CN109621732A - A kind of rapid detection method of molecular screen membrane - Google Patents
A kind of rapid detection method of molecular screen membrane Download PDFInfo
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- CN109621732A CN109621732A CN201811519512.3A CN201811519512A CN109621732A CN 109621732 A CN109621732 A CN 109621732A CN 201811519512 A CN201811519512 A CN 201811519512A CN 109621732 A CN109621732 A CN 109621732A
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- membrane
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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- Chemical Kinetics & Catalysis (AREA)
- Sampling And Sample Adjustment (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of rapid detection methods of molecular screen membrane.This method comprises: molecular screen membrane membrane tube one end is blocked, by the non-valve side of other end connecting detection device, detection device valve side connects vacuum pump；The detection device includes communicating pipe, threeway, vacuum meter, valve, and wherein threeway Single port is connect with vacuum meter, and Single port is controlled to a vacuum pump through valve, the last one port with membrane tube by connecting communicating pipe when use；Detection device valve, vacuum pump are opened, membrane tube is unqualified if vacuum degree cannot reach setting numerical value, does not need to carry out next step operation；If vacuum degree reaches requirement, detection device valve is closed after vacustat, closes vacuum pump, starts timing；Setting numerical value is decayed to vacuum degree, stops timing；Judge molecular screen membrane quality according to the vacuum degree retention time, when the vacuum degree retention time within the set range, judge membrane tube qualified product to be measured；When the vacuum degree retention time not within the set range, judge that membrane tube product quality is unqualified.This method equipment is simple, easy to operate, detection time is short, is particularly suitable for detecting a large amount of molecular screen membrane products in time.
Description
Technical field
The invention belongs to the technical fields of inorganic material preparation and detection, are related specifically to through vacuum method Quick test tube
The method of formula molecular screen membrane quality.
Background technique
Membrane separation technique compared with conventional separation techniques have low energy consumption, pollution less, be easy to couple with other separation processes,
Use condition is mild, is easy to the advantages that amplifying, and is widely used in many industrial circles.Molecular screen membrane is as inoranic membrane
One kind have many advantages, such as that high temperature resistant, anticorrosive, high mechanical strength, separation flux are big, with more uniform cellular structure and easily
The architectural characteristic of modulation.NaA type molecular screen membrane is with the fastest developing speed, and NaA molecular sieve has octatomic ring cellular structure, effective aperture
For 0.42nm, hydrophily is very strong, therefore separating property outstanding is shown in terms of organics dehydration.Type T molecular sieve film silicon
Aluminium ratio is 3~4, and hydrophily is only second to NaA type molecular screen membrane, adsorbs aperture in 0.5nm or so, and have good acidproof
Property.
The separation and permeation flux of molecular screen membrane determine the quality of film quality.Qualified molecular screen membrane is with higher
Separation and certain membrane flux.Under scanning electron microscope, film surface shows higher crystallinity, uncrystallized zeolite granular
With colloidal particles almost without or seldom, without apparent gap between zeolite, and form a large amount of twin structures.Film surface is whole
It shows continuous, uniform, fine and close.The unqualified molecular screen membrane product that separation is not high, membrane flux is excessive, it may be possible to synthesize
Crystal does not generate fine and close, continuous film layer in film surface in the process, and crystallinity is not high, and the gap of intracrystalline pore is excessive；And film is logical
Measure too low unqualified molecular screen membrane product, it may be possible to which film surface colloid is excessive, and crystal duct and surface intracrystalline pore is completely stifled
Extremely or membrane tube synthesis rear surface do not clean up thoroughly not can enter so as to cause moisture surface holes road reach separation effect
Fruit.
