CN108821300A - One kind preparing CaSiO by discarded silicon slag3Method - Google Patents
One kind preparing CaSiO by discarded silicon slag3Method Download PDFInfo
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention belongs to field of silicate technology, more particularly to one kind to prepare CaSiO by discarded silicon slag3Method.This method comprises the following steps：Firstly, being uniformly mixed with sodium hydroxide by discarded silicon slag is levigate, obtain mixing material；Secondly, adding water after material roasting will be mixed, and it is stirred dissolution, filters, obtain sodium silicate solution and adjust pH value, impurity is taken out in purification；Again, it will be calcined after limestone crushing, obtain active calcium oxide, and active calcium oxide is added into water emulsification, obtain calcium hydroxide emulsion；Finally, calcium hydroxide emulsion is mixed in proportion with sodium silicate solution, hydro-thermal reaction produces CaSiO3And sodium hydroxide solution, inspissation crystallize to obtain sodium hydroxide return and mention silicon.The present invention provides a kind of hydro-thermal method and prepares the micro-nano CaSiO of morphology controllable3Method, by change additive and additive whether is added type and additive amount may be implemented to CaSiO3The control of pattern.
Description
Technical field
The invention belongs to field of silicate technology, more particularly to one kind to prepare CaSiO by discarded silicon slag3Method.
Background technique
Siliceous mineral up to more than 79 in nature, rich reserves.Natural high-quality mineral have crystal, quartz etc..Often
In the metallurgical mineral seen such as zinc oxide ore, lateritic nickel ore, boron magnesium ore, cupric oxide ore resource and metallurgical secondary resource flyash
Silicon resource rich in.
Traditional method utilizes these resources, is generally conceived to the extraction and application of wherein high level non-ferrous metal, such as zinc oxide
Mine is generally conceived to extraction zinc and lead, lateritic nickel ore are conceived to extraction nickel and cobalt (partially recycled iron), flyash are conceived to extraction
Aluminium therein etc., and the big silicon of content cannot be utilized rationally, become waste discharge, caused serious environmental pollution and resource
Waste (general containing acid or alkali).The stockpiling of silicon slag not only land occupation, also wastes resource, because of the remaining of leaching agent or reactant
Huge pressure is generated to environment.
Also industrial waterglass is made in the silicon extraction in silicate phase by some or the precipitation method produce precipitated silica (hard charcoal
It is black), because white carbon black particle size range is wide, agglomeration is obvious, be only used in rubber or coating common, of low grade, performance without
Method meets the needs of high-end rubber, coating, plastics, ceramic industry, and it is even more impossible to enter cosmetics, pharmaceuticals industry, added value is lower,
And domestic only 3,000,000 tons or so of annual consumption.
With the development of micro Nano material chemical synthesis process, hydro-thermal method mild, product advantages of good crystallization, production with its reaction condition
The advantages such as product are controllable are valued by people.In recent years in the monodispersity of micro-and nano-particles and size, pattern control and scale
Metaplasia produces aspect and achieves significant progress.
Summary of the invention
(1) technical problems to be solved
For existing technical problem, the present invention provides a kind of hydro-thermal method and prepares the micro-nano CaSiO of morphology controllable3's
Method may be implemented by changing the type that additive and additive whether is added and additive amount to CaSiO3The control of pattern
System.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include：
One kind preparing CaSiO by discarded silicon slag3Method, include the following steps：
It is S1, levigate：It is discarded silicon slag is dry, broken and levigate, obtain levigate silicon slag；
S2, mixing：The levigate silicon slag is uniformly mixed with sodium hydroxide, obtains mixing material；
S3, roasting：The material that is mixed is roasted, roasting material is obtained；
S4, dissolution filtering：The roasting material is added into water, and is stirred dissolution, filters, obtains sodium silicate solution；
S5, purification：Adjust the pH value of the sodium silicate solution；
S6, calcining：It will be calcined after limestone crushing, obtain active calcium oxide；
S7, emulsification：The active calcium oxide is added to the water, is stirred while adding, and filters and weeds out insoluble impurity particle,
Obtain calcium hydroxide emulsion；
S8, causticization：By the calcium hydroxide emulsion and the sodium silicate solution with molar ratio together with hydrothermal reaction kettle is added,
Stirring evenly reacts it, described to filter after reaction, is placed in oven and dried to obtain CaSiO after washing3；
S9, crystallization：Mixed solution is obtained in the step S8, crystallizes the mixed solution inspissation to obtain sodium hydroxide,
Return mentions silicon, and obtained water continues cycling through utilization.
