CN109012225A - Self-supporting Li-ABW molecular screen membrane is used to separate the application of calcium ion in hard water - Google Patents
Self-supporting Li-ABW molecular screen membrane is used to separate the application of calcium ion in hard water Download PDFInfo
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- CN109012225A CN109012225A CN201810840385.0A CN201810840385A CN109012225A CN 109012225 A CN109012225 A CN 109012225A CN 201810840385 A CN201810840385 A CN 201810840385A CN 109012225 A CN109012225 A CN 109012225A
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- abw
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- molecular screen
- hard water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/028—Molecular sieves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
Abstract
The invention discloses the applications of calcium ion in self-supporting Li-ABW molecular screen membrane separation hard water, and used self-supporting Li-ABW molecular screen membrane diameter is 40mm, with a thickness of 6~8mm, in the case where operation pressure difference is 0.01~0.09MPa, to Ca in hard water2+The hard water that concentration is 100~400mg/L carries out UF membrane, and separative efficiency is 99.8% or more.The self-supporting Li-ABW molecular screen membrane that the present invention is prepared using solid waste circulating fluid bed coal ash as raw material, low in cost, environmentally protective, membrane separation device is simple, operation is convenient, separative efficiency is high.
Description
Technical field
The invention belongs to apply molecular screen membrane softened water field, and in particular to be used for using self-supporting Li-ABW molecular screen membrane
Separate the application of the calcium ion in water.
Background technique
The use of hard water can bring many puzzlements to daily life and industrial production, and especially high calcium and magnesium ion is drawn
The problems such as scale problems risen will be greatly reduced the heat transfer efficiency of boiler, and serious scale can cause the bursting of boilers.Currently, hard water
Softening method specifically includes that ion-exchange, absorption method, dosing tenderizer, electrochemistry tenderizer and membrane separation process[1].Its
In, membrane separation process due to its is easy to operate, water separating membrane good, condensed water discharge of fine quality less, save the advantages that occupied area by
Concern[2].However, there is more demanding, equipment investment, fortune to intake pressure in the organic high molecular layer for being currently used in water softening
Row cost and membrane module high cost problem.
Molecular screen membrane is a kind of novel inorganic membrane material with molecule Yu ion screening function, has general inoranic membrane
The features such as high high-temp stability, resist chemical, high mechanical strength, high membrane flux, and have that molecular sieve bore diameter is uniform, specific surface concurrently
The advantages such as product is big, absorption and ion-exchange capacity are strong, are most potential one of membrane materials.The synthesis of conventional molecular sieve membrane is main
It is on porous carrier such as aluminium oxide carrier or supporter by Vacuum-assisted method method, crystal seed method, plug-hole method, microwave heating
Method, pulsed laser deposition and electrophoretic deposition synthesis have the molecular screen membrane of supporter.However, molecular sieve crystal particle is propping up
The degree of roughness of random growth and supporter on support body can seriously affect the performance of molecular screen membrane, and the use of supporter
So that the preparation cost of molecular screen membrane increases considerably.Self-supporting molecular screen membrane is the New Polycrystalline zeolite membrane reported in recent years,
Its synthetic method is simple, film properties are excellent[3,4].He Yan[3]The method using geo-polymer converted in-situ molecular sieve is reported,
It is successfully prepared NaA self-supporting molecular screen membrane of good performance, has inquired into its application study in terms of sea water desalination.As a result table
Bright: the NaA molecular sieve membrane surface compact of this method preparation, uniformly, compression strength reaches 57.6MPa, for 25 DEG C of temperature, quality
The NaCl solution that percentage is 3.5%, as film thickness is reduced to 2mm from 9.4mm, the flux of water increases to 4.74Kg/ from 0.42
m2·h.When film thickness is more than 9.4mm, the rejection to Na ion is more than 99.5%.It advances rashly[4]Deng with calcined kaolin and water glass
Glass is that raw material prepares geo-polymer, using hydrothermal synthesis method fabricated in situ self-supporting faujasite (abbreviation FAU type) film.It is logical
Cross infiltration evaporation experiment investigated self-supporting FAU type zeolite membrane to the permeation flux of ethanol/water mixture system and separation because
Number.The result shows that: under conditions of feeding temperature is 50 DEG C, the content of ethyl alcohol is 70% in raw material, FAU type zeolite membrane have compared with
High permeation flux and separation factor, permeation flux and separation factor respectively reach 1.41kg/m2H and 16.8.