Currently, the research of molecular screen membrane gradually enters large-scale production and engineering stage from laboratory stage.With
The increase of membrane tube output, membrane tube test problems become increasingly conspicuous.There are two types of detection method apply than wide: " dead end method " be by
Film sealing is fixed in membrane module, and being passed through gas makes membrane tube two sides keep certain pressure difference, keeps certain temperature and time, is led to
The gas permeation flux for crossing gas flowmeter measurement membrane tube, the quality of membrane tube is judged according to flux；" infiltration evaporation experiment detection
Method " is that membrane tube is packed into membrane module, and water-containing organic solvent is flowed in molecular screen membrane film layer side, and carrier side vacuumizes, passes through
It detects under certain temperature, the quality of unit time penetrating fluid and solution composition judge the quality of membrane tube.Above-mentioned detection method,
Device process is complicated, cumbersome, detection time is long, and the molecular screen membrane product of mass production can not be accomplished to examine in time
Assessment valence.Therefore, it is extremely urgent to develop a kind of quickly and effectively molecular screen membrane detection method.
Summary of the invention
The technical problem to be solved by the present invention is to complicated for conventional molecular sieve membrane detection method device process, operation is numerous
Trivial, the disadvantages of detection time is long, provides and a kind of is sentenced by retention time of detection membrane tube under the conditions of certain vacuum degree to detect
The method of disconnected molecular screen membrane quality.This method equipment is simple, easy to operate, detection time is short, is particularly suitable for a large amount of molecular sieves
Film product is detected in time.
The present invention is a kind of rapid detection method of molecular screen membrane, is carried out as steps described below:
(1) molecular screen membrane membrane tube one end is blocked, by the non-valve side of other end connecting detection device, detection device valve
Side connects vacuum pump；
(2) opening detecting device valve opens vacuum pump, and membrane tube is unqualified if vacuum degree cannot reach setting numerical value,
It does not need to carry out next step operation；If vacuum degree reaches requirement, operation detection in next step is carried out to vacustat；
(3) detection device valve is closed, vacuum pump is closed, starts timing；
(4) setting numerical value is decayed to vacuum degree, stops timing；
(5) molecular screen membrane quality is judged according to the vacuum degree retention time, when the vacuum degree retention time is in setting range
It is interior, judge membrane tube qualified product to be measured；When the vacuum degree retention time not within the set range, judge membrane tube product matter
It measures unqualified；
The detection device includes communicating pipe, threeway, vacuum meter, valve, and wherein threeway Single port is connect with vacuum meter,
Single port is controlled to a vacuum pump through valve, the last one port with membrane tube by connecting communicating pipe when use.
In the method for the present invention, the molecular screen membrane is the tubular types such as NaA type molecular screen membrane, type T molecular sieve film, ZSM-5 type load
Load type molecular screen membrane it is one or more.
Tubing, threeway, connector in detection device of the present invention preferably use stainless steel material；Valve preferably uses needle valve.
The method of the present invention is compared with existing molecular screen membrane detection method, and beneficial outcomes are: apparatus and process is simple, operation
Simplicity, detection speed is fast, is suitble to the detection of high-volume membrane tube.By retention time of the membrane tube under certain vacuum degree, can sentence
The quality of disconnected molecular screen membrane quality.And can tentatively conclude the problem membrane tube institute problem, so as to adjust with improve molecule
The process of sieve membrane synthesis.Detection method of the invention and infiltration evaporation experiment detection method compare test, wherein permeating
Vaporization experiment detection is detected at 80 DEG C using 95wt/% ethyl alcohol, almost the same to membrane tube evaluation testing result.
Detailed description of the invention
Fig. 1 is the quick overhaul flow chart of molecular screen membrane in the embodiment of the present invention.
Fig. 2 is the infiltration evaporation experimental provision structural schematic diagram of existing molecular screen membrane.
In Fig. 2: 1 magnetic stirring apparatus, 2 constant temperature oil baths, 3 membrane tubes, 4 water/alcohol mixture head tank, 5 membrane modules, 6 silicon
Glue vacuum tube, 7 cold-traps, 8 vacuum buffer bottles, 9 vacuum meters, 10 vacuum pumps.
