CN107840342A - Utilize the method for the direct synthetic calcium silicate of soda lime sintering process red mud - Google Patents
Utilize the method for the direct synthetic calcium silicate of soda lime sintering process red mud Download PDFInfo
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- CN107840342A CN107840342A CN201711229229.2A CN201711229229A CN107840342A CN 107840342 A CN107840342 A CN 107840342A CN 201711229229 A CN201711229229 A CN 201711229229A CN 107840342 A CN107840342 A CN 107840342A
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- calcium silicate
- red mud
- soda lime
- sintering process
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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
- C01B33/24—Alkaline-earth metal silicates
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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
- C01P2006/10—Solid density
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- Silicates, Zeolites, And Molecular Sieves (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a kind of method using the direct synthetic calcium silicate of soda lime sintering process red mud, belong to field of heat insulating materials.Method comprises the following steps：S1, raw material slurry preparation：Soda lime sintering process red mud and silica and water are pressed into liquid-solid ratio 10 30:1 mixed preparing raw material is starched, wherein, calcium silicon mol ratio is 0.83 1 in the raw material slurry after preparation:1；S2, hydrothermal synthesis method prepare calcium silicate material slurry：Step S1 raw material is starched into 180 300 DEG C of 20h of stirring reaction 6 in confined conditions, obtains calcium silicate material slurry；S3, calcium silicate powder material synthesis：The step S2 calcium silicate material slurries obtained are cooled down at room temperature, solid product and water are obtained by separating, then the solid product after separation is dried and removes moisture removal, obtains tobermorite or/and eakleite.The present invention is simple to operate, and process is few, and cost is low, and preparation efficiency is high, realizes the high value added utilization of waste material.
Description
Technical field
The invention belongs to field of heat insulating materials, is related to a kind of side using the direct synthetic calcium silicate of soda lime sintering process red mud
Method.
Background technology
Calcium silicates class material is using tobermorite, eakleite, wollastonite as the material that mainly forms, because with special
Physicochemical property and be widely used, be mainly used in the insulation of the heating and ventilating equipments such as metallurgy, building materials, weaving, power system and pipeline,
And the field such as ship heat-insulation and heat-preservation.
Calcium silicate hydrate crystalline articles include two kinds：One kind is tobermorite type, is called tobermorite (5CaO
6SiO2·5H2O), maximum operation (service) temperature is 650 DEG C, typically using static hydrothermal synthesis；Another kind is eakleite (6CaO
6SiO2·H2O) type, temperature in use can reach 1000 DEG C, typically using dynamic autoclaved technology.Influence eakleite technology of preparing
Key factor is feedstock property, which determine the solubility of original components, influences CaO-SiO2-H2The reaction of O hydro-thermal reaction systems
Course and product, therefore select excellent siliceous raw material, calcareous raw material, additive particularly important.Conventionally produced calcium silicates
Class material, its siliceous raw material are usually that industrial waterglass is generated under melting condition using diatomite or quartz sand and alkali,
In the preparation process of raw material, it is necessary to using the high-quality silicon ore such as a large amount of quartz sands, diatomite and soda ash or sodium sulphate in fusing kiln
Congruent melting in stove, then it is made after cooling crush dissolving, so that the selection of siliceous raw material needs to exploit and consume quartz and silicon
A large amount of non-renewable silicon mineral resources such as diatomaceous earth, while calcareous raw material is in addition to carbide slag, can also lime stone coke or
The independent lime calcining of the high-grade fuels such as anthracite and refined lime breast, energy consumption and cost are big, resource and environment are influenceed big.
With the development of aluminum i ndustry and the reduction of bauxitic ore grade, red mud yield will be increasing.From 2009 with
Come, about 60,000,000 tons of red mud is discharged in the whole world every year.China discharges red mud more than 30,000,000 tons every year, and accumulation red mud storage is high
Up to 200,000,000 tons.At present either box dam stockpiling, fill out sea can not all solve red mud harm problem.Contain substantial amounts of calcium oxide in red mud
And silica, but be not utilized effectively so far, cause the secondary waste of renewable resource.Therefore, in land resource increasingly
Nervous, environmental protection is paid attention to increasingly, especially today in recycling economy sustainable development, and red mud pollution has turned into the comprehensive regulation
One of people's focus of interest, the research comprehensively utilized to red mud also into it is extremely urgent the problem of.At present, it is also not public
Open a kind of method that the direct synthetic calcium silicate of soda lime sintering process red mud is utilized using soda lime sintering process red mud.
