CN101913613A - Process for synthesizing aciform wollastonite powder by desiliconizing alkaline liquor - Google Patents
Process for synthesizing aciform wollastonite powder by desiliconizing alkaline liquor Download PDFInfo
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- CN101913613A CN101913613A CN 201010254879 CN201010254879A CN101913613A CN 101913613 A CN101913613 A CN 101913613A CN 201010254879 CN201010254879 CN 201010254879 CN 201010254879 A CN201010254879 A CN 201010254879A CN 101913613 A CN101913613 A CN 101913613A
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- alkali lye
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Abstract
The invention discloses a process for synthesizing aciform wollastonite powder by desiliconizing alkaline liquor, comprising the following steps: mixing the alkaline liquor obtained by pre-desiliconizing potassium-rich rock or flyash or gangue with calcium hydroxide based on that the mole ratio of the silicon oxide in the desiliconizing alkaline liquor to the calcium hydroxide is 0.95-1.05, placing in a reactor for constant temperature reaction for 2-4h at the temperature of 180-280 DEG C, filtering and washing the slurry obtained by reaction, preparing the obtained caustic alkaline liquor into kali salt products or feeding the obtained caustic alkaline liquor to the pre-desiliconizing section for recycling, and drying, calcining, crushing and sieving the afwillite filter cake to obtain the aciform wollastonite powder. The aciform wollastonite powder product prepared by the invention has favorable performance, and can meet the high requirements of industries such as plastics, painting, rubber, ceramics and the like on the fine quality aciform wollastonite powder products.
Description
Technical field
The present invention relates to a kind of technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye.
Background technology
In that water-insoluble potassium ore deposit and aluminous fly-ash or high alumina coal gangue resource are carried out in the industrialized utilization process, by potassium rich rock or flyash or coal gangue raw material gained desiliconization filtrate, be its through the filtrate that pre-desilication reaction, filtering separation obtain, its main component is Na
2SiO
3(K
2SiO
3) and NaOH (KOH).For the recycle that realizes alkali, the economic benefit that improves technological process, with the SiO in the desiliconization filtrate
2With alkali (Na
2O and K
2O) realizing effectively separating, and be made into the good high value added product of market outlook, is the important component part of this type of comprehensive utilization of resources Technology.
Wollastonite is a kind of calcareous white metasilicate crystallization powder, and pattern is generally needle-like, radial or fibrous agrregate.The fibrous wollastonite powder of high-purity, high length-diameter ratio, high whiteness can be used as the filler and the strengthening agent of plastics, rubber after surface modification treatment.Because natural wollastonite resource especially high-quality wollastonite mine is constantly exploited and is consumed, modern industry development simultaneously is more and more higher to the specification of quality of wollastonite powder material, utilizes the high-quality wollastonite powder of other raw mineral materials synthetic to become a kind of mineral powder technology of preparing with essential industry using value.
In that water-insoluble potassium ore deposit and aluminous fly-ash or high alumina coal gangue resource are carried out in the industrialized utilization process, by potassium rich rock or flyash or coal gangue raw material gained desiliconization filtrate, be its through the filtrate that pre-desilication reaction, filtering separation obtain, its main component is Na
2SiO
3(K
2SiO
3) and NaOH (KOH).Its preparation process " technology of preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock (application number: 201010121250.2) " and " high alumina coal gangue, coal ash alkali solution-off silicon prepare hydrated aluminum silicate technology (application number: 201010114787.6) " detailed record is arranged in two patents of invention.
Summary of the invention
The purpose of this invention is to provide a kind of technology of utilizing potassium rich rock or flyash or coal gangue desiliconization alkali lye to prepare the acicular wollastonite powder.This method adopts the SiO in the slaked lime precipitation desiliconization alkali lye
2, generating the hydrated calcium silicate filter cake, the needle shape wollastonite powder product is made in drying, calcining, pulverizing, screening, and potassic mixed alkali liquor is used to produce the sylvite product, and the pure cerium hydroxide soda lye directly is sent to the pre-desiliconization workshop section recycle of front.The present invention is SiO in potassium rich rock or flyash or the coal gangue
2The efficient utilization of component provides a new technological approaches.
