CN109110771A - A method of waterglass is prepared using catalytic gasification lime-ash - Google Patents
A method of waterglass is prepared using catalytic gasification lime-ash Download PDFInfo
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- CN109110771A CN109110771A CN201811062977.0A CN201811062977A CN109110771A CN 109110771 A CN109110771 A CN 109110771A CN 201811062977 A CN201811062977 A CN 201811062977A CN 109110771 A CN109110771 A CN 109110771A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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Abstract
The present invention relates to a kind of method for preparing waterglass using catalytic gasification lime-ash, this method, through acid dissolution, removes wherein most Al using catalytic gasification lime-ash as raw material2O3、Fe2O3Impurity, and to thick SiO2Product is separated by solid-liquid separation, then obtains pure SiO after washed, drying2, it is reacted under the conditions of atmospheric low-temperature with NaOH finally and prepares water glass solution.The present invention is by preparing waterglass using catalytic gasification ash, alleviate the long-term accumulation bring environmental problem of gasification ash, simultaneously, utilize the higher feature of catalytic gasification ash reactivity, the larger step of the energy consumptions such as calcination activation and pressurised extraction is omitted, compared with the preparation for completing waterglass under temperate condition, the preparation cost of waterglass is reduced, economic benefit is improved.
Description
Technical field
The invention belongs to solid waste resource recoveries during coal utilization to utilize field, utilize catalysis what is involved is a kind of
The method that gasification lime-ash prepares waterglass.
Background technique
With flourishing for coal chemical industry, leading technology of the coal gasification as coal chemical industry is had received widespread attention.Gas
Solid waste of the ashing slag as Coal Gasification, yield increase year by year.The lime-ash that gasifies is coal in high temperature weakly reducing atmosphere
Remaining solid matter after lower sufficiently reaction, accounts for 20% or so of gasified raw material coal, main component is SiO2、Al2O3.This
Outside, also contain part Fe2O3、TiO2、CaO、MgO、Na2O、K2O、SO3、P2O5Deng.
For a long time, air storage is the major way of processing gasification lime-ash.The method occupies a large amount of arable lands, and in lime-ash
It containing heavy metal and acidic materials, through chronic sun exposure, wind, drenches with rain, easily forms acid water and overflow and permeated with heavy metal ion, made
At the serious pollution of soil, water body.
Currently, the comprehensive utilization of lime-ash is concentrated mainly on construction material, roadbed material etc., but these still fall within it is extensive
The Land use systems of type and equally exist heavy metal infiltration, to cause the risk of secondary pollution to soil, water body.
Waterglass is commonly called as sodium silicate, molecular formula Na2O·mSiO2, wherein m is the modulus of waterglass, is a kind of solvable
The silicate of property, is made of the silica and alkali metal of different proportion.It is adopted in industry in order to prepare the higher waterglass of modulus more
It is calcined at a high temperature of 1300-1400 DEG C with silica flour and soda ash, then waterglass is produced in dissolution in high-temperature high pressure water.Waterglass
Modulus value is bigger, and viscosity is higher, and solvability in water is lower.When modulus is greater than 3.0, can only be dissolved in hot water, to making
With making troubles；Modulus, which is dissolved in water again for the waterglass of 2.6-2.8, higher intensity, under construction for manufacturing fast solid carbon dioxide
Mud, rapid hardening waterproofing agent, acid-resisting concrete, heat-resisting gelling etc.；And the waterglass of modulus 2.0 or so is easy to control during the reaction
System, for manufacturing white carbon black, zeolite molecular sieve, washing powder, soap, dyeing auxiliaries, bleaching agent etc. in chemical production.