Therefore, being badly in need of one kind can utilize soda lime sintering process red mud directly to synthesize silicon using soda lime sintering process red mud
The method of sour calcium, to solve the problems, such as that current soda lime sintering process red mud storage is big, it is wide to take up an area, pollution is heavy and it is difficult to handle, simultaneously
A kind of new raw material is searched out for the preparation of calcium silicate material, realizes the high value added utilization of waste material.
The content of the invention
(1) technical problems to be solved
In order to solve the above mentioned problem of prior art, the present invention is provided one kind and directly synthesized using soda lime sintering process red mud
The method of calcium silicates, this method can effectively utilize the valuable constituent in soda lime sintering process red mud, be the system of calcium silicate material
It is standby to have found new raw material and method, while solve that current soda lime sintering process red mud storage is big, it is wide to take up an area, pollution weight and processing
The problem of difficult, realize the high value added utilization of waste material.
(2) technical scheme
In order to achieve the above object, the main technical schemes that the present invention uses include：
A kind of method using the direct synthetic calcium silicate of soda lime sintering process red mud, comprise the following steps：
S1, raw material slurry preparation：Soda lime sintering process red mud and silica and water are pressed into liquid-solid ratio 10-30:1 mixing is matched somebody with somebody
Raw material slurry processed, wherein, calcium silicon mol ratio is 0.83-1 in the raw material slurry after preparation:1；
S2, hydrothermal synthesis method prepare calcium silicate material slurry：By step S1 180-300 DEG C in confined conditions of raw material slurry
Stirring reaction 6-20h, obtain calcium silicate material slurry；
S3, calcium silicate powder material synthesis：The step S2 calcium silicate material slurries obtained are cooled down at room temperature,
Obtain solid product and water by separating, then the solid product after separation dried and removes moisture removal, obtain tobermorite or/and
Eakleite.
According to the present invention, the mixing speed of the step S2 is 150-300r/min.
According to the present invention, when silico-calcium mol ratio is 0.83-0.91:1st, liquid-solid ratio 15-20:1st, reaction temperature 180-
250 DEG C, the reaction time be 8-18h and when mixing speed is 200-300r/min, synthesize tobermorite；
When silico-calcium mol ratio is 0.93-1:1st, liquid-solid ratio 10-30:1st, reaction temperature be 200-250 DEG C, the reaction time be
When 8-16h and mixing speed are 150-300r/min, synthesize eakleite；
When silico-calcium mol ratio is 0.85-0.93:1st, liquid-solid ratio 22-28:1st, reaction temperature be 200-300 DEG C, reaction when
Between be 6-18h and when mixing speed is 180-280r/min, synthesize eakleite and tobermorite.
According to the present invention, in the step S2, the raw material slurry uses oil bath heating mode, salt bath heating mode and electricity
Any of mode of heating controlling reaction temperature.
According to the present invention, the drying temperature of the step S3 is 90-180 DEG C.
(3) beneficial effect
On the premise of additive and other material compositions is not added, the present invention is only with soda lime sintering process red mud, two
Three kinds of raw materials of silica and water, cooled down, be separated by filtration and back tender by simple mixed material, a step Hydrothermal Synthesiss, room temperature
Sequence, with regard to that can prepare calcium silicate material product, method of the invention is simple to operate, and preparation section is few, and production efficiency is high, is produced into
This low, valuable constituent calcium oxide and silica being effectively utilized in soda lime sintering process red mud, it is the preparation of calcium silicate material
New raw material and method are have found, while solves that current soda lime sintering hair red mud storage is big, takes up an area wide, pollution weight and processing
The problem of difficult, realize the high value added utilization of waste material, energy-conserving and environment-protective.
Flow is simple in whole building-up process, and no discarded object and pollutant produce, low for equipment requirements, easily realize industry
Change；In building-up process, by adjusting process parameter, the calcium silicate products that can obtain different crystal forms and physicochemical property (avenges silico-calcium
Stone or/and eakleite).
Embodiment
In order to preferably explain the present invention, in order to understand, below by embodiment, present invention work is retouched in detail
State.
Embodiment 1
S1, raw material slurry preparation：Soda lime sintering process red mud is mixed with silica and distilled water, stir preparation
Go out raw material slurry, wherein, in mixed raw material slurry, calcium silicon mol ratio Ca/Si is 0.83:1, the liquid-solid ratio L/S during raw material is starched are
20:1；
S2, hydrothermal synthesis method prepare calcium silicate material slurry：Raw material slurry is placed in closed reactor, and is placed on 180
DEG C oil bath pan in heat 8h (oil bath temperature heats 8h after reaching 180 DEG C), while with 300r/min speed in heating process
Degree is stirred, and hydro-thermal reaction makes it generate tobermorite slurry；
Herein, raw material slurry is contained primarily to providing a kind of confined reaction condition, certainly also using closed reactor
Other closed measures can be taken.
