CN1110353C - Missing yarn examination method for hollow fibre composite membrane separator - Google Patents

Missing yarn examination method for hollow fibre composite membrane separator Download PDF

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Publication number
CN1110353C
CN1110353C CN98113915A CN98113915A CN1110353C CN 1110353 C CN1110353 C CN 1110353C CN 98113915 A CN98113915 A CN 98113915A CN 98113915 A CN98113915 A CN 98113915A CN 1110353 C CN1110353 C CN 1110353C
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China
Prior art keywords
gas
separator
composite membrane
membrane separator
hollow
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Expired - Fee Related
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CN98113915A
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CN1231940A (en
Inventor
任常青
赵勇
刘富强
邢丹敏
曹义鸣
邓麦村
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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Publication of CN1110353C publication Critical patent/CN1110353C/en
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Abstract

The present invention relates to a missing yarn examining method for a hollow-fibre composite membrane separator. Mixed gas to be separated is compressed to server as raw gas sent into a membrane separator, penetrating air for 1 or 2 to 5 yarns at the penetrating air side is taken to carry out gas separation analysis, and if the fast gas (gas with large penetration rate in the mixed gas) concentration in the penetrating gas is lower than that of other hollow fibres, the hollow fibre or the hollow fibres must have missing yarns. The present invention can examine the coating situation of some yarns in a separator, and enhances the qualified rate of a separator product through the treatment to the missing yarns.

Description

A kind of hollow fiber composite membrane separator missing yarn examination method
The present invention relates to membrane separation technique.It provides a kind of hollow fiber composite membrane separator to leak silk or the incomplete detection method of coating.The method is analyzed infiltration pneumatolytic part with instrument such as chromatograph or oxygen analyser etc., can detect Lou silk or the incomplete hollow-fibre membrane of coating accurately and rapidly, improves the gas separation coefficient of composite membrane separator.
Gas separation membrane is a kind of membrane technology of divided gas flow.Since 1979, Monsanto company has separated since the industrialization for the first time gas film, and gas film separates very great development, has occupied suitable important proportion in the film separation process.Early stage film infiltration coefficient is little, and permeability is low, makes membrane process expense height.And also have a unfavorable conditions, be exactly its poor selectivity of the high high polymer of permeability; Otherwise, the high polymer that permeability is low, its selectivity is good.The high polymer of most of glassy states all has high permeability coefficient to gas, so they separate of great use gas.Also be spun into asymmetric hollow fiber easily with low porosity (less than 0.01%).But these doughnuts have been too many holes concerning gas separates really, so can not use.If also want to utilize the high polymer of these glassy states, will try to make the porosity of doughnut very low so (less than 10 -7%) or try the hole on doughnut surface is bottled up.Coat skim material on counterdie, the infiltration coefficient of film is reduced, selectivity does not reduce.Monsanto company once proposed to have the notion " resistance composite membrane " of historic significance, the method for silicon rubber with vacuum coating, was coated on the asymmetric macromolecule counterdie, to repair the defective on the macromolecule counterdie.Because the gas permeability of silicon rubber is big, so the separating property of this composite membrane depends primarily on asymmetric counterdie.Because the compacted zone of asymmetric counterdie as thin as a wafer, so the more original homogeneous membrane of infiltration coefficient has a very significant increase, and can satisfy industrialized needs.Up to now, gas film separates in many aspects to be used, as recover hydrogen from synthetic ammonia tailgas, and separated oxygen, nitrogen or carbon dioxide from air, separation of helium etc. from natural gas.
The general structure of doughnut gas film separator as shown in Figure 1, hollow fiber bundle one end is an opening, raw material is made shell side leave with rage, the infiltration make a journey leave with rage, at this moment doughnut can bear higher pressure.Owing in manufacturing the process of hollow fiber composite membrane, can produce the place that coating is incomplete or leak silk.Like this, lip-deep some defective of asymmetric counterdie does not obtain repairing, and whole membrane separator separating property is reduced greatly.
Detecting the method for leaking silk in the past is that whole separator is measured.Be exactly to use two kinds of pure gas respectively to membrane separator measurement gas flow Q 1, Q 2, use formula J=Q/A Δ pt then, α=J 1/ J 2Calculate the separation of two kinds of gases.If the separation of gas is too low, then this separator can't reach the separating effect of hope, and a separator is just scrapped.Such as for the nitrogen hydrogen separator, if nitrogen hydrogen separation α H2/N2=3.9, such separation is too low, often can't meet the demands.If the doughnut coating in the separator is incomplete, the porous supporting film directly contacts with gas.The hollow-fibre membrane of face coat is the resistance composite membrane, and is different with the characteristic of perforated membrane, and the surface porosity factor of the counterdie of resistance composite membrane is in than the scope of broad (<10 -4%) all have than higher gas separation coefficient.And if the porosity of common perforated membrane is greater than 10 -7%, the gas separation coefficient of this film will drop to very little value.Therefore, exist the separator that leaks silk or the incomplete hollow-fibre membrane of coating will obviously reduce the gas separation coefficient of whole separator.
The object of the present invention is to provide a kind of detection method of hollow fiber composite membrane separator, it can detect the coating situation of certain rhizoid in the separator, and borrows the qualification rate that this processing of leaking silk is improved the separator product.
The invention provides a kind of hollow fiber composite membrane separator missing yarn examination method, it is characterized in that mist compression to be separated is sent into membrane separator as unstripped gas, the infiltration gas of getting 1 or 2~5 rhizoids at infiltrating gas side one by one carries out the gas compartment analysis, if the concentration of relative other doughnut of fast gas (the big gas of permeability in the mist) concentration is low in the infiltration gas, can conclude that this root or these macaroni yarns dimension must have the silk of leakage.
The gas film separating mechanism is dissolving a--diffusion mechanism, according to this mechanism, and the film that gas separation coefficient is little, the concentration of fast gas is also little in its infiltration gas.And according to hollow-fibre membrane N 2-H 2The Mathematical Modeling of separator separation process obtains y o = β - β 2 - 4 ( P 2 / P 1 ) ( α - 1 ) α · X o 2 ( P 2 / P 1 ) ( α - 1 )
Wherein: P 1--raw gas pressure, MPa
P 2--infiltration atmospheric pressure, MPa
y o--H in the infiltration gas 2Concentration
x o--H in the unstripped gas 2Concentration
β=(α-1)(x o+P 2/P 1)+1
From last formula also as can be seen along with the increase of α (gas separation coefficient), y oValue also increases gradually, and the present invention utilizes special detection head, entangles separator infiltration gas and surveys a rhizoid or several silk, makes the infiltration gas in it enter chromatographic probe tube.According to the chromatography result,, can conclude that so this rhizoid must be incomplete for leaking silk or coating if when the concentration of fast gas is starkly lower than other rhizoid.With adhesive such as epoxy resin the outlet of infiltration gas is sealed, just can improve the gas separation effect of whole separator.
The present invention is not only applicable to composite membrane, can also be used in non-composite membrane because spinning process produces the detection of defective.
By embodiment in detail the present invention is described in detail below in conjunction with accompanying drawing.
Accompanying drawing 1 is a hollow fiber composite membrane cyclone separator arrangement schematic diagram.
Accompanying drawing 2 is test H 2Schematic diagram.
Embodiment 1
Making the hydrogen/nitrogen ratio is that 1: 4 mist feeds silicon rubber/polysulfone hollow fibre composite membrane N 2/ H 2Separator.The concentration that records hydrogen in the gaseous mixture at infiltrating gas side is 0.225, because this concentration is very low, concludes that therefore this composite membrane separator must have the silk of leakage.So in separator epoxy sealing head one side, separator is put the opening flange, fastens a rhizoid with sampling Rubber end shown in Figure 2.Record H in some doughnut infiltration gas 2Content have only 0.20, so conclude that these silks are for leaking silk.With epoxy resin the outlet of these infiltration gas is sealed.And then survey the whole separating effect of separator, record H in the infiltration gas 2Content be 0.378.
Embodiment 2
Make the oxygen permeable membrane separator with the polyether sulfone composite hollow fiber membrane, make compressed air feed this hollow fiber composite membrane separator.Record at infiltrating gas side that concentration of oxygen is 0.21 in the gaseous mixture,, conclude that therefore this composite membrane separator must have the silk of leakage because this concentration is very low.So in separator epoxy sealing head one side, separator is changed the opening flange, fastens a rhizoid with sampling head shown in Figure 2.Record O in some doughnut infiltration gas 2Content have only 0.181, so conclude that these silks are for leaking silk.With epoxy resin these infiltration gas is sealed by mouth.And then survey the whole separating effect of separator, record O in the infiltration gas 2Content be 0.308.

