CN106861444A - A kind of micro-filtration, milipore filter regenerative agent and preparation method thereof - Google Patents
A kind of micro-filtration, milipore filter regenerative agent and preparation method thereof Download PDFInfo
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- CN106861444A CN106861444A CN201710187333.3A CN201710187333A CN106861444A CN 106861444 A CN106861444 A CN 106861444A CN 201710187333 A CN201710187333 A CN 201710187333A CN 106861444 A CN106861444 A CN 106861444A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/168—Use of other chemical agents
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Abstract
The invention discloses a kind of micro-filtration, milipore filter regenerative agent and preparation method thereof, the regenerative agent, by the active alkali potassium hydroxide without sodium ion, water treatment agent ATMP and intercalating agent K-IAO are prepared from for raw material, successively to adding K-IAO in deionized water, potassium hydroxide and ATMP obtain regenerative agent finished product after stirring, regenerative agent finished product adds deionized water to be diluted to the regenerative agent aqueous solution that concentration is 1%, for food industry, petrochemical industry, sewage disposal, micro-filtration in steel industry, the cleaning and regeneration of milipore filter；The present invention has excellent micro-filtration, milipore filter power of regeneration, it is easy to which excessively aqueous energy, organic polymer compatibility is good, with the effect for significantly inhibiting the formation of the crystal structures such as calcium, magnesium, the almost noresidue inside film surface or fenestra；And long-term use causes that the permanent flux downward trend of film is significantly inhibited.
Description
Technical field
The present invention relates to micro-filtration, milipore filter regenerating reagent technical field, specifically a kind of micro-filtration, milipore filter regenerative agent and
Its preparation method.
Background technology
Various micro-filtrations, milipore filter are widely used in food industry, petrochemical industry, sewage disposal, steel industry, mainly exist
Applied in the processing steps such as removal of impurities, macromolecular substances extraction, desalination, decolouring, organic matter concentration, water-oil separating；Micro-filtration, milipore filter
Regeneration technology have critically important influence for the production efficiency and production cost of membrane separation process, wherein regenerative agent performance is it
One of key factor.
Film regenerative agent is trapped the chemical solution of material as clean film surface, fenestra inside and dissolving, for recovering
The effective penetrating area of film, increases net water flux and plays an important roll；At present, the most frequently used film regenerative agent such as NaOH, by
It is stronger in adhesion, it is difficult to be flush with water, film surface is residued in, especially calcium of the alkali inside fenestra easily and in retention material
Calcium ions and magnesium ions in magnesium ion, and water form hard-packed crystal, cause the permanent of the penetrating area of film and net water flux
Decline, for retaining the dissolving of material, cleansing power is limited, and its regeneration effect is unsatisfactory for single NaOH in addition, therefore
Limit its range of application；Conventional intercalating agent such as ethylenediamine tetra-acetic acid (EDTA), its chelant ability significantly, but cannot increase hydrogen
The discharge capacity of sodium oxide molybdena, the formation for suppressing calcium and magnesium crystal structure in fenestra has no remarkable result, and chelant ability is simultaneously
Will not increase due to the increase of basicity and temperature, range of application is restricted.
