CN104741007A - Preparation method of membrane separation layer for water treatment - Google Patents
Preparation method of membrane separation layer for water treatment Download PDFInfo
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- CN104741007A CN104741007A CN201510177546.9A CN201510177546A CN104741007A CN 104741007 A CN104741007 A CN 104741007A CN 201510177546 A CN201510177546 A CN 201510177546A CN 104741007 A CN104741007 A CN 104741007A
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- colloidal sol
- deionized water
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Abstract
The invention relates to the field of membranes for water treatment, and particularly relates to a preparation method of a membrane separation layer for water treatment. The method comprises the following steps: grinding aluminium isopropoxide; adding the aluminium isopropoxide into hot deionized water to carry out magnetic stirring; adding nitric acid in batches, and stirring until a solution is clear and transparent; adding a dispersant and a defoamer, and uniformly stirring; and putting a support body in a sol, then gelatinizing and drying the obtained product. According to the method, by controlling the temperature of hydrolysis and the application amount of deionized water, a relatively stable sol can be prepared; an appropriate amount of dispersant added in the sol contributes to improving the wettability of the sol and the surface of the support body, so that the film-forming quality is improved, and cracks can be avoided; and due to the adoption of a classified drying method, a homogeneous and transparent non-crack xerogel membrane can be obtained.
Description
Technical field
The present invention relates to water treatment film field, is a kind of preparation method of water treatment UF membrane layer specifically.
Background technology
Membrane technology is contemporary new and effective isolation technics, is the product of multi-crossed disciplines, compared with traditional isolation technics, it have efficient, energy-conservation, process is easy to control, easy to operate, environmental friendliness, easily and the advantage such as other technologies are integrated.Membrane technology extensively and is effectively applied to the fields such as the energy, electronics, petrochemical industry, medical and health, biochemistry, environment, food, defines emerging high-tech industry.At present, being applied in membrane technology is inoranic membrane more widely, and it has high temperature resistant, the advantage such as mechanical strength is high, chemical stability good, long service life relative to organic film.Inoranic membrane generally adopts supporter to increase the mechanical strength of film, and separating layer is then the core of membrane technology.When separating layer adopts sol-gel process to prepare, colloidal sol is the key substance basis of separating layer.Existing colloidal sol preparation is hydrolyzing metallic salts, makes polycondensation between alcohol molecules of salt form cross-linking products; But prior art is good not owing to controlling amount of water and temperature, causes colloidal sol very unstable, causes film forming even not.
Summary of the invention
For above-mentioned technical problem, the invention provides that technique is simple, the preparation method of the uniform separating layer of film forming.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of preparation method of water treatment UF membrane layer, and it comprises the following steps:
(1) prepare colloidal sol: added by ground aluminium isopropoxide in the deionized water of heat and carry out magnetic agitation, then add nitric acid in batches, be stirred to solution clear, then add dispersant and defoamer stirs, obtain colloidal sol.
(2) apply: supporter is immersed in colloidal sol, then supporter is upwards lifted out colloidal sol liquid level, make supporter to apply one deck liquid film;
(3) gelation: the supporter scribbling liquid film is positioned in the atmosphere containing steam and continues film forming, make liquid film be transformed into gel mould;
(4) dry: to adopt classification seasoning dry to gel mould.
As preferably, the mol ratio of aluminium isopropoxide and deionized water is 1:(95--105); The temperature of deionized water is 80 DEG C--90 DEG C.
As preferably, concentration of nitric acid is 1.65mol/L, and the mol ratio of itself and aluminium isopropoxide is (0.15-0.3): 1.
As preferably, nitric acid is divided equally three times and is added, and each interval time is 1h.
As preferably, described dispersant is Disponer-W511, and addition is the 0.15%--0.3% of solution quality; Described defoamer is DeformW-0506, and addition is the 0.02%--0.04% of solution quality.
As preferably, pull rate during coating is 5-15cm/ min.
As preferably, first preliminarily dried 10min at 80 DEG C of temperature time dry, is then cooled to 50 DEG C of dry 20min, then is down to drying at room temperature 10min.
From the above, this method passes through the consumption of controlled hydrolysis temperature and deionized water, can make to prepare comparatively stable colloidal sol; Meanwhile, in colloidal sol, add the wetability that suitable dispersant and defoamer contribute to improving colloidal sol and supporting body surface, improve quality of forming film, can avoid occurring crackle; In addition that adopt classification seasoning can obtain homogeneous transparent and flawless xerogel film.