To achieve these goals, the present invention adopts following technical proposals.
A kind of synthetic needle shape wollastonite powder body technology of potassium rich rock or flyash or coal gangue desiliconization alkali lye that utilizes, this method comprises the following steps:
First step, is 0.95～1.05 to mix desiliconization alkali lye and calcium hydroxide by the silicon oxide in the desiliconization alkali lye and the mol ratio of calcium hydroxide, add entry 180～280 ℃ of following isothermal reactions 2～4 hours in reactor, wherein, water and desiliconization alkali lye is as liquid, with liquid-solid mass ratio as solid calcium hydroxide be 5～8;
Second step, the slip that obtains of reaction after filtration with washing after, after the filtrate that obtains and washings merged,, or return recycle in the step (1) as the raw material of producing the sylvite product;
Third step, the filter cake after filtering is dry in loft drier, obtain hydration calcium silicate powder;
The 4th step, hydration calcium silicate powder are pulverized through calcining, and screening obtains the acicular wollastonite powder.
Wherein, desiliconization alkali lye used in the present invention is the technology (application number: 201010121250.2) make by preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock, the concrete preparation process of desiliconization alkali lye is as follows: be with potassium rich rock fragmentation, homogenize, make broken ore, potassium rich rock broken ore and desiliconization alkali lye are ground raw pulp together, raw pulp 180 ℃～250 ℃ following constant temperature 1～4 hour in reactor, reaction obtains pre-desilication reaction slip through dilution, filtration, backflush, gained filtrate is desiliconization alkali lye, as the raw material of synthetic acicular wollastonite powder.Desiliconization alkali lye used in the present invention can also be to prepare the technology of hydrated aluminum silicate by high alumina coal gangue, coal ash alkali solution-off silicon (application number: 201010114787.6) make, the concrete preparation process of desiliconization alkali lye is as follows: this technology comprises the technology of high alumina bastard coal crystal soda solution-off silicon and the alkali solution-off silicon technology of aluminous fly-ash.The high alumina coal gangue leaches with alkali lye then through calcining and activating, solid-liquid separation, and filtrate is sodium silicate solution; Aluminous fly-ash need not the calcining and activating operation, direct alkali solution-off silicon, and solid-liquid separation, filtrate is sodium silicate solution.Two kinds of method gained water glass filtrates are desiliconization alkali lye, as the raw material of synthetic acicular wollastonite powder.
In the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye of the present invention, in described first step, be 60～200rpm in reaction kettle for reaction 20-30 minute stir speed (S.S.) in earlier stage, prevent the material sedimentation, after stirring 20-30 minute, close stirring, make it to generate fibrous product.
In the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye of the present invention, in described first step, the desiliconization alkali lye that uses is secondary rainbow brightness syenite desiliconization filtrate, it is the mixed alkali liquor of potassium hydroxide and sodium hydroxide, through reaction, filtrate that obtains after the filtration and washings are the mixed alkali liquors of potassium hydroxide and sodium hydroxide, as the raw material of producing the sylvite product.
In the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye of the present invention, in described first step, the desiliconization alkali lye that uses is calcining coal gangue desiliconization filtrate, through reaction, filtrate that obtains after the filtration and washings are the pure cerium hydroxide soda lyes, return recycle in the step (1).
In the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye of the present invention, in described third step, filter cake carries out drying in loft drier, the exsiccant temperature is 100～200 ℃, dry 1～3 hour, after the drying, the water ratio in the hydration calcium silicate powder that obtains is that the mass percent of free water water ratio is less than 2%.
In the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye of the present invention, in described the 4th step, the calcining temperature of hydration calcium silicate powder is 800～1000 ℃, calcines 1～3 hour.