Preferably, in the step S2, required for the dosage of sodium hydroxide is reacted completely just for silicon in levigate silicon slag
1.0 times of sodium hydroxide theoretical amount~1.6 times.
Preferably, in the step S3, the temperature of roasting is 300 DEG C~550 DEG C, and the constant temperature time of roasting is 50min
~250min.
Preferably, in the step S4, the solid-liquid mass ratio for roasting material and water is 1:2~1:10, the temperature of stirring
It is 60 DEG C~90 DEG C, the time of stirring is 60min~150min.
Preferably, in the step S5, hydrochloric acid is selected to adjust the pH value of sodium silicate solution, pH value is 11~11.5.
Preferably, in the step S7, the concentration of calcium hydroxide emulsion is 120gL-1~260gL-1。
Preferably, in the step S8, molar ratio 0.9：1~1.3：1.
Preferably, in the step S8, it is 10% that mass percentage is added simultaneously into the hydrothermal reaction kettle
Additive.
Preferably, the additive is one in cetyl trimethylammonium bromide, lauryl sodium sulfate and sodium chloride
Kind.
Preferably, in the step S8, the temperature reacted in hydrothermal reaction kettle is 180 DEG C~240 DEG C, reaction when
Between be 4h~12h, dry temperature is 90 DEG C~120 DEG C in an oven, and the dry time is 6h~12h.
(3) beneficial effect
The beneficial effects of the invention are as follows：
1, provided by the invention that CaSiO is prepared by discarded silicon slag3Method closed using discarded silicon slag as raw material using hydro-thermal
At technology, CaSiO is prepared by precipitating reagent of calcium hydroxide emulsion3, reaction condition is mild, product advantages of good crystallization, product morphology controllable.
2, provided by the invention that CaSiO is prepared by discarded silicon slag3Method, it is obtained threadiness and needle-shaped CaSiO3, chemistry
Stability is good, high-temperature stability is good, dielectric properties are good, and added value of product is high, in papermaking, high-grade ceramic, rubber and NEW TYPE OF COMPOSITE
The fields such as material have a wide range of applications.
3, provided by the invention that CaSiO is prepared by discarded silicon slag3Method, the repeatable benefit of the sodium hydroxide generated in the process
With.
4, provided by the invention that CaSiO is prepared by discarded silicon slag3Method, for metallurgy industry discard silicon slag recycling and
Innoxious use provides an approach.
Detailed description of the invention
Fig. 1 is CaSiO obtained in the embodiment of the present invention 13SEM spectrum；
Fig. 2 is CaSiO obtained in the embodiment of the present invention 23SEM spectrum；
Fig. 3 is CaSiO obtained in the embodiment of the present invention 33SEM spectrum.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
Present embodiment proposes a kind of by discarded silicon slag preparation CaSiO3Method, include the following steps：
It is S1, levigate：It is discarded silicon slag is dry, broken and levigate, obtain levigate silicon slag；
S2, mixing：The levigate silicon slag is uniformly mixed with sodium hydroxide, obtains mixing material；
S3, roasting：The material that is mixed is roasted, roasting material is obtained；
S4, dissolution filtering：The roasting material is added into water, and is stirred dissolution, filters, obtains sodium silicate solution；
S5, purification：Adjust the pH value of the sodium silicate solution；
S6, calcining：It will be calcined after limestone crushing, obtain active calcium oxide；
S7, emulsification：The active calcium oxide is added to the water, is stirred while adding, and filters and weeds out insoluble impurity particle,
Obtain calcium hydroxide emulsion；
S8, causticization：By the calcium hydroxide emulsion and the sodium silicate solution with molar ratio together with hydrothermal reaction kettle is added,
Stirring evenly reacts it, described to filter after reaction, is placed in oven and dried to obtain CaSiO after washing3；
S9, crystallization：Mixed solution is obtained in the step S8, crystallizes the mixed solution inspissation to obtain sodium hydroxide,
Return mentions silicon, and obtained water continues cycling through utilization.
