CN106315614A - Preparation method of modified Y-type molecular sieve - Google Patents

Preparation method of modified Y-type molecular sieve Download PDF

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Publication number
CN106315614A
CN106315614A CN201610763029.4A CN201610763029A CN106315614A CN 106315614 A CN106315614 A CN 106315614A CN 201610763029 A CN201610763029 A CN 201610763029A CN 106315614 A CN106315614 A CN 106315614A
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China
Prior art keywords
molecular sieve
type molecular
alkali
preparation
modification
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CN201610763029.4A
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Chinese (zh)
Inventor
孙浩
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Hope Technology (tianjin) Ltd By Share Ltd
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Hope Technology (tianjin) Ltd By Share Ltd
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Priority to CN201610763029.4A priority Critical patent/CN106315614A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • 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
    • C01B39/24—Type Y
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/56—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with multiple filtering elements, characterised by their mutual disposition
    • B01D46/62—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with multiple filtering elements, characterised by their mutual disposition connected in series
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/06—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with moving adsorbents, e.g. rotating beds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/72—Organic compounds not provided for in groups B01D53/48 - B01D53/70, e.g. hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/81—Solid phase processes
    • B01D53/82—Solid phase processes with stationary reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/204—Inorganic halogen compounds
    • B01D2257/2045—Hydrochloric acid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027

Abstract

The invention discloses a preparation method of a modified Y-type molecular sieve. The preparation method is characterized in that a NaY molecular sieve, alkali and water are mixed in proportion, a water solution of the molecular sieve and alkali is beaten, and the molecular sieve is subjected to alkali treatment at the temperature of 80-120 DEG C for 5-24 h; the Y-type molecular sieve subjected to alkali treatment is subjected to ion exchange and then subjected to hydrothermal roasting at the temperature of 500-600 DEG C for 1-2 h, and the modified Y-type molecular sieve is obtained. Calcium ions are used for modifying the Y-type molecular sieve, a layer of calcium is formed on the surface of the molecular sieve through exchange of calcium and sodium, organic waste gas containing alcohol can be effectively adsorbed by means of the performance of a complex compound prepared from calcium ions and alcoholic hydroxyl groups, and the dissociation temperature of the complex compound is lower, so that the desorption temperature of the molecular sieve is reduced, and the energy consumption of an enterprise is reduced during treatment of waste gas.