General micro-filtration, milipore filter can form the concentration polarization of retention material during UF membrane in the side of film
Layer, the even part having enters inside fenestra, causes the decline of membrane area and the reduction of the penetrating amount of water purification, this membrane area
Decline is temporary transient, typically can carry out film regeneration by physical means such as recoil, vibration, ultrasonic waves, and addition contains hydrogen
The solution of sodium oxide molybdena or phosphoric acid is circulated the chemical means such as dissolving trapped substance and is regenerated；Traditional sodium hydroxide solution is again
After life, because NaOH is than less easily crossing inside the more small fenestra of water, especially aperture ratio, almost without washing away machinery
Power, thus results in NaOH and is remained in fenestra, remains in the alkali combination trapped substance in film or separates solution, cleaning and prepares
Calcium, magnesium compound crystal can be formed with the calcium in water, magnesium ion, if this crystalloid is formed in inside fenestra, fenestra can be caused
Block, and due to this crystalloid and membrane material combination closely, unless any special measures be typically difficult regenerate, this membrane area
Drop to it is permanent；In recent years, researcher is carried out to active alkali and the property of polyphosphate without sodium ion
Research, it is found that its surface adhesion is small without the active alkali of sodium ion, is relatively easily flush with water completely, especially in fenestra
Some washing water quantities such as inside are small, and the less region of mechanical force, and its alkali residual quantity is relatively small for suppressing in fenestra
Calcium, the formation of magnesium crystal structure have remarkable effect；Polyphosphate can substantially increase albumen, grease, polysaccharide polymer
Dispersibility of the matter in water, can accelerate to retain the speed that material is removed from film surface, accelerate the speed of film regeneration, improve film
The effect of regeneration；In addition, intercalating agent, especially chelant ability regenerated with the intercalating agent that temperature and basicity rise and rises in film
The combination of calcium ions and magnesium ions and residual alkali in fenestra can further be suppressed in journey, the membrane material high-alkali for high temperature resistant was regenerating
The crystal formed in journey can further suppress.
The content of the invention
It is an object of the invention to provide a kind of with the active alkali without sodium ion, water treatment agent and intercalating agent as former
Material, as obtained in stabilization process, with excellent micro-filtration, milipore filter power of regeneration, was easy to aqueous energy, and organic polymer is simultaneous
Capacitive, and have in regenerative process significantly inhibit the crystal structures such as calcium, magnesium formed the micro-filtration of effect, milipore filter regenerative agent and its
Preparation method, to solve the problems, such as to be proposed in above-mentioned background technology.
To achieve the above object, the present invention provides following technical scheme：
A kind of micro-filtration, milipore filter regenerative agent, by the active alkali without sodium ion be potassium hydroxide excellent discharge capacity,
Water treatment agent be ATMP to the dispersibility of macromolecular substances, in aqueous slkali to organic matter solvability
Improve and chelating agent is for the sequestering power collective effect realization of calcium ions and magnesium ions in water.
As further scheme of the invention：The active alkali without sodium ion is potassium hydroxide, and intercalating agent is grape
Saccharic acid potassium, water treatment agent is ATMP；Each raw material is respectively according to the proportioning of mass percent：Potassium hydroxide
30%~45%, ATMP content 6%~10%, K-IAO 5%~15%, deionized water 30%~
59%.
As further scheme of the invention：The preparation method of the micro-filtration, milipore filter regenerative agent, including following step
Suddenly：
1) first, by each raw material of formula ratio, K-IAO is added in deionized water, stirring causes that K-IAO exists
It is completely dissolved in deionized water；
2) secondly, in step 1) potassium hydroxide is added in the gluconic acid aqueous solutions of potassium for preparing, 15min is with up to hydrogen for stirring
Potassium oxide is completely dissolved；
3) last, in step 2) containing of preparing add liquid water treatment agent amino in intercalating agent, the aqueous solution of active alkali
Trimethylene phosphonic, stirs, and obtains regenerative agent finished product, and proportion of the regenerative agent finished product being made under the conditions of 20 DEG C is 1.25
~1.50g/ml.
Regenerative agent finished product adds deionized water, the regenerative agent aqueous solution that concentration is 1% is diluted to, for food industry, stone
The cleaning and regeneration of micro-filtration, milipore filter in chemical industry, sewage disposal, steel industry, concentration is the pH value of the 1% regenerative agent aqueous solution
It is 12.5~14.0.
