CN102926197A - Manufacturing method of support cloth for preparation of ion exchange membrane - Google Patents
Manufacturing method of support cloth for preparation of ion exchange membrane Download PDFInfo
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- CN102926197A CN102926197A CN2012104616032A CN201210461603A CN102926197A CN 102926197 A CN102926197 A CN 102926197A CN 2012104616032 A CN2012104616032 A CN 2012104616032A CN 201210461603 A CN201210461603 A CN 201210461603A CN 102926197 A CN102926197 A CN 102926197A
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Abstract
The invention relates to the technical field of chemical industry production, in particular to a manufacturing method of support cloth for preparation of an ion exchange membrane. The manufacturing method comprises the steps that polyvinyl chloride fibers of which the diameters are 0.03-0.06 mm are adopted as raw materials, and irradiated by 60Co gamma-rays for activation; then the fibers are soaked in polytetrafluoroethylene emulsion; the polyvinyl chloride fibers are subjected to high-temperature treatment in an oxygen-free environment to obtain tetrafluoride polyvinyl chloride fibers to be cut for use; the tetrafluoride polyvinyl chloride fibers for use are woven into cloth in a prismatic crossing manner; a warp distance and a weft distance are both 0.12-0.18 mm; and compaction treatment is conducted. The manufacturing method has the advantages that the ion exchange membrane is very high in mechanical strength and chemical stability, and can be used in extreme conditions such as strong acid, strong alkali, an organic solvent and high temperature.
Description
Technical field
The present invention relates to a kind of chemical production technical field, be specifically related to a kind of manufacture method of the supports cloth for the ion-exchange film preparation.
Background technology
As the amberplex of the core component in the electrodialysis, its film properties directly affects the performance of whole electrodialysis plant.Nineteen fifty, American W.J uda has at first invented amberplex and preparation method thereof.Amberplex at that time is heterogeneous membrane, all by the anion and cation exchange resin powder respectively mixing with binder and with strengthen screen cloth and suppress and form.Afterwards, the U.S. and Japan had developed again homogeneous ion-exchange membrane and preparation method thereof in succession.
Since eighties of last century, amberplex and relevant technology thereof develop rapidly, are widely used in water treatment, environmental protection, the energy and cleaner production.At present, for the Application in Chemical Engineering condition for harshness, development have excellent ion-selective permeability, low resistance, high machinery, chemical stability amberplex one-tenth the task of top priority.For the preparation of alkaline anion-exchange membrane, because inevitable mechanical strength on film, chemical stability etc. cause great impact in the halomethylation step in the traditional route.As for cation-exchange membrane, substantially be with chlorosulfonic acid or the concentrated sulfuric acid as sulfonating agent, also be that the mechanical strength, chemical stability etc. on film causes great impact.
Film-forming method mainly contains impregnation method, irradiation method, rubbing method etc. at present, and wherein impregnation method is because material cost is high, large to equipment corrosion, the problems such as the bad control of stability of masking; The masking difficulty is large, the high in cost of production consequence and irradiation method is because the problems such as the uniformity, irradiation bomb cause.And rubbing method is most possibly high-performance processed, low cost, high mechanical properties, a kind of film-forming method that chemical stability is good comparatively speaking.
Homogeneous ion-exchange membrane has excellent chemical property, has replaced gradually heterogeneous membrane in each Application Areas.And with the phase film that rubbing method prepares, all have superiority in film kind, film properties, chemical stability, manufacturing cost etc.
So for the emphasis of the research and development of amberplex be placed on mainly that preparation is high temperature resistant, the supports cloth that is used for the ion-exchange film preparation of non-oxidizability, corrosion-resistant, organic solvent-resistant.Supports cloth for the preparation of homogeneous membrane mainly contains terylene cloth, nylon cloth, polyvinyl chloride fibre cloth etc. at present, and these cloth generally can not anti-strong acid of while and highly basic.When particularly preparing Bipolar Membrane, have simultaneously strong acid and highly basic to exist in the both sides of film, the performance of supports cloth has directly been affected high mechanical properties, the chemical stability of film.We are for above present situation, on the basis of forefathers' research, the specific (special) requirements for preparing the electrodialysis homogeneous ion-exchange membrane for rubbing method, series of studies and exploitation have been carried out, through to multiple experimental study and the contrast of carrying out for the supports cloth of masking, finally employing polyvinyl chloride and polytetrafluoroethylene (PTFE) Compound Fabric have been developed, solved the simultaneously problem of anti-strong acid and highly basic of common supports cloth, also solved the problem of the organic solvent-resistant of film, supports cloth of the present invention can prepare various homogeneous-phase anion exchange films, cation-exchange membrane, Bipolar Membrane, the diffusion dialysis film, the chlor-alkali film, fuel cell membranes etc.