The one kind of catalytic gasification lime-ash as gasification lime-ash.Due to joined catalyst in coal, during catalytic gasification, urge
Agent can with siliceous mineral qualitative response in coal and activate, cause in catalytic gasification lime-ash containing a large amount of high activities, be easily recycled
SiO2, raw material of industry waterglass is prepared by its high efficiency extraction and in a mild condition, environmental problem can be alleviated, make full use of money
Source, and the preparation cost of waterglass can be reduced, it increases economic efficiency.Therefore, waterglass is prepared using catalytic gasification lime-ash as raw material
It has important practical significance.Being not found through retrieval using catalytic gasification lime-ash is that raw material prepares the existing of raw material of industry waterglass
Technology.
Summary of the invention
It using catalytic gasification lime-ash is raw material that the present invention, which provides a kind of, and the method for waterglass is prepared under the conditions of atmospheric low-temperature.
Technical solution of the present invention includes that acid reacts at low temperature with catalytic gasification ash, makes most of minerals in coal
Al2O3、Fe2O3Deng dissolution, recycle caustic alkali under the conditions of atmospheric low-temperature with SiO in acid leaching residue2Reaction, to prepare water glass
Glass.Since catalytic gasification ash is relative to gangue or combustion ash, have the characteristics that more high reaction activity, roasting can be saved and lived
The larger step of energy consumptions such as change and pressurised extraction, greatly reduces the preparation cost of waterglass, provides for the production of waterglass
New method.
The technical solution adopted by the present invention are as follows:
(1) the catalytic gasification lime-ash of coal is added in the acid that concentration is 0.2-8 mol/L and is stirred, in 30-90 DEG C of dissolution 0.2-4
H reacts it sufficiently；
(2) solution after above-mentioned reaction is separated by solid-liquid separation, to solid matter wash, and by the solid matter after washing in
Dry 0.5-10 h, obtains catalytic gasification acid sludge at 30-200 DEG C；
(3) NaOH aqueous solution is carried out reacting 30-200 min at 40-98 DEG C with catalytic gasification acid sludge, after cooling, filtering
To water glass solution.
The catalytic gasification lime-ash of coal as described above is that the coal of supported catalyst is carried out gasification reaction to obtain, wherein coal
Catalyst mode of loading is mainly mechanical mixing, infusion process and ultrasonic immersing method.
The mechanical mixing the following steps are included:
Coal is ground, it is dry after mixed with a certain amount of catalyst, and this mixture is ground, obtains mechanical mixture
Method prepares the coal of supported catalyst.
The infusion process the following steps are included:
Catalyst is dissolved into the water, catalyst aqueous solution is formed, then this solution is mixed and is sufficiently stirred with coal dust, is made
Catalyst is impregnated into coal.Dry 2-12 h, obtains under the conditions of the coal slurry after this impregnation catalyst agent is finally placed in 50-150 DEG C
The coal of supported catalyst.
The ultrasonic immersing method the following steps are included:
Catalyst is put into aqueous solution, and places it in supersonic generator and makes it completely dissolved, it is water-soluble to obtain catalyst
Then this solution is poured into coal and is stirred, while is placed in supersonic generator by liquid, keep dipping of the catalyst in coal more equal
It is even.Dry 2-12 h, obtains the coal of supported catalyst under the conditions of the coal slurry after this impregnation catalyst agent is finally placed in 50-150 DEG C.
The catalyst is Na2SO4、K2SO4、K2CO3、Na2CO3, it is one or more of in CaO.The load capacity of catalyst is 1
Kg coal loads 0.5-4.0 mol catalyst.
The acid being added in catalytic gasification lime-ash as described above is that hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, acetic acid are one such
Or it is several.The concentration of acid solution is 0.2-8.0 mol/L, and the volume of acid solution and the weight ratio of catalytic gasification lime-ash are 5-50
ml/g。
The NaOH solution concentration of step (3) as described above is 0.2-1.4 mol/L, NaOH solution volume and catalytic gasification acid
The mass ratio of slag is 1-50 mL/g.
