CN107117621A - A kind of preparation method of magnesium fluosilicate - Google Patents
A kind of preparation method of magnesium fluosilicate Download PDFInfo
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- CN107117621A CN107117621A CN201610098802.XA CN201610098802A CN107117621A CN 107117621 A CN107117621 A CN 107117621A CN 201610098802 A CN201610098802 A CN 201610098802A CN 107117621 A CN107117621 A CN 107117621A
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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
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention belongs to magnesium fluosilicate field, more particularly to a kind of preparation method of magnesium fluosilicate.The method that the present invention is provided comprises the following steps：A), fluosilicic acid and magnesia are reacted in water, and the pH of question response system stops reaction after being changed into 3~4, obtains reaction solution；B), the reaction solution be concentrated into that quality is changed into original at 100~120 DEG C 15~40%, obtain the first crystallized product and concentrate；C) after, the concentrate is concentrated into quality is changed into original 30~50% at 100~120 DEG C, crystallisation by cooling obtains the second crystallized product；D), first crystallized product and the second crystallized product are dried, and obtain magnesium fluosilicate.
Description
Technical field
The invention belongs to magnesium fluosilicate field, more particularly to a kind of preparation method of magnesium fluosilicate.
Background technology
Magnesium fluosilicate is a kind of colourless or white diamond or acicular crystal, tasteless, relative density 1.788, by
Easily hydrolyzed when hot and produce silicon tetrafluoride gas, soluble in water, 648 grams/10 grams water of solubility under normal temperature and pressure,
It is anti-frequently as concrete intensifier, concrete hardening retarders, rubber latex solidified agent, preservative and textile
Moth agent is used.
At present, it is industrial that magnesium fluosilicate is mainly produced using magnesia neutralisation, but existing magnesia is neutralized
Method production technology exist magnesium fluosilicate product yield it is low the problem of.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of magnesium fluosilicate, using this hair
The yield when method of bright offer prepares magnesium fluosilicate is higher.
The invention provides a kind of preparation method of magnesium fluosilicate, comprise the following steps：
A), fluosilicic acid and magnesia are reacted in water, and the pH of question response system stops after being changed into 3~4
Only react, obtain reaction solution；
B), the reaction solution be concentrated into that quality is changed into original at 100~120 DEG C 15~40%, obtain
First crystallized product and concentrate；
C) after, the concentrate is concentrated into quality is changed into original 30~50% at 100~120 DEG C, cooling
Crystallization, obtains the second crystallized product；
D), first crystallized product and the second crystallized product are dried, and obtain magnesium fluosilicate.
It is preferred that, the mol ratio of the fluosilicic acid and magnesia is (0.5~1.5)：1.
It is preferred that, in step b), the reaction solution is removed before being concentrated, first in the reaction solution
Precipitation.
It is preferred that, in step d), the temperature of the drying is 55~70 DEG C.
It is preferred that, in step d), the time of the drying is 10~15min.
It is preferred that, the step a) is specially：
The mixture and raw materials of magnesium oxide of fluosilicic acid and water are reacted, and the pH of question response system is changed into 3~4
Stop reaction afterwards, obtain reaction solution.
It is preferred that, the content of fluosilicic acid is 15~30wt% in the mixture of the fluosilicic acid and water.
It is preferred that, the raw materials of magnesium oxide is magnesia.
It is preferred that, the content of magnesia is 70~90wt% in the magnesia.