Specific embodiment
To make those skilled in the art better understand technical solution of the present invention, 1 comes to this hair with reference to the accompanying drawing
The molecular screen membrane rapid detection method of bright offer is described in detail, it is clear that described embodiment is only the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
All other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Following example is specifically carried out as steps described below using the rapid detection method of molecular screen membrane of the present invention:
(1) molecular screen membrane membrane tube one end is blocked, by the non-valve side of other end connecting detection device, detection device valve
Side connects vacuum pump；The detection device includes that communicating pipe, threeway, vacuum meter, valve, wherein threeway Single port and vacuum meter connect
It connects, Single port is controlled to a vacuum pump through valve, the last one port with membrane tube by connecting communicating pipe when use；Specific embodiment
Select NaA molecular sieve membrane product, length 800mm, pipe outside diameter 12mm, bore 8mm.
(2) opening detecting device valve opens vacuum pump, the film if vacuum degree (gauge pressure) cannot reach 0.095Mpa or more
Manage it is unqualified, do not need carry out next step operation；If vacuum degree (gauge pressure) reaches 0.095Mpa requirement, to vacustat
Carry out operation detection in next step；
(3) detection device valve is closed, vacuum pump is closed, starts timing；
(4) 0.09Mpa is decayed to vacuum degree (gauge pressure), stops timing；
(5) molecular screen membrane quality is judged according to the vacuum degree retention time, when the vacuum degree retention time is in 10-20min
In range above, membrane tube qualified product to be measured is judged；When the vacuum degree retention time not within the set range, judge film
Pipe product quality is unqualified.
Embodiment 1
800mm long NaA molecular sieve membrane is taken, membrane tube one end is blocked, the other end connects hose, and the connection of the hose other end has
The vacuum pump of vacuum meter.Vacuum degree is 0.097Mpa after opening vacuum pump 10s, keeps 1min vacuum degree constant, closes vacuum pump
Start timing；Vacuum degree becomes 0.09Mpa, stops timing, Shi Changwei 13.5min.Fig. 2 infiltration evaporation is used to the membrane tube later
Experimental provision carries out the detection of membrane flux and separation, and testing result is shown in Table 1.
Embodiment 2
800mm long NaA molecular sieve membrane is taken, membrane tube one end is blocked, the other end connects hose, and the connection of the hose other end has
The vacuum pump of vacuum meter.Vacuum degree is 0.097Mpa after opening vacuum pump 10s, keeps 1min vacuum degree constant, closes vacuum pump
Start timing；Vacuum degree becomes 0.09Mpa, stops timing, Shi Changwei 16.6min.It is real using infiltration evaporation to the membrane tube later
Experiment device carries out the detection of membrane flux and separation, and testing result is shown in Table 1.
Embodiment 3
800mm long NaA molecular sieve membrane is taken, membrane tube one end is blocked, the other end connects hose, and the connection of the hose other end has
The vacuum pump of vacuum meter.Vacuum degree is 0.097Mpa after opening vacuum pump 10s, keeps 1min vacuum degree constant, closes vacuum pump
Start timing；Vacuum degree becomes 0.09Mpa, stops timing, Shi Changwei 5.3min.The membrane tube is tested using infiltration evaporation later
Device carries out the detection of membrane flux and separation, and testing result is shown in Table 1.
Embodiment 4
800mm long NaA molecular sieve membrane is taken, membrane tube one end is blocked, the other end connects hose, and the connection of the hose other end has
The vacuum pump of vacuum meter.Vacuum degree is 0.097Mpa after opening vacuum pump 10s, keeps 1min vacuum degree constant, closes vacuum pump
Start timing；Vacuum degree becomes 0.09Mpa, stops timing, Shi Changwei 27.1min.It is real using infiltration evaporation to the membrane tube later
Experiment device carries out the detection of membrane flux and separation, and testing result is shown in Table 1.