In the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye of the present invention, in described the 4th step, the calcining of hydration calcium silicate powder can be selected rotary calcining stove or fluidized bed calcination stove for use.
Method of the present invention has following characteristics:
(1) in potassium rich rock or flyash or the coal gangue pre-desilicification process, by the SiO of part stripping
2Make the needle shape wollastonite powder product by this technological process, improved the economic benefit of resource utilization and commercial run.
(2) by the alkali (Na in the slaked lime precipitate and separate desiliconization filtrate
2O and K
2O), silicon (SiO
2), realized the recycle of alkali lye.
(3) excellent property of the acicular wollastonite powder product of employing the present invention preparation can satisfy the requirement of industries such as plastics, coating, rubber, pottery to high-quality acicular wollastonite powder product.
Embodiment
Embodiment 1
Raw material 1: secondary rainbow brightness syenite desiliconization filtrate, chemical ingredients following (g/L):
Measure 400mL secondary rainbow brightness syenite desiliconization filtrate and mix [SiO with 39.34g calcium hydroxide
2(the SiO in the coal gangue desiliconization filtrate
2): the CaO mol ratio is 1.0], add 300mL distilled water [wherein, distilled water and desiliconization alkali lye (comprising wherein silicon oxide and sodium oxide and potassium oxide etc.) are as liquid, with the liquid-solid mass ratio as solid calcium hydroxide be 6], in reactor, stir, be warming up to 220 ℃ of isothermal reaction 4h; The slime vacuum suction filtration that reaction obtains after finishing with three washing leaching cakes of 600mL distillation moisture, obtains 256.30g hydrated calcium silicate filter cake (water ratio 72%) then; First-time filtrate and wash water merge, and obtain the 1.25L causticized alkali liquor, its chemical ingredients following (g/L):
Above-mentioned 256.30g hydrated calcium silicate filter cake is placed electric drying oven with forced convection, dried 1 hour down, obtain the 71.69g hydration calcium silicate powder, its chemical ingredients following (%) at 260 ℃:
Above-mentioned 71.69g calcium silicate hydrate powder is placed box experimental electric furnace, calcined 1 hour down, obtain 60.62g wollastonite powder product at 900 ℃.Observe under scanning electron microscope, wollastonite is an acicular crystals, and length is 6～12 μ m, diameter 100～200nm, and length-to-diameter ratio is about 30～120.Wollastonite content in the goods is 95.0%, dioxide-containing silica 51.23%, and calcium oxide content 45.86%, every index reaches the specification of quality of the first grade of wollastonite industry standard (JC/T 535-2007).
Embodiment 2
Raw material 2: calcining coal gangue desiliconization filtrate, chemical ingredients following (g/L):
Measure 500mL calcining coal gangue desiliconization filtrate and mix [SiO with 37.60g calcium hydroxide
2(the SiO in the coal gangue desiliconization filtrate
2): the CaO mol ratio is 1.0], add 200mL distilled water [wherein, distilled water and desiliconization alkali lye (comprising wherein silicon oxide and sodium oxide and potassium oxide etc.) are as liquid, with the liquid-solid mass ratio as solid calcium hydroxide be 6], in reactor, stir, be warming up to 240 ℃ of following isothermal reaction 3h; The slurry vacuum filtration washing that reaction obtains after finishing obtains 212.86g hydrated calcium silicate filter cake (water ratio 68%), obtains the 1.20L causticized alkali liquor.
Above-mentioned 212.86g hydrated calcium silicate filter cake is placed electric drying oven with forced convection, dried 1 hour down, obtain the 68.12g hydration calcium silicate powder, its chemical ingredients following (%) at 260 ℃:
Above-mentioned 71.69g calcium silicate hydrate powder is placed box experimental electric furnace, calcined 1 hour down, obtain 60.62g product wollastonite powder at 950 ℃.Its chemical ingredients is as follows:
Wollastonite content in the goods is 91.2%, and every index reaches the specification of quality of the first grade of wollastonite industry standard (JC/T 535-2007).
