CN101134572A - Method for processing and separating ultra-fine molecular sieve by employing inorganic membrane integral system - Google Patents
Method for processing and separating ultra-fine molecular sieve by employing inorganic membrane integral system Download PDFInfo
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- CN101134572A CN101134572A CNA2006101219990A CN200610121999A CN101134572A CN 101134572 A CN101134572 A CN 101134572A CN A2006101219990 A CNA2006101219990 A CN A2006101219990A CN 200610121999 A CN200610121999 A CN 200610121999A CN 101134572 A CN101134572 A CN 101134572A
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Abstract
The present invention relates to process of treating and separating superfine molecular sieve in an integrated inorganic film system. The process can perform liquid-solid separation of superfine molecular sieve in high efficiency, combine the reaction treatment and continuous separation of molecular sieve, treating molecular sieve with acid and base without need of neutralization, and obtain molecular sieve with high performance.
Description
Technical field
The present invention relates to a kind of method that adopts inorganic membrane integral system processing and separating ultra-fine molecular sieve.
Background technology
Superfine molecular sieves refers to the molecular sieve particle diameter below 1 μ m, especially less than the close grain molecular sieve of 0.5 μ m, compares with the big crystal grain molecular sieve of routine, has plurality of advantages such as activity is high, selectivity is good.Along with the progress of industry science and technology such as oil refining, chemical industry, its production and application are also more and more widely.A significant problem that faces in the superfine molecular sieves production at present is how to carry out high efficiency liquid-solid separation, and does not influence product performance.In general, molecular sieve is thin more, and its separating difficulty is big more, and particularly nano level molecular sieve is suspended state in liquid, and traditional gravity settling almost can't use; And be the various filtering techniques of filtration medium with the filter cloth, its separation efficiency is very low, and the filtered solution quality also is difficult to guarantee; Adopt ultracentrifuge, solution its efficient lower to solid content is extremely low; Add the flocculation agent filtration and then can influence product performance.Therefore, the liquid-solid separation of superfine molecular sieves often becomes the principal element that influences product yield, cost, quality.
Mineral membrane has separation efficiency height, corrosion-resistant, advantages such as energy consumption is low, device is simple, processing ease in the liquid-solid separation of micron and submicron particle.At present, the application of mineral membrane mainly be the purification of water treatment, industrial chemicals liquid, the catalyst recovery in the liquid-solid catalytic reaction and the filtering separation in the production of inorganic.CN1289632A has reported and has adopted mineral membrane to carry out the reaction separation method of the inorganic superfine powder body of ultrafine yttria, super fine zinc oxide; CN1170775C has reported the separation method that adopts film-integration hydrothermal reaction superfine titanium dioxide; CN1377875A has reported that then mineral membrane is used for the catalyst separating recovery method that p-aminophenol is produced; Chinese patent application 01108189.9 is applied to biological respinse with ceramic-film tube.Mineral membrane is used for the catalyst preparation process especially liquid-solid separation of superfine molecular sieves and then not appearing in the newspapers of processing.
The crystallization last handling process is generally all arranged in the molecular sieve production process, comprise that repetitive scrubbing removes foreign ion, acid, alkali or salt are handled the performance that improves molecular sieve etc.Generally adopt at present and in reaction vessel, carry out acid, alkali or salt processing earlier, enter next step operation after filter cloth filtration or ultracentrifugation separate.Adopt filter cloth to filter or the isolating method of ultracentrifuge, active high close grain molecular sieve is easy to run and decreases when separation and washing, and product yield is low; If add flocculation agent before filtration or the separation, then unformed material also can be sneaked in the molecular sieve finished product, influences the product activity.When adopting acid, alkaline purification, especially during acid treatment, the traditional filtering material generally all is difficult to bear the corrosion of treatment solution, if the solution after will handling neutralizes, then treatment effect does not reach requirement.Simultaneously, this treating processes is an intermittent operation, inefficiency.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts inorganic membrane integral system processing and separating ultra-fine molecular sieve, this method can be carried out the liquid-solid separation of superfine molecular sieves expeditiously, the reaction treatment of molecular sieve can also be combined with separating continuously, and need not neutralization when adopting acid-alkali treatment, can guarantee the performance of molecular sieve effectively.