Description

A kind of preparation method of the Y type molecular sieve of modification
Technical field
The invention belongs to molecular sieve preparation field, be specifically related to the preparation method of the Y type molecular sieve of a kind of modification.
Background technology
Zeolite runner Adsorption Concentration device uses adsorption-desorption-concentration to incinerate three continuous programs, is mainly used in organic The improvement of waste gas；It is particularly suitable for Wind Volume, low concentration occasion.This adsorbent equipment, with ceramic fibre as base material, is made cellular Big disk colyliform system, wheel surface coating hydrophobic zeolite do adsorbent, therefore zeolite, namely the type of molecular sieve and Character directly determines the treatment effect of organic exhaust gas.The modification technology of research molecular screen material, including changing molecular sieve pore passage knot Structure, surface polarity, it is thus achieved that there is the Y type molecular sieve of merit, and screening is applicable to dividing of different VOC Son sieve is used for researching and developing novel molecular sieve and absorbs-be desorbed resource recovery technology.Molecular sieve adsorption effect of the prior art only exists 80%, can not completely adsorb, and the temperature being desorbed needs is high, energy consumption is bigger.
Summary of the invention
For the problems referred to above, the present invention provides the preparation method of the Y type molecular sieve of a kind of modification, can contain alcohols by active adsorption Temperature needed for the organic exhaust gas of compound, and desorption is relatively low, reduces the Energy in use of enterprise.
The present invention solves the preparation side that above-mentioned technical problem be the technical scheme is that the Y type molecular sieve of a kind of modification Method, it is characterised in that comprise the following steps:
(1) NaY molecular sieve, alkali and water are mixed according to the mass ratio of 1～2: 0.5～2: 4～10, by molecular sieve and alkali Aqueous solution is pulled an oar, and under the temperature conditions of 80～120 DEG C, molecular sieve is implemented alkali and processes 5～24h；
(2) the alkali-treated Y type molecular sieve that step (1) obtains being carried out ion exchange, molecular sieve butt joins dense Degree is in the Ca saline solution of 0.5～2mol/L, the mol ratio of molecular sieve and calcium be 1:1～1.5,80～100 DEG C of stirrings 4～ 10h, at least carries out primary ions exchange；
(3) being filtered by the molecular sieve that step (2) obtains, hydrothermal calcine 500～600 DEG C carry out 1～2h, obtain modification Y type molecular sieve.
Further, the alkali of described step (1) is sodium hydroxide or sodium metaaluminate.
Further, after described step (1) carries out alkali process to molecular sieve, filter, filter cake Ca saline in step (2) Solution washs several times, controls the pH value of filtrate between 5～7.
Further, the calcium salt in described step (2) is calcium chloride or dalcium biphosphate.
Further, described step (2) is repeated twice.
Further, described step (3) is repeated four times.
The Y type molecular sieve of a kind of modification, it is characterised in that prepared by the method described in above-mentioned any one.
It is an advantage of the current invention that: 1, the present invention uses calcium ion modification Y type molecular sieve, by the exchange of calcium Yu sodium, be The surface of molecular sieve form one layer of calcium, utilize calcium ion and alcoholic extract hydroxyl group to form the performance of complex, can effectively adsorb containing alcohol Organic exhaust gas, and the dissociation temperature of complex is relatively low so that the desorption temperature of molecular sieve reduces, and reduces when exhaust-gas treatment The energy consumption of enterprise；
2, existing Y type molecular sieve is prepared method of modifying and be all employ greatly substantial amounts of ammonium salt, is causing the same of environmental pollution Time so that subsequent treatment cost is greatly increased, and the present invention does not use the reagent of Nitrogen-and Phosphorus-containing, environmentally friendly.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is clearly and completely described, it is clear that described reality Executing example is a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area The every other embodiment that art personnel are obtained under not making creative work premise, broadly falls into the model of present invention protection Enclose.
Embodiment 1:
(1) NaY molecular sieve, alkali and water are mixed according to the mass ratio of 1: 0.5: 10, the aqueous solution of molecular sieve with alkali is beaten Slurry, implements alkali to molecular sieve under the temperature conditions of 80～120 DEG C and processes 5h；
(2) the alkali-treated Y type molecular sieve that step (1) obtains being carried out ion exchange, molecular sieve butt joins dense In the degree Ca saline solution for 0.5mol/L, molecular sieve is 1:1 with the mol ratio of calcium, 80～100 DEG C of stirrings 4～10h,
(3) being filtered by the molecular sieve that step (2) obtains, hydrothermal calcine 500～600 DEG C carry out 1～2h, repeat step (2) and step (3) obtain modification Y type molecular sieve.
The alkali of described step (1) is sodium hydroxide or sodium metaaluminate.
After molecular sieve being carried out alkali process in described step (1), filtering, the Ca saline solution in filter cake step (2) is washed Wash several times, control the pH value of filtrate between 5～7.
Calcium salt in described step (2) is calcium chloride or dalcium biphosphate.
Utilize the molecular sieve obtained in embodiment 1 to be coated on zeolite runner, carry out exhaust-gas treatment test, technological process: Gas collection+chemical absorbing+zeolite runner+catalysis burning
Major pollutants: isoamyl alcohol, ethanol etc., containing a small amount of HCl
Treatment scale: 16000m3/h
Treatment effeciency: 96%
Desorption temperature is less than 200 DEG C.
Process introduction: to enterprise's metformin hydrochloride workshop VOCs treatment, waste gas employing wet scrubbing+remove Mist, all waste gases are by multistage filtering as pretreatment, and effective dust intercepted contained by waste gas is to prevent from blocking zeolite, and goes Except partial organic substances administers pressure to alleviate succeeding body technique, after process, waste gas enters zeolite runner and concentrates+catalysis burning (CO) main process.Treatment effeciency is up to 96%, inlet gas concentration 300mg/m3, it is 12mg/m after process3, far below Tianjin " industrial undertaking's Volatile organic emissions controls standard " (DB12/524-2014) is to pharmaceuticals industry limit value 40mg/m3Requirement.
Various embodiments above only in order to technical scheme to be described, is not intended to limit；Although with reference to aforementioned each reality Execute example the present invention has been described in detail, it will be understood by those within the art that: its still can to aforementioned respectively Technical scheme described in embodiment is modified, or the most some or all of technical characteristic is carried out equivalent；And These amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.