Oil bath heating mode can be substituted for salt bath heating or Electric heating, as long as disclosure satisfy that uniform heating, realize
Accurate controlling reaction temperature.
S3, calcium silicate powder material synthesis：Reacted tobermorite slurry is cooled down under room temperature (about 25 DEG C), led to
Cross separation and obtain solid product and water, then the tobermorite after separation is dried at 120 DEG C and removes moisture removal, produces solid-state
Tobermorite product (is shown in Table 1).
Herein, can be according to actual production demand (quality, energy consumption, cost, environmental protection and safety) the rational solid-liquid of selection
Separation equipment, such as filtering equipment, precipitation apparatus, filter plant, precipitation apparatus, vacuum equipment, centrifuge.
Embodiment 2-10
Similar with the synthesis step of embodiment 1, embodiment 2-10 is rubbed by adjusting calcium silicon in the step S1 of building-up process
Your when ginseng such as drying temperature in liquid-solid ratio L/S, the hydrothermal temperature in step S2, hydro-thermal time and mixing speed, step S3
Said conditions synthesize different calcium silicate materials.Synthesis situations of the embodiment 2-10 to different calcium silicate materials is specifically as shown in table 1.
Synthesis situations of the embodiment 2-10 of table 1 to different calcium silicate materials.
It is as it can be seen from table 1 anti-by adjusting silico-calcium mol ratio, liquid-solid ratio, hydrothermal temperature, hydro-thermal in building-up process
Between seasonable and the parameter such as mixing speed, the calcium silicates class product of different crystal forms and physicochemical property can obtain.Specifically, when silico-calcium rubs
Your ratio is 0.83-0.91:1st, liquid-solid ratio 15-20:1st, reaction temperature is 180-250 DEG C, the reaction time is 8-18h and stirring speed
Spend for 200-300r/min when, synthesize tobermorite.When silico-calcium mol ratio is 0.93-1:1st, liquid-solid ratio 10-30:1st, react
When temperature is 200-250 DEG C, the reaction time is 8-16h and mixing speed is 150-300r/min, synthesize eakleite.Work as silicon
Calcium mol ratio is 0.85-0.93:1st, liquid-solid ratio 22-28:1st, reaction temperature is 200-300 DEG C, the reaction time is 6-18h and is stirred
When to mix speed be 180-280r/min, synthesize the mix products of eakleite and tobermorite.
The physical and chemical performance parameter of the embodiment 1-10 calcium silicate materials prepared is contrasted below, specific physical and chemical performance
Parameter is as shown in table 2.
The embodiment 1-10 of table 2 calcium silicate material type and its parameter value contrast table
The oil factor of powder is directed to be slowly added into vegetable oil (being usually linseed oil) in 100 grams of powders, and side edged is mixed
With, when can stick into a glob of with loose granule to powder, the oily amount that is consumed, in gram.
From table 2 it can be seen that no matter the product of embodiment 1-10 synthesis is tobermorite, or eakleite, or snow
The mix products of silicoglaserite and eakleite, with the increase of the bulk density of product, oil factor then accordingly reduces.This is probably
Because when product grain is in state of aggregation, the space between product grain is smaller, causes oil factor to reduce.
The technique effect of the present invention is embodied in the following aspects：
On the premise of additive and other material compositions is not added, the present invention is only with soda lime sintering process red mud, two
Three kinds of raw materials of silica and water, cooled down, be separated by filtration and back tender by simple mixed material, a step Hydrothermal Synthesiss, room temperature
Sequence, with regard to that can prepare calcium silicate material product, method of the invention is simple to operate, and preparation section is few, and production efficiency is high, is produced into
This low, valuable constituent calcium oxide and silica being effectively utilized in soda lime sintering process red mud, it is the preparation of calcium silicate material
New raw material and method are have found, while solves that current soda lime sintering hair red mud storage is big, takes up an area wide, pollution weight and processing
The problem of difficult, realize the high value added utilization of waste material, energy-conserving and environment-protective.
Flow is simple in whole building-up process, and no discarded object and pollutant produce, low for equipment requirements, easily realize industry
Change.In building-up process, by adjusting process parameter, the calcium silicate products that can obtain different crystal forms and physicochemical property (avenges silico-calcium
Stone or/and eakleite).
