CN105819458B - A kind of method that eakleite is prepared using disodium metasilicate calcium - Google Patents
A kind of method that eakleite is prepared using disodium metasilicate calcium Download PDFInfo
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- CN105819458B CN105819458B CN201610189180.1A CN201610189180A CN105819458B CN 105819458 B CN105819458 B CN 105819458B CN 201610189180 A CN201610189180 A CN 201610189180A CN 105819458 B CN105819458 B CN 105819458B
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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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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2006/32—Thermal properties
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Abstract
The present invention provides a kind of method that eakleite is prepared using disodium metasilicate calcium, comprises the following steps：Disodium metasilicate calcium is mixed with sodium hydroxide solution, subsequent temperature-gradient method is to 200~260 DEG C and 1~8h of insulation reaction；Reaction product is filtered and dried successively, obtains eakleite.The method of the present invention uses the industrial residue containing alkali for containing disodium metasilicate calcium, and as raw material, its is cheap and easy to get, stable performance, so as to greatly reduce the production cost of eakleite；In addition, the method for the present invention is simple to operate, the reaction time is short, particularly suitable for industrialization production.
Description
Technical field
The present invention relates to a kind of preparation method of eakleite, and hard silicon is prepared using disodium metasilicate calcium more particularly to one kind
The method of calcium stone.
Background technology
Eakleite (Ca6[Si6O17](OH)2) be calcium-silicate thermal insulation material main mineral constituent, the insulation being made from it
Materials'use temperature can reach more than 1000 DEG C, while eakleite has that unit weight is small, high high-temp stability is good, thermal conductivity factor
Low advantage, thus it is widely used in the primary raw material as light heat-insulating fire proofing material.
At present, the preparation method of eakleite is mainly hydrothermal synthesis method, and this method is by by calcareous raw material and siliceous original
Material is placed in autoclave after mixing by a certain percentage to be reacted to obtain eakleite.However, employed in this method
Siliceous raw material is the solid materials such as quartz sand or the high white carbon of price of complete crystallization mostly, required for course of reaction when
Between it is longer；Therefore, the method for producing eakleite using prior art has the shortcomings that production cost is high, time-consuming for production.Such as
What finds the siliceous raw material that a kind of cost is cheap, the market supply is sufficient, while and can enough shortens the production time one of eakleite
It is directly people's urgent problem to be solved.
The content of the invention
The present invention provides a kind of method that eakleite is prepared using disodium metasilicate calcium, and it, which is utilized, contains disodium metasilicate calcium
Industrial residue containing alkali has the advantages that production cost is low, the reaction time is short as siliceous raw material.
The present invention provides a kind of method that eakleite is prepared using disodium metasilicate calcium, comprises the following steps：
Disodium metasilicate calcium is mixed with sodium hydroxide solution, subsequent temperature-gradient method to 200~260 DEG C and insulation reaction 1~
8h；
Reaction product is filtered and dried successively, obtains eakleite.
In the present invention, temperature-gradient method is advantageous to eakleite and crystallized during the course of the reaction, good so as to be formed
Crystal formation, while it is also beneficial to be lifted the physical property of eakleite.
Further, the temperature-gradient method process includes：10~15min is incubated at 130~150 DEG C, at 150~180 DEG C
10~12min is incubated, 8~12min is incubated at 180~200 DEG C, 1~8h is incubated at 200~260 DEG C；In addition, the segmentation rises
The heating rate of temperature is 1~5 DEG C/min.
In the present invention, the dosage to sodium hydroxide solution and concentration do not limit strictly, such as the disodium metasilicate
Calcium can be with 1g with the sodium hydroxide solution：(15~40) mL ratio is mixed, and the sodium hydroxide solution is dense
Degree can be 5~60g/L.
The disodium metasilicate calcium that the present invention uses can come from the industrial residue containing alkali containing disodium metasilicate calcium, such as can come
From soda lime sintered clinker dissolution NaAlO2Remaining filter residue afterwards.In industrial solid containing alkali waste residue (such as Bayer process red mud, sintering process
Red mud etc.) recovery alkali after waste residue can be utilized, so as to reduce the consumption of raw material in production process, reduce production cost；It is special
It is not the main thing for the soda lime sintered clinker for using high-alkali low calcium proportioning mutually for NaAlO2And Na2CaSiO4, wherein NaAlO2
Enter liquid phase in process in leaching, so as to leave with disodium metasilicate calcium (Na2CaSiO4) be main thing phase filter residue, the filter residue
Chemical composition includes：Na220~25wt% of O；28~32wt% of CaO；SiO228~32wt%；Al2O32~5wt%, its
Alkali content height (Na2O content is more than 20wt%), and Nature comparison is stable under condition of normal pressure in aqueous, if not located
Reason, not only wastes substantial amounts of alkali, and be unfavorable for following process and the processing of industrial solid waste residue.
