to ensure the complete reaction of fluosilicic acid, it is heated to after material liquid pH value reaches 9, the fluorine silicon in feed liquid
Acid has realized complete reaction.
Further, in step 3, the aluminun fluoride solution excessive value of addition is 10%.10% aluminum fluoride excessive value can ensure that fluorine
Change the normal reaction between sodium and aluminum fluoride, while avoid the aluminun fluoride solution of excessive addition from causing mixed liquid concentration further to drop
It is low, reduce reaction speed between the two.
Brief description of the drawings
Fig. 1 is a kind of schematic flow sheet for the method that ice crystal is produced using fluosilicic acid waste liquid of the present invention.
Embodiment
Below by embodiment, the present invention is further detailed explanation：
Embodiment 1：
A kind of method that ice crystal is produced using fluosilicic acid waste liquid as shown in Figure 1, is comprised the following steps：
Step 1: the preparation of Fluorinse：
1) by the fluosilicic acid waste liquid after decontamination be made concentration be 12% silicate fluoride solution and pour into steel lining plastic reactor, then
The soda ash of excessive addition 10% into steel lining plastic reactor（Soda ash purity is 98%）Feed liquid is formed, feed liquid is stirred and is heated to 70
DEG C, until material liquid pH value is 9；Chemical equation is：H2SiF6+3Na2CO3→6NaF+SiO2+3CO2+H2O；
2) filter：Feed liquid after filtering and heating, silica being filtered out, filtrate is sodium fluoride liquid, then by sodium fluoride liquid system
Standby is the Fluorinse that concentration of sodium fluoride is 20%；
Step 2: the preparation of aluminun fluoride solution：
1）By the fluosilicic acid waste liquid after decontamination be made concentration be 12% silicate fluoride solution and pour into steel lining plastic reactor, then
By reaction ratio alundum (Al2O3) is added into steel lining plastic reactor（The purity of alundum (Al2O3) is 96%）Form feed liquid, stirring
Feed liquid is simultaneously heated to 80 DEG C, until without particle in feed liquid；Chemical equation is：H2SiF6+Al2O3→2AlF3+SiO2+H2O；
2）Filtering：Feed liquid after filtering and heating, silica is filtered out, filtrate is to be fluorinated aluminium liquid, then will be fluorinated aluminium liquid system
Standby is the Fluorinse that aluminum fluoride concentration is 12%；
Step 3：The synthesis of ice crystal：
1）Fluorinse is put into synthesis reactor, then excessive 10% aluminun fluoride solution formation mixed liquor is added into synthesis reactor,
Mixed liquor is heated to 100 DEG C, until there is no crystal grain generation in synthesis reactor；Chemical equation is：3NaF+AlF3→Na3AlF6；
2）Filter mixed liquor, filter out ice crystal and heat water washing, then dry, dry, obtain ice crystal finished product.
Embodiment 2：
The difference of embodiment 2 and embodiment 1 is, the purity of soda ash is 96%, the purity of alundum (Al2O3) is 95%；Step
Feed liquid is heated to material liquid pH value as 8.5 in one；In step 3, the excessive value of aluminun fluoride solution addition is 9%, heating-up temperature 95
℃。
Embodiment 3：
The difference of embodiment 3 and embodiment 1 is, the purity of soda ash is 97%, the purity of alundum (Al2O3) is 98%；Step
Feed liquid is heated to material liquid pH value as 8 in one；In step 3, the excessive value of aluminun fluoride solution addition is 11%, heating-up temperature 98
℃。
Ice crystal is prepared by using the present invention, the quality and conversion ratio of ice crystal can be effectively improved, while realizes fluorine silicon
The efficient utilization of acid waste liquid, avoids the waste of fluosilicic acid in fluosilicic acid waste liquid, is the development of enterprise while environmental protection
Create more values.
Above-described is only embodiments of the invention, and the general knowledge such as known concrete structure and characteristic is not made herein in scheme
Excessive description., without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these should also be considered as protection scope of the present invention, and these are implemented all without the influence present invention
Effect and practical applicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as embodiment can be used for the content for explaining claim.
Claims (4)
- A kind of 1. method that ice crystal is produced using fluosilicic acid waste liquid, it is characterised in that comprise the following steps：Step 1: the preparation of Fluorinse：Fluosilicic acid waste liquid after decontamination is poured into steel lining plastic reactor, then the excessive addition 5% ~ 10% into steel lining plastic reactor Soda ash form feed liquid, stirring feed liquid is simultaneously heated to 70 DEG C, until material liquid pH value is 8 ~ 9；Chemical equation is：H2SiF6+ 3Na2CO3→6NaF+SiO2+3CO2+H2O；Filtering：Feed liquid after filtering and heating, filters out silica, and filtrate is Fluorinse；Step 2: the preparation of aluminun fluoride solution：Fluosilicic acid waste liquid after decontamination is poured into steel lining plastic reactor, then added by reaction ratio into steel lining plastic reactor Alundum (Al2O3) forms feed liquid, stirs feed liquid and is heated to 80 DEG C, until without particle in feed liquid；Chemical equation is：H2SiF6+ Al2O3→2AlF3+SiO2+H2O；Filtering：Feed liquid after filtering and heating, filters out silica, and filtrate is aluminun fluoride solution；Step 3：The synthesis of ice crystal：Fluorinse is put into synthesis reactor, then excessive 9% ~ 11% aluminun fluoride solution formation mixing is added into synthesis reactor Liquid, heating mixed liquor is to 95 DEG C ~ 100 DEG C, until there is no crystal grain generation in synthesis reactor；Chemical equation is：3NaF+AlF3→ Na3AlF6；Filter mixed liquor, filter out ice crystal and heat water washing, then dry, dry, obtain ice crystal finished product.
- 2. the method according to claim 1 that ice crystal is produced using fluosilicic acid waste liquid, it is characterised in that：It is prepared by ice crystal During fluosilicic acid waste liquid concentration be 12%, soda ash purity is more than 96%, the purity of alundum (Al2O3) is more than 95%.
- 3. the method according to claim 2 that ice crystal is produced using fluosilicic acid waste liquid, it is characterised in that：In step 1, Heating to feed liquid is until material liquid pH value is 9.
- 4. the method according to claim 3 that ice crystal is produced using fluosilicic acid waste liquid, it is characterised in that：In step 3, The aluminun fluoride solution excessive value of addition is 10%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109231247A (en) * | 2018-11-28 | 2019-01-18 | 达州励志环保科技有限公司 | A kind of method that the by-product of fluosilicic acid legal system aluminum fluoride prepares ice crystal |
| CN115196660A (en) * | 2022-06-22 | 2022-10-18 | 中石化南京工程有限公司 | Method and system for producing cryolite from fluosilicic acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629800A (en) * | 2016-09-30 | 2017-05-10 | 王显权 | Method for producing cryolite from fluosilicic acid waste liquid |
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- 2017-12-11 CN CN201711311636.8A patent/CN107857286A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629800A (en) * | 2016-09-30 | 2017-05-10 | 王显权 | Method for producing cryolite from fluosilicic acid waste liquid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109231247A (en) * | 2018-11-28 | 2019-01-18 | 达州励志环保科技有限公司 | A kind of method that the by-product of fluosilicic acid legal system aluminum fluoride prepares ice crystal |
| CN115196660A (en) * | 2022-06-22 | 2022-10-18 | 中石化南京工程有限公司 | Method and system for producing cryolite from fluosilicic acid |
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Application publication date: 20180330 |