Detailed description of the invention
The preparation method of water treatment UF membrane layer of the present invention is introduced in detail below in conjunction with embodiment:
First, by levigate for aluminium isopropoxide grinder, then aluminium isopropoxide is added heat deionized water in carry out magnetic agitation; The mol ratio of aluminium isopropoxide and deionized water is 1:(95-105); The temperature of deionized water is 80 DEG C--90 DEG C, the method for heating water bath can be utilized to maintain the temperature of deionized water then, and with nitric acid as peptizing agent, add nitric acid all in three batches, each interval time is about 1h, then is stirred to solution clear.The colloidal sol transparency generated when making peptizing agent with nitric acid is high, and not easily separates out precipitation.Because the addition of nitric acid is different, by causing, the pH value of solution is different, thus has an impact to Sol-Gel process and the final alumina sol formed.The addition of nitric acid is too low or too high, can cause the precipitation of particle, cause particle aggregation.The concentration of nitric acid that this method adopts is 1.65mol/L, and its mol ratio with aluminium isopropoxide be (0.15-0.3): 1, and the alumina sol of generation is like this stablized, transparent; Add the Disponer-W511 dispersant of 0.15%--0.3% and the DeformW-0506 defoamer of 0.02%--0.04% again, and stir, stand-by.Only have supporting body surface and colloidal sol to have good wetability, just can guarantee the uniformity of film and the stability of dry run.Otherwise colloidal sol is difficult to sprawl in supporting body surface, or form local defect in the dry run of gel mould.Therefore, in colloidal sol, add the wetability that suitable dispersant contributes to improving colloidal sol and supporting body surface.Meanwhile, because stirring and refluxing can produce a lot of bubble, when film, bubble hinders the moistening of colloidal sol and supporter, suppresses the generation of bubble by adding defoamer.
Then, supporter is immersed in above-mentioned colloidal sol, then supporter is upwards lifted out colloidal sol liquid level with the speed of 5-15cm/min, at this moment supporter will cover the uniform liquid film of one deck.
Then, the supporter scribbling liquid film is positioned in the atmosphere containing steam, proceeds hydrolysis in film forming procedure and polymerisation thus be transformed into gel mould.
Finally, classification is dry.Dry run is exactly residual moisture, organic group and organic solvent in removing wet gel.The final structure of xerogel film depends on that colloidal sol starts to be formed the structure of wet gel film, and xerogel film essence is contracted or the wet gel film of alteration of form.And first preliminarily dried 10min at 80 DEG C of temperature, be then cooled to 50 DEG C of dry 20min, the drier rule of the classification of being down to drying at room temperature 10min can obtain homogeneous transparent and flawless xerogel film.As carried out drying 80 DEG C or 50 DEG C always, generate although avoid large crystal, because drying is too fast, film surface will produce ununiform shrinkage with inside, easily makes film peeling.
Embodiment 1
Get the levigate aluminium isopropoxide of 1mol to add in the deionized water of the 95mol of 80 DEG C and carry out magnetic agitation, maintain the temperature of deionized water with heating water bath; The nitric acid 1/33L adding 1.65 mol/L again stirs, the above-mentioned nitric acid adding 1/33L after about 1h again stirs, after about 1h, third time adds the above-mentioned nitric acid stirring of 1/33L, adds 0.15% Disponer-W511 dispersant and 0.02% DeformW-0506 defoamer, namely obtain colloidal sol after about 30min; The supporter prepared is placed in colloidal sol, liquid level is lifted out with the speed of 5cm/min, be placed in steam atmosphere film forming again, finally preliminarily dried 10min at 80 DEG C of temperature, then 50 DEG C of dry 20min are cooled to, be down to drying at room temperature 10min again, obtain uniform separating layer, average pore size about 0.6 μm.
Embodiment 2
Get the levigate aluminium isopropoxide of 1mol to add in the deionized water of the 100mol of 85 DEG C and carry out magnetic agitation, maintain the temperature of deionized water with heating water bath; The nitric acid 0.05L adding 1.65 mol/L again stirs, the above-mentioned nitric acid adding 0.05L after about 1h again stirs, after about 1h, third time adds the above-mentioned nitric acid stirring of 0.05L, adds 0.25% Disponer-W511 dispersant and 0.03% DeformW-0506 defoamer, namely obtain colloidal sol after about 30min; The supporter prepared is placed in colloidal sol, liquid level is lifted out with the speed of 10cm/min, be placed in steam atmosphere film forming again, finally preliminarily dried 10min at 80 DEG C of temperature, then 50 DEG C of dry 20min are cooled to, be down to drying at room temperature 10min again, obtain uniform separating layer, average pore size about 0.4 μm.
Embodiment 3
Get the levigate aluminium isopropoxide of 1mol to add in the deionized water of the 105mol of 90 DEG C and carry out magnetic agitation, maintain the temperature of deionized water with heating water bath; The nitric acid 2/33L adding 1.65 mol/L again stirs, the above-mentioned nitric acid adding 2/33L after about 1h again stirs, after about 1h, third time adds the above-mentioned nitric acid stirring of 2/33L, adds 0.3% Disponer-W511 dispersant and 0.04% DeformW-0506 defoamer, namely obtain colloidal sol after about 30min; The supporter prepared is placed in colloidal sol, liquid level is lifted out with the speed of 15cm/min, be placed in steam atmosphere film forming again, finally preliminarily dried 10min at 80 DEG C of temperature, then 50 DEG C of dry 20min are cooled to, be down to drying at room temperature 10min again, obtain uniform separating layer, average pore size about 0.5 μm.