The present inventor it has been investigated that：Above-mentioned disodium metasilicate calcium (Na2CaSiO4) in alkaline medium and hydro-thermal reaction bar
Can voluntarily it be decomposed under part, it need not add other dealkalize agent during dealkalize, and will not change solid phase calcium silicon before and after dealkalize
Mol ratio, therefore the alkali in disodium metasilicate calcium is directly decomposed under high-temperature alkaline environment, and remaining solid phase slag is used to prepare
Eakleite, so as to complete the present invention.
In the present invention, the reaction can be carried out in autoclave.It is possible to further control the reaction
Absolute pressure is 0.6~3.5MPa.
Furthermore, it is possible to carry out the reaction under agitation, and it is 100-300r/ that can control the speed of the stirring
min。
Further, before the drying is carried out, the filter cake that can also be formed to the filtering washs；Washing can
To be carried out using hot water, the temperature of hot water can be 70~100 DEG C, and hot wash-water dosage and the hard silico-calcium of butt in filter cake
The ratio of stone can be 5~30ml：1g.
It it is 90~120 DEG C it is possible to further control the temperature of the drying, drying time is 1~3h.
The present invention utilizes eakleite prepared by disodium metasilicate calcium, and moisture content (weight/mass percentage composition) is less than after tested
2.0%, it is suitable with the moisture content for the eakleite that prior art is prepared, and quality meets relevant criterion level.Especially
It is that the eakleite includes the fibrous crystal body of draw ratio 20~40；Average aspect ratio is 30 or so；It is in addition, described hard
The thermal conductivity factor of silicoglaserite is 0.04~0.045W/ (mK)；Rupture strength is 0.6~0.9MPa.
The implementation of the present invention program, at least has the advantage that：
1st, the present invention is to contain the industrial residue containing alkali of disodium metasilicate calcium as raw material, and its is cheap and easy to get, stable performance, from
And greatly reduce the production cost of eakleite；In addition, the preparation method of the present invention is simple to operate, particularly reaction time
It is short, it is consequently adapted to industrialization production.
2nd, method of the invention makes alkali with the shape of caustic solution while eakleite is prepared using disodium metasilicate calcium
Formula is recycled, and removal process does not add other dealkalize agent, and raw material and production and processing cost decrease.
3rd, method of the invention can effectively solve the problem that the problem of consumption of disodium metasilicate calcium and higher value application, so as to be production
The eakleite of high-quality is laid a good foundation, and has larger application value.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of eakleite prepared by the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of eakleite prepared by the embodiment of the present invention 1.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with embodiments of the invention, to this
Technical scheme in inventive embodiments is clearly and completely described, it is clear that described embodiment is that a part of the invention is real
Apply example, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creation
Property work under the premise of the every other embodiment that is obtained, belong to the scope of protection of the invention.
Embodiment 1
Raw material disodium metasilicate calcium comes from soda lime sintered clinker dissolution NaAlO used by the present embodiment2Remaining filter afterwards
Slag, its chemical composition are shown in Table 1.
Chemical composition (the content unit of the disodium metasilicate calcium raw material of table 1：Wt%)
The method for preparing eakleite using above-mentioned disodium metasilicate calcium, it is specially：
The piece alkali that purity is 99wt% is weighed, is completely dissolved in 600g distilled water, being configured to about 600mL concentration is
50g/L or so sodium hydroxide solution, it is standby.
The above-mentioned disodium metasilicate calcium of 20.0g or so is weighed, is added into the above-mentioned 600mL prepared sodium hydroxide solution,
After stirring, it is placed in the test-type autoclave that dischargeable capacity is 1L, the absolute pressure for controlling reaction is 2.5MPa, and
It is stirred, is heated up in a manner of 3 DEG C/min heating rate and temperature-gradient method, wherein dividing with 100rpm or so speed
Section temperature-rise period be：12min is incubated at 140 DEG C or so, 10min is incubated at 165 DEG C or so, 8min is incubated at 190 DEG C or so,
230 DEG C or so insulation reaction 3h.
After reaction terminates, reaction product is cooled to 90 DEG C, then filtered, is in temperature by the filter cake being filtrated to get
2h or so is dried at 110 DEG C, obtains the eakleite that moisture content is less than 2.0%.