Compared with prior art, the invention provides a kind of preparation method of magnesium fluosilicate.The present invention is provided
Method comprise the following steps：A), fluosilicic acid and magnesia are reacted in water, question response system
PH stops reaction after being changed into 3~4, obtains reaction solution；B), the reaction solution is concentrated at 100~120 DEG C
It is changed into original 15~40% to quality, obtains the first crystallized product and concentrate；C), the concentrate
After quality is changed into original 30~50% are concentrated at 100~120 DEG C, crystallisation by cooling obtains the second crystallization
Product；D), first crystallized product and the second crystallized product are dried, and obtain magnesium fluosilicate.This
Invention is by controlling the endpoint pH of fluosilicic acid and oxidation reactive magnesium and being crystallized using two-step enrichment, effectively suppression
Hydrolysis of the magnesium fluosilicate in preparation process is made, so as to improve final obtained magnesium fluosilicate product
Yield.Test result indicates that, the method provided using the present invention prepares the fluorination aluminum that purity is more than 95%
During product, its yield is more than 59%.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that institute
The embodiment of description is only a part of embodiment of the invention, rather than whole embodiments.Based on this hair
Embodiment in bright, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
The invention provides a kind of preparation method of magnesium fluosilicate, comprise the following steps：
A), fluosilicic acid and magnesia are reacted in water, and the pH of question response system stops after being changed into 3~4
Only react, obtain reaction solution；
B), the reaction solution be concentrated into that quality is changed into original at 100~120 DEG C 15~40%, obtain
First crystallized product and concentrate；
C) after, the concentrate is concentrated into quality is changed into original 30~50% at 100~120 DEG C, cooling
Crystallization, obtains the second crystallized product；
D), first crystallized product and the second crystallized product are dried, and obtain magnesium fluosilicate.
In the present invention, fluosilicic acid and magnesia are reacted in water first.Wherein, the fluorine silicon
The mol ratio of acid and magnesia is preferably (0.5~1.5)：1, more preferably (0.66~1.43)：1, most
Preferably 1：1；The temperature of the reaction is preferably room temperature.The pH of question response system stops anti-after being changed into 3~4
Should, obtain reaction solution.
In one embodiment that the present invention is provided, the reaction solution is prepared in such a way：
The mixture and raw materials of magnesium oxide of fluosilicic acid and water are reacted, and the pH of question response system is changed into 3~4
Stop reaction afterwards, obtain reaction solution.
In the preparation method that the above embodiment of the present invention is provided, in the mixture of the fluosilicic acid and water
Fluosilicic acid content is preferably 15~30wt%, more preferably 20~25wt%；The raw materials of magnesium oxide is preferably water chestnut
Magnesia；Content of magnesia in the magnesia is preferably 70~90wt%, more preferably 80~85wt%；Institute
The mol ratio for stating magnesia in fluosilicic acid and magnesia is preferably (0.5~1.5)：1, more preferably
(0.66~1.43)：1, most preferably 1：1；The temperature of the reaction is preferably room temperature.
Obtain after the reaction solution, the reaction solution is concentrated into quality under the conditions of 100~120 DEG C is changed into former
15~40% come.Magnesium fluosilicate crystal is constantly separated out from reaction solution in concentration process, after concentration terminates,
Separation of solid and liquid, obtains the first crystallized product and concentrate.Wherein, first crystallized product is fluosilicic acid
Magnesium crystal.In the present invention, the temperature of the concentration is 100~120 DEG C, preferably 105~110 DEG C；Institute
The quality for stating reaction solution after concentration is changed into original 15~40%, preferably becomes original 20~40%.In this hair
In one embodiment of bright offer, the quality of reaction solution is changed into original 20~30% after the concentration；At this
Invent in another embodiment provided, the quality of reaction solution is changed into original 35~40% after the concentration.
In the present invention, to reduce the impurity content in the first crystallized product and concentrate, the reaction solution is entering
Before row concentration, the precipitation in the reaction solution is preferably first removed.In the present invention, the reaction is removed
The concrete mode of precipitation in liquid is：After being filtered to the reaction solution, filter residue is removed.
Obtain after concentrate, the concentrate is concentrated into quality under the conditions of 100~120 DEG C is changed into original
30~50%, crystallisation by cooling afterwards.Magnesium fluosilicate crystal is constantly separated out in crystallisation by cooling, after concentration terminates,
Separation of solid and liquid, obtains the second crystallized product, second crystallized product also magnesium fluosilicate crystal.
In the present invention, the temperature of the concentration is 100~120 DEG C, preferably 105~110 DEG C；After the concentration
The quality of concentrate is changed into original 30~50%, preferably becomes original 38~50%.There is provided in the present invention
In one embodiment, the quality of concentrate is changed into original 38~40% after the concentration；In present invention offer
Another embodiment in, the quality of concentrate is changed into original 45~50% after the concentration.