Claims (7)

1. the preparation method of a modified Y type molecular sieve, it is characterised in that comprise the following steps:
(1) NaY molecular sieve, alkali and water are mixed according to the mass ratio of 1～2: 0.5～2: 4～10, water-soluble by molecular sieve and alkali Liquid is pulled an oar, and under the temperature conditions of 80～120 DEG C, molecular sieve is implemented alkali and processes 5～24h；
(2) the alkali-treated Y type molecular sieve that step (1) obtains being carried out ion exchange, molecular sieve butt joins concentration and is In the Ca saline solution of 0.5～2mol/L, molecular sieve is 1:1～1.5,80～100 DEG C of stirrings 4～10h with the mol ratio of calcium, extremely Carry out primary ions exchange less；
(3) being filtered by the molecular sieve that step (2) obtains, hydrothermal calcine 500～600 DEG C carry out 1～2h, obtain the Y of modification Type molecular sieve.
The preparation method of the Y type molecular sieve of a kind of modification the most according to claim 1, it is characterised in that described step (1) Alkali be sodium hydroxide or sodium metaaluminate.
The preparation method of the Y type molecular sieve of a kind of modification the most according to claim 1, it is characterised in that described step (1) In molecular sieve is carried out alkali process after, filter, filter cake with the Ca aqueous salt solu-tion in step (2) several times, controls filtrate PH value is between 5～7.
The preparation method of the Y type molecular sieve of a kind of modification the most according to claim 1, it is characterised in that described step (2) In calcium salt be calcium chloride or dalcium biphosphate.
The preparation method of the Y type molecular sieve of a kind of modification the most according to claim 1, it is characterised in that described step (2) It is repeated twice.
The preparation method of the Y type molecular sieve of a kind of modification the most according to claim 1, it is characterised in that described step (3) It is repeated four times.
7. a modified Y type molecular sieve, it is characterised in that prepared by the method described in claim 1～6 any one.
CN201610763029.4A 2016-08-29 2016-08-29 Preparation method of modified Y-type molecular sieve Pending CN106315614A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108128785A (en) * 2018-03-02 2018-06-08 浙江大学 Using nickel amine complex as the method for template one-step synthesis ITE zeolite molecular sieves
CN113145064A (en) * 2021-03-12 2021-07-23 苏州科技大学 Preparation method of clay mineral-based VOCs adsorbent

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2125314A1 (en) * 1994-06-07 1995-12-08 Raymond Le Van Mao Zeolite materials with enhanced ion exchange capacity
CN1151906A (en) * 1995-12-13 1997-06-18 中国科学院大连化学物理研究所 Zeolite refrigerating absorbent capable of replacing freon
CN1962047A (en) * 2006-10-17 2007-05-16 太原理工大学 Method for preparing molecular sieve absorbent with high adsorption capacity
CN101708183A (en) * 2009-11-10 2010-05-19 浙江大学 Method for improving haemostatic effect of external-use zeolite haemostatic

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2125314A1 (en) * 1994-06-07 1995-12-08 Raymond Le Van Mao Zeolite materials with enhanced ion exchange capacity
CN1151906A (en) * 1995-12-13 1997-06-18 中国科学院大连化学物理研究所 Zeolite refrigerating absorbent capable of replacing freon
CN1962047A (en) * 2006-10-17 2007-05-16 太原理工大学 Method for preparing molecular sieve absorbent with high adsorption capacity
CN101708183A (en) * 2009-11-10 2010-05-19 浙江大学 Method for improving haemostatic effect of external-use zeolite haemostatic

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王晓峰: ""二氧化碳中含氧有机物的吸附分离"", 《中国优秀硕士学位论文全文数据库（电子期刊）工程科技Ｉ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108128785A (en) * 2018-03-02 2018-06-08 浙江大学 Using nickel amine complex as the method for template one-step synthesis ITE zeolite molecular sieves
CN108128785B (en) * 2018-03-02 2020-02-14 浙江大学 Method for synthesizing ITE zeolite molecular sieve by using nickel-amine complex as template agent in one step
CN113145064A (en) * 2021-03-12 2021-07-23 苏州科技大学 Preparation method of clay mineral-based VOCs adsorbent

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Application publication date: 20170111