Claims (6)
1. technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye, it is characterized in that: this technology may further comprise the steps:
First step, is 0.95～1.05 to mix desiliconization alkali lye and calcium hydroxide by the silicon oxide in the desiliconization alkali lye and the mol ratio of calcium hydroxide, add entry in reactor in 180～280 ℃ of following isothermal reactions 2～4 hours, wherein, water and desiliconization alkali lye is as liquid, with liquid-solid mass ratio as solid calcium hydroxide be 5～8;
Second step, the slip that obtains of reaction after filtration with washing after, after the filtrate that obtains and washings merged,, or return recycle in the step (1) as the raw material of producing the sylvite product;
Third step, the filter cake after filtering is dry in loft drier, obtain hydration calcium silicate powder;
The 4th step, hydration calcium silicate powder are pulverized through calcining, and screening obtains the acicular wollastonite powder.
2. the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye according to claim 1, it is characterized in that: in described first step, in reaction kettle for reaction 20-30 minute stir speed (S.S.) in earlier stage is 60～200rpm, prevent the material sedimentation, after stirring 20-30 minute, close stirring, make it to generate fibrous product.
3. the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye according to claim 1 and 2, it is characterized in that: in described first step, the desiliconization alkali lye that uses is secondary rainbow brightness syenite desiliconization filtrate, through reaction, filtrate that obtains after the filtration and washings are the mixed alkali liquors of potassium hydroxide and sodium hydroxide, as the raw material of producing the sylvite product.
4. the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye according to claim 1 and 2, it is characterized in that: in described first step, the desiliconization alkali lye that uses is calcining coal gangue desiliconization filtrate, through reaction, filtrate that obtains after the filtration and washings are the pure cerium hydroxide soda lyes, return recycle in the step (1).
5. the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye according to claim 1 and 2, it is characterized in that: in described third step, filter cake carries out drying in loft drier, the exsiccant temperature is 100～200 ℃, dry 1～3 hour, after the drying, the water ratio in the hydration calcium silicate powder that obtains is that the mass percent of free water water ratio is less than 2%.
6. the technology of utilizing the synthetic acicular wollastonite powder of desiliconization alkali lye according to claim 1 and 2, it is characterized in that: in described the 4th step, the calcining temperature of hydration calcium silicate powder is 800～1000 ℃, calcines 1～3 hour.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674380A (en) * | 2012-05-25 | 2012-09-19 | 中南大学 | Method for synthesizing tobermorite whiskers by sodium silicate |
| CN103641125A (en) * | 2013-12-26 | 2014-03-19 | 张延大 | Method for synthesizing wollastonite with high length-diameter ratio by using industrial waste residue resource |
| CN103708478A (en) * | 2013-12-30 | 2014-04-09 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | Preparation method of tobermorite |
| CN104258804A (en) * | 2014-09-10 | 2015-01-07 | 陕西科技大学 | Comprehensive utilization method of coal gangue |
| CN104828834A (en) * | 2014-02-12 | 2015-08-12 | 中国科学院过程工程研究所 | Method of preparing tobermorite from fly ash and application thereof |
| CN105692632A (en) * | 2014-11-27 | 2016-06-22 | 中国科学院过程工程研究所 | Method for preparing tobermorite by use of silicon slag obtained after acid-process fly ash treatment for aluminium extraction |
| CN105753000A (en) * | 2016-02-29 | 2016-07-13 | 同济大学 | Preparation method and application method of hydrated calcium silicate seed crystal |
