CN109632678A - A kind of detection method of polyamide composite film piece residual amine content - Google Patents
A kind of detection method of polyamide composite film piece residual amine content Download PDFInfo
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- CN109632678A CN109632678A CN201811372265.9A CN201811372265A CN109632678A CN 109632678 A CN109632678 A CN 109632678A CN 201811372265 A CN201811372265 A CN 201811372265A CN 109632678 A CN109632678 A CN 109632678A
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- 150000001412 amines Chemical class 0.000 title claims abstract description 63
- 238000001514 detection method Methods 0.000 title claims abstract description 30
- 239000004952 Polyamide Substances 0.000 title claims abstract description 15
- 229920002647 polyamide Polymers 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 239000003480 eluent Substances 0.000 claims abstract description 27
- 239000012528 membrane Substances 0.000 claims abstract description 26
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004817 gas chromatography Methods 0.000 claims abstract description 4
- 235000019441 ethanol Nutrition 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims 2
- 238000012360 testing method Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 3
- 238000005375 photometry Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 238000011155 quantitative monitoring Methods 0.000 abstract 1
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 58
- 229940018564 m-phenylenediamine Drugs 0.000 description 58
- 239000000523 sample Substances 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000002835 absorbance Methods 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 235000013399 edible fruits Nutrition 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000012496 blank sample Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000000306 component Substances 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 2
- 201000004624 Dermatitis Diseases 0.000 description 1
- 208000001647 Renal Insufficiency Diseases 0.000 description 1
- -1 alcohol compound Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 201000006370 kidney failure Diseases 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000010412 perfusion Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012088 reference solution Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of detection method of chemical residue, in particular to a kind of detection methods of polyamide composite film piece residual amine content.The present invention is to wash out technique by the way that reverse osmosis membrane is remained amine content；Using alcohol solution as eluent；Amine content detects in eluate；Finally diaphragm residual amine content is calculated obtained.The present invention provides the detection methods that a kind of easy, efficient diaphragm residual amine wash-off and instrument test combine.Residual amine eluent uses the alcohol solution of 20~100wt%, pass through the heating immersion treatment of diaphragm certain time in eluent, eluate is converted into diaphragm using amine content in UV, visible light scene photometry or gas chromatography test eluate and is remained amine content.This method eluate ingredient is simple, and it is convenient to prepare, and eluate easily detects, the Quantitative Monitoring suitable for reverse osmosis membrane residual amine content.
Description
Technical field
The present invention relates to a kind of detection methods of polyamide composite film piece residual amine content.
Background technique
Reverse-osmosis membrane element is the core component of seawater desalination system by film method, is rolled by reverse osmosis membrane.It is reverse osmosis
The production of diaphragm mainly generates polyamide supporting layer using the progress water phase on porous support membrane and oily phase interfacial reaction.Industrially
M-phenylene diamine (MPD) is mostly used to be reacted as aqueous phase monomers.
M-phenylene diamine (MPD) chemical property is more active, unstable in air, Yi Fasheng oxidation reaction.M-phenylene diamine (MPD) has certain
Toxicity, be absorbed into vivo through skin and eating, repeatedly or Long Term Contact may cause skin allergy, may have to kidney and blood
It influences, leads to the lesions such as kidney failure, be put into three classes carcinogenic substance.If m-phenylene diamine (MPD) residual content in diaphragm is more, can make
Diaphragm slowly turns yellow, or even blacks, meanwhile, also have an impact to film properties.Production process Zhong Mo producer would generally use pickling, alkali
The washing that equal rinsing process carry out residual amine is washed, but because the difference of technique and the limitation of working condition, still have different degrees of
Aromatic amine residual.It if the film with more residual amine is used in drink water purifying engineering, will be absorbed by the body, generate potential
Health hazard.