Summary of the invention
The present invention is directed to deficiency of the prior art, propose a kind of supports cloth that rubbing method prepares the homogeneous ion-exchange membranes such as homogeneous phase anode membrane, homogeneous phase cavity block, Bipolar Membrane, diffusion dialysis film, chlor-alkali film, fuel cell membranes that can be used for.The present invention also aims to provide a kind of and can make manufacture method and the relevant parameter that economy, high performance rubbing method prepare the supports cloth of amberplex.
For reaching this purpose, the present invention is achieved by following technical proposals:
(1) selecting wire diameter is that the polyvinyl chloride fibre silk of 0.03-0.06mm is raw material, under-10 ℃ of-1 ℃ of conditions, with 60Co gamma-radiation constant temperature irradiation activation, irradiation dose is 1KGy-3KGy, again the filament after the activation is immersed in the ptfe emulsion that mass concentration is 5-30%, soak time is 2-20 minute, allow polytetrafluoroethylene (PTFE) fully be adsorbed on polyvinyl chloride fibre silk surface, again the vinyl chloride fibers silk is carried out high-temperature process under oxygen-free environment, treatment temperature is 250 ℃-350 ℃, making the polytetrafluoroethylene (PTFE) that is adsorbed on vinyl fiber silk surface be melt into liquid film coats fully to the vinyl fiber silk, get final product to such an extent that wire diameter is the polyvinyl chloride fibre of the tetrafluoroethylene protection of 0.05-0.08mm, be called for short tetrafluoro polyvinyl chloride silk, this tetrafluoro polyvinyl chloride silk cutting is for subsequent use;
(2) tetrafluoro polyvinyl chloride silk is woven into cloth with the mode that prismatic intersects, warp interval and parallel interval all are 0.12mm-0.18mm, the angle of warp and parallel is the 80-90 degree, is woven into to carry out densification behind the cloth and process, and the thickness that makes this cloth is 0.09mm-0.11mm; Preparation-obtained cloth is the supports cloth for the ion-exchange film preparation.
Mixed solution with styrene, divinylbenzene, benzoyl peroxide is processed to get preparation liquid through the heating prepolymerization, the preparation liquid scraping fluid on above-mentioned supports cloth, after carrying out cross-linking reaction with 90-180 ℃ temperature again, obtain the basement membrane for the preparation of various homogeneous ion-exchange membranes, the sulfonation in sulfonated liquid of this basement membrane can obtain cation-exchange membrane; Chloromethylation then amination can obtain anion-exchange membrane; The one side sulfonation, another side chloromethylation, amination can obtain Bipolar Membrane.
Beneficial effect: with the prepared various homogeneous ion-exchange membranes of supports cloth of the present invention owing to there is supports cloth to exist, so its mechanical strength is very good.Because the filament of supports cloth of the present invention coats with tetrafluoroethylene, the chemical stability of the various amberplexes that prepare with supports cloth of the present invention is very good, can various strong acid, use under the harsh conditions such as highly basic, organic solvent, high temperature.
Description of drawings
Fig. 1 tetrafluoro polyvinyl chloride supports cloth preparation flow schematic diagram
Fig. 2 tetrafluoro polyvinyl chloride silk structural representation
The structural representation of Fig. 3 supports cloth
The specific embodiment
The below specifies enforcement of the present invention:
Embodiment 1
Press the process of the preparation flow schematic diagram shown in the accompanying drawing 1; selecting wire diameter is that the polyvinyl chloride fibre silk of 0.05mm is raw material; condition under-8 ℃ of temperature; with 60Co gamma-radiation constant temperature irradiation activation; irradiation dose is 2KGy; again the filament after the activation is immersed in 20% the ptfe emulsion; soak time is 5 minutes; allow polytetrafluoroethylene (PTFE) fully be adsorbed on polyvinyl chloride fibre silk surface; again the vinyl chloride fibers silk is carried out high-temperature process under oxygen-free environment; treatment temperature is 270 ℃; making the polytetrafluoroethylene (PTFE) that is adsorbed on vinyl fiber silk surface be melt into liquid film coats fully to the vinyl fiber silk; get final product to such an extent that wire diameter is the polyvinyl chloride fibre of the tetrafluoroethylene protection of 0.07mm, be called for short tetrafluoro polyvinyl chloride silk, it is for subsequent use that this tetrafluoro polyvinyl chloride silk is cut into certain-length.In the present embodiment, employed tetrafluoro polyvinyl chloride silk structure as shown in Figure 2.