As further scheme of the invention：The micro-filtration, the preparation method of milipore filter regenerative agent are comprised the following steps：
1) ionized water 1600-2750g is removed, is added in the container equipped with agitator, 450-600g conducts are added at room temperature
The K-IAO of chelating agent, at the uniform velocity stirring mixing 15min to K-IAO are completely dissolved；
2) to step 1) gluconic acid aqueous solutions of potassium in add without sodium ion active alkali potassium hydroxide solid 1500-
2250g, potassium hydroxide purity is 98%, in 0.5-2h is reacted under 25 DEG C of -40 DEG C of temperature conditionss, is stirred completely molten to potassium hydroxide
Solution；
3) to step 2) in the aqueous solution containing chelating agent and active alkali, add 300-550g as the ammonia of water treatment agent
Base trimethylene phosphonic, concentration is adjusted to for the 1% regenerative agent aqueous solution with deionized water or active alkali, and its pH value is 12.5-
14.0, control regenerative agent aqueous solution gross mass for 5000g, obtain finished product.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is utilized by the active alkali without sodium ion, water
Inorganic agent and intercalating agent are raw material Membrane cleaning regenerative agent as obtained in stabilization process, are configured to containing the present invention again with water
The solution of the raw percent by volume of agent 0.5%~3.0%, for carrying out cleaning and regeneration to contaminated micro-filtration, milipore filter, there is excellent
Micro-filtration, milipore filter power of regeneration, it will be apparent that be easy to aqueous energy, organic polymer compatibility is good, and in regenerative process have
There are the effect for significantly inhibiting the formation of the crystal structures such as calcium, magnesium, the almost noresidue inside film surface or fenestra；Film regeneration efficiency
It is high；Film regeneration technology is simple simultaneously, it is easy to operate, membrane material, dirt and condition of water quality are applicable wide in range；Not only film recovery time
Shorten, film regeneration effect improves, and long-term use causes that the permanent flux downward trend of film is significantly inhibited, so as to prolong
The service life for having grown film relaxes film regeneration right, the production cost for reducing membrane separation process, increased the production efficiency of film
The requirement of condition of water quality；This big bright micro-filtration, milipore filter regenerative agent can be widely applied to food industry, petrochemical industry, at sewage
In reason, steel industry.
Brief description of the drawings
Fig. 1 is that regenerative agent of the present invention suppresses micro-filtration, the permanent flux downward trend figure of milipore filter.
Fig. 2 is that regenerative agent of the present invention shortens micro-filtration, the tendency chart of milipore filter recovery time.
Specific embodiment
The technical scheme of this patent is described in more detail with reference to specific embodiment.
Embodiment 1
Fig. 1, a kind of micro-filtration, milipore filter regenerative agent and preparation method thereof are referred to, the regenerative agent is made by K-IAO
It is chelating agent, potassium hydroxide is prepared from as the active alkali without sodium ion, ATMP as water treatment agent,
Specifically preparation method is：
Ionized water 2500g is removed, is added in the container equipped with agitator, add 600g glucose in uniform stirring at room temperature
Sour potassium, persistently mixes 15 minutes, after confirmation is completely dissolved, 1500g purity is subsequently added for 98% potassium hydroxide solid, in 25 DEG C
2.0h is reacted under temperature conditionss, after confirmation is completely dissolved, 300g ATMPs is added, with deionized water or activity
It is 12.5~14.0 that alkali adjusts the regenerative agent aqueous solution pH that concentration is 1%, controls regenerative agent aqueous solution gross mass for 5000g, is obtained
To finished product 1.
The experiment of the cleaning efficiency of finished product 1 is as follows：
It is 50ppm (with CaCO with the water hardness3Meter) water prepare be about containing the concentration of finished product 1 2.5% aqueous solution conduct
Regenerative agent, the polysulfones material milipore filter to the dalton of molecular cut off about 1,000,000 carries out pressure flush, every time cleaning about 1h, clearly
Temperature control is washed at 50 DEG C, after with the water hardness be 50ppm (with CaCO3Meter) water pressure flush about 0.5h, rinse temperature control
At 50 DEG C, the net water flux for repeating above-mentioned 100 caudacorias of regenerative process declines about 2.7%.