The invention has the following advantages over the prior art:
1. catalytic gasification ash used in the present invention is compared with preparing the common quartz of waterglass, gangue or power plant combustion ash
Have the characteristics that reactivity is high, it is living to be not required to carry out it reaction that calcination activation can reach after gangue or combustion ash activation
Property, save the energy consumption of calcination activation process；
2. present invention reaction temperature in waterglass preparation process is lower, the system of waterglass can be completed at 100 DEG C or less
It is standby, waterglass is prepared at 1300-1400 DEG C compared to quartz and soda ash, largely reduces reaction process energy consumption；
3. present invention reaction pressure during preparing waterglass is normal pressure, adding compared to combustion ash or gangue needs
The higher waterglass of modulus can be just obtained in pressure ring border, reduce equipment investment cost, while avoiding operational danger；
4. the present invention is in waterglass preparation process, the NaOH solution concentration used is relatively low, and NaOH solution and catalysis gas
The liquid-solid ratio for changing acid sludge is relatively small, prepares waterglass compared to using gangue or power plant combustion ash as raw material, is greatly saved
The usage amount of NaOH；
5. modulus of water glass prepared by the present invention is higher, and is reacted with NaOH and can once reach 2.0 or so, compared to combustion
Ashing or gangue need and NaOH solution is through multiple circular response, reduces process complexity.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail, but invention protection scope is not limited in described
Hold.
Embodiment 1
1) use mechanical mixing by raw coal (ash component analysis is shown in Table 1) and catalyst K2CO3By 2.0 mol catalyst/kg coal
It is loaded, then it is gasified to obtain catalytic gasification ash；
2) acetic acid and catalytic gasification ash that concentration is 8 mol/L carry out acidleach with the ratio of 30.0 mL/g of liquid-solid ratio at 60 DEG C
3 h are reacted, catalytic gasification acid sludge is then obtained after separation of solid and liquid, washing, drying and other steps；
3) concentration is 0.50 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 30.0 mL/g at 98 DEG C
120 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
Embodiment 2
1) use mechanical mixing by raw coal (coal same as Example 1) and catalyst K2CO3By 2.5 mol catalyst/kg
Coal is loaded, and is then gasified to obtain catalytic gasification ash to it；
2) concentration is 0.2 mol/L oxalic acid/sulfuric acid/mixed in hydrochloric acid sour (molar ratio 2:3:3) and catalytic gasification ash with liquid-solid ratio
The ratio of 50.0 mL/g carries out 1 h of acid-leaching reaction at 90 DEG C, is then urged after separation of solid and liquid, washing, drying and other steps
Change gasification acid sludge；
3) concentration is 0.44 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 25.0 ml/g at 90 DEG C
30 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
Embodiment 3
1) use mechanical mixing by raw coal (coal same as Example 1) and catalyst n a2CO3/ CaO(molar ratio 3:1) into
Row mixing, raw coal are loaded by 4.0 mol catalyst/kg coal with catalyst, are then gasified to obtain catalytic gasification to it
Ash；
2) to carry out acidleach at 50 DEG C with the ratio of 20 mL/g of liquid-solid ratio anti-for the oxalic acid and catalytic gasification ash that concentration is 7 mol/L
2 h are answered, catalytic gasification acid sludge is then obtained after separation of solid and liquid, washing, drying and other steps；
3) concentration is 0.88 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 12.5 ml/g at 90 DEG C
180 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
Embodiment 4
1) use infusion process by raw coal (coal same as Example 1) and catalyst K2CO3/ CaO(molar ratio 2:1) it is mixed
It closes, raw coal is loaded with catalyst by 3.0 mol catalyst/kg coal, is then gasified to obtain catalytic gasification ash to it；
2) sulfuric acid and oxalic acid mixed acid (molar ratio 2:1) and catalytic gasification ash that concentration is 3 mol/L are with 15.0 mL/g of liquid-solid ratio