The needs of needs or diaphragm safety of paddling detection based on the research of reverse osmosis membrane rinsing process, it is necessary to diaphragm
Residual amine is detected.For the cleaning technique of m-phenylene diamine (MPD) in diaphragm, acid-water-alkali-water washing is generally used in production process
Technique, process is cumbersome.In addition, if eluent complicated component, last eluate complicated component, in addition to water and m-phenylene diamine (MPD)
Outside, there are also the presence of other compositions, also higher for testing and analyzing requirement.Currently, for m-phenylene diamine (MPD) in reverse osmosis membrane
The entire detection method for washing out, detecting and being converted to diaphragm amine content finds no standard or document report.Reverse osmosis membrane
Residual amine has more serious harmfulness to human body, and residual amine will be slow into product water in paddle technique or engineering, because
This, the detection that diaphragm remains amine content is particularly important, has no special report or patent disclosure before this.
Summary of the invention
A kind of polyamide composite film piece of the present invention remains the detection method of amine content, and residual amine washes out technique letter in this method
Single, eluate detection is easy sample preparation and equipment operation, can effectively detect the content of residual amine in reverse osmosis membrane, solve
Safety detection requirement that reverse osmosis membrane residual amine rinsing process is studied and diaphragm is paddled.
It is described that technical scheme is as follows.
A kind of detection method of reverse osmosis membrane residual amine content, includes the following steps:
(1) reverse osmosis membrane residual amine content washes out technique；Using alcohol solution as eluent；
(2) amine content detects in eluate；
(3) diaphragm residual amine content calculates.
It is 30~100 DEG C that reverse osmosis membrane described in step (1), which remains amine content and washes out technique eluent temperature, preferably
It is 50~80 DEG C.
Reverse osmosis membrane described in step (1) remains amine content and washes out technique, and diaphragm is cut into certain area, marks the face
Product is A, is put into the eluent for being heated to certain temperature, and shading sealing prevents m-phenylene diamine (MPD) from largely aoxidizing in soaking process；
Soaking time is greater than 0.5h, preferably 1~4h.
Step (1) described eluent refer to water have certain compatibility alcohol compound, methanol, ethyl alcohol, isopropanol,
N-butanol, isobutanol, ethylene glycol, any one or a few the aqueous solution in glycerine；To avoid interfering, the water of solution is prepared
Using pure water.
Difference of step (1) eluent according to alcohols solubility and the difference to m-phenylene diamine (MPD) Effect of retrograde perfusion, concentration
Range is 20~100wt%, preferably 30~80wt%.
Amine content detection uses ultraviolet-visible spectrophotometry or gas chromatography in eluate described in step (2).
The color development area that m-phenylene diamine (MPD) detects on ultraviolet-uisible spectrophotometer is mainly near 290nm, water and fat
Alcohols does not develop the color in the region；Blank reference solution uses eluent blank sample；Test temperature absorbs peak intensity to m-phenylene diamine (MPD)
There are minor impacts for degree, to avoid causing error, can warm to room temperature eluate and eluent blank sample perseverance.
The m-phenylene diamine (MPD) of different quality is added in eluent, is configured to certain density m-phenylene diamine (MPD) standard solution, it is excellent
0~100mg/L of concentration range is selected, eluent blank sample is as reference.It is ordinate, extinction that result, which is made m-phenylene diamine (MPD) concentration,
Angle value is the standard curve of abscissa.
287 DEG C of m-phenylene diamine (MPD) boiling point, if vapourizing temperature is higher, and m-phenylene diamine (MPD) content is lower, to gas chromatograph and
Gas chromatographic column has higher requirements, and gas chromatography tests m-phenylene diamine (MPD) content in eluate, can refer to chemical industry standard HG/
T 3401-2006, according to the difference of gas chromatographic column and gas chromatograph, testing conditions should be according to being actually adjusted.
