CN105540601A - Method for producing sodium metasilicate pentahydrate - Google Patents
Method for producing sodium metasilicate pentahydrate Download PDFInfo
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- CN105540601A CN105540601A CN201610051622.6A CN201610051622A CN105540601A CN 105540601 A CN105540601 A CN 105540601A CN 201610051622 A CN201610051622 A CN 201610051622A CN 105540601 A CN105540601 A CN 105540601A
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- Prior art keywords
- metasilicate pentahydrate
- pentahydrate sodium
- mixed solution
- sodium
- production method
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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
Abstract
The invention relates to a method for producing sodium metasilicate pentahydrate. Sodium hydroxide solid, silica fume and water are mixed, a mixed solution with the mass concentration of sodium hydroxide being 37-39% is obtained, the mixed solution is placed at the temperature of 60-80 DEG C for conducting a reaction for 30-90 minutes, then the mixed solution obtained after the reaction is filtered, filtered clear liquid is taken and subjected to modulus adjustment, the adjusted modulus is 0.6-1.6, the clear liquid obtained after modulus adjustment is subjected to crystallization at the temperature of 40-52 DEG C, and the sodium metasilicate pentahydrate is obtained. The method for producing the sodium metasilicate pentahydrate has the advantages that the reaction condition is convenient to control, and product quality is good.
Description
Technical field
The present invention relates to the production technology of Starso, particularly a kind of production method of metasilicate pentahydrate sodium.
Background technology
The conventional production process of Starso is for raw material with quartz sand and caustic soda, react at 100-150 DEG C after certain density sodium hydroxide solution and quartz sand are mixed according to a certain percentage, carry out the explained hereafter such as mode transfer, crystallization and drying again to form, the granularity of usual quartz sand is between 100-325 order.Except taking quartz sand as the main production of raw material, in existing technique, with wollastonite, (main component is for CaSiO in addition
3), (main component is SiCl to polycrystalline silicon production waste materials
4), useless silica gel, Serpentine ore residue after extracting magnesium, diatomite, cullet, flyash, bauxitic clay extract the preparation technology that aluminum sulfate dregs, zirconium oxychloride by-product waste lye etc. are raw material employing wet method or dry method, these techniques all have employed waste or inexpensive raw material is raw material, in the hope of reducing production cost and reducing environmental pollution, but not easily to remove with technological process the reasons such as difficult control due to impurity, above-mentioned technique in production application on all there is the restriction of application scale and scope.
The patent No. is the production method that the Chinese invention patent of 201510566278.X discloses a kind of metasilicate pentahydrate sodium, described production method comprises the following steps: (1) take dioxide-containing silica as the quartz sand of 99.3-100% and sodium oxide content be the caustic soda of 45 ~ 50% is reaction raw materials, the weight ratio 1:1.5-1.8 of described quartz sand and described caustic soda, under the condition of pressure 0.6-1.6MPa, temperature 150-200 DEG C, react 4-12 hour, obtain the thick liquid of liquid sodium silicate; (2) at 80-95 DEG C of temperature, in the thick liquid of described liquid sodium silicate, add flocculation agent, stir 30-60 minute, leave standstill 10-15 hour, obtain flocculation liquid, in described flocculation liquid, add flocculating aids, device filters after filtration, obtains water glass refined liquid and filter residue; (3) caustic soda being 50% by described water glass refined liquid and sodium oxide content mixes according to the ratio of weight ratio 1.5-2.5:1, and obtained silicon-dioxide and sodium oxide total content are the metasilicate pentahydrate sodium melt liquid of 55-60%; (4) described metasilicate pentahydrate sodium melt liquid is cooled, in described metasilicate pentahydrate sodium melt liquid, pass into pressurized air while cooling, carry out airflow stirring, make the temperature of described metasilicate pentahydrate sodium melt liquid be cooled to 65-70 DEG C; (5) above-mentioned cooled metasilicate pentahydrate sodium melt liquid and small-particle crystal seed are carried out abundant mix and blend, described metasilicate pentahydrate sodium melt liquid is made to be attached to described small-particle seed surface equably, again after cooling, make described metasilicate pentahydrate sodium melt liquid in described small-particle seed surface solidification crystallization; (6) after crystallization, then through air-cooled or water-cooled, be cooled to less than 50 DEG C, sieve through 18-30 mesh sieve, to obtain final product.
The production method of metasilicate pentahydrate sodium disclosed in above-mentioned patent is take dioxide-containing silica as the quartz sand of 99.3-100% and sodium oxide content be the caustic soda of 45 ~ 50% is reaction raw materials, still there is impurity and not easily remove the problem rambunctious with technological process in it, thus apply scale and scope less.
