CN104402019A - Solid-phase preparation method of fly ash zeolite molecular sieve - Google Patents
Solid-phase preparation method of fly ash zeolite molecular sieve Download PDFInfo
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- CN104402019A CN104402019A CN201410661353.6A CN201410661353A CN104402019A CN 104402019 A CN104402019 A CN 104402019A CN 201410661353 A CN201410661353 A CN 201410661353A CN 104402019 A CN104402019 A CN 104402019A
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- C01—INORGANIC CHEMISTRY
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/20—Faujasite type, e.g. type X or Y
- C01B39/22—Type X
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Abstract
The invention discloses a solid-phase preparation method of a fly ash zeolite molecular sieve, and relates to a method for preparing a fly ash zeolite molecular sieve. The method comprises steps of calcining grinded fly ash, deironing, mixing the grinded fly ash with sodium hydroxide solid, adding sodium metaaluminate for adjusting Si/Al molar ratio, grinding and mixing, performing crystallization reaction, washing, drying, and finally obtaining the zeolite molecular sieve with productive rate being 93 to 95 percent. The method is simple in operation, without needing process of preparing hydrous gel, saves the use of clean water, results in less waste production after the completion of the crystallization, greatly reduces environmental pollution caused by waste discharge, is short in reaction time, energy-saving, and high in utilization rate of raw materials and product yield, low in system reaction pressure, and avoids high requirements on reaction equipment, and the CEC value of a 4A type zeolite product is 223.86 mmol/100g, reaching 80.15 percent that of a relative commodity zeolite, and having high adsorption capability to heavy metals and organic wastewater.
Description
Technical field
The present invention relates to solid waste resource recovery field, is a kind of environment-friendly preparation method thereof of high yield coal ash zeolite adsorbent of molecular sieve.
Background technology
Flyash, also known as flying dust, is the waste of coal-burning power plant's pulverized coal friring discharge, containing a small amount of carbon, crystal (quartz, mullite) and a large amount of sillico aluminate glass body, with SiO
2and Al
2o
3be main (accounting for 60%-80%).Within 2013, China's flyash quantity discharged reaches 5.32 hundred million tons, rate of increase 2.31%, and China's flyash adds up accumulating amount and reached 3,700,000,000 tons.The disposal options of current flyash, based on ash disposal area stacking, both took tract, caused again soil erosion, environmental pollution and disruption of ecological balance.Therefore effective disposal of flyash and recycling are the important subject of China's environmental science circle.At present, China's utilization of fly ash rate is only 41.7%, is mainly used in the aspects such as building material made, construction work, road engineering, production cost is high, and its technology content and added value are all lower, therefore in the urgent need to finding low processing cost, and the method that added value of product is high.Zeolite is a kind of inorganic microporous material be widely used in the commercial runs such as catalysis, absorption and ion-exchange.Commercial synthesis zeolite generally all adopts silicate, aluminate, caustic alkali etc., the high and complex process of cost, expensive, and natural zeolite resource-constrained, this limits zeolite output to a great extent.The composition of flyash is similar to the presoma of natural zeolite, therefore, utilizes coal ash for manufacturing not only to expand the recycling approach of flyash for zeolite, improves flyash value-added content of product, also for artificial zeolite have found a kind of raw material of cheapness.
In recent years, the research of coal ash molecular sieve synthetic zeolite is utilized to be incorporated in environment pollution control.Main application: heavy metal component in curing soil, carries out the reparation of contaminated soil, and effectively can remove the easily elimination metal ion such as copper, nickel, zinc, chromium, Be very effective is better than clay; For purifying acid pit water; Remove the Cu in industrial sewage
2+, Cd
2+, Fe
3+, As
3+, Pb
2+etc. heavy metal ion, the sorbing materials such as synthetic zeolite from flyash specific activity charcoal, silica gel have higher absorption property; As soil additive, low-quality coal ash zeolite contains amorphous silicon and other trace elements of a large amount of amorphous aluminosilicate and incomplete zeolitization, is also the beneficiating ingredient of improvement soil; For removing ammonia nitrogen and the phosphoric acid salt of COD in waste water and lower concentration.The research of coal ash zeolite process organic waste water shows, it has good absorption property, therefore utilizes aboundresources, and cheap flyash synthetic adsorbent just progressively replaces conventional adsorbent dominant position in the treatment of waste water.