It is discarded silicon slag is broken, levigate to 170 mesh~230 mesh, it is preferable that will to discard in present embodiment step S1
Silicon slag is levigate to 200 mesh, and obtained levigate silicon slag can preferably be mixed with sodium hydroxide.Wherein, it discards in silicon slag and contains
There are the impurity such as a small amount of aluminium, iron and calcium.
In present embodiment step S2, the dosage of sodium hydroxide is that silicon reacts required hydrogen completely just in levigate silicon slag
1.0 times of sodium oxide molybdena theoretical amount~1.6 times.
In present embodiment step S3, the temperature of roasting is 300 DEG C~550 DEG C, the constant temperature time of roasting be 50min~
The chemical reaction of such as formula (1), (2) occurs in roasting process for 250min.
SiO2+ 2NaOH=Na2SiO3+H2O (1)
Na2SiO3+ 2NaOH=Na4SiO4+H2O (2)
In present embodiment step S4, the solid-liquid mass ratio for roasting material and water is 1:2~1:10, the temperature of stirring is
60 DEG C~90 DEG C, the time of stirring is 60min~150min.
In present embodiment step S5, precipitated since other acid are easy to generate with calcium ion, so hydrochloric acid is selected to adjust
The pH value of sodium silicate solution, pH value are 11~11.5.Due to carry out alkali process silicon slag when, sodium hydroxide be it is excessive, in this way add
On the one hand the hydrochloric acid entered can neutralize excessive sodium hydroxide, generate water and sodium chloride solution.On the other hand, hydrochloric acid can and it is a small amount of
The sodium silicate solution of (3% or so) reacts, and generates hydrated SiO 2 precipitating and sodium chloride solution, while a small amount of aluminium in step S3
The sodium aluminate generated with sodium hydroxide reaction, can react with hydrochloric acid and generate aluminium hydroxide and sodium chloride.It is a small amount of in sodium silicate solution
Impurity (such as do not precipitate complete aluminium, iron and calcium etc.) be adsorbed and removed by aluminium hydroxide, precipitation of silica, promote the product of product
Matter.More particularly to such as formula (3), (4) chemical reaction.
Na2SiO3+2H++(n-1)H2O→2Na++SiO2·nH2O↓ (3)
NaAlO2+H++H2O→Na++Al(OH)3↓ (4)
In present embodiment step S6, after limestone crushing to 2cm~5cm, it is placed in Muffle furnace and calcines.
In present embodiment step S7, it will take out after active calcium oxide furnace cooling, be added to the water while hot, when being added
Stirring is filtered with heat release and is weeded out insoluble impurity particle, and the concentration for obtaining calcium hydroxide emulsion is 120gL-1~260gL-1, and in particular to as formula (5) chemically react.
CaO+H2O→Ca(OH)2 (5)
In present embodiment step S8, by calcium hydroxide emulsion and sodium silicate solution with molar ratio 0.9：1~1.3：1 one
With addition hydrothermal reaction kettle, and the additive that 2ml~10ml that mass percentage is 10% is added stirs evenly, and carries out anti-
It answers.Wherein, cetyl trimethylammonium bromide (CTAB), lauryl sodium sulfate (SDS) and sodium chloride can be selected in additive
(NaCl) any one in, and the temperature of hydro-thermal reaction is 180 DEG C~240 DEG C, and the reaction time is 4h~12h.Reaction knot
It is filtered after beam, is put into after washing in baking oven and CaSiO is obtained with the dry 6h~12h of 90 DEG C~120 DEG C of temperature3.Added by changing
The type and additive amount for adding agent may be implemented to CaSiO3The control of pattern.It is obtained when the additive of addition is CTAB
CaSiO3In fibrous structure；When the additive of addition is SDS, CaSiO obtained3In whisker structure；When the additive of addition
For NaCl or when being added without additive, CaSiO obtained3In elongated piece structure.It is chemically reacted more particularly to such as formula (6).
Ca(OH)2+Na2SiO3=CaSiO3↓+2NaOH (6)
In present embodiment step S9, step S8 can obtain the mixed solution of sodium hydroxide and sodium chloride, pass through inspissation
Crystallization obtains sodium hydroxide.Since the solubility with temperature variation of sodium chloride is little, the solubility of sodium hydroxide is bigger than sodium chloride
Very much, it and varies with temperature very big.During inspissation crystallization, sodium chloride is first crystallized out, and crystallizes out after sodium hydroxide.