Summary of the invention
Technical problem to be solved by this invention is: the production method providing a kind of metasilicate pentahydrate sodium of easily-controlled reaction conditions.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of production method of metasilicate pentahydrate sodium, sodium hydrate solid, SILICA FUME and water are mixed, obtaining sodium hydroxide mass concentration is the mixed solution of 37-39%, 30-90min is reacted under described mixed solution being placed in 60-80 DEG C of condition, then filtered by reacted mixed solution, get the clear liquid after filtration and carry out mode transfer, adjustment modulus is 0.6-1.6, clear liquid after mode transfer is carried out crystallization under 40-52 DEG C of condition, obtains described metasilicate pentahydrate sodium.
Beneficial effect of the present invention is:
(1) temperature of reaction can reduce to 60-80 DEG C by the 100-150 of prior art DEG C, and caustic soda can be utilized to dissolve and reaction liberated heat, reality only needs to consume little electrical energy, simultaneously can Reaction time shorten, without the need to carrying out under high-temperature and high-pressure conditions, effectively can reduce the energy consumption of production, and reaction conditions is convenient to control, and then large-scale application can be realized;
(2) design of the mixed solution of 37-39% mass concentration, effectively can improve the quality product that product yield also ensures to have had, and specifically, the too low meeting of mixed liquid concentration makes reaction slack-off, affects quality product; Mixed liquid concentration is too high comparatively large to equipment corrosion, also affects quality product; The metasilicate pentahydrate sodium that the present invention obtains can reach national premium grads standard;
(3) clear liquid adjustment modulus is between 0.6-1.6, water glass effectively can be converted into Starso, and modulus departs from high or the preparation being all unfavorable for product on the low side;
(4) SILICA FUME can be turned waste into wealth, realize resource circulation utilization.
Embodiment
By describing technology contents of the present invention in detail, being realized object and effect, be explained below in conjunction with embodiment.
The design of most critical of the present invention is: adopt SILICA FUME and sodium hydroxide be raw material to prepare metasilicate pentahydrate sodium, thus there is easily-controlled reaction conditions and the advantage easily removed of impurity.
The production method of a kind of metasilicate pentahydrate sodium provided by the invention, sodium hydrate solid, SILICA FUME and water are mixed, obtaining sodium hydroxide mass concentration is the mixed solution of 37-39%, 30-90min is reacted under described mixed solution being placed in 60-80 DEG C of condition, then filtered by reacted mixed solution, get the clear liquid after filtration and carry out mode transfer, adjustment modulus is 0.6-1.6, clear liquid after mode transfer is carried out crystallization under 40-52 DEG C of condition, obtains described metasilicate pentahydrate sodium.
SILICA FUME also cry silicon ash, be iron alloy when smelting duriron and industrial silicon (Pure Silicon Metal), or zircon sand electric smelting method produce zirconium white time, produce the SiO that a large amount of volatility is very strong in electric furnace
2with Si gas, collect form after gaseous emission with the condensation of air rapid oxidation, be mainly used in the industry such as cement and refractory materials and be used as dopant or additive, part SILICA FUME is still put aside as useless because quality and performance is difficult to reach application requiring.Because SILICA FUME has little, the active high characteristic of granularity, mean particle size generally at 1 microns, main component SiO
2content, generally more than 90%, therefore can be used for producing Starso by purification processes.
Do not have in prior art any file open using SILICA FUME as raw material for production metasilicate pentahydrate sodium.Reason may be: on the one hand, and the understanding of the understanding of those skilled in the art to SILICA FUME and the application at specific field thereof not enough; On the other hand, those skilled in the art generally believe that the purification of SILICA FUME exists certain difficulty, thus always can not using SILICA FUME as the raw material preparing metasilicate pentahydrate sodium.Present inventor finds through long-term experiment, using SILICA FUME as the raw material producing metasilicate pentahydrate sodium, its temperature of reaction is lower than adopting quartz sand, reaction times is shorter than quartz sand, concrete temperature of reaction can reduce to 60-80 DEG C by 100-150 DEG C, without the need to carrying out under high-temperature and high-pressure conditions, effectively can reduce energy consumption, SILICA FUME can be turned waste into wealth again simultaneously, realize resource circulation utilization.
In mixed solution, the ratio of sodium hydrate solid, SILICA FUME and water is not specifically limited, simultaneously the purity of sodium hydroxide also do not limit, as long as the mass concentration of sodium hydroxide is 37-39% in mixed solution.