Adopt conventional hydrothermal method by after synthetic zeolite from flyash first from Holler in 1985 etc., the synthetic technology such as salt-melting method, microwave heating method, alkali fusion, two-step approach, the synthesis of interpolation crystal seed, microwave assisting method is emerged in large numbers gradually.Conventional hydrothermal synthesis method, salt-melting method and microwave method zeolite conversion ratio are lower, and crystal formation is impure; Though two-step approach can synthesize single structure zeolite, produce the remaining flyash after a large amount of extraction silicon; Add crystal seed in crystal seed method to turn brilliant at flyash and play the guiding role for during zeolite, the generation of other zeolite stray crystals can be greatly reduced, raising degree of crystallinity, but quartz in flyash and mullite can not transform completely; Alkali fusion is melting under 500-600 DEG C of high temperature after flyash and alkali being mixed, then through hydro-thermal reaction synthetic zeolite.Alkali fusion research finds that NaOH is than KOH and Na
2cO
3there is higher silicon extraction yield and transformation efficiency; Significantly improve zeolite conversion ratio, and obtain the zeolite of single kind by Si/Al in adjustment gel.Wang Chunfeng etc. adopt alkali fusion synthesis to reach 82.93% and 84.31% of corresponding commodity zeolite without stray crystal NaA and NaX coal ash zeolite CEC.
But prior synthesizing method all needs large water gaging as solvent, and complex steps, the productive rate of product is 60-85%, and input-output ratio is low, increases synthesis cost; After having reacted, molecular sieve needs a large amount of clear water to wash with the separation of mother liquor, brings alkaline pollution to environment.Therefore, the key that the oligosaprobic technology of preparing of a kind of low power consuming is flyash suitability for industrialized production zeolite is researched and developed.
At present, synthetic method such as hydrothermal method, salt-melting method, microwave heating method, alkali fusion, two-step approach, the synthesis of interpolation crystal seed, the microwave assisting method etc. of coal ash zeolite all need large water gaging as solvent, and the productive rate of product is low, and input-output ratio is low, increase synthesis cost; After having reacted, molecular sieve needs a large amount of clear water to wash with the separation of mother liquor, brings alkaline pollution to environment.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method for preparing solid phase of coal ash zeolite molecular sieve is provided, simple, the green cheap novel method for synthesizing of the method technique, to prepare the coal ash zeolite sorbent material compared with high absorption capacity, raw material availability and productive rate.
The present invention is achieved through the following technical solutions:
Flyash, also known as flying dust, is the waste of coal-burning power plant's pulverized coal friring discharge, containing a small amount of carbon, crystal (quartz, mullite) and a large amount of sillico aluminate glass body, with SiO
2and Al
2o
3be main (accounting for 60%-80%), the solid phase preparing technique process process of coal ash zeolite molecular sieve is as follows:
(1) take the flyash of 20 g through ground 300 mesh sieves, be placed in retort furnace in loading nickel crucible and calcine 2 hours at 650 DEG C, after being cooled to room temperature with furnace temperature, carry out deironing with highly-effective magnetic separator.
(2) take the flyash after 10 g deironing oven dry, 5 g NaOH solid particulates are joined in the flyash after deironing oven dry, obtain sode ash mixture, sodium metaaluminate is added in sode ash mixture, to adjust its silica alumina ratio to n (SiO
2)/n (Al
2o
3)=2.2-3.0, obtains solids mixing material, solids mixing material is put into agate mortar and carries out grinding and stirring 30-60 minute.
(3) in polytetrafluoro stainless steel cauldron, 27 g deionized waters are added, by the solids mixing material after grinding is stirred, put into reactor, carry out crystallization, condition is 90 DEG C, and 3.5-4.0 hour, obtains crystallization product, this crystallization product is carried out filtering and washing to pH<9,80 DEG C of oven dry are coal ash zeolite molecular sieve.
Principle of the present invention:
The solid phase synthesis starting stage, mixed being incorporated between whole amorphous silicon oxide of raw material is spread; System temperature raises subsequently, in the process of material diffusion, carries out continuous condensation between silicone hydroxyl, polycondensation goes out moisture, unbodied silicon oxide is gradually to crystal transition, and crystallization process constantly carries out, and the continuous condensation of silicone hydroxyl finally makes solid material be converted to molecular sieve crystal under solid state shape.