Later, the sodium hydroxide return after crystallization is mentioned into silicon.
Now in conjunction with Figure of description and specific embodiment, the present invention is further described：
Embodiment 1
Embodiment 1 proposes a kind of by discarded silicon slag preparation CaSiO3Method, include the following steps：
It is S1, levigate：Discarded silicon slag group used becomes：SiO2- 65.68%, Fe2O3- 6.64%, Al2O3- 2.86%, CaO-
3.02%, MgO-2.43%, NiO-0.08%, it is discarded silicon slag is dry, broken and levigate to 200 mesh, obtain levigate silicon slag；
S2, mixing：Levigate silicon slag is uniformly mixed with sodium hydroxide, the amount that sodium hydroxide is added is that silicon is just complete in silicon slag
1.2 times of sodium hydroxide theoretical amount needed for full response obtain mixing material；
S3, roasting：Material will be mixed to be placed in Muffle furnace, in 550 DEG C of at a temperature of constant temperature calcining 120min, roasted
Material；
S4, dissolution filtering：With solid-to-liquid ratio 1:7 ratio adds water to roasting material, and is stirred dissolution, leaching temperature 80
DEG C, dissolution time 90min is filtered after dissolution, obtains sodium silicate solution and filter residue, and filter residue is spare；
S5, purification：Hydrochloric acid is added into sodium silicate solution, the pH value of sodium silicate solution is adjusted to 11, filtering removal is not
Molten object, sodium silicate solution are spare；
S6, calcining：After limestone crushing to 2cm~5cm, it is placed in Muffle furnace, in 1150 DEG C of temperature lower calcination 2h,
Obtain active calcium oxide；
S7, emulsification：It will be taken out after active calcium oxide furnace cooling, be added to the water while hot, stir while adding with heat release, and
Filtering weeds out insoluble impurity particle, and obtaining concentration is 180gL-1Calcium hydroxide emulsion；
S8, causticization：By sodium silicate solution after calcium hydroxide emulsion and purification with molar ratio 1：1 is added hydro-thermal reaction together
Kettle, and be added 5ml mass percentage be 10% CTAB solution, stir evenly, 220 DEG C at a temperature of reaction 6h after mistake
Filter, is put into baking oven after washing, obtains CaSiO in 90 DEG C of at a temperature of dry 6h3；
S9, crystallization：Mixed solution inspissation is crystallized to obtain by the mixed solution that sodium hydroxide and sodium chloride are obtained in step S8
Sodium hydroxide, return mention silicon, and obtained water continues cycling through utilization.
As shown in Figure 1, for using CaSiO made from the above method3, it is in fibrous structure.CaSiO3Fiber is as a kind of new
Type inorganic filler, the feature good with its chemical stability, high-temperature stability is good, dielectric properties are good, in papermaking, high-grade ceramic, rubber
The fields such as glue and advanced composite material (ACM) have a wide range of applications, for comparing white carbon black, CaSiO3Fiber consumption and added value are equal
Much higher than white carbon black.
Embodiment 2
Embodiment 2 proposes a kind of by discarded silicon slag preparation CaSiO3Method, include the following steps：
It is S1, levigate：Discarded silicon slag group used becomes：SiO2- 35.68%, Fe2O3- 15.64%, Al2O3- 2.86%, CaO-
5.02%, ZnO-0.85%, it is discarded silicon slag is dry, broken and levigate to 200 mesh, obtain levigate silicon slag；
S2, mixing：Levigate silicon slag is uniformly mixed with sodium hydroxide, the amount that sodium hydroxide is added is that silicon is just complete in silicon slag
1.4 times of sodium hydroxide theoretical amount needed for full response obtain mixing material；
S3, roasting：Material will be mixed to be placed in Muffle furnace, in 550 DEG C of at a temperature of constant temperature calcining 150min, roasted
Material；
S4, dissolution filtering：With solid-to-liquid ratio 1:6 ratio adds water to roasting material, and is stirred dissolution, leaching temperature 80
DEG C, dissolution time 100min is filtered after dissolution, obtains sodium silicate solution and filter residue, and filter residue is spare；
S5, purification：Hydrochloric acid is added into sodium silicate solution, the pH value of sodium silicate solution is adjusted to 11.5, filtering removal
Insoluble matter, sodium silicate solution are spare；
S6, calcining：After limestone crushing to 2cm~5cm, it is placed in Muffle furnace, in 1150 DEG C of temperature lower calcination 2h,
Obtain active calcium oxide；
S7, emulsification：It will be taken out after active calcium oxide furnace cooling, be added to the water while hot, stir while adding with heat release, and
Filtering weeds out insoluble impurity particle, and obtaining concentration is 220gL-1Calcium hydroxide emulsion；
S8, causticization：By sodium silicate solution after calcium hydroxide emulsion and purification with molar ratio 1：1 is added hydro-thermal reaction together
Kettle, and be added 5ml mass percentage be 10% SDS solution, stir evenly, 220 DEG C at a temperature of reaction 6h after filter,
It is put into baking oven after washing, obtains CaSiO in 100 DEG C of at a temperature of dry 6h3；
S9, crystallization：Mixed solution inspissation is crystallized to obtain by the mixed solution that sodium hydroxide and sodium chloride are obtained in step S8
Sodium hydroxide, return mention silicon, and obtained water continues cycling through utilization.