From foregoing description, beneficial effect of the present invention is:
(1) temperature of reaction can reduce to 60-80 DEG C by the 100-150 of prior art DEG C, and caustic soda can be utilized to dissolve and reaction liberated heat, reality only needs to consume little electrical energy, simultaneously can Reaction time shorten, without the need to carrying out under high-temperature and high-pressure conditions, effectively can reduce the energy consumption of production, and reaction conditions is convenient to control, and then large-scale application can be realized;
(2) design of the mixed solution of 37-39% concentration, effectively can improve the quality product that product yield also ensures to have had, and specifically, the too low meeting of mixed liquid concentration makes reaction slack-off, affects quality product; Mixed liquid concentration is too high comparatively large to equipment corrosion, also affects quality product; The metasilicate pentahydrate sodium that the present invention obtains can reach national premium grads standard;
(3) clear liquid adjustment modulus is between 0.6-1.6, water glass effectively can be converted into Starso, and modulus departs from high or the preparation being all unfavorable for product on the low side;
(4) SILICA FUME can be turned waste into wealth, realize resource circulation utilization.
Further, described SILICA FUME is purified to the SiO in SILICA FUME
2purity be more than 99%.
Seen from the above description, can to SiO
2the purity SILICA FUME that do not reach 99% purify, the SILICA FUME be about to containing certain impurity carries out purification processes, mainly adopts the pipeline iron filings, the ZrO that carry secretly in the operation removal SILICA FUME such as rapid subsidence separations, diluted acid leaching, cleaning
2, Al
2o
3, Fe
2o
3, the impurity such as CaO, MgO, by main component SiO
2content brings up to more than 99%, can ensure the conforming product rate of the metasilicate pentahydrate sodium prepared.
Further, the filter residue after filtration is added in described mixed solution.
Seen from the above description, filter residue can be continued to add in mixed solution participating in reaction, filter residue is fully recycled.
Further, described crystallization adopts the mode of adding Starso crystal seed to carry out.
Seen from the above description, crystallization can adopt crystallization method of the prior art, and such as, mode by adding crystal seed carries out condensing crystal.
Further, the metasilicate pentahydrate sodium of acquisition is carried out successively concentrate, solid-liquid separation and drying.The metasilicate pentahydrate sodium of acquisition being concentrated into solid content is 56-58%, then carries out solid-liquid separation and drying successively, and the temperature of described drying is 60-65 DEG C.
Seen from the above description, the metasilicate pentahydrate sodium obtained can be carried out as stated above successively concentrating, solid-liquid separation and drying after crystallization, solid-liquid separation can adopt automatic piston whizzer to carry out, and drying can adopt atomization granulating drying technology continuously to carry out.
Embodiments of the invention one are:
The production method of the metasilicate pentahydrate sodium of the present embodiment, its concrete steps are:
1, purify: the SILICA FUME being 96% by the purity of producing electric-melting zirconia collection carries out purification processes, adopt the operations such as rapid subsidence separation, diluted acid leaching, cleaning to remove the pipeline iron filings, the ZrO that carry secretly in SILICA FUME
2, Al
2o
3, Fe
2o
3, the impurity such as CaO, MgO, by main component SiO
2content brings up to more than 99%;
2, mix: added by sodium hydroxide in SILICA FUME slurry, being made into concentration of lye is in proportion 38%, is uniformly mixed;
3, react: react 60 minutes under reactor being heated to 60 DEG C of temperature;
4, filter: filtered by reacted material pressure filter, filter residue Returning reactor continues reaction;
5, mode transfer: the clear liquid after filtering is carried out mode transfer, clear liquid adjustment modulus is 1;
6, crystallization: when solution temperature is at 50 DEG C, start to add crystal seed, add-on is 6% of product volume, carries out condensing crystal;
7, it is dry: when in reactor, material is concentrated into solid content 56%, blowing carries out solid-liquid separation in automatic piston whizzer, adopt atomization granulating drying technology continuously to obtain metasilicate pentahydrate sodium again, drying temperature controls at 65 DEG C, the metasilicate pentahydrate sodium of obtained the present embodiment.