Tetrafluoro polyvinyl chloride silk is woven into cloth with the mode that prismatic intersects, and as shown in Figure 3, warp interval and parallel interval are 0.15mm all, carry out densification behind the cloth that is woven into and process, and the thickness that makes this cloth is 0.1mm.With styrene be 75%, divinylbenzene 25%, benzoyl peroxide be that 1% mixed solution is processed to get preparation liquid through the heating prepolymerization, the preparation liquid scraping fluid on above-mentioned supports cloth, after carrying out cross-linking reaction with 170 ℃ temperature again, obtain the basement membrane for the preparation of various homogeneous ion-exchange membranes.
This basement membrane take silver sulfate as catalyst, was carried out sulfonation 15 hours take the concentrated sulfuric acid as sulfonating agent under 46 ℃, can obtain homogeneous phase cation exchange film through cooling, ion exchange capacity is 0.7 milliequivalent/gram film.Embodiment 2
The preparation method of basement membrane such as embodiment 1 are identical.
With this basement membrane take butter of tin as catalyst, under 52 ℃, carried out chloromethylation 16 hours take chloromethyl ether as chloromethylation reagent, get the chloromethane basement membrane of chloromethylation after the cooling, carried out the season ammonification 12 hours with 30% trimethylamine aqueous solution in 30 ℃ at last, can obtain homogeneous-phase anion exchange film, ion exchange capacity is 1.2 milliequivalents/gram film.
Embodiment 3
Selecting wire diameter is that the polyvinyl chloride fibre silk of 0.07mm is raw material; condition under-6 ℃ of temperature; with 60Co gamma-radiation constant temperature irradiation activation; irradiation dose is 3KGy; again the filament after the activation is immersed in 20% the ptfe emulsion; soak time is 8 minutes; allow polytetrafluoroethylene (PTFE) fully be adsorbed on polyvinyl chloride fibre silk surface; again the vinyl chloride fibers silk is carried out high-temperature process under oxygen-free environment; treatment temperature is 280 ℃; making the polytetrafluoroethylene (PTFE) that is adsorbed on vinyl fiber silk surface be melt into liquid film coats fully to the vinyl fiber silk; get final product to such an extent that wire diameter is the polyvinyl chloride fibre of the tetrafluoroethylene protection of 0.09mm; be called for short tetrafluoro polyvinyl chloride silk, it is for subsequent use that this tetrafluoro polyvinyl chloride silk is cut into certain-length.
Tetrafluoro polyvinyl chloride silk is woven into cloth with the mode that prismatic intersects, and warp interval and parallel interval are 0.15mm all, carry out densification behind the cloth that is woven into and process, and the thickness that makes this cloth is 0.15mm.With styrene be 75%, divinylbenzene 25%, benzoyl peroxide be that 1% mixed solution is processed to get preparation liquid through the heating prepolymerization, the preparation liquid scraping fluid on above-mentioned supports cloth, after carrying out cross-linking reaction with 175 ℃ temperature again, obtain the basement membrane for the preparation of various homogeneous ion-exchange membranes.
The one side of this basement membrane was carried out sulfonation 12 hours take the concentrated sulfuric acid as sulfonating agent under 47 ℃, then another side carried out chloromethylation 14 hours take chloromethyl ether as chloromethylation reagent under 50 ℃, carry out the season ammonification 8 hours with 30% trimethylamine aqueous solution in 30 ℃ again, can obtain Bipolar Membrane.
Claims (1)
1. a supports cloth manufacture method that is used for the ion-exchange film preparation is characterized in that, comprises the steps:
(1) selecting wire diameter is that the polyvinyl chloride fibre silk of 0.03-0.06mm is raw material, under-10 ℃ of-1 ℃ of conditions, with 60Co gamma-radiation constant temperature irradiation activation, irradiation dose is 1KGy-3KGy, again the filament after the activation is immersed in the ptfe emulsion that mass concentration is 5-30%, soak time is 2-20 minute, allow polytetrafluoroethylene (PTFE) fully be adsorbed on polyvinyl chloride fibre silk surface, again the vinyl chloride fibers silk is carried out high-temperature process under oxygen-free environment, treatment temperature is 250 ℃-350 ℃, making the polytetrafluoroethylene (PTFE) that is adsorbed on vinyl fiber silk surface be melt into liquid film coats fully to the vinyl fiber silk, get final product to such an extent that wire diameter is the polyvinyl chloride fibre of the tetrafluoroethylene protection of 0.05-0.08mm, be called for short tetrafluoro polyvinyl chloride silk, this tetrafluoro polyvinyl chloride silk cutting is for subsequent use;
(2) tetrafluoro polyvinyl chloride silk is woven into cloth with the mode that prismatic intersects, warp interval and parallel interval all are 0.12mm-0.18mm, the angle of warp and parallel is the 40-60 degree, is woven into to carry out densification behind the cloth and process, and the thickness that makes this cloth is 0.09mm-0.11mm; Preparation-obtained cloth is the supports cloth for the ion-exchange film preparation.
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