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CN109762382A - Thermal polymerization nanofiltration film preparation coating liquid and application method - Google Patents

Thermal polymerization nanofiltration film preparation coating liquid and application method Download PDF

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Publication number
CN109762382A
CN109762382A CN201811603591.6A CN201811603591A CN109762382A CN 109762382 A CN109762382 A CN 109762382A CN 201811603591 A CN201811603591 A CN 201811603591A CN 109762382 A CN109762382 A CN 109762382A
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China
Prior art keywords
coating liquid
parts
thermal polymerization
film preparation
preparation coating
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Pending
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CN201811603591.6A
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Chinese (zh)
Inventor
王春浩
胡晓宇
梁恩宾
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Tianjin Motimo Membrane Technology Co Ltd
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Tianjin Motimo Membrane Technology Co Ltd
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Priority to CN201811603591.6A priority Critical patent/CN109762382A/en
Publication of CN109762382A publication Critical patent/CN109762382A/en
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Abstract

The invention belongs to field of membrane preparation, and in particular to a kind of thermal polymerization nanofiltration film preparation coating liquid and application method.Thermal polymerization nanofiltration film preparation coating liquid includes following content of component: 2-10 parts of charge adjusting agent, 0.5-5 parts of crosslinking agent, and 10-20 parts of chain-transferring agent, 2-10 parts of initiator, 0.1-1 parts of surfactant and 100 parts of aqueous solvent.The present invention takes water as a solvent production hollow fiber nanofiltration membrane, and serialization external pressure production model, the shorter cost of process is lower, can also reduce carrying capacity of environment.