Embodiments of the invention two are:
The production method of the metasilicate pentahydrate sodium of the present embodiment, its concrete steps are:
1, purify: the SILICA FUME being 90% by the purity of producing electric-melting zirconia collection carries out purification processes, adopt the operations such as rapid subsidence separation, diluted acid leaching, cleaning to remove the pipeline iron filings, the ZrO that carry secretly in SILICA FUME
2, Al
2o
3, Fe
2o
3, the impurity such as CaO, MgO, by main component SiO
2content brings up to more than 99%;
2, mix: added by sodium hydroxide in SILICA FUME slurry, being made into concentration of lye is in proportion 38%, is uniformly mixed;
3, react: react 30 minutes under reactor being heated to 80 DEG C of temperature;
4, filter: filtered by reacted material pressure filter, filter residue Returning reactor continues reaction;
5, mode transfer: the clear liquid after filtering is carried out mode transfer, clear liquid adjustment modulus is 1.6;
6, crystallization: when solution temperature is at 48 DEG C, start to add crystal seed, add-on is 5% of product volume, carries out condensing crystal;
7, it is dry: when in reactor, material is concentrated into solid content 58%, blowing carries out solid-liquid separation in automatic piston whizzer, adopt atomization granulating drying technology continuously to obtain metasilicate pentahydrate sodium again, drying temperature controls at 62 DEG C, the metasilicate pentahydrate sodium of obtained the present embodiment.
Embodiments of the invention three are:
The production method of the metasilicate pentahydrate sodium of the present embodiment, sodium hydrate solid, SILICA FUME and water are mixed, obtaining sodium hydroxide mass concentration is the mixed solution of 37%, 30min is reacted under described mixed solution being placed in 60 DEG C of conditions, then reacted mixed solution is filtered, filter residue after filtering is added continuation participation reaction in described mixed solution, get the clear liquid after filtration and carry out mode transfer, adjustment modulus is 0.6, clear liquid after mode transfer is added under 40 DEG C of conditions crystal seed and carry out crystallization, obtain described metasilicate pentahydrate sodium.The metasilicate pentahydrate sodium of acquisition being concentrated into solid content is 56%, then carries out solid-liquid separation and drying successively, and the temperature of described drying is 60 DEG C.
Embodiments of the invention four are:
The production method of the metasilicate pentahydrate sodium of the present embodiment, sodium hydrate solid, SILICA FUME and water are mixed, obtaining sodium hydroxide mass concentration is the mixed solution of 39%, 90min is reacted under described mixed solution being placed in 80 DEG C of conditions, then reacted mixed solution is filtered, filter residue after filtering is added continuation participation reaction in described mixed solution, get the clear liquid after filtration and carry out mode transfer, adjustment modulus is 1.6, clear liquid after mode transfer is added under 52 DEG C of conditions crystal seed and carry out crystallization, obtain described metasilicate pentahydrate sodium.The metasilicate pentahydrate sodium of acquisition being concentrated into solid content is 58%, then carries out solid-liquid separation and drying successively, and the temperature of described drying is 65 DEG C.
Embodiments of the invention five are:
The production method of the metasilicate pentahydrate sodium of the present embodiment, sodium hydrate solid, SILICA FUME and water are mixed, obtaining sodium hydroxide mass concentration is the mixed solution of 38%, 70min is reacted under described mixed solution being placed in 70 DEG C of conditions, then reacted mixed solution is filtered, filter residue after filtering is added continuation participation reaction in described mixed solution, get the clear liquid after filtration and carry out mode transfer, adjustment modulus is 1, clear liquid after mode transfer is added under 46 DEG C of conditions crystal seed and carry out crystallization, obtain described metasilicate pentahydrate sodium.The metasilicate pentahydrate sodium of acquisition being concentrated into solid content is 57%, then carries out solid-liquid separation and drying successively, and the temperature of described drying is 63 DEG C.
Quality examination
Metasilicate pentahydrate sodium embodiment one to embodiment five prepared carries out quality examination, and detected result and quality standard (HG/T2568-2008) is contrasted, and comparing result is as shown in table 1.Table 1 is the quality measurements table of metasilicate pentahydrate sodium of the present invention.
Table 1
Known according to table 1, the quality of the metasilicate pentahydrate sodium that the embodiment of the present invention prepares to embodiment five all meets national premium grads index.
In sum, the production method of metasilicate pentahydrate sodium provided by the invention have reaction conditions be convenient to control and the advantage of good product quality.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalents utilizing description of the present invention to do, or be directly or indirectly used in relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. the production method of a metasilicate pentahydrate sodium, it is characterized in that, sodium hydrate solid, SILICA FUME and water are mixed, obtaining sodium hydroxide mass concentration is the mixed solution of 37-39%, reacts 30-90min, then filtered by reacted mixed solution under described mixed solution being placed in 60-80 DEG C of condition, get the clear liquid after filtration and carry out mode transfer, adjustment modulus is 0.6-1.6, and the clear liquid after mode transfer is carried out crystallization under 40-52 DEG C of condition, obtains described metasilicate pentahydrate sodium.