1 embodiment of table tests and analyzes result
Claims (3)
1. a kind of rapid detection method of molecular screen membrane, it is characterised in that: the following steps are included:
(1) molecular screen membrane membrane tube one end is blocked, by the non-valve side of other end connecting detection device, detection device valve side
Connect vacuum pump；
(2) opening detecting device valve opens vacuum pump, and membrane tube is unqualified if vacuum degree cannot reach setting numerical value, is not required to
Carry out next step operation；If vacuum degree reaches requirement, operation detection in next step is carried out to vacustat；
(3) detection device valve is closed, vacuum pump is closed, starts timing；
(4) setting numerical value is decayed to vacuum degree, stops timing；
(5) molecular screen membrane quality is judged according to the vacuum degree retention time, when the vacuum degree retention time within the set range, sentence
Break membrane tube qualified product to be measured；When the vacuum degree retention time not within the set range, judge membrane tube product quality not
It is qualified；
The detection device includes communicating pipe, threeway, vacuum meter, valve, and wherein threeway Single port is connect with vacuum meter, one end
It mouthful is controlled to a vacuum pump through valve, the last one port with membrane tube by connecting communicating pipe when use.
2. the rapid detection method of molecular screen membrane according to claim 1, it is characterised in that: the molecular screen membrane membrane tube is
The loaded molecular screen membrane of the tubular types such as NaA type molecular screen membrane, type T molecular sieve film, type ZSM 5 molecular sieve film it is one or more.
3. the rapid detection method of molecular screen membrane according to claim 1, it is characterised in that: tubing in detection device,
Stainless steel material is selected in threeway；Valve selects needle valve.
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| CN201811519512.3A CN109621732A (en) | 2018-12-12 | 2018-12-12 | A kind of rapid detection method of molecular screen membrane |
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Citations (6)
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| CN204352765U (en) * | 2014-12-12 | 2015-05-27 | 湖南沁森环保高科技有限公司 | A kind of reverse-osmosis membrane element vacuum test and benefit adhesive dispenser |
| JP2015186776A (en) * | 2014-03-26 | 2015-10-29 | 三菱化学株式会社 | Zeolite membrane evaluation method |
| CN105841894A (en) * | 2016-03-24 | 2016-08-10 | 山东九章膜技术有限公司 | Detecting method and detecting instrument for airtightness value of reverse osmosis membrane component |
| CN205981581U (en) * | 2016-08-25 | 2017-02-22 | 珠海格力电器股份有限公司 | Testing arrangement of RO membrane filter core |
| CN206082203U (en) * | 2016-10-09 | 2017-04-12 | 成都美富特膜科技有限公司 | A gas tightness detection device for membrane post |
| CN207756005U (en) * | 2017-12-15 | 2018-08-24 | 安徽普朗膜技术有限公司 | The test device of tubular type membrane flux |
-
2018
- 2018-12-12 CN CN201811519512.3A patent/CN109621732A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015186776A (en) * | 2014-03-26 | 2015-10-29 | 三菱化学株式会社 | Zeolite membrane evaluation method |
| CN204352765U (en) * | 2014-12-12 | 2015-05-27 | 湖南沁森环保高科技有限公司 | A kind of reverse-osmosis membrane element vacuum test and benefit adhesive dispenser |
| CN105841894A (en) * | 2016-03-24 | 2016-08-10 | 山东九章膜技术有限公司 | Detecting method and detecting instrument for airtightness value of reverse osmosis membrane component |
| CN205981581U (en) * | 2016-08-25 | 2017-02-22 | 珠海格力电器股份有限公司 | Testing arrangement of RO membrane filter core |
| CN206082203U (en) * | 2016-10-09 | 2017-04-12 | 成都美富特膜科技有限公司 | A gas tightness detection device for membrane post |
| CN207756005U (en) * | 2017-12-15 | 2018-08-24 | 安徽普朗膜技术有限公司 | The test device of tubular type membrane flux |
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Application publication date: 20190416 |