The above-mentioned eakleite being prepared is detected, wherein X-ray diffractogram is as shown in figure 1, scanning electron microscope (SEM) photograph
As shown in Figure 2.From fig. 1, it can be seen that it is above-mentioned be prepared for eakleite；As can be seen from Figure 2, the above-mentioned eakleite being prepared
For fibrous crystal body, its draw ratio 20~40, average aspect ratio is 30 or so.
In addition, the above-mentioned physicochemical property that eakleite is prepared is entered according to the method in GB 11968-2006 standards
Row detection, the results showed that：The rupture strength of eakleite is 0.81MPa, and thermal conductivity factor is 0.043W/ (mK).
Embodiment 2
Raw material disodium metasilicate calcium comes from soda lime sintered clinker dissolution NaAlO used by the present embodiment2Remaining filter afterwards
Slag, its chemical composition are shown in Table 2.
Chemical composition (the content unit of the disodium metasilicate calcium raw material of table 2：Wt%)
| Composition | Na2O | CaO | SiO2 | Al2O3 | K2O | MgO | Fe2O3 | LOI |
| Content | 22.37 | 29.45 | 30.86 | 2.04 | 0.84 | 0.89 | 0.82 | 11.87 |
The method for preparing eakleite using above-mentioned disodium metasilicate calcium, it is specially：
The piece alkali that purity is 99wt% is weighed, is completely dissolved in 800g distilled water, being configured to about 800mL concentration is
10g/L or so sodium hydroxide solution, it is standby.
The above-mentioned disodium metasilicate calcium of 20.0g or so is weighed, is added into the above-mentioned 800mL prepared sodium hydroxide solution,
After stirring, it is placed in the test-type autoclave that dischargeable capacity is 1L, the absolute pressure for controlling reaction is 3.0MPa, and
It is stirred, is heated up in a manner of 2 DEG C/min heating rate and temperature-gradient method, wherein dividing with 200rpm or so speed
Section temperature-rise period be：15min is incubated at 150 DEG C or so, 12min is incubated at 180 DEG C or so, 10min is incubated at 210 DEG C or so,
In 260 DEG C or so insulation reaction 2h.
After reaction terminates, reaction product is cooled to 90 DEG C, then filtered, is in temperature by the filter cake being filtrated to get
2h is dried at 90 DEG C, obtains the eakleite that moisture content is less than 2.0%, its X-ray diffractogram is similar to Fig. 1, and is fiber
Shape crystalline solid, draw ratio 20~40, average aspect ratio are 30 or so.
In addition, the above-mentioned physicochemical property that eakleite is prepared is entered according to the method in GB 11968-2006 standards
Row detection, the results showed that：The rupture strength of eakleite is 0.76MPa, and thermal conductivity factor is 0.044W/ (mK).
Embodiment 3
Raw material disodium metasilicate calcium comes from soda lime sintered clinker dissolution NaAlO used by the present embodiment2Remaining filter afterwards
Slag, its chemical composition are shown in Table 3.
Chemical composition (the content unit of the disodium metasilicate calcium raw material of table 3：Wt%)
| Composition | Na2O | CaO | SiO2 | Al2O3 | K2O | MgO | Fe2O3 | LOI |
| Content | 21.09 | 29.00 | 29.32 | 2.78 | 0.67 | 0.71 | 0.93 | 14.87 |
The method for preparing eakleite using above-mentioned disodium metasilicate calcium, it is specially：
The piece alkali that purity is 99wt% is weighed, is completely dissolved in 500g distilled water, being configured to about 500mL concentration is
20g/L or so sodium hydroxide solution, it is standby.
The above-mentioned disodium metasilicate calcium of 20.0g or so is weighed, is added into the above-mentioned 500mL prepared sodium hydroxide solution,
After stirring, it is placed in the test-type autoclave that dischargeable capacity is 1L, the absolute pressure for controlling reaction is 3.0MPa, and
It is stirred, is heated up in a manner of 5 DEG C/min heating rate and temperature-gradient method, wherein dividing with 250rpm or so speed
Section temperature-rise period be：10min is incubated at 130 DEG C or so, 10min is incubated at 150 DEG C or so, 12min is incubated at 180 DEG C or so,
In 210 DEG C or so insulation reaction 6h.
After reaction terminates, reaction product is cooled to 90 DEG C, then filtered, is in temperature by the filter cake being filtrated to get
2h is dried at 120 DEG C, obtains the eakleite that moisture content is less than 2.0%, its X-ray diffractogram is similar to Fig. 1, and is fiber
Shape crystalline solid, draw ratio 20~40, average aspect ratio are 30 or so.