The reaction process of solid phase synthesis is the process spreading rearrangement between material, reaction occurs between solid-state reactant, there is not the dissolving as occurring in liquid phase gel, reset the process of regrowth, because the water-content in solid system is extremely low, only can provide the water molecules of reactant character, these water moleculess serve the effect of a reaction initiator.The storeroom of visible initial reaction stage is reset and is played great impact to reaction process, and the difference of liquid phase mechanism and solid phase diffusion mechanism embodies the most obvious at this moment.For the method for solid-phase thermal synthesis, just have partial pore to be formed in the amorphous stage of initial reaction stage, and now crystal is also far from growth.Owing to being comparatively loose metamict, aperture is at this moment greater than the standard aperture (5.2-5.5) of molecular sieve crystal.Along with carrying out further of growth, the further growth of unbodied silicon skeleton, condensation, grown up to the crystalline structure in standard aperture gradually.
Compared with the route of traditional water heat transfer molecular sieve, solid-phase synthesis has following obvious feature: high zeolite product yield, significantly increase reactor single still utilization ratio, decrease pollutent significantly, simplify synthesis step, the pressure in save energy and reaction process reduces.
Embodiment
Embodiment 1
The solid phase preparing technique process process of 4A type coal ash zeolite molecular sieve is as follows:
(1) take the flyash of 20g through ground 300 mesh sieves, be placed in retort furnace in loading nickel crucible and calcine 2 hours at 650 DEG C, after being cooled to room temperature with furnace temperature, carry out deironing with highly-effective magnetic separator.
(2) XRF is adopted to measure flyash after pretreatment elementary composition, wherein SiO
2with Al
2o
3content be respectively 68.9 wt.% and 20.1 wt.%.Take the flyash after 10g deironing oven dry, 5 grams of NaOH join in the flyash after deironing oven dry by mass ratio NaOH/ flyash=1/2, obtain sode ash mixture, according to the stoichiometric equation of 4A type zeolite, joined by sodium metaaluminate 6.18g in sode ash mixture, adjustment silica alumina ratio is to n (SiO
2)/n (Al
2o
3)=2.2, obtain solids mixing material, solids mixing material is put into agate mortar and carries out grinding 10 minutes, then mixture is put into 250mL Erlenmeyer flask, magnetic agitation 1.0 hours.
(3) by Si content mol ratio n (H in flyash after water molecules and 10 g deironing
2o)/n (Si)=1.3, adds deionized water 27g in polytetrafluoro stainless steel cauldron, by the solids mixing material after grinding is stirred, put into reactor, carry out crystallization, condition is 90 DEG C, 3.5 hours, obtain crystallization product, this crystallization product is carried out filtering and washing to pH<9,80 DEG C of oven dry, cross 300 mesh sieves, be detected as 4A type coal ash zeolite molecular sieve to solid XRD, productive rate is 91%.
Embodiment 2
The solid phase preparing technique process process of Na-P1 type coal ash zeolite molecular sieve is as follows:
(1) take the flyash of 20g through ground 300 mesh sieves, be placed in retort furnace in loading nickel crucible and calcine 2 hours at 650 DEG C, after being cooled to room temperature with furnace temperature, carry out deironing with highly-effective magnetic separator.
(2) flyash after 10 g deironing oven dry is taken, in mass ratio NaOH/ flyash=1/2 5 g NaOH are joined deironing dry after flyash in, obtain sode ash mixture, 8.42g sodium metaaluminate is added in sode ash mixture, to adjust its silica alumina ratio to n (SiO
2)/n (Al
2o
3)=3.0, obtain solids mixing material, solids mixing material is put into agate mortar and carries out grinding 10 minutes, then mixture is put into 250mL Erlenmeyer flask, magnetic agitation 1.0 hours.
(3) by Si content mol ratio n (H in flyash after water molecules and 10 g deironing
2o)/n (Si)=1.3, adds deionized water 27g in polytetrafluoro stainless steel cauldron, by the solids mixing material after grinding is stirred, put into reactor, carry out crystallization, condition is 90 DEG C, 3.5 hour, obtain crystallization product, this crystallization product is carried out filtering and washing to pH<9,80 DEG C of oven dry, obtain 9.3g coal ash zeolite molecular sieve, cross 300 mesh sieves, be detected as Na-P1 type coal ash zeolite molecular sieve to solid XRD, productive rate is 91%.