The accompanying drawing summary
Fig. 1 is the process flow diagram that adopts inorganic membrane integral system processing and separating ultra-fine molecular sieve according to the present invention.
Detailed Description Of The Invention
The inorganic membrane integral system of indication of the present invention comprises the symmetrical or asymmetric perforated membrane (such as 37038 type film pipes of environmental protection Co., Ltd of Yue Yangxin section, 37036 type film pipes etc.) by the inorganic metal of acidproof or alkali, metal oxide or pottery preparation; With reaction or the cut-back tank of the supporting suitable material of selecting according to reaction/treatment conditions of inoranic membrane, pump and respective lines; Backpurge system.
Method of the present invention is that superfine molecular sieves membrane sepn and aftertreatment technology is integrated, forms complete, successive production process, and can avoid traditional neutralization that influences molecular sieve performance and flocculation step.Its detailed process is as follows:
1) with superfine molecular sieves dry powder or slurries in reaction vessel with the washings dilution or add the chemical reagent reaction treatment, when wherein diluting with washings, weaker concn can be 0.001～0.9 of original content, temperature can or be heated to 30～99 ℃ for normal temperature; When adding chemical reagent and handling, the consumption of chemical reagent is about 1～50% based on the molecular sieve dry weight, and can at normal temperatures or be heated to 30～300 ℃ of reactions 0.5～300 hour;
2) will dilute or reaction treatment after the feed liquid that contains superfine molecular sieves continuously to feed the aperture under the pressure of 0.05～1MPa be in the inorganic film tube of 0.01～1 μ m, partially liq medium wherein and foreign ion see through the micropore diameter of mineral membrane outside the cross-flow vent pipe, feed liquid cycles through film pipe and continuous enrichment after the film pipe flows out, reach at 15～50% o'clock to the superfine molecular sieves solid content, to be diluted to solid content be 0.1～30% or add the chemical reagent reaction to add washings in feed liquid;
3) feed liquid is continued circulation and feed the film pipe, impurity ion content is less than normality in penetrating fluid, for example less than 100mg/L, perhaps the reaction treatment of superfine molecular sieves reaches specified requirement, for example penetrating fluid pH value is 6～8, perhaps in the molecular sieve during non-skeleton metal ion processed clean (uv raman spectroscopy characterizes skeleton metal ion peak nothing but), stop dilution washing or reaction treatment;
4) material continues circulation to be concentrated into solid content is 30～60% subsequently, and enrichment feed liquid drying is obtained superfine molecular sieves dry powder.
The solid content of the feed liquid that contains superfine molecular sieves after dilution that obtains in the step 1) of the inventive method or the reaction treatment is 5～30% based on the dry weight of molecular sieve.
Drying in the step 4) of the inventive method can be carried out according to ordinary method, for example in the spraying drying of carrying out under 200-300 ℃ or the tray dried of carrying out under 100-150 ℃.
The washings of the inventive method is selected from water or organic solvent, and organic solvent can be selected ketone, alcohol, ester compounds such as acetone, butanone, ethanol, propyl alcohol, tetraethyl orthosilicate, silicic acid four butyl esters for use.
The chemical reagent that the inventive method is selected for use is that acid is as nitric acid, hydrochloric acid, dilute sulphuric acid, acetic acid etc.; Alkali such as sodium hydroxide, tetraethyl ammonium hydroxide, TPAOH etc.; Or salt such as ammonium nitrate, ammonium chloride etc.
The reaction or the cut-back tank that comprise in the inorganic membrane integral system that the inventive method adopts, the pH value of the selection of pump and respective lines and treatment condition, especially reagent treatment is relevant.Alkalescence or neutrallty condition adopt materials such as stainless steel down, and acidic conditions adopts acidproof pipeline and acid proof pumps such as acid-resistant container, lining tetrafluoroethylene or glass reinforced plastic such as lining enamel or lining glass reinforced plastic down.