Obtain after the first crystallized product and the second crystallized product, first crystallized product and second are crystallized
Product is dried.The temperature of the drying is preferably 55~70 DEG C, more preferably 60~65 DEG C；It is described dry
The dry time is preferably 10~15min；The promising infared dryer of the equipment used of the drying.Dry
After end, magnesium fluosilicate product is obtained.
The present invention is crystallized by controlling fluosilicic acid with the endpoint pH of oxidation reactive magnesium and using two-step enrichment,
Hydrolysis of the magnesium fluosilicate in preparation process effectively is inhibited, so as to improve final obtained magnesium fluosilicate
The yield of product.In the preferred embodiment that the present invention is provided, by controlling fluosilicic acid and magnesia to exist
Dosage in water, reduces fluosilicic acid and aoxidizes water of the magnesium fluosilicate of reactive magnesium generation in reaction solution
Solution degree, so as to further improve the yield of final obtained magnesium fluosilicate product.Test result indicates that,
When the method provided using the present invention prepares fluorination aluminum products of the purity more than 95%, its yield is more than 59%.
For the sake of becoming apparent from, it is described in detail below by following examples.
Embodiment 1
By 700g 20.58wt% silicate fluoride solution and 50g magnesias (content of magnesia 80.01wt%)
Add to be stirred with sticking plaster in plastic beaker and to react uniform, to pH value=3~4, stop reaction,
Obtain reaction solution；Reaction solution is filtered, and the filtrate being filtrated to get is concentrated by evaporation in two steps at 105 DEG C,
First step filtrate is concentrated into 20~30wt%, filters while hot, obtains filtrate and filtrate；The filtrate is entered again
Row second step is concentrated by evaporation to after 38~40wt%, is put into crystallizer crystallisation by cooling, is centrifuged afterwards
To crystallization；The crystallization is merged with above-mentioned filtrate, then with laboratory far infrared drying device 60~
10~15min is dried at 65 DEG C, weighs obtain 108g finished products after drying.
The finished product is analyzed using infrared spectrometer, and by obtained spectrogram and magnesium fluosilicate mark
The infrared spectrogram of quasi- sample is compared, and spectrum curve is consistent, and it is fluorine to illustrate finished product produced by the present invention
Magnesium silicate.
Obtained finished product is vaporized at 120 DEG C, 3g residues are obtained, so as to calculate fluorine in finished product
Silicic acid content of magnesium is 105g, and then it is 97.2% to calculate magnesium fluosilicate content in finished product.
Product yield is calculated, as a result for：108/166 × 100%=65.1%.
Embodiment 2
By 700g 20.58wt% silicate fluoride solution and 75g magnesias (content of magnesia 80.01wt%)
Add to be stirred with sticking plaster in plastic beaker and to react uniform, to pH value=3~4, stop reaction,
Obtain reaction solution；Reaction solution is filtered, and the filtrate being filtrated to get is concentrated by evaporation in two steps at 105 DEG C,
First step filtrate is concentrated into 20~30wt%, filters while hot, obtains filtrate and filtrate；The filtrate is entered again
Row second step is concentrated by evaporation to after 38~40wt%, is put into crystallizer crystallisation by cooling, is centrifuged afterwards
To crystallization；The crystallization is merged with above-mentioned filtrate, then with laboratory far infrared drying device 60~
It is dried to weigh after drying for 10~15 minutes at 65 DEG C and obtains 110.3g finished products.
Obtained finished product is vaporized at 120 DEG C, 5.2g residues are obtained, so as to calculate in finished product
Magnesium fluosilicate content is 105.1g, and then it is 95.3% to calculate magnesium fluosilicate content in finished product.
Product yield is calculated, as a result for：110.3/166 × 100%=66.45%.