Embodiment 3
The solid phase preparing technique process process of NaX type coal ash zeolite molecular sieve is as follows:
(1) take the flyash of 20g through ground 300 mesh sieves, be placed in retort furnace in loading nickel crucible and calcine 2 hours at 650 DEG C, after being cooled to room temperature with furnace temperature, carry out deironing with highly-effective magnetic separator.
(2) flyash after 10g deironing oven dry is taken, 5 grams of NaOH join in the flyash after deironing oven dry by mass ratio NaOH/ flyash=1/2, obtain sode ash mixture, according to the stoichiometric equation of 4A type zeolite, joined by sodium metaaluminate 6.74g in sode ash mixture, adjustment silica alumina ratio is to n (SiO
2)/n (Al
2o
3)=2.4, obtain solids mixing material, solids mixing material is put into agate mortar and carries out grinding 10 minutes, then mixture is put into 250mL Erlenmeyer flask, magnetic agitation 0.5 hour.
(3) by Si content mol ratio n (H in flyash after water molecules and 10 g deironing
2o)/n (Si)=1.3, adds deionized water 27g in polytetrafluoro stainless steel cauldron, by the solids mixing material after grinding is stirred, put into reactor, carry out crystallization, condition is 90 DEG C, 4.0 hours, obtain crystallization product, this crystallization product is carried out filtering and washing to pH<9,80 DEG C of oven dry, obtain 9.5g coal ash zeolite molecular sieve, cross 300 mesh sieves, NaX type coal ash zeolite molecular sieve is detected as to solid XRD.
Claims (2)
1. a method for preparing solid phase for coal ash zeolite molecular sieve, is characterized in that, described method comprises following process:
(1) take the flyash of 20 g through ground 300 mesh sieves, be placed in retort furnace in loading nickel crucible and calcine 2 hours at 650 DEG C, after being cooled to room temperature with furnace temperature, carry out deironing with highly-effective magnetic separator;
(2) take the flyash after 10 g deironing oven dry, 5 g NaOH solid particulates are joined in the flyash after deironing oven dry, obtain sode ash mixture, sodium metaaluminate is added in sode ash mixture, to adjust its silica alumina ratio to n (SiO
2)/n (Al
2o
3)=2.2-3.0, obtains solids mixing material, solids mixing material is put into agate mortar and carries out grinding and stir 30-60 minute;
(3) in polytetrafluoro stainless steel cauldron, 27 g deionized waters are added, by the solids mixing material after grinding is stirred, put into reactor, carry out crystallization, condition is 90 DEG C, and 3.5-4.0 hour, obtains crystallization product, this crystallization product is carried out filtering and washing to pH<9,80 DEG C of oven dry are coal ash zeolite molecular sieve.
2. the method for preparing solid phase of a kind of coal ash zeolite molecular sieve according to claim 1, it is characterized in that, described flyash is also known as flying dust, it is the waste of coal-burning power plant's pulverized coal friring discharge, containing a small amount of carbon, crystal (quartz, mullite) and a large amount of sillico aluminate glass body, with SiO
2and Al
2o
3be main (accounting for 60%-80%).