The technical principle of the present invention is described above in association with embodiment.These descriptions are intended merely to explain the present invention
Principle, and limiting the scope of the invention can not be construed in any way.Based on explanation herein, art technology
Personnel, which need not pay creative work, can associate other embodiments of the present invention, and these modes fall within this
Within invention protection domain.
Claims (5)
- A kind of 1. method using the direct synthetic calcium silicate of soda lime sintering process red mud, it is characterised in that comprise the following steps：S1, raw material slurry preparation：Soda lime sintering process red mud and silica and water are pressed into liquid-solid ratio 10-30:1 mixed preparing is former Slurry, wherein, calcium silicon mol ratio is 0.83-1 in the raw material slurry after preparation:1；S2, hydrothermal synthesis method prepare calcium silicate material slurry：By step S1 raw material slurry 180-300 DEG C of stirring in confined conditions 6-20h is reacted, obtains calcium silicate material slurry；S3, calcium silicate powder material synthesis：The step S2 calcium silicate material slurries obtained are cooled down at room temperature, passed through Separation obtains solid product and water, then dries the solid product after separation and removes moisture removal, obtains tobermorite or/and hard silicon Calcium stone.
- 2. the method for the direct synthetic calcium silicate of soda lime sintering process red mud is utilized as claimed in claim 1, it is characterised in that institute The mixing speed for stating step S2 is 150-300r/min.
- 3. the method for the direct synthetic calcium silicate of soda lime sintering process red mud is utilized as claimed in claim 2, it is characterised in that when Silico-calcium mol ratio is 0.83-0.91:1st, liquid-solid ratio 15-20:1st, reaction temperature be 180-250 DEG C, the reaction time be 8-18h and When mixing speed is 200-300r/min, synthesize tobermorite；When silico-calcium mol ratio is 0.93-1:1st, liquid-solid ratio 10-30:1st, reaction temperature be 200-250 DEG C, reaction time 8- When 16h and mixing speed are 150-300r/min, synthesize eakleite；When silico-calcium mol ratio is 0.85-0.93:1st, liquid-solid ratio 22-28:1st, reaction temperature be 200-300 DEG C, the reaction time be When 6-18h and mixing speed are 180-280r/min, synthesize eakleite and tobermorite.
- 4. the method for the direct synthetic calcium silicate of soda lime sintering process red mud is utilized as claimed in claim 3, it is characterised in that In the step S2, the raw material slurry is using the control of any of oil bath heating mode, salt bath heating mode and Electric heating Reaction temperature processed.
- 5. the method for the direct synthetic calcium silicate of soda lime sintering process red mud is utilized as claimed in claim 4, it is characterised in that institute The drying temperature for stating step S3 is 90-180 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109020459A (en) * | 2018-08-24 | 2018-12-18 | 内蒙古中建亚太建材科技有限公司 | A kind of method that red mud from sintering process prepares tobermorite type heat preservation fireproofing material |
| CN114736685A (en) * | 2022-03-04 | 2022-07-12 | 大唐同舟科技有限公司 | Method for producing water-retaining soil conditioner by using alkali-containing solid waste |
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| CN101734673A (en) * | 2008-11-20 | 2010-06-16 | 贵阳宝源阳光硅业有限公司 | Calcium silicate and preparation method thereof |
| CN104477926A (en) * | 2014-12-31 | 2015-04-01 | 东北大学设计研究院（有限公司） | Method for producing xonotlite and aluminum oxide by using coal ash alkaline leaching sintering hydrothermal method |
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2017
- 2017-11-29 CN CN201711229229.2A patent/CN107840342B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101734673A (en) * | 2008-11-20 | 2010-06-16 | 贵阳宝源阳光硅业有限公司 | Calcium silicate and preparation method thereof |
| CN104477926A (en) * | 2014-12-31 | 2015-04-01 | 东北大学设计研究院（有限公司） | Method for producing xonotlite and aluminum oxide by using coal ash alkaline leaching sintering hydrothermal method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109020459A (en) * | 2018-08-24 | 2018-12-18 | 内蒙古中建亚太建材科技有限公司 | A kind of method that red mud from sintering process prepares tobermorite type heat preservation fireproofing material |
| CN114736685A (en) * | 2022-03-04 | 2022-07-12 | 大唐同舟科技有限公司 | Method for producing water-retaining soil conditioner by using alkali-containing solid waste |
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