As shown in Fig. 2, for using CaSiO made from the above method3, it is in whisker structure.It is compared with embodiment 1, difference adds
Add the type of agent, CaSiO3The draw ratio of fiber is different.
Embodiment 3
Embodiment 3 proposes a kind of by discarded silicon slag preparation CaSiO3Method, include the following steps：
It is S1, levigate：Discarded silicon slag group used becomes：SiO2- 85.46%, Fe2O3- 2.67%, Al2O3- 5.51%, CaO-
0.93%, ZnO-1.07%, it is discarded silicon slag is dry, broken and levigate to 200 mesh, obtain levigate silicon slag；
S2, mixing：Levigate silicon slag is uniformly mixed with sodium hydroxide, the amount that sodium hydroxide is added is that silicon is just complete in silicon slag
1.0 times of sodium hydroxide theoretical amount needed for full response obtain mixing material；
S3, roasting：Material will be mixed to be placed in Muffle furnace, in 550 DEG C of at a temperature of constant temperature calcining 120min, roasted
Material；
S4, dissolution filtering：With solid-to-liquid ratio 1:8 ratio adds water to roasting material, and is stirred dissolution, leaching temperature 80
DEG C, dissolution time 120min is filtered after dissolution, obtains sodium silicate solution and filter residue, and filter residue is spare；
S5, purification：Hydrochloric acid is added into sodium silicate solution, the pH value of sodium silicate solution is adjusted to 11.5, filtering removal
Insoluble matter, sodium silicate solution are spare；
S6, calcining：After limestone crushing to 2cm~5cm, it is placed in Muffle furnace, in 1150 DEG C of temperature lower calcination 2h,
Obtain active calcium oxide；
S7, emulsification：It will be taken out after active calcium oxide furnace cooling, be added to the water while hot, stir while adding with heat release, and
Filtering weeds out insoluble impurity particle, and obtaining concentration is 140gL-1Calcium hydroxide emulsion；
S8, causticization：By sodium silicate solution after calcium hydroxide emulsion and purification with molar ratio 1.05：1 together be added hydro-thermal it is anti-
Answer kettle, and be added 5ml mass percentage be 10% NaCl solution, stir evenly, 200 DEG C at a temperature of reaction 8h after mistake
Filter, is put into baking oven after washing, obtains CaSiO in 120 DEG C of at a temperature of dry 8h3；
S9, crystallization：Mixed solution inspissation is crystallized to obtain by the mixed solution that sodium hydroxide and sodium chloride are obtained in step S8
Sodium hydroxide, return mention silicon, and obtained water continues cycling through utilization.
As shown in figure 3, for using CaSiO made from the above method3, it is in elongated piece structure.Needle-shaped CaSiO3, because of its change
The feature that stability is good, high-temperature stability is good, dielectric properties are good is learned, in papermaking, high-grade ceramic, rubber and advanced composite material (ACM) etc.
Field has a wide range of applications, only papermaking one, and annual requirement is i.e. up to only 40,000,000 tons, and price and added value are higher.This
Invent it is with the obvious advantage, for metallurgy industry discard silicon slag recycling and innoxious use provide an approach.