Applicant discloses " a kind of synthetic method of block Li-ABW zeolite " (Chinese Patent Application No.:
201810126623.1)[5], this method is by CFB flyash: white carbon black: lithium hydroxide: the mass ratio of deionized water is 1:0.18:
0.1~0.12:0.96~1 is mixed and stirred, and through molding, maintenance, is demoulded, is obtained block CFB fly ash geopolymer, by block CFB powder
Coal ash geopolymer is placed in reaction kettle, through Li+Guidance synthesis is dried to obtain the block Li-ABW boiling with certain mechanical strength
Stone.
Applicant is not had found by a large amount of domestic patent of system reviews and documents and materials about self-supporting Li-ABW
Molecular screen membrane separates the relevant report of the method for calcium ion.
It is relevant references below:
[1] Zhang Yafeng, An Luyang, Wang Yunan, Xu Xinwei, Zhang Litao, Song Dihui, in water hardness minimizing technology study into
Exhibition, Coal dressing and comprehensive utilization, 12 (2017) 54-63.
[2] Yuan Junsheng, Jiao Liang, Liu Jie are studied, water treatment technology, 38 (11) (2012) using nanofiltration membrane softening concentrated seawater
81-83。
[3] He Yan, the research of geo-polymer converted in-situ NaA molecular sieve preparating mechanism and application, Guangxi University (2013).
[4] advance rashly, Wang Yipin, Liu Jing, He Yan, Liu Xingdong, Cui Xuemin, geo-polymer fabricated in situ faujasite film and
Its infiltration evaporation performance, silicate journal, 9 (2013) 1244-1250.
[5] Zhang Yaojun, He Panyang, Chen Hao, Han Zhichao, Zhang Ye, Liu Licai, a kind of synthesis side of block Li-ABW zeolite
Method, Chinese Patent Application No.: 201810126623.1.
Summary of the invention
The object of the present invention is to provide the applications that self-supporting Li-ABW molecular screen membrane is used to separate calcium ion.
According to applicant's the study found that self-supporting Li-ABW molecular screen membrane can be used in water softening separates in hard water
Calcium ion.
Used self-supporting Li-ABW molecular screen membrane diameter is 40mm, with a thickness of 6~8mm, operate pressure difference be 0.01~
0.09MPa, Ca in hard water2+Concentration is 100~400mg/L.
Specifically implement according to the following steps:
(1) self-supporting Li-ABW molecular screen membrane is fixed in membrane filter, membrane filter is connected by pipeline, buffering fills
It sets and vacuum pump, demarcates water flux.
(2) different Ca are prepared2+The CaCl of concentration2Solution is as simulation hard water.
(3) hard water described in step (2) is added in membrane filter described in step (1), opens vacuum pump, and by slow
Flushing device adjusts pressure difference.
(4) penetrating fluid is collected, the Ca in penetrating fluid is detected by inductively coupled plasma atomic emission (ICP-OES)2+
The concentration of ion.
Self-supporting Li-ABW molecular screen membrane of the invention is used to separate the application of calcium ion, and innovation is:
The self-supporting Li-ABW molecular screen membrane prepared using solid waste circulating fluid bed coal ash as raw material is low in cost,
It is environmentally protective；To Ca in hard water2+Concentration be 100~400mg/L hard water carry out UF membrane, separative efficiency be 99.8% with
On, and membrane separation device is simple, operation is convenient.
Detailed description of the invention
Fig. 1 is the photo in kind of self-supporting Li-ABW molecular screen membrane.Wherein, (a) figure is diameter 40mm, with a thickness of 4mm's
Photo, (b) figure is diameter 40mm, and with a thickness of the photo of 6mm, (c) figure is diameter 40mm, with a thickness of the photo of 8mm；
Fig. 2 is the schematic device for water demineralization；
Fig. 3 is the FESEM photo of the obtained self-supporting Li-ABW molecular screen membrane of example 1.
Below in conjunction with drawings and examples, the present invention is described in further detail.