In addition, the above-mentioned physicochemical property that eakleite is prepared is entered according to the method in GB 11968-2006 standards
Row detection, the results showed that：The rupture strength of eakleite is 0.64MPa, and thermal conductivity factor is 0.045W/ (mK).
Reference examples 1
Reference examples 1 are other same as Example 1 in addition to heating mode is continuous warming, wherein：
Continuous warming is specially：Be warming up to 230 DEG C by 140 DEG C with 3 DEG C/min heating rate, it is total be incubated the reaction time with
Embodiment 1 is identical, obtains the eakleite that moisture content is less than 2.0%.
After testing, the eakleite that reference examples 1 are prepared is fibrous crystal body, and its draw ratio 10~20 is average long
Footpath ratio is 15 or so；In addition, the thermal conductivity factor for the eakleite that reference examples 1 are prepared is 0.055W/ (mK).
Thus illustrate, temperature-gradient method of the invention is advantageous to eakleite and crystallized during the course of the reaction, so as to be formed
Good crystal formation, while it is also beneficial to be lifted the physical property of eakleite.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (6)
- A kind of 1. method that eakleite is prepared using disodium metasilicate calcium, it is characterised in that comprise the following steps：Disodium metasilicate calcium is mixed with sodium hydroxide solution, subsequent temperature-gradient method is to 200~260 DEG C and 1~8h of insulation reaction；Reaction product is filtered and dried successively, obtains eakleite；The heating rate of the temperature-gradient method is 1~5 DEG C/min；The disodium metasilicate calcium comes from soda lime sintered clinker dissolution NaAlO2Remaining filter residue afterwards;The chemical composition of the filter residue includes：Na2O 20~25wt%, CaO 28~32wt%, SiO228~32wt%, Al2O3 2~5wt%；The absolute pressure for controlling the reaction is 0.6~3.5MPa.
- 2. according to the method for claim 1, it is characterised in that the temperature-gradient method process includes：In 130~150 DEG C of guarantors 10~15min of temperature, 10~12min is incubated at 150~180 DEG C, and 8~12min is incubated at 180~200 DEG C, in 200~260 DEG C of guarantors 1~8h of temperature.
- 3. method according to any one of claims 1 to 2, it is characterised in that the disodium metasilicate calcium and the sodium hydroxide Solution is with 1g：(15~40) mL ratio is mixed, and the concentration of the sodium hydroxide solution is 5~60g/L.
- 4. method according to any one of claims 1 to 2, it is characterised in that carry out the reaction under agitation, and control The speed of the stirring is 100-300r/min.
- 5. method according to any one of claims 1 to 2, it is characterised in that the temperature for controlling the drying is 90~120 DEG C, drying time is 1~3h.
- 6. method according to any one of claims 1 to 2, it is characterised in that the eakleite includes draw ratio 20~40 Fibrous crystal body.
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| RO93046A2 (en) * | 1985-07-25 | 1987-11-30 | Institutul Politehnic"Traian Vuia",Ro | PROCESS FOR OBTAINING XONOTLYTE-LIKE CALCIUM SILICATE AND SYNTHETIC WOLLASTONITE |
| CN103539138A (en) * | 2013-11-11 | 2014-01-29 | 内蒙古大唐国际再生资源开发有限公司 | Method for preparing xonotlite by utilizing desiliconized alkali liquor |
| CN104556170A (en) * | 2014-12-31 | 2015-04-29 | 东北大学设计研究院（有限公司） | Method for producing wollastonite and aluminum oxide through fly ash alkali leaching and sintering hydrothermal method |
| CN104709914A (en) * | 2013-12-12 | 2015-06-17 | 神华集团有限责任公司 | Xonotlite material and xonotlite thermal-insulation material and their preparation methods |
-
2016
- 2016-03-28 CN CN201610189180.1A patent/CN105819458B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO93046A2 (en) * | 1985-07-25 | 1987-11-30 | Institutul Politehnic"Traian Vuia",Ro | PROCESS FOR OBTAINING XONOTLYTE-LIKE CALCIUM SILICATE AND SYNTHETIC WOLLASTONITE |
| CN103539138A (en) * | 2013-11-11 | 2014-01-29 | 内蒙古大唐国际再生资源开发有限公司 | Method for preparing xonotlite by utilizing desiliconized alkali liquor |
| CN104709914A (en) * | 2013-12-12 | 2015-06-17 | 神华集团有限责任公司 | Xonotlite material and xonotlite thermal-insulation material and their preparation methods |
| CN104556170A (en) * | 2014-12-31 | 2015-04-29 | 东北大学设计研究院（有限公司） | Method for producing wollastonite and aluminum oxide through fly ash alkali leaching and sintering hydrothermal method |
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