2. the production method of metasilicate pentahydrate sodium according to claim 1, is characterized in that, described SILICA FUME is purified to the SiO in SILICA FUME
2purity be more than 99%.
3. the production method of metasilicate pentahydrate sodium according to claim 1, is characterized in that, is added in described mixed solution by the filter residue after filtering.
4. the production method of metasilicate pentahydrate sodium according to claim 1, is characterized in that, described crystallization adopts the mode of adding Starso crystal seed to carry out.
5. the production method of metasilicate pentahydrate sodium according to claim 1, is characterized in that, is carried out successively by the metasilicate pentahydrate sodium of acquisition concentrating, solid-liquid separation and drying.
6. the production method of metasilicate pentahydrate sodium according to claim 5, is characterized in that, the metasilicate pentahydrate sodium of acquisition being concentrated into solid content is 56-58%, then carries out solid-liquid separation and drying successively, and the temperature of described drying is 60-65 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610051622.6A CN105540601B (en) | 2016-01-26 | 2016-01-26 | A kind of production method of metasilicate pentahydrate sodium |
| CN201810025779.0A CN108046281A (en) | 2016-01-26 | 2016-01-26 | A kind of production method of the metasilicate pentahydrate sodium of good product quality |
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|---|---|---|---|
| CN201610051622.6A CN105540601B (en) | 2016-01-26 | 2016-01-26 | A kind of production method of metasilicate pentahydrate sodium |
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| CN201810025779.0A Division CN108046281A (en) | 2016-01-26 | 2016-01-26 | A kind of production method of the metasilicate pentahydrate sodium of good product quality |
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| CN105540601A true CN105540601A (en) | 2016-05-04 |
| CN105540601B CN105540601B (en) | 2018-02-06 |
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| CN201610051622.6A Active CN105540601B (en) | 2016-01-26 | 2016-01-26 | A kind of production method of metasilicate pentahydrate sodium |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044819A (en) * | 2016-06-07 | 2016-10-26 | 临沂长荣环保科技有限公司 | Environment-friendly joint production method of polyaluminum chloride-sodium metasilicate |
| CN116457311A (en) * | 2020-08-12 | 2023-07-18 | Pq硅巴西有限公司 | Stable solutions of sodium and iron silicate, method for producing said solutions and use thereof |
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| CN1607177A (en) * | 2003-10-13 | 2005-04-20 | 刘增刚 | Production method of sodium metasilicate pentahydrate |
| CN101837984A (en) * | 2010-05-07 | 2010-09-22 | 南昌大学 | Method for preparing sodium methasilicate pentahydrate |
| CN103738973A (en) * | 2013-12-17 | 2014-04-23 | 柳州东风化工股份有限公司 | Preparation method of sodium metasilicate pentahydrate |
| CN105197949A (en) * | 2015-09-08 | 2015-12-30 | 昌邑市龙港无机硅有限公司 | Production method of sodium metasilicate pentahydrate |
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2016
- 2016-01-26 CN CN201810025779.0A patent/CN108046281A/en not_active Withdrawn
- 2016-01-26 CN CN201610051622.6A patent/CN105540601B/en active Active
Patent Citations (4)
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| CN1607177A (en) * | 2003-10-13 | 2005-04-20 | 刘增刚 | Production method of sodium metasilicate pentahydrate |
| CN101837984A (en) * | 2010-05-07 | 2010-09-22 | 南昌大学 | Method for preparing sodium methasilicate pentahydrate |
| CN103738973A (en) * | 2013-12-17 | 2014-04-23 | 柳州东风化工股份有限公司 | Preparation method of sodium metasilicate pentahydrate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044819A (en) * | 2016-06-07 | 2016-10-26 | 临沂长荣环保科技有限公司 | Environment-friendly joint production method of polyaluminum chloride-sodium metasilicate |
| CN106044819B (en) * | 2016-06-07 | 2018-02-27 | 临沂长荣环保科技有限公司 | A kind of environmentally friendly aluminium polychloride sodium metasilicate Joint Production method |
| CN116457311A (en) * | 2020-08-12 | 2023-07-18 | Pq硅巴西有限公司 | Stable solutions of sodium and iron silicate, method for producing said solutions and use thereof |
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| Publication number | Publication date |
|---|---|
| CN108046281A (en) | 2018-05-18 |
| CN105540601B (en) | 2018-02-06 |
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