Diaphragm residual amine content meter described in step (3) refers at last according to eluate volume and m-phenylene diamine (MPD) concentration, diaphragm
Area is converted into the content of m-phenylene diamine (MPD) in unit area.Diaphragm remains amine content and is labeled as C1, unit mg/m2；Eluate
Volume markings are V, unit L；M-phenylene diamine (MPD) concentration markers are C in eluate2, unit mg/L；Diaphragm area is labeled as A,
Unit is m2.The calculation formula that diaphragm remains amine content is as follows: c1=c2×V/A
The utility model has the advantages that reverse osmosis membrane residual amine can be sufficiently dissolved in the application, and effectively detected, and the application
Detection mode it is simple and easy to operate, the addition of alcohol type organic is so that m-phenylene diamine (MPD) is easier to be washed out；Purple also can be used in the present invention
Outer visible honourable photometry, without adding color developing agent, test is rapidly and efficiently, lower to sample and equipment requirement.
Specific embodiment
In order to deepen the understanding of the present invention, technical solution of the present invention is described in further detail below with reference to embodiment.It is following
Embodiment is merely provided as explanation rather than limiting the invention.
Embodiment 1
The ultralow die mould reverse osmosis membrane of producer A is chosen as experiment film, cuts out the circular film 3 of 32mm diameter
Piece, the Duplicate Samples as diaphragm sample.The ethanol water 200ml or so that 50wt% is prepared with pure water and dehydrated alcohol, as
Eluent.30ml or so is taken with graduated cylinder, pours into blue lid reagent bottle, and ready 1 diaphragm sample is put into bottle, other 2
Piece diaphragm sample does same processing.Remaining eluent is as blank reference.The blue lid reagent bottle and sky of diaphragm sample will be housed
White reference is put into 70 DEG C of baking ovens, and after placing 2h, carry sample is cooled to room temperature, and is carried out using ultraviolet-visible spectrophotometer
Absorbance value obtained and m-phenylene diamine (MPD) standard curve are compared, obtain m-phenylene diamine (MPD) content in eluate by absorbance detection,
The average value of three Duplicate Samples is taken, diaphragm residual amine content is finally calculated according to diaphragm residual amine calculation formula, calculates knot
Fruit is shown in Table 1.
Embodiment 2
The bitter type reverse osmosis membrane of producer A is chosen as experiment film, cuts out the circular film 3 of 32mm diameter
Piece, the Duplicate Samples as diaphragm sample.The ethanol water 200ml or so that 50wt% is prepared with pure water and dehydrated alcohol, as
Eluent.30ml or so is taken with graduated cylinder, pours into blue lid reagent bottle, and ready 1 diaphragm sample is put into bottle, other 2
Piece diaphragm sample does same processing.Remaining eluent is as blank reference.The blue lid reagent bottle and sky of diaphragm sample will be housed
White reference is put into 70 DEG C of baking ovens, and after placing 2h, carry sample is cooled to room temperature, and is carried out using ultraviolet-visible spectrophotometer
Absorbance value obtained and m-phenylene diamine (MPD) standard curve are compared, obtain m-phenylene diamine (MPD) content in eluate by absorbance detection,
The average value of three Duplicate Samples is taken, diaphragm residual amine content is finally calculated according to diaphragm residual amine calculation formula, calculates knot
Fruit is shown in Table 1.
Embodiment 3
The ultralow die mould reverse osmosis membrane of producer A is chosen as experiment film, cuts out the circular film 3 of 32mm diameter
Piece, the Duplicate Samples as diaphragm sample.The isopropanol water solution 200ml or so that 50wt% is prepared with pure water and isopropanol, as
Eluent.30ml or so is taken with graduated cylinder, pours into blue lid reagent bottle, and ready 1 diaphragm sample is put into bottle, other 2
Piece diaphragm sample does same processing.Remaining eluent is as blank reference.The blue lid reagent bottle and sky of diaphragm sample will be housed
White reference is put into 80 DEG C of baking ovens, and after placing 2h, carry sample is cooled to room temperature, and is carried out using ultraviolet-visible spectrophotometer
Absorbance value obtained and m-phenylene diamine (MPD) standard curve are compared, obtain m-phenylene diamine (MPD) content in eluate by absorbance detection,
The average value of three Duplicate Samples is taken, diaphragm residual amine content is finally calculated according to diaphragm residual amine calculation formula, calculates knot
Fruit is shown in Table 1.