Ratio 4 h of acid-leaching reaction is carried out at 70 DEG C, then obtained after separation of solid and liquid, washing, drying and other steps catalytic gasification acid
Slag；
3) concentration is 0.55 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 20.0 ml/g at 90 DEG C
90 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
Embodiment 5
1) use infusion process by raw coal (coal same as Example 1) and catalyst n a2CO3/ K2CO3(molar ratio 1:1) presses 0.5
Mol catalyst/kg coal is loaded, and is then gasified to obtain catalytic gasification ash to it；
2) sulfuric acid that concentration is 1 mol/L and hydrochloric acid (molar ratio 1:1) mixed acid and catalytic gasification ash are with liquid-solid ratio for 35 mL/g
Ratio 0.2 h of acid-leaching reaction is carried out at 80 DEG C, then obtain catalytic gasification after separation of solid and liquid, washing, drying and other steps
Acid sludge；
3) concentration is 0.20 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 50.0 ml/g at 90 DEG C
200 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
Embodiment 6
1) use infusion process by raw coal (coal same as Example 1) and catalyst n a2CO3/ K2SO4(molar ratio 1:1) presses 1.0
Mol catalyst/kg coal is loaded, and is then gasified to obtain catalytic gasification ash to it；
2) hydrochloric acid and acetic acid (molar ratio 2:1) mixed acid and catalytic gasification ash that concentration is 6 mol/L are with 25.0 mL/g of liquid-solid ratio
Ratio 3 h of acid-leaching reaction is carried out at 30 DEG C, then obtained after separation of solid and liquid, washing, drying and other steps catalytic gasification acid
Slag；
3) concentration is 1.10 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 10.0 ml/g at 60 DEG C
60 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
Embodiment 7
1) use ultrasonic immersing method by raw coal (coal same as Example 1) and catalyst n a2SO4/ K2SO4(molar ratio 1:1)
It is loaded by 2.5 mol catalyst/kg coal, then it is gasified to obtain catalytic gasification ash；
2) hydrochloric acid and catalytic gasification ash that concentration is 5 mol/L carry out acid-leaching reaction with the ratio of 5 mL/g of liquid-solid ratio at 70 DEG C
Then 4 h obtain catalytic gasification acid sludge after separation of solid and liquid, washing, drying and other steps；
3) concentration is 1.40 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 1.0 ml/g at 40 DEG C
150 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
Embodiment 8
1) use ultrasonic immersing method by raw coal (coal same as Example 1) and catalyst n a2SO4By 1.5 mol catalyst/kg
Coal is loaded, and is then gasified to obtain catalytic gasification ash to it；
2) sulfuric acid and nitric acid (molar ratio 3:1) mixed acid and catalytic gasification ash that concentration is 4 mol/L are with 10 mL/g's of liquid-solid ratio
Ratio carries out 4 h of acid-leaching reaction at 50 DEG C, and catalytic gasification acid sludge is then obtained after separation of solid and liquid, washing, drying and other steps；
3) concentration is 0.40 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 40.0 mL/g at 95 DEG C
100 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
Embodiment 9
1) use ultrasonic immersing method by raw coal (coal same as Example 1) and catalyst K2SO4By 3.5 mol catalyst/kg
Coal is loaded, and is then gasified to obtain catalytic gasification ash to it；
2) sulfuric acid and acetic acid (molar ratio 2:1) mixed acid and catalytic gasification ash that concentration is 6 mol/L are with 8 mL/g's of liquid-solid ratio
Ratio carries out 3 h of acid-leaching reaction at 40 DEG C, and catalytic gasification acid sludge is then obtained after separation of solid and liquid, washing, drying and other steps；
3) concentration is 1.40 mol/L NaOH solution and catalytic gasification acid sludge are with ratio that liquid-solid ratio is 5.0 ml/g at 75 DEG C
130 min of lower reaction obtain water glass solution after cooling, filtering.
To SiO in catalytic gasification acid sludge ingredient2Content is measured using Silicon Molybdenum Blue Spectrophotometry, SiO2Extraction rate
And the measurement of modulus of water glass is according to the method in national standard GB/T 4209-2008.SiO in acid sludge2Content, SiO2Recovery rate,
Modulus of water glass is shown in Table 2.