Specific embodiment
By applicant, further study show that, self-supporting Li-ABW molecular screen membrane can be used in separating calcium ion, below
Embodiment in, applicant provide self-supporting Li-ABW molecular screen membrane separation calcium ion application example.It should be noted that with
Under embodiment only for preferably annotating the present invention, the present invention is not limited to these Examples.
The preparation method of self-supporting Li-ABW molecular screen membrane, according to Chinese patent application (application number:
201810126623.1) method carry out, it may be assumed that
Raw material use CFB flyash, white carbon black, lithium hydroxide and deionized water, wherein CFB flyash, white carbon black,
Lithium hydroxide, deionized water mass ratio be 1:0.18:0.1~0.12:0.96~1.
(1) CFB flyash is purchased from Co., Ltd of Zhun Neng group of Shenhua.Using preceding drying, vibromill grinding 30 seconds.
The main oxides of CFB flyash form (mass percent): SiO2(35.14%), CaO (2.86%), Al2O3
(45.35%), Na2O (0.08%), MgO (0.23%), K2O (0.34%), Fe2O3(2.61%), TiO2(1.82%), P2O5
(0.12%), SO3(0.54%), LOI (10.91%).
(2) white carbon black (precipitation method) are purchased from Shanghai Bei Mo Industrial Co., Ltd., white powder, SiO2Content >=90%, than
Surface area: 200m2/g。
(3) lithium hydroxide (anhydrous), is purchased from Shanghai Mike's woods biochemical technology Co., Ltd, analytical reagents, molecular weight:
23.95g/mol。
(4) deionized water, laboratory self-control.
(5) referring to fig. 2, membrane separation device is made of membrane filter, buffer unit and vacuum pump 10.Wherein, membrane filter
By Buchner funnel 1, bottle,suction 2, self-supporting Li-ABW molecular screen membrane 3 and O-ring composition, concrete function is by self-supporting Li-
ABW molecular screen membrane 3 is fixed in Buchner funnel 1 with O-ring.
Buffer unit is made of bottle,suction 5, two way cock 6, quadrature tube 7 and diplopore plug 8 and differential pressure regulator 9, specifically
It is assembled according to Fig. 2.
Vacuum pump 10 uses circulating water type vacuum pump, is purchased from Zhengzhou Great Wall Instrument Ltd., model SHB- III.
(6) membrane separation device is assembled according to Fig. 2, simulation hard water addition is sealed with self-supporting Li-ABW molecular screen membrane 3
In Buchner funnel 1, vacuum pump 10 is opened, and adjust pressure difference with differential pressure regulator 9.
(9) filtrate is collected, the Ca in ICP-OES detection filtrate is used2+Concentration.
(10) preparation of self-supporting Li-ABW molecular screen membrane is specifically implemented according to the following steps:
1) CFB flyash is weighed by formula ratio；
2) white carbon black is weighed by formula ratio；
3) weighed CFB flyash is uniformly mixed with white carbon black, obtains mixture；
4) lithium hydroxide is weighed by formula ratio, be placed in beaker；
5) deionized water is weighed by formula ratio, dissolves lithium hydroxide；
6) lithium hydroxide solution is placed in blender, by the mixture merging blender of step 3), is stirred to get
Even slurry；
7) slurry is contained into die for molding, mold is diameter 40mm, with a thickness of the disk stainless steel mould of 2~10mm.
Mold is sealed with plastic film hermetic bag, is placed in 80 DEG C of maintenances in insulating box and is demoulded afterwards for 24 hours, obtains block CFB geopolymer；
8) above-mentioned block CFB geopolymer is placed in reaction kettle, it is 0~4mol/L that 50mL concentration is added into reaction kettle
Lithium hydroxide solution, seal kettle, in 120~180 DEG C, under self-generating pressure, through Li+It takes out, does after 12~36h of guidance reaction
It is dry, obtain self-supporting Li-ABW molecular screen membrane.
It is self-supporting Li-ABW molecular screen membrane separation calcium ion below using specific embodiment:
Embodiment 1:
(1) diameter 40mm is taken, the self-supporting Li-ABW molecular screen membrane (a of Fig. 1 schemes) of thickness 4mm is fixed on cloth with O-ring
In family name's funnel.
(2) according to assembling membrane separation device shown in Fig. 2.