Embodiment 4
The bitter type reverse osmosis membrane of producer A is chosen as experiment film, cuts out the circular film 3 of 32mm diameter
Piece, the Duplicate Samples as diaphragm sample.The isopropanol water solution 200ml or so that 50wt% is prepared with pure water and isopropanol, as
Eluent.30ml or so is taken with graduated cylinder, pours into blue lid reagent bottle, and ready 1 diaphragm sample is put into bottle, other 2
Piece diaphragm sample does same processing.Remaining eluent is as blank reference.The blue lid reagent bottle and sky of diaphragm sample will be housed
White reference is put into 80 DEG C of baking ovens, and after placing 2h, carry sample is cooled to room temperature, and is carried out using ultraviolet-visible spectrophotometer
Absorbance value obtained and m-phenylene diamine (MPD) standard curve are compared, obtain m-phenylene diamine (MPD) content in eluate by absorbance detection,
The average value of three Duplicate Samples is taken, diaphragm residual amine content is finally calculated according to diaphragm residual amine calculation formula, calculates knot
Fruit is shown in Table 1.
1 reverse osmosis membrane of table remains amine content
| Embodiment | Diaphragm remains amine content/mg/m2 |
| Embodiment 1 | 82 |
| Embodiment 2 | 98 |
| Embodiment 3 | 75 |
| Embodiment 4 | 91 |
As can be seen from Table 1, the residual amine content of identical reverse osmosis membrane is close in different embodiments, illustrates according to this hair
The wash-off and content detection of almost all residual amine may be implemented under suitable testing conditions in bright method.
Claims (9)
1. a kind of detection method of polyamide composite film piece residual amine content, which comprises the steps of:
(1) reverse osmosis membrane residual amine content washes out technique, using alcohol solution as eluent；
(2) amine content in eluate is detected；
(3) diaphragm residual amine content calculates.
2. a kind of detection method of polyamide composite film piece residual amine content according to claim 1, it is characterised in that: step
Suddenly it is 30~100 DEG C that reverse osmosis membrane residual amine content, which washes out technique eluent temperature, in (1).
3. a kind of detection method of polyamide composite film piece residual amine content according to claim 2, it is characterised in that: step
Suddenly it is 50~80 DEG C that reverse osmosis membrane residual amine content, which washes out technique eluent temperature, in (1).
4. a kind of detection method of polyamide composite film piece residual amine content according to claim 1, it is characterised in that: step
Suddenly the residual of reverse osmosis membrane described in (1) amine content, which washes out in technique, seals diaphragm shading, and soaking time is greater than 0.5h.
5. a kind of detection method of polyamide composite film piece residual amine content according to claim 4, it is characterised in that: step
Suddenly the residual of reverse osmosis membrane described in (1) amine content, which washes out in technique, seals diaphragm shading, 1~4h of soaking time.
6. a kind of detection method of polyamide composite film piece residual amine content according to claim 1, it is characterised in that: institute
State eluent refer in methanol, ethyl alcohol, propyl alcohol, n-butanol, isobutanol, ethylene glycol or glycerine any one or a few
Aqueous solution.
7. a kind of detection method of polyamide composite film piece residual amine content according to claim 1, it is characterised in that: institute
The concentration range for stating eluent is 20~100wt%.
8. a kind of detection method of polyamide composite film piece residual amine content according to claim 7, it is characterised in that: institute
The concentration range for stating eluent is 30~80wt%.
9. a kind of detection method of polyamide composite film piece residual amine content according to claim 1, it is characterised in that: step
Suddenly in eluate described in (2) amine content detection use ultraviolet-visible spectrophotometry or gas chromatography, the wavelength used for
285nm~295nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905577A (en) * | 2020-08-12 | 2020-11-10 | 浙江奥氏环境科技有限公司 | Method for reducing content of residual amine of reverse osmosis membrane |
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| CN111905577A (en) * | 2020-08-12 | 2020-11-10 | 浙江奥氏环境科技有限公司 | Method for reducing content of residual amine of reverse osmosis membrane |
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Application publication date: 20190416 |