In the methods of the invention, behind inorganic film tube work certain hour, have the micropore that solid materials stops up mineral membrane, influence the flux of film, therefore need to adopt pressurized air interval backflushing membrane module, for example adopt pressurized air blowback face, make attached to the material on the face to come off and import in the mobile molecular sieve pulp.
Describe the present invention in detail below in conjunction with accompanying drawing:
As shown in the figure, superfine molecular sieves dry powder or slurries mix with washings or chemical reagent in cut-back tank or reaction vessel 1, under whipped state, handle for some time (temperature can be passed through to feed steam or chilled water modulation in the cover of centre), feed liquid after the processing is pressed into mineral membrane separator 3 through prefilter 2, recycle pump 6, and cross-flow is passed through in mineral membrane separator 3; The partially liq medium is through under meter 5 discharging, enrichment feed liquid return cut-back tank or reaction vessel 1 again.Feed liquid constantly circulates between mineral membrane separator 3 and cut-back tank or reaction vessel 1, and because the separation of liquid medium and continuous enrichment, when feed concentration reaches certain set(ting)value, in feed liquid, add washings or chemical reagent, repeat above process, to reach in specified requirement or the molecular sieve non-skeleton metal ion less than the reaction treatment of certain set(ting)value or superfine molecular sieves processed when clean for impurity ion content in penetrating fluid, stop dilution washing or reaction treatment, material continues circulation and concentrates with oozing out constantly of dilution or reaction solution between container and inorganic film tube subsequently, and enrichment feed liquid drying is obtained superfine molecular sieves dry powder.Among the figure recoiling device 4 in working cycle regularly or not timing ground to the penetrating fluid pressurization, to the recoil of film pipe, recover the flux of film.
The inventive method is compared with separation method with the processing of existing superfine molecular sieves, and significantly advantage is: 1) yield height, can hold back active high close grain molecular sieve effectively when separation and washing; 2) membrane separation unit and treatment unit is integrated, form the serialization production process, technical process is simple, the production efficiency height; 3) handle with separates before and after need not neutralization or interpolation flocculation agent, product performance are unaffected; 4) the foreign ion washing separates totally the product purity height; 5) acid-alkali-corrosive-resisting, the scope of application is extensive.
Embodiment
All wt percentage number average by weight in this specification sheets.
Embodiment 1The washing of ultra-fine ZSM-5 molecular sieve separates
With 1229 liters of solid contents be 10% and the pH value be 13 ZSM-5 molecular sieve pulp (d=1.22g/cm
3) (material is 316L to the cut-back tank 1 of packing into, 5m
3) in, at room temperature adding deionized water, to be diluted to solid content be 5%, is conveyed into pump 6 (material is 321) that (flow velocity is 40m
3/ h) mineral membrane tripping device 3 (37038 type film pipes that adopt environmental protection company limited of Yue Yangxin section to provide, the film pore directly is 0.2 μ m) carry out solid-liquid separation (pressure is 0.3MPa), portion water, foreign ion and unformed material ooze out through inorganic face and give off outside the system, enrichment slurries return cut-back tank 1, so circulating and being concentrated into concentration is solid content about 25%, adding deionized water then in cut-back tank 1 is diluted to and enters mineral membrane tripping device 3 once more behind the solid content about 8% and carry out solid-liquid separation, dilution washing and separation so repeatedly, circulate after four times, recording penetrating fluid pH value is 7.6; Stop washing, slurries continue circulation, and to be concentrated into solid content about 35%, by spraying drying (230 ℃), obtains 145 kilograms in ZSM-5 molecular sieve then, yield 96.7%, and the molecular sieve median size is 270 nanometers.