| CN105839188A (en) * | 2015-01-14 | 2016-08-10 | 中国科学院过程工程研究所 | Method of producing calcium silicate crystal whiskers with fly ash desilication liquid |
| CN114920253A (en) * | 2022-06-16 | 2022-08-19 | 江西广源化工有限责任公司 | Superfine wollastonite and preparation method and application thereof |
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| CN103553061A (en) * | 2013-10-14 | 2014-02-05 | 郴州四方立投资有限公司 | Method for synthesis of wollastonite |
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| CN101798095A (en) * | 2010-03-10 | 2010-08-11 | 昊青薪材（北京）技术有限公司 | Process for preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock |
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2010
- 2010-08-16 CN CN 201010254879 patent/CN101913613B/en active Active
Patent Citations (1)
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| CN101798095A (en) * | 2010-03-10 | 2010-08-11 | 昊青薪材（北京）技术有限公司 | Process for preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock |
Non-Patent Citations (1)
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|---|
| 《Theoretical Foundations of Chemical Engineering》 20081231 K. G. Grigoryan et al. Synthesis of Calcium Hydromonosilicate from Diatomite under Hydrothermal Conditions and Its Transformation into Wollastonite 第583页右栏第2～4段 1-6 第42卷, 第5期 2 * |
Cited By (17)
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| CN102674380B (en) * | 2012-05-25 | 2013-08-14 | 中南大学 | Method for synthesizing tobermorite whiskers by sodium silicate |
| CN102674380A (en) * | 2012-05-25 | 2012-09-19 | 中南大学 | Method for synthesizing tobermorite whiskers by sodium silicate |
| CN103641125A (en) * | 2013-12-26 | 2014-03-19 | 张延大 | Method for synthesizing wollastonite with high length-diameter ratio by using industrial waste residue resource |
| CN103641125B (en) * | 2013-12-26 | 2015-05-13 | 张延大 | Method for synthesizing wollastonite with high length-diameter ratio by using industrial waste residue resource |
| CN103708478A (en) * | 2013-12-30 | 2014-04-09 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | Preparation method of tobermorite |
| CN103708478B (en) * | 2013-12-30 | 2015-11-25 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | A kind of preparation method of tobermorite |
| CN104828834B (en) * | 2014-02-12 | 2017-08-25 | 中国科学院过程工程研究所 | A kind of use coal ash for manufacturing for tobermorite method and its application |
| CN104828834A (en) * | 2014-02-12 | 2015-08-12 | 中国科学院过程工程研究所 | Method of preparing tobermorite from fly ash and application thereof |
| CN104258804A (en) * | 2014-09-10 | 2015-01-07 | 陕西科技大学 | Comprehensive utilization method of coal gangue |
| CN104258804B (en) * | 2014-09-10 | 2016-05-25 | 陕西科技大学 | A kind of method of comprehensive utilization of gangue |
| CN105692632A (en) * | 2014-11-27 | 2016-06-22 | 中国科学院过程工程研究所 | Method for preparing tobermorite by use of silicon slag obtained after acid-process fly ash treatment for aluminium extraction |
| CN105692632B (en) * | 2014-11-27 | 2018-11-13 | 中国科学院过程工程研究所 | A method of preparing tobermorite with gained white residue after acid treatment aluminum-extracted pulverized fuel ash |
| CN105839188A (en) * | 2015-01-14 | 2016-08-10 | 中国科学院过程工程研究所 | Method of producing calcium silicate crystal whiskers with fly ash desilication liquid |
| CN105839188B (en) * | 2015-01-14 | 2018-11-27 | 中国科学院过程工程研究所 | A method of calcium silicate whisker is prepared using flyash desiliconization liquid |
| CN105753000A (en) * | 2016-02-29 | 2016-07-13 | 同济大学 | Preparation method and application method of hydrated calcium silicate seed crystal |
| CN114920253A (en) * | 2022-06-16 | 2022-08-19 | 江西广源化工有限责任公司 | Superfine wollastonite and preparation method and application thereof |
| CN114920253B (en) * | 2022-06-16 | 2023-10-03 | 江西广源化工有限责任公司 | Superfine wollastonite and preparation method and application thereof |
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