Above-mentioned embodiment is used for illustrative purposes only, and be not limitation of the present invention, the those of ordinary skill of relevant technical field, without departing from the spirit and scope of the present invention, can also make various change and modification, therefore all equivalent technical schemes also should belong to category of the present invention.
Claims (7)
1. a water treatment preparation method for UF membrane layer, it comprises the following steps:
(1) prepare colloidal sol: added by ground aluminium isopropoxide in the deionized water of heat and carry out magnetic agitation, then add nitric acid in batches, be stirred to solution clear, then add dispersant and defoamer stirs, obtain colloidal sol;
(2) apply: supporter is immersed in colloidal sol, then supporter is upwards lifted out colloidal sol liquid level, make supporter to apply one deck liquid film;
(3) gelation: the supporter scribbling liquid film is positioned in the atmosphere containing steam and continues film forming, make liquid film be transformed into gel mould;
(4) dry: to adopt classification seasoning dry to gel mould.
2. method according to claim 1, is characterized in that: the mol ratio of aluminium isopropoxide and deionized water is 1:(95--105); The temperature of deionized water is 80 DEG C--90 DEG C.
3. method according to claim 2, is characterized in that: concentration of nitric acid is 1.65mol/L, and the mol ratio of itself and aluminium isopropoxide is (0.15-0.3): 1.
4. method according to claim 3, it is characterized in that: nitric acid is divided equally three times and added, each interval time is 1h.
5. method according to claim 1, it is characterized in that: described dispersant is Disponer-W511, addition is the 0.15%--0.3% of solution quality; Described defoamer is DeformW-0506, and addition is the 0.02%--0.04% of solution quality.
6. method according to claim 1, is characterized in that: pull rate during coating is 5-15cm/ min.
7. method according to claim 1, is characterized in that: first preliminarily dried 10min at 80 DEG C of temperature time dry, is then cooled to 50 DEG C of dry 20min, then is down to drying at room temperature 10min.
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| CN201510177546.9A CN104741007A (en) | 2015-04-16 | 2015-04-16 | Preparation method of membrane separation layer for water treatment |
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| CN201510177546.9A CN104741007A (en) | 2015-04-16 | 2015-04-16 | Preparation method of membrane separation layer for water treatment |
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| CN104741007A true CN104741007A (en) | 2015-07-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107945938A (en) * | 2017-11-16 | 2018-04-20 | 安徽天大铜业有限公司 | A kind of polyimides coats toughness electromagnetic wire |
| CN115725101A (en) * | 2022-11-21 | 2023-03-03 | 乌镇实验室 | Preparation method of nano alumina/polyimide high-temperature dielectric composite film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4968426A (en) * | 1987-12-11 | 1990-11-06 | Norton Company | Fine alpha alumina ultrafiltration membranes |
| CN101069819A (en) * | 2007-03-29 | 2007-11-14 | 西北农林科技大学 | Method for preparing composite ceramic super-filtering film on porous stainless steel substrate |
| CN103272563A (en) * | 2013-05-17 | 2013-09-04 | 武汉理工大学 | Preparation method of aluminum hydroxide film |
-
2015
- 2015-04-16 CN CN201510177546.9A patent/CN104741007A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4968426A (en) * | 1987-12-11 | 1990-11-06 | Norton Company | Fine alpha alumina ultrafiltration membranes |
| CN101069819A (en) * | 2007-03-29 | 2007-11-14 | 西北农林科技大学 | Method for preparing composite ceramic super-filtering film on porous stainless steel substrate |
| CN103272563A (en) * | 2013-05-17 | 2013-09-04 | 武汉理工大学 | Preparation method of aluminum hydroxide film |
Non-Patent Citations (1)
| Title |
|---|
| 李祥锋: "用于水处理陶瓷膜材料的制备研究", 《青岛理工大学硕士学位论文》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107945938A (en) * | 2017-11-16 | 2018-04-20 | 安徽天大铜业有限公司 | A kind of polyimides coats toughness electromagnetic wire |
| CN107945938B (en) * | 2017-11-16 | 2019-09-13 | 安徽天大铜业有限公司 | A kind of polyimides cladding toughness electromagnetic wire |
| CN115725101A (en) * | 2022-11-21 | 2023-03-03 | 乌镇实验室 | Preparation method of nano alumina/polyimide high-temperature dielectric composite film |
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Application publication date: 20150701 |