Embodiment 2The salt of nano-beta molecular sieve is handled and is separated with washing
With 1538 liters of solid contents 25% nano-beta molecular sieve (Na
2O content is 1%) slurries (d=1.30g/cm
3) (material is 0Cr18Ni9Ti to the reaction vessel 1 of packing into, 5m
3) in, add 150 kilograms in ammonium nitrate, in the reaction vessel chuck, feed steam and be warmed up to 90 ℃ (vapor pressure is approximately 0.3MPa), constant temperature 1 hour closes steam then, opens cooling water temperature to normal temperature, is conveyed into pump 6 (material is 321) that (flow velocity is 40m
3/ h) mineral membrane tripping device 3 (37036 type film pipes that adopt environmental protection company limited of Yue Yangxin section to provide, the film pore directly is 0.1 μ m) carry out solid-liquid separation (pressure is 0.2MPa), portion water, foreign ion and unformed material ooze out through inorganic face and give off outside the system, enrichment slurries return reaction vessel 1, so circulation is concentrated into solid content about 40%, adding deionized water then in container 1 is diluted to and enters mineral membrane tripping device 3 once more behind the solid content about 10% and carry out solid-liquid separation, the dilution washing separates 7 times so repeatedly, adopts a meter beta-molecular sieve sample detection Na
2O content stops washing less than 0.05%, and slurries continue circulation, and to be concentrated into solid content be about 45%, by tray dried (120 ℃), obtains 492 kilograms of nano-beta molecular sieves then, yield 98.4%, and the molecular sieve median size is 100 nanometers.
Embodiment 3The acid treatment of superfine Ti ZSM-5 molecular sieve with separate
With 1613 liters of solid contents 20% superfine Ti ZSM-5 molecular sieve pulp (d=1.242/cm
3) lining enamelled reaction vessel 1 (5m packs into
3) in, add the hydrochloric acid double centner of 37% concentration, in the reaction vessel chuck, feed steam and be warmed up to 90 ℃ (vapor pressure is approximately 0.3MPa), constant temperature 3 hours, close steam then, open cooling water temperature, be conveyed into through glass steel pipeline with acid proof pump 6 (lining tetrafluoroethylene pump) that (flow velocity is 40m to normal temperature
3/ h) mineral membrane tripping device 3 (37036 type film pipes that environmental protection company limited of Yue Yangxin section provides, the aperture is 0.1 μ m) carry out solid-liquid separation (pressure is 0.2MPa), portion water, foreign ion and unformed material ooze out through inorganic face and give off outside the system, enrichment slurries return reaction vessel 1, so circulation is concentrated into solid content about 25%, adding deionized water then in container 1 is diluted to and enters mineral membrane tripping device 3 once more behind the solid content about 8% and carry out solid-liquid separation, the dilution washing separates 6 times so repeatedly, and recording penetrating fluid pH value is 6.5; Stop washing, slurries continue circulation, and to be concentrated into solid content about 42%, then by tray dried (120 ℃), obtain 380 kilograms in superfine Ti ZSM-5 molecular sieve, yield 95%, the molecular sieve median size is 200 nanometers, estimate through the phenol hydroxylation reactive behavior, its transformation efficiency is 23%.
Comparative Examples 1The washing of adopting the ultracentrifugation machine to carry out ultra-fine ZSM-5 molecular sieve separates
With 1229 liters of solid contents be 10% and the pH value be 13 ZSM-5 molecular sieve pulp (d=1.22g/cm
3) (material is 316L to the cut-back tank of packing into, 5m
3) in, be conveyed into pump (material is 321) that (flow velocity is 20m
3/ h) ultracentrifuge (oasis, Nanjing machine works product, LWS420*1680-ND type horizontal centrifuge) carries out solid-liquid separation, portion water, foreign ion, unformed material and part superfine crystal particle molecular sieve are separated into liquid phase through hypervelocity and discharge, and solid phase (mainly being molecular sieve and water) is unloaded to cut-back tank (5m by scraper
3), and adding deionized water in cut-back tank, to be diluted to solid content about 5%, separating, washing is 7 times so repeatedly, records liquid phase PH valve less than 9; Stop washing, solid phase is collected, by spraying drying (260 ℃), obtain ZSM-5 molecular sieve double centner then, yield 66.7%, the molecular sieve median size is 300 nanometers.