It is 50ppm (with CaCO with the water hardness3Meter) water prepare containing 30% NaOH (NaOH) solution about 2.5%
The aqueous solution carries out pressure flush as regenerative agent, the polysulfones material milipore filter to the dalton of molecular cut off about 1,000,000, clear every time
Wash about 1h, cleaning temperature is controlled at 50 DEG C, after with the water hardness be 50ppm (with CaCO3Meter) water pressure flush about 0.5h, rinse
Temperature control is at 50 DEG C；The net water flux for repeating above-mentioned 100 caudacorias of regenerative process declines about 41.0%.
Two groups of regenerative agents suppress micro-filtration, the permanent flux downward trend of milipore filter and see accompanying drawing 1, by the data in accompanying drawing 1
As can be seen that temperature, the time, basicity, the water hardness and membrane material it is identical in the case of, carry out 100 cleaning and regenerations
Afterwards, the film for being regenerated with regenerative agent of the present invention, permanent throughput loss about 3.0%, the film of traditional alkali regenerative agent regeneration permanently leads to
Amount loss reach 40%, because the throughput loss that high-temperature alkali and calcium ions and magnesium ions are caused cannot almost regenerate, thus the present invention for
Extension membrane lifetime, suppressing the permanent flux decline of film has remarkable effect.
Embodiment 2
A kind of micro-filtration, milipore filter regenerative agent and preparation method thereof, the regenerative agent is by K-IAO as chelating agent, hydrogen
Potassium oxide is prepared from as the active alkali without sodium ion, ATMP as water treatment agent, specific preparation side
Method is：
Ionized water 2000g is removed, is added in the container equipped with agitator, add 450g Portugals at the uniform velocity under stirring condition at room temperature
Grape saccharic acid potassium, persistently mixes 15 minutes, after confirmation is completely dissolved.The potassium hydroxide solid that 1850g purity is 98% is subsequently added,
React 1.0h under 32 DEG C of temperature conditionss, after confirmation is completely dissolved, add 550g ATMPs, with deionized water or
Active alkali is adjusted to the regenerative agent aqueous solution pH about 12.5~14.0 that concentration is 1%, and control regenerative agent aqueous solution gross mass is about
5000g, obtains finished product 2.
The experiment of the cleaning efficiency of finished product 2 is as follows：
It is 20ppm (with CaCO with the water hardness3Meter) water prepare the aqueous solution containing the concentration of finished product 2 about 2.5% as again
Raw agent, the ceramic material milipore filter to the dalton of molecular cut off about 500,000 of filtering aloe plant extract solution about 5h pressurizes
Rinse, the film net water flux drops to the 17% of design flux before regeneration, clean about 2h, cleaning temperature is controlled at 70 DEG C, used afterwards
It is 20ppm (with CaCO with the water hardness3Meter) water pressure flush about 0.5h, rinse temperature control at 40 DEG C, regeneration caudacoria it is net
Water flux recovers to the 93.5% of design flux.
It is 20ppm (with CaCO with the water hardness3Meter) water prepare the water containing 39% concentration of sodium hydroxide solution about 2.5%
Solution enters as regenerative agent, the ceramic material milipore filter to the dalton of molecular cut off about 500,000 of filter plant extract solution about 5h
Row pressure flush, the film net water flux drops to the 21% of design flux before regeneration, cleans about 2h, and cleaning temperature is controlled 70
DEG C, after with the water hardness be 20ppm (with CaCO3Meter) water pressure flush about 0.5h, rinse temperature control at 40 DEG C, after regeneration
The net water flux of film recovers to the 72.2% of design flux, and two groups of regenerative agents suppress what the permanent flux of micro-filtration, milipore filter declined
Trend is as shown in the table：
Table 1：Recover micro-filtration, the temporary flux downward trend of milipore filter
From the data of table 1 as can be seen that in the case of temperature, time, basicity, water hardness all same, according to implementation
The more traditional alkali regeneration of membrane flux of the regeneration of regenerative agent finished product 2 prepared by example 2 improves about 50% or so, illustrates regeneration of the invention
Agent has stronger trapped