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106076212A (en) * | 2016-06-22 | 2016-11-09 | 河北大学 | A kind of technique utilizing waterworks sludge to prepare hydrogel zeolite and the application of hydrogel zeolite |
| CN108383131A (en) * | 2018-02-10 | 2018-08-10 | 西安建筑科技大学 | A method of flyash being prepared into different zeolites using solid phase transformation method |
| CN111847475A (en) * | 2020-07-31 | 2020-10-30 | 中国矿业大学(北京) | Preparation method of 13X molecular sieve and 13X molecular sieve |
| CN112592720A (en) * | 2020-12-15 | 2021-04-02 | 中国矿业大学 | Method for preparing composite curing agent by taking fly ash as raw material and application of composite curing agent in repairing mining area soil |
| CN112642394A (en) * | 2019-10-10 | 2021-04-13 | 萍乡市捷龙环保科技有限公司 | Preparation method of honeycomb zeolite molecular sieve adsorbent |
| CN113028436A (en) * | 2021-02-08 | 2021-06-25 | 华北电力大学 | System and method for removing pollutants in coal-fired flue gas |
| CN113753914A (en) * | 2021-10-08 | 2021-12-07 | 吉林化工学院 | Preparation method of fly ash-based FER structure zeolite |
| CN113893815A (en) * | 2021-11-17 | 2022-01-07 | 太原科技大学 | Ceramsite-zeolite composite high-performance adsorbing material and preparation method thereof |
| CN115385356A (en) * | 2022-08-11 | 2022-11-25 | 浙江大学 | Method for preparing 13X molecular sieve by using fly ash solid phase |
| CN115477312A (en) * | 2022-09-21 | 2022-12-16 | 宁夏大学 | Method for preparing NaX molecular sieve by solid-like phase method |
| CN115770609A (en) * | 2022-11-17 | 2023-03-10 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
| CN116119680A (en) * | 2023-01-17 | 2023-05-16 | 西南科技大学 | Method for solidifying nonferrous metal tailings by using 4A zeolite and solidified body thereof |
| CN116462206A (en) * | 2023-05-11 | 2023-07-21 | 浙江大学 | Method for preparing zeolite from fly ash |
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| CN1389399A (en) * | 2002-07-08 | 2003-01-08 | 中国地质大学（武汉） | Synthesis of zeolite with flyash |
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2014
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| CN1389399A (en) * | 2002-07-08 | 2003-01-08 | 中国地质大学（武汉） | Synthesis of zeolite with flyash |
Non-Patent Citations (1)
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|---|---|---|---|---|
| CN106076212B (en) * | 2016-06-22 | 2018-10-23 | 河北大学 | A kind of application for the technique and hydrogel zeolite preparing hydrogel zeolite using waterworks sludge |
| CN106076212A (en) * | 2016-06-22 | 2016-11-09 | 河北大学 | A kind of technique utilizing waterworks sludge to prepare hydrogel zeolite and the application of hydrogel zeolite |
| CN108383131A (en) * | 2018-02-10 | 2018-08-10 | 西安建筑科技大学 | A method of flyash being prepared into different zeolites using solid phase transformation method |
| CN112642394A (en) * | 2019-10-10 | 2021-04-13 | 萍乡市捷龙环保科技有限公司 | Preparation method of honeycomb zeolite molecular sieve adsorbent |
| CN111847475A (en) * | 2020-07-31 | 2020-10-30 | 中国矿业大学(北京) | Preparation method of 13X molecular sieve and 13X molecular sieve |
| CN112592720A (en) * | 2020-12-15 | 2021-04-02 | 中国矿业大学 | Method for preparing composite curing agent by taking fly ash as raw material and application of composite curing agent in repairing mining area soil |
| CN113028436A (en) * | 2021-02-08 | 2021-06-25 | 华北电力大学 | System and method for removing pollutants in coal-fired flue gas |
| CN113753914B (en) * | 2021-10-08 | 2023-12-29 | 吉林化工学院 | Preparation method of fly ash-based FER structure zeolite |
| CN113753914A (en) * | 2021-10-08 | 2021-12-07 | 吉林化工学院 | Preparation method of fly ash-based FER structure zeolite |
| CN113893815A (en) * | 2021-11-17 | 2022-01-07 | 太原科技大学 | Ceramsite-zeolite composite high-performance adsorbing material and preparation method thereof |
| CN115385356A (en) * | 2022-08-11 | 2022-11-25 | 浙江大学 | Method for preparing 13X molecular sieve by using fly ash solid phase |
| CN115385356B (en) * | 2022-08-11 | 2024-01-05 | 浙江大学 | Method for preparing 13X molecular sieve by utilizing fly ash solid phase |
| CN115477312A (en) * | 2022-09-21 | 2022-12-16 | 宁夏大学 | Method for preparing NaX molecular sieve by solid-like phase method |
| CN115770609A (en) * | 2022-11-17 | 2023-03-10 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
| CN115770609B (en) * | 2022-11-17 | 2024-04-19 | 华电电力科学研究院有限公司 | Preparation method of fly ash-based Fe/ZSM-5 mesoporous molecular sieve catalyst |
| CN116119680A (en) * | 2023-01-17 | 2023-05-16 | 西南科技大学 | Method for solidifying nonferrous metal tailings by using 4A zeolite and solidified body thereof |
| CN116462206A (en) * | 2023-05-11 | 2023-07-21 | 浙江大学 | Method for preparing zeolite from fly ash |
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Application publication date: 20150311 |