Comparative Examples 2Superfine Ti ZSM-5 molecular sieve acidifying post neutralization also adopts the filter cloth filtration washing to separate
With 1613 liters of solid contents 20% superfine Ti ZSM-5 molecular sieve pulp (d=1.24g/cm
3) lining enamelled reaction vessel (5m packs into
3) in, the hydrochloric acid double centner that adds 37% concentration, in the reaction vessel chuck, open steam and be warmed up to 90 ℃ (vapor pressure is approximately 0.3MPa), constant temperature 3 hours closes steam then, opens cooling water temperature to normal temperature, with ammoniacal liquor slurries are neutralized, filter in whizzer (the SS300-1500 type of Zhangjiagang Huada Centrifugal Manufacturing Co., Ltd.) with filter cloth (as 9503 type filter clothes of Dalian filter cloth factory), filter cake deionized water repetitive scrubbing, salt concn is lower than 100mg/L in washings; Stop washing, filter cake is by tray dried (120 ℃), obtain 310 kilograms in superfine Ti ZSM-5 molecular sieve, yield 77.5%, the molecular sieve median size is 210 nanometers, estimate through the phenol hydroxylation reactive behavior, phenol conversion is 18%, than using mineral membrane without the direct isolating transformation efficiency in neutralization back low 5%.
Table 1 embodiment effect comparison table
| Separation method | Superfine molecular sieves slurries type | Could operate continuously | Yield, % | Product performance | |
| Embodiment 1 | Inorganic membrane integral system | Ultra-fine ZSM-5 molecular sieve pulp | Can | 96.7 | |
| Embodiment 2 | The nano-beta molecular sieve slurries | Can | 98.4 | ||
| Embodiment 3 | Superfine Ti ZSM-5 molecular sieve pulp | Can | 95 | Phenol hydroxylation reaction conversion ratio 23% | |
| Comparative Examples 1 | Ultracentrifuge | Ultra-fine ZSM-5 molecular sieve pulp | Can | 66.7 | |
| Comparative Examples 2 | Filter cloth | Superfine Ti ZSM-5 molecular sieve pulp | Not | 77.5 | Phenol hydroxylation reaction conversion ratio 18% |
Claims (8)
1. one kind is adopted inorganic membrane integral system to handle and the method for separating ultra-fine molecular sieve, may further comprise the steps:
1) with superfine molecular sieves dry powder or slurries in reaction vessel with the washings dilution or add the chemical reagent reaction treatment, when wherein diluting with washings, weaker concn is 0.001～0.9 of an original content, temperature is normal temperature or is heated to 30～99 ℃; When adding chemical reagent and handling, the consumption of chemical reagent is 1～50% based on the molecular sieve dry weight, and at normal temperatures or be heated to 30～300 ℃ of reactions 0.5～300 hour;
2) will dilute or reaction treatment after the feed liquid that contains superfine molecular sieves continuously to feed the aperture under the pressure of 0.05～1MPa be in the inorganic film tube of 0.01～1 μ m, partially liq medium wherein and foreign ion see through the micropore diameter of mineral membrane outside the cross-flow vent pipe, feed liquid cycles through film pipe and continuous enrichment after the film pipe flows out, reach at 15～50% o'clock to the superfine molecular sieves solid content, to be diluted to solid content be 0.1～30% or add the chemical reagent reaction to add washings in feed liquid;
3) feed liquid is continued circulation and feed the film pipe, impurity ion content is less than normality in penetrating fluid, perhaps the reaction treatment of superfine molecular sieves reaches specified requirement, and perhaps non-skeleton metal ion is processed when clean in the molecular sieve, stops dilution washing or reaction treatment;
4) material continues circulation to be concentrated into solid content is 30～60% subsequently, and enrichment feed liquid drying is obtained superfine molecular sieves dry powder.
2. proceed in the penetrating fluid foreign matter content less than 100mg/L according to the process of claim 1 wherein in step 3), or penetrating fluid pH value is 6～8, perhaps uv raman spectroscopy characterizes skeleton metal ion peak nothing but.
3. according to the process of claim 1 wherein that described inorganic membrane integral system comprises mineral membrane, with supporting reaction or cut-back tank, pump and respective lines and the back-purge system of mineral membrane.