(3) pure water flux of the self-supporting Li-ABW molecular screen membrane under different pressure differences is demarcated, the results are shown in Table 1, so
Diaphragm is dried afterwards.
(4) CaCl of 200mg/L is prepared2Solution is as simulation hard water.
(5) simulation hard water addition is sealed in the Buchner funnel of self-supporting Li-ABW molecular screen membrane, opens vacuum pump, and
Adjusting pressure difference with buffer unit is 0.06MPa.
(6) penetrating fluid is collected, the Ca in ICP-OES detection filtrate is used2+Concentration is 0.37mg/L, and separative efficiency is
99.8%.
Table 1: the pure water flux (kg/m under self-supporting Li-ABW molecular screen membrane difference pressure difference2·h)
Embodiment 2:
(1) diameter 40mm is taken, the self-supporting Li-ABW molecular screen membrane (b of Fig. 1 schemes) of thickness 6mm is fixed on cloth with O-ring
In family name's funnel.
(2) according to assembling membrane separation device shown in Fig. 2.
(3) pure water flux of the self-supporting Li-ABW molecular screen membrane under different pressure differences is demarcated, the results are shown in Table 1, so
Diaphragm is dried afterwards.
(4) CaCl of 400mg/L is prepared2Solution is as simulation hard water.
(5) simulation hard water addition is sealed in the Buchner funnel of self-supporting Li-ABW molecular screen membrane, opens vacuum pump, and
Adjusting pressure difference with buffer unit is 0.06MPa.
(6) penetrating fluid is collected, the Ca in ICP-OES detection filtrate is used2+Concentration is 0.29mg/L, and separative efficiency is
99.9%.
Embodiment 3:
(1) diameter 40mm is taken, the self-supporting Li-ABW molecular screen membrane (c of Fig. 1 schemes) of thickness 8mm is fixed on cloth with O-ring
In family name's funnel.
(2) according to assembling membrane separation device shown in Fig. 2.
(3) pure water flux of the self-supporting Li-ABW molecular screen membrane under different pressure differences is demarcated, the results are shown in Table 1, so
Diaphragm is dried afterwards.
(4) CaCl of 400mg/L is prepared2Solution is as simulation hard water.
(5) simulation hard water addition is sealed in the Buchner funnel of self-supporting Li-ABW molecular screen membrane, opens vacuum pump, and
Adjusting pressure difference with buffer unit is 0.06MPa.
(6) penetrating fluid is collected, the Ca in ICP-OES detection filtrate is used2+Concentration is 0.29mg/L, and separative efficiency is
99.9%.
Claims (3)
1. the application that self-supporting Li-ABW molecular screen membrane is used to separate calcium ion in hard water.
2. application as described in claim 1, which is characterized in that the self-supporting Li-ABW molecular screen membrane diameter is 40mm,
With a thickness of 6~8mm, operation pressure difference is 0.01~0.09MPa, Ca in hard water2+Concentration is 100mg/L~400mg/L.
3. application as claimed in claim 2, which is characterized in that the implementation steps of calcium ion are as follows in specific separation hard water:
(1) self-supporting Li-ABW molecular screen membrane is fixed in membrane filter, by pipeline connect membrane filter, buffer unit and
Vacuum pump demarcates water flux；
(2) with CaCl2Solution prepares Ca as simulation hard water2+Concentration is the hard water solution of 100mg/L~400mg/L；
(3) hard water described in step (2) is added in membrane filter described in step (1), opens vacuum pump, and pass through buffering dress
Setting and adjusting pressure difference is 0.01~0.09MPa；
(4) penetrating fluid is collected, the Ca in penetrating fluid is detected by inductively coupled plasma atomic emission (ICP-OES)2+Ion
Concentration.
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| CN201810840385.0A CN109012225B (en) | 2018-07-27 | 2018-07-27 | Application of self-supporting Li-ABW molecular sieve membrane in separation of calcium ions in hard water |
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Cited By (2)
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| CN110975647A (en) * | 2019-11-26 | 2020-04-10 | 西安建筑科技大学 | Preparation method and application of ZnO/CuO semiconductor composite inorganic film |
| CN111632575A (en) * | 2019-03-01 | 2020-09-08 | 诺和锐驰科技有限责任公司 | Composite adsorbent and preparation method thereof |
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