Claims (1)

1. hollow fiber composite membrane separator missing yarn examination method, it is characterized in that mist compression to be separated is sent into membrane separator as unstripped gas, the infiltration gas of getting 1 or 2~5 rhizoids at infiltrating gas side one by one carries out the gas compartment analysis, if the concentration of relative other doughnut of fast gas concentration is low in the infiltration gas, conclude that then this root or these doughnuts must have the silk of leakage.
CN98113915A 1998-04-16 1998-04-16 Missing yarn examination method for hollow fibre composite membrane separator Expired - Fee Related CN1110353C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN98113915A CN1110353C (en) 1998-04-16 1998-04-16 Missing yarn examination method for hollow fibre composite membrane separator

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Application Number Priority Date Filing Date Title
CN98113915A CN1110353C (en) 1998-04-16 1998-04-16 Missing yarn examination method for hollow fibre composite membrane separator

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CN1231940A CN1231940A (en) 1999-10-20
CN1110353C true CN1110353C (en) 2003-06-04

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102580547B (en) * 2011-12-29 2014-05-14 新奥科技发展有限公司 Membrane module testing method
CN103100307B (en) * 2013-03-05 2014-07-23 天津工业大学 Characterization method of interface combination condition of enhancement type hollow fiber membrane

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08285792A (en) * 1995-04-14 1996-11-01 Kanegafuchi Chem Ind Co Ltd Defect detection method for hollow yarn membrane in hollow yarn membrane module
JPH0999341A (en) * 1995-10-03 1997-04-15 Morikawa Sangyo Kk Manufacture of lost foam pattern having under-cut part and device thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08285792A (en) * 1995-04-14 1996-11-01 Kanegafuchi Chem Ind Co Ltd Defect detection method for hollow yarn membrane in hollow yarn membrane module
JPH0999341A (en) * 1995-10-03 1997-04-15 Morikawa Sangyo Kk Manufacture of lost foam pattern having under-cut part and device thereof

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