4. according to the method for claim 3, wherein the material of reaction or cut-back tank, pump and respective lines depends on treatment condition, under alkalescence or neutrallty condition, adopt materials such as stainless steel, and under acidic conditions, adopt acidproof pipeline and acid proof pumps such as acid-resistant container, lining tetrafluoroethylene or glass reinforced plastic such as lining enamel or lining glass reinforced plastic.
5. according to the process of claim 1 wherein that washings is water or organic solvent; Chemical reagent is acid, alkali or salt; And need not to carry out acid-base neutralisation or flocculation before and after handling.
6. according to the method for claim 5, wherein said organic solvent is selected from acetone, butanone, ethanol, propyl alcohol, tetraethyl orthosilicate or silicic acid four butyl esters, and described chemical reagent is selected from nitric acid, hydrochloric acid, dilute sulphuric acid, acetic acid, sodium hydroxide, tetraethyl ammonium hydroxide, TPAOH, ammonium nitrate or ammonium chloride.
7. according to the process of claim 1 wherein that described mineral membrane is symmetry or the asymmetric porous-film by inorganic metal, metal oxide or pottery preparation.
8. according to the process of claim 1 wherein,, make attached to the material on the face to come off and import in the mobile molecular sieve pulp preferably by high-pressure air blowback face with pressurized air interval backflushing membrane module.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101219990A CN101134572A (en) | 2006-08-30 | 2006-08-30 | Method for processing and separating ultra-fine molecular sieve by employing inorganic membrane integral system |
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|---|---|---|---|
| CNA2006101219990A CN101134572A (en) | 2006-08-30 | 2006-08-30 | Method for processing and separating ultra-fine molecular sieve by employing inorganic membrane integral system |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145301A (en) * | 2010-12-29 | 2011-08-10 | 中国天辰工程有限公司 | Method for washing micron-level molecular sieve containing nano impurities |
| CN103084204A (en) * | 2011-10-27 | 2013-05-08 | 中国石油化工股份有限公司 | Method for treating slurry containing nanometer beta molecular sieve |
| CN103752083A (en) * | 2014-02-14 | 2014-04-30 | 大连龙泰科技发展有限公司 | Filtering separation method for nanometer molecular sieve slurry |
| CN103964464A (en) * | 2013-01-30 | 2014-08-06 | 中国石油天然气股份有限公司 | Preparation method of NaY molecular sieve with improved degree of crystallinity, dispersibility and stability |
| CN113428871A (en) * | 2021-07-12 | 2021-09-24 | 宁夏美邦寰宇化学有限公司 | Separation and purification method and separation and purification system of titanium-silicon molecular sieve |
-
2006
- 2006-08-30 CN CNA2006101219990A patent/CN101134572A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145301A (en) * | 2010-12-29 | 2011-08-10 | 中国天辰工程有限公司 | Method for washing micron-level molecular sieve containing nano impurities |
| CN103084204A (en) * | 2011-10-27 | 2013-05-08 | 中国石油化工股份有限公司 | Method for treating slurry containing nanometer beta molecular sieve |
| CN103084204B (en) * | 2011-10-27 | 2015-03-25 | 中国石油化工股份有限公司 | Method for treating slurry containing nanometer beta molecular sieve |
| CN103964464A (en) * | 2013-01-30 | 2014-08-06 | 中国石油天然气股份有限公司 | Preparation method of NaY molecular sieve with improved degree of crystallinity, dispersibility and stability |
| CN103964464B (en) * | 2013-01-30 | 2016-05-11 | 中国石油天然气股份有限公司 | A kind of NaY molecular sieve preparation method that improves degree of crystallinity, dispersiveness and stability |
| CN103752083A (en) * | 2014-02-14 | 2014-04-30 | 大连龙泰科技发展有限公司 | Filtering separation method for nanometer molecular sieve slurry |
| CN103752083B (en) * | 2014-02-14 | 2016-04-06 | 大连龙泰科技发展有限公司 | A kind of filter separation method of nanometer molecular sieve slurry |
| CN113428871A (en) * | 2021-07-12 | 2021-09-24 | 宁夏美邦寰宇化学有限公司 | Separation and purification method and separation and purification system of titanium-silicon molecular sieve |
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