The ash component of 1 raw coal of table is analyzed
SiO under 2 different condition of table in embodiment2Content, extraction rate and modulus of water glass
Claims (8)
1. a kind of method for preparing waterglass using catalytic gasification lime-ash, it is characterised in that the following steps are included:
(1) the catalytic gasification lime-ash of coal is added in the acid that concentration is 0.2-8 mol/L and is stirred, in 30-90 DEG C of dissolution 0.2-4
H reacts it sufficiently；
(2) solution after above-mentioned reaction is separated by solid-liquid separation, to solid matter wash, and by the solid matter after washing in
Dry 0.5-10 h, obtains catalytic gasification acid sludge at 30-200 DEG C；
(3) NaOH aqueous solution is carried out reacting 30-200 min at 40-98 DEG C with catalytic gasification acid sludge, after cooling, filtering
To water glass solution.
2. a kind of method for preparing waterglass using catalytic gasification lime-ash as described in claim 1, it is characterised in that the coal
Catalytic gasification lime-ash be that the coal of supported catalyst is carried out gasification reaction to obtain, wherein the catalyst mode of loading of coal is machine
Tool mixing method, infusion process and ultrasonic immersing method.
3. a kind of method for preparing waterglass using catalytic gasification lime-ash as claimed in claim 2, it is characterised in that the machine
Tool mixing method the following steps are included:
Coal is ground, it is dry after mixed with a certain amount of catalyst, and this mixture is ground, obtains mechanical mixture
Method prepares the coal of supported catalyst.
4. a kind of method for preparing waterglass using catalytic gasification lime-ash as claimed in claim 2, it is characterised in that the leaching
Stain method the following steps are included:
Catalyst is dissolved into the water, catalyst aqueous solution is formed, then this solution is mixed and is sufficiently stirred with coal dust, is made
Catalyst is impregnated into coal, and dry 2-12 h, obtains under the conditions of the coal slurry after this impregnation catalyst agent is finally placed in 50-150 DEG C
The coal of supported catalyst.
5. a kind of method for preparing waterglass using catalytic gasification lime-ash as claimed in claim 2, it is characterised in that described super
Sound infusion process the following steps are included:
Catalyst is put into aqueous solution, and places it in supersonic generator and makes it completely dissolved, it is water-soluble to obtain catalyst
Then this solution is poured into coal and is stirred, while is placed in supersonic generator by liquid, keep dipping of the catalyst in coal more equal
It is even,
Dry 2-12 h, obtains supported catalyst under the conditions of the coal slurry after this impregnation catalyst agent is finally placed in 50-150 DEG C
Coal.
6. a kind of method for preparing waterglass using catalytic gasification lime-ash as claimed in claim 2, it is characterised in that
The catalyst is Na2SO4、K2SO4、K2CO3、Na2CO3, it is one or more of in CaO, the load capacity of catalyst is 1 kg coal
Load 0.5-4.0 mol catalyst.
7. a kind of method for preparing waterglass using catalytic gasification lime-ash as described in claim 1, it is characterised in that described
The acid being added in catalytic gasification lime-ash is one or more of hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, acetic acid, and the concentration of acid solution is
0.2-8.0 mol/L, the volume of acid solution and the weight ratio of catalytic gasification lime-ash are 5-50 ml/g.
8. a kind of method for preparing waterglass using catalytic gasification lime-ash as described in claim 1, it is characterised in that the step
Suddenly (3) NaOH solution concentration is 0.2-1.4 mol/L, and NaOH solution volume and the mass ratio of catalytic gasification acid sludge are 1-50 mL:
1g。
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Cited By (1)
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| CN112408407A (en) * | 2020-12-04 | 2021-02-26 | 鞍钢集团矿业有限公司 | Method for preparing high-modulus water glass by using iron tailings |
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| CN101259965A (en) * | 2008-01-11 | 2008-09-10 | 邱家俊 | Method for preparing soluble glass from coal gangue |
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Application publication date: 20190101 |