Embodiment 3
By 1000g 20.58wt% silicate fluoride solution and 50g magnesias (content of magnesia 80.01wt%)
Add to be stirred with sticking plaster in plastic beaker and to react uniform, to pH value=2~2.5, stop reaction,
Obtain reaction solution；Reaction solution is filtered, and the filtrate being filtrated to get is concentrated by evaporation in two steps at 105 DEG C,
First step filtrate is concentrated into 20~30wt%, filters while hot, obtains filtrate and filtrate；The filtrate is entered again
Row second step is concentrated by evaporation to after 38~40wt%, is put into crystallizer crystallisation by cooling, is centrifuged afterwards
To crystallization；The crystallization is merged with above-mentioned filtrate, then with laboratory far infrared drying device 60~
It is dried to weigh after drying for 10~15 minutes at 65 DEG C and obtains 105.9g finished products.
Obtained finished product is vaporized at 120 DEG C, 3.5g residues are obtained, so as to calculate in finished product
Magnesium fluosilicate content is 102.4g, and then it is 96.7% to calculate magnesium fluosilicate content in finished product.
Product yield is calculated, as a result for：105.9/166 × 100%=63.8%.
Embodiment 4
By 700g 20.58wt% silicate fluoride solution and 50g magnesias (content of magnesia 80.01wt%)
Add to be stirred with sticking plaster in plastic beaker and to react uniform, to pH value=3~4, stop reaction,
Obtain reaction solution；Reaction solution is filtered, and the filtrate being filtrated to get is concentrated by evaporation in two steps at 105 DEG C,
First step filtrate is concentrated into 35~40wt%, filters while hot, obtains filtrate and filtrate；The filtrate is entered again
Row second step is concentrated by evaporation to after 45~50wt%, is put into crystallizer crystallisation by cooling, is centrifuged afterwards
To crystallization；The crystallization is merged with above-mentioned filtrate, then with laboratory far infrared drying device 60~
It is dried to weigh after drying for 10~15 minutes at 65 DEG C and obtains 98.2g finished products.
Obtained finished product is vaporized at 120 DEG C, 2.2g residues are obtained, so as to calculate in finished product
Magnesium fluosilicate content is 96g, and then it is 97.8% to calculate magnesium fluosilicate content in finished product.
Product yield is calculated, as a result for：98.2/166 × 100%=59.1%.
Described above is only the preferred embodiment of the present invention, it is noted that for the general of the art
For logical technical staff, under the premise without departing from the principles of the invention, some improvement and profit can also be made
Decorations, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of magnesium fluosilicate, comprises the following steps：
A), fluosilicic acid and magnesia are reacted in water, and the pH of question response system stops after being changed into 3~4
Only react, obtain reaction solution；
B), the reaction solution be concentrated into that quality is changed into original at 100~120 DEG C 15~40%, obtain
First crystallized product and concentrate；
C) after, the concentrate is concentrated into quality is changed into original 30~50% at 100~120 DEG C, cooling
Crystallization, obtains the second crystallized product；
D), first crystallized product and the second crystallized product are dried, and obtain magnesium fluosilicate.
2. according to the method described in claim 1, it is characterised in that the fluosilicic acid and magnesia rub
You are than being (0.5~1.5)：1.
3. according to the method described in claim 1, it is characterised in that in step b), the reaction solution
Before being concentrated, the precipitation in the reaction solution is first removed.
4. according to the method described in claim 1, it is characterised in that in step d), the drying
Temperature is 55~70 DEG C.
5. method according to claim 4, it is characterised in that in step d), the drying
Time is 10~15min.
6. according to the method described in claim 1, it is characterised in that the step a) is specially：
The mixture and raw materials of magnesium oxide of fluosilicic acid and water are reacted, and the pH of question response system is changed into 3~4
Stop reaction afterwards, obtain reaction solution.
7. method according to claim 6, it is characterised in that the mixture of the fluosilicic acid and water
The content of middle fluosilicic acid is 15~30wt%.
8. method according to claim 6, it is characterised in that the raw materials of magnesium oxide is magnesia.
9. method according to claim 8, it is characterised in that magnesia contains in the magnesia
Measure as 70~90wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111792648A (en) * | 2020-07-24 | 2020-10-20 | 昆明合起工贸有限公司 | Process for producing ferrous fluorosilicate |
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