Description

Thermal polymerization nanofiltration film preparation coating liquid and application method
Technical field
The invention belongs to field of membrane preparation, and in particular to a kind of thermal polymerization nanofiltration film preparation coating liquid and application method.
Background technique
It currently, the preparation of hollow fiber nanofiltration membrane mostly uses internal pressure, and is the interfacial polymerization of batch production.And it is continuous Outside the pale of civilization pressure production hollow fiber nanofiltration membrane also uses interfacial polymerization;Interface sentence polymerization needs a large amount of organic solvents, pollutes ring Border, and complexity is post-processed, improve production cost.
Summary of the invention
The purpose of the present invention is to overcome the defects in the prior art, provides a kind of thermal polymerization nanofiltration film preparation coating liquid And application method.
The present invention to achieve the above object, using following technical scheme:
A kind of thermal polymerization nanofiltration film preparation coating liquid, including following content of component: 2-10 parts of charge adjusting agent, crosslinking 0.5-5 parts of agent, 10-20 parts of chain-transferring agent, 2-10 parts of initiator, 0.1-1 parts of surfactant and 100 parts of aqueous solvent.
The charge adjusting agent includes negative charge control agents, positive charge control agents and neutral regulator.
The positive charge control agents include diethyl enamine, diallyldimethylammonium chloride, Methacrylamide propyl Trimethyl ammonium chloride or MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride;The negative charge control agents include metering system Acid, methacrylic sulfonic acid, methyl styrenesulfonic acid or 2- Methacrylamide -2- methyl propane sulfonic acid;The neutral adjusting Agent includes Methacrylamide, and dimethylacrylamide, vinylacetate, hydroxyethyl methacrylate or methacrylic acid are sweet Grease.
The chain-transferring agent is sodium hypophosphite, isopropanol or mercaptoethanol.
The crosslinking agent be diethyl allyl diglycol, glycerol dimethacrylate, polyethylene glycol dimethacrylate, Or ethylene glycol dimethacrylate.
The initiator is ammonium persulfate, potassium peroxydisulfate or hydrogen peroxide.
The surfactant be lauryl sodium sulfate, dodecyl sodium sulfate, dodecyl trimethyl ammonium chloride, Or polyethylene glycol.
The invention also includes a kind of methods using the coating liquid preparation nanofiltration membrane, include the following steps: film 1) Silk infiltration in coating liquid, high-speed air is blown away swim after, into flat-temperature zone, low speed nitrogen is used to heat film wire;2) it has reacted Cheng Hou is soaked in RO water overnight to get product;Wherein, coating liquid infiltrating time 5-60s;High-speed air purge time 1- 5min;Thermostat temperature is 60-80 degree, heating time 5-20min.
Compared with prior art, the beneficial effects of the present invention are:
The present invention takes water as a solvent production hollow fiber nanofiltration membrane, and serialization external pressure production model, the shorter cost of process is more It is low, carrying capacity of environment can also be reduced.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, implement below with reference to best The present invention is described in further detail for example.
Embodiment 1: the preparation of coating liquid: charge adjusting agent 2- Methacrylamide -2- methyl propane sulfonic acid 10kg, crosslinking Agent polyethylene glycol dimethacrylate 1kg, chain-transferring agent sodium hypophosphite 10kg, initiator ammonium persulfate 10kg, surface-active Agent lauryl sodium sulfate 0.3kg, water 100kg are mixed to get.Film wire infiltration 10s, high-speed air in coating liquid are swept into 5min, Into flat-temperature zone, film wire is heated using low speed nitrogen, temperature is 80 degree, time 5min.After the reaction was completed, it is soaked in mistake in RO water Night is to get product.
Embodiment 2: coating liquid: diallyldimethylammonium chloride 5kg, glycerol dimethacrylate 0.5kg, hypophosphorous acid Sodium 12kg, potassium peroxydisulfate 5kg, polyethylene glycol 0.1kg, water 100kg;Film wire infiltration 10s, high-speed air in coating liquid are swept 3min heats film wire using low speed nitrogen, temperature is 70 degree, time 8min into flat-temperature zone.After the reaction was completed, it is soaked in RO Overnight to get product in water.
Embodiment 3: coating liquid: methacrylic sulfonic acid 4kg, ethylene glycol dimethacrylate 1kg, sodium hypophosphite 20kg, Ammonium persulfate 2kg, dodecyl sodium sulfate 0.2kg, water 100kg.Film wire infiltration 40s, high-speed air in coating liquid are swept 5min heats film wire using low speed nitrogen, temperature is 80 degree, time 16min into flat-temperature zone.After the reaction was completed, it is soaked in RO Overnight to get product in water.
Embodiment 4: coating liquid: hydroxy-ethyl acrylate 10kg, glycerol dimethacrylate 5kg, isopropanol 15kg, over cure Sour sodium 10kg, lauryl sodium sulfate 0.5kg, water 100kg.Film wire infiltration 60s, high-speed air in coating liquid are swept into 4min, Into flat-temperature zone, film wire is heated using low speed nitrogen, temperature is 80 degree, time 5min.After the reaction was completed, it is soaked in mistake in RO water Night is to get product.
Embodiment 5: coating liquid: dimethylacrylamide 2kg, glycerol dimethacrylate 2kg, mercaptoethanol 16kg, Potassium peroxydisulfate 6kg, dodecyl trimethyl ammonium chloride 1kg, water 100kg.By film wire infiltration 30s, high-speed air in coating liquid 5min is swept, into flat-temperature zone, heats film wire using low speed nitrogen, temperature is 70 degree, time 10min.After the reaction was completed, it is soaked in Overnight to get product in RO water.
Embodiment 6: coating liquid: glyceral methacrylate 8kg, ethylene glycol dimethacrylate 1kg, isopropanol 10kg, ammonium persulfate 2kg, dodecyl sodium sulfate 0.3kg, water 100kg.By film wire infiltration 5s, high-speed air in coating liquid 1min is swept, into flat-temperature zone, heats film wire using low speed nitrogen, temperature is 60 degree, time 20min.After the reaction was completed, it is soaked in Overnight to get product in RO water.
7 coating liquid of embodiment: styrene sulfonic acid 10kg, glycerol dimethacrylate 5kg, sodium hypophosphite 20kg, over cure Sour ammonium 7kg, lauryl sodium sulfate 0.6kg, water 100kg.Film wire infiltration 10s, high-speed air in coating liquid are swept into 5min, into Enter flat-temperature zone, heats film wire using low speed nitrogen, temperature is 80 degree, time 5min.After the reaction was completed, it is soaked in mistake in RO water Night is to get product.
Comparative example 1: being added without charge adjusting agent in coating liquid, remaining is same as Example 1.
Comparative example 2: being not added chain-transferring agent in coating liquid, remaining is same as Example 1.
Comparative example 3: being added without surfactant in coating liquid, remaining is same as Example 1.
Nano filter membrane separating property test method
Test fluid: 2000mg/L magnesium sulfate (MgSO is used4) solution testing.
Operating parameter: it is tested using nanofiltration membrane evaluation instrument, pressure 0.5MPa, 25 DEG C, pH=7.0, the rate of recovery 15%.
Calculation formula:
Rejection R=(CI-CO)/CI* 100%, wherein CIFor conductance of intaking, COTo be discharged conductance;
Flux F=V/ (A*T), wherein V is to produce water volume, and A is membrane area, and T is time of measuring.
The comparison of 1 nano filter membrane separating property of table.
Table 1
Flux (LMH) Rejection (%)
Embodiment 1 32 91
Embodiment 2 29 85
Embodiment 3 35 89
Embodiment 4 32 88
Embodiment 5 33 89
Embodiment 6 34 87
Embodiment 7 30 90
Comparative example 1 8 90
Comparative example 2 12 91
Comparative example 3 28 73
Conclusion: using this method can be obtained rejection 85% or more nanofiltration membrane wherein surfactant be introduced as it is each The abundant dissolution of component provides guarantee, is the important guarantee (comparative example 3) of rejection.And charge adjusting agent, chain-transferring agent are The important guarantee of enough flux.
The above is only a preferred embodiment of the present invention, for those of ordinary skill in the art, according to the present invention Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to the present invention Limitation.