Embodiment 4
Embodiment 4 proposes a kind of by discarded silicon slag preparation CaSiO3Method, include the following steps：
It is S1, levigate：Discarded silicon slag group used becomes：SiO2- 71.64%, Fe2O3- 9.84%, Al2O3- 5.02%, CaO-
0.93%, MgO-1.61%, NiO-0.08%, it is discarded silicon slag is dry, broken and levigate to 200 mesh, obtain levigate silicon slag；
S2, mixing：Levigate silicon slag is uniformly mixed with sodium hydroxide, the amount that sodium hydroxide is added is that silicon is just complete in silicon slag
1.1 times of sodium hydroxide theoretical amount needed for full response obtain mixing material；
S3, roasting：Material will be mixed to be placed in Muffle furnace, in 450 DEG C of at a temperature of constant temperature calcining 90min, roasted
Material；
S4, dissolution filtering：With solid-to-liquid ratio 1:5 ratio adds water to roasting material, and is stirred dissolution, leaching temperature 80
DEG C, dissolution time 90min is filtered after dissolution, obtains sodium silicate solution and filter residue, and filter residue is spare；
S5, purification：Hydrochloric acid is added into sodium silicate solution, the pH value of sodium silicate solution is adjusted to 11, filtering removal is not
Molten object, sodium silicate solution are spare；
S6, calcining：After limestone crushing to 2cm~5cm, it is placed in Muffle furnace, in 1150 DEG C of temperature lower calcination 2h,
Obtain active calcium oxide；
S7, emulsification：It will be taken out after active calcium oxide furnace cooling, be added to the water while hot, stir while adding with heat release, and
Filtering weeds out insoluble impurity particle, and obtaining concentration is 140gL-1Calcium hydroxide emulsion；
S8, causticization：By sodium silicate solution after calcium hydroxide emulsion and purification with molar ratio 1.05：1 together be added hydro-thermal it is anti-
Answer in kettle and stir evenly, 220 DEG C at a temperature of reaction 6h after filter, be put into baking oven after washing, 90 DEG C at a temperature of it is dry
Dry 6h obtains CaSiO3；
S9, crystallization：Mixed solution inspissation is crystallized to obtain by the mixed solution that sodium hydroxide and sodium chloride are obtained in step S8
Sodium hydroxide, return mention silicon, and obtained water continues cycling through utilization.
Using CaSiO made from the above method3, it is the CaSiO that sodium chloride solution obtains with additive3Pattern is identical, is in needle
Shape grain structure.Because the amount for the sodium chloride that hydrochloric acid is reacted with excessive sodium hydrate, makes CaSiO enough3Pattern
For acicular texture.
Method provided by the invention, using hydrothermal synthesis technology, is heavy with calcium hydroxide emulsion using discarded silicon slag as raw material
Shallow lake agent prepares CaSiO3.By to reaction temperature, material proportion, the reaction time, reactant concentration, whether be added additive and
The type of additive and the control of additive amount are realized to CaSiO3The control of pattern.
Meanwhile discarded silicon slag is from the mineral acidleach such as zinc oxide ore, lateritic nickel ore, flyash, boron magnesium ore, cupric oxide ore
Slag, ammonia leaching residue and sulfuric acid, ammonium hydrogen sulfate roasting dissolution slag, improve the greenization added value of above-mentioned resource.
The technical principle of the invention is described above in combination with a specific embodiment, these descriptions are intended merely to explain of the invention
Principle shall not be construed in any way as a limitation of the scope of protection of the invention.Based on explaining herein, those skilled in the art
It can associate with other specific embodiments of the invention without creative labor, these modes fall within this hair
Within bright protection scope.
Claims (10)
1. a kind of prepare CaSiO by discarded silicon slag3Method, which is characterized in that include the following steps：
It is S1, levigate：It is discarded silicon slag is dry, broken and levigate, obtain levigate silicon slag；
S2, mixing：The levigate silicon slag is uniformly mixed with sodium hydroxide, obtains mixing material；
S3, roasting：The material that is mixed is roasted, roasting material is obtained；
S4, dissolution filtering：The roasting material is added into water, and is stirred dissolution, filters, obtains sodium silicate solution；
S5, purification：Adjust the pH value of the sodium silicate solution；
S6, calcining：It will be calcined after limestone crushing, obtain active calcium oxide；
S7, emulsification：The active calcium oxide is added to the water, is stirred while adding, and filters and weeds out insoluble impurity particle, is obtained
Calcium hydroxide emulsion；
S8, causticization：By the calcium hydroxide emulsion and the sodium silicate solution with molar ratio together with hydrothermal reaction kettle is added, stir
Uniformly react it, it is described to filter after reaction, it is placed in oven and dried to obtain CaSiO after washing3；
S9, crystallization：Mixed solution is obtained in the step S8, crystallizes the mixed solution inspissation to obtain sodium hydroxide, is returned
Silicon is mentioned, obtained water continues cycling through utilization.