Claims (8)

1. a kind of thermal polymerization nanofiltration film preparation coating liquid, which is characterized in that including following content of component: charge adjusting agent 2- 10 parts, 0.5-5 parts of crosslinking agent, 10-20 parts of chain-transferring agent, 2-10 parts of initiator, 0.1-1 parts of surfactant and aqueous solvent 100 parts.
2. thermal polymerization nanofiltration film preparation coating liquid according to claim 1, which is characterized in that the charge adjusting agent Including negative charge control agents, positive charge control agents and neutral regulator.
3. thermal polymerization nanofiltration film preparation coating liquid according to claim 2, which is characterized in that the positive charge is adjusted Agent includes diethyl enamine, diallyldimethylammonium chloride, Methacrylamide hydroxypropyltrimonium chloride or metering system Acyloxyethyl trimethyl ammonium chloride;The negative charge control agents include methacrylic acid, methacrylic sulfonic acid, methyl styrene Sulfonic acid or 2- Methacrylamide -2- methyl propane sulfonic acid;The neutral regulator includes Methacrylamide, dimethyl propylene Acrylamide, vinylacetate, hydroxyethyl methacrylate or glyceral methacrylate.
4. thermal polymerization nanofiltration film preparation coating liquid according to claim 1, which is characterized in that the chain-transferring agent is Sodium hypophosphite, isopropanol or mercaptoethanol.
5. thermal polymerization nanofiltration film preparation coating liquid according to claim 1, which is characterized in that the crosslinking agent is two Ethylene glycol, glycerol dimethacrylate, polyethylene glycol dimethacrylate or ethylene glycol dimethacrylate Ester.
6. thermal polymerization nanofiltration film preparation coating liquid according to claim 1, which is characterized in that the initiator was Ammonium sulfate, potassium peroxydisulfate or hydrogen peroxide.
7. thermal polymerization nanofiltration film preparation coating liquid according to claim 1, which is characterized in that the surfactant For lauryl sodium sulfate, dodecyl sodium sulfate, dodecyl trimethyl ammonium chloride or polyethylene glycol.
8. a kind of method using the described in any item coating liquid preparation nanofiltration membranes of claim 1-7, which is characterized in that including under State step: 1) by film wire infiltration in coating liquid, high-speed air is blown away swim after, into flat-temperature zone, heated using low speed nitrogen Film wire;2) it after the reaction was completed, is soaked in RO water overnight to get product;Wherein, coating liquid infiltrating time 5-60s;High-speed air Purge time 1-5min;Thermostat temperature is 60-80 degree, heating time 5-20min.
CN201811603591.6A 2018-12-26 2018-12-26 Thermal polymerization nanofiltration film preparation coating liquid and application method Pending CN109762382A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111001310A (en) * 2019-12-23 2020-04-14 天津膜天膜科技股份有限公司 Preparation method of environment-friendly nanofiltration membrane
CN119349747A (en) * 2024-12-30 2025-01-24 北京东雷恒业环保科技有限公司 A high-salt wastewater treatment membrane and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN1816385A (en) * 2003-04-01 2006-08-09 库诺公司 Hydrophilic membrane and process for making the same
WO2010086852A1 (en) * 2009-01-29 2010-08-05 Ben-Gurion University Of The Negev Research And Development Authority A method for modifying composite membranes for liquid separations
CN102029117A (en) * 2009-09-29 2011-04-27 中国科学院大连化学物理研究所 Method for modifying surface of ultrafiltration membrane
CN102294176A (en) * 2011-08-17 2011-12-28 浙江大学 High permeability nanofiltration membrane containing zwitterion and preparation method thereof
CN107469651A (en) * 2017-08-22 2017-12-15 中国海洋大学 A kind of preparation method and applications of high flux crosslinked polyimide solvent resistant NF membrane

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111001310A (en) * 2019-12-23 2020-04-14 天津膜天膜科技股份有限公司 Preparation method of environment-friendly nanofiltration membrane
CN119349747A (en) * 2024-12-30 2025-01-24 北京东雷恒业环保科技有限公司 A high-salt wastewater treatment membrane and preparation method thereof

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Application publication date: 20190517