2. according to claim 1 prepare CaSiO by discarded silicon slag3Method, which is characterized in that in the step S2,
The dosage of sodium hydroxide is silicon reacts required sodium hydroxide theoretical amount completely just in levigate silicon slag 1.0 times~1.6 times.
3. according to claim 1 prepare CaSiO by discarded silicon slag3Method, which is characterized in that in the step S3,
The temperature of roasting is 300 DEG C~550 DEG C, and the constant temperature time of roasting is 50min~250min.
4. according to claim 1 prepare CaSiO by discarded silicon slag3Method, which is characterized in that in the step S4,
The solid-liquid mass ratio for roasting material and water is 1:2~1:10, the temperature of stirring is 60 DEG C~90 DEG C, and the time of stirring is 60min
~150min.
5. according to claim 1 prepare CaSiO by discarded silicon slag3Method, which is characterized in that in the step S5,
Hydrochloric acid is selected to adjust the pH value of sodium silicate solution, pH value is 11~11.5.
6. according to claim 1 prepare CaSiO by discarded silicon slag3Method, which is characterized in that in the step S7,
The concentration of calcium hydroxide emulsion is 120gL-1~260gL-1。
7. according to claim 1 prepare CaSiO by discarded silicon slag3Method, which is characterized in that in the step S8,
Molar ratio is 0.9：1~1.3：1.
8. according to any one of claims 1 to 7 prepare CaSiO by discarded silicon slag3Method, which is characterized in that described
In step S8, the additive that mass percentage is 10% is added simultaneously into the hydrothermal reaction kettle.
9. according to claim 8 prepare CaSiO by discarded silicon slag3Method, which is characterized in that the additive be ten
One of six alkyl trimethyl ammonium bromides, lauryl sodium sulfate and sodium chloride.
10. according to claim 9 prepare CaSiO by discarded silicon slag3Method, which is characterized in that in the step S8
In, the temperature reacted in hydrothermal reaction kettle is 180 DEG C~240 DEG C, and the time of reaction is 4h~12h, is dried in an oven
Temperature is 90 DEG C~120 DEG C, and the dry time is 6h~12h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810886294.0A CN108821300B (en) | 2018-08-06 | 2018-08-06 | Preparation of CaSiO from waste silicon slag3Method (2) |
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| CN112591757A (en) * | 2021-01-04 | 2021-04-02 | 南京工大环境科技有限公司 | Method for preparing white carbon black and sponge copper from organic silicon slurry residues |
| CN114524408A (en) * | 2022-02-14 | 2022-05-24 | 浙江大学 | Environment-friendly comprehensive recycling method of organic silicon pulp residues |
| CN114849673A (en) * | 2022-05-31 | 2022-08-05 | 浙江皇马科技股份有限公司 | Method for preparing magnesium silicate adsorbent with high specific surface area |
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| CN112591757A (en) * | 2021-01-04 | 2021-04-02 | 南京工大环境科技有限公司 | Method for preparing white carbon black and sponge copper from organic silicon slurry residues |
| CN114524408A (en) * | 2022-02-14 | 2022-05-24 | 浙江大学 | Environment-friendly comprehensive recycling method of organic silicon pulp residues |
| CN114849673A (en) * | 2022-05-31 | 2022-08-05 | 浙江皇马科技股份有限公司 | Method for preparing magnesium silicate adsorbent with high specific surface area |
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| CN116376368A (en) * | 2023-04-23 | 2023-07-04 | 刘闽瑶 | Micro-excitation low-carbon energy-saving coating and preparation method thereof |
| CN116376368B (en) * | 2023-04-23 | 2024-01-26 | 刘闽瑶 | Micro-excitation low-carbon energy-saving coating and preparation method thereof |
| CN117466305A (en) * | 2023-12-07 | 2024-01-30 | 广州瑞云材料科技有限公司 | Calcium silicate with friction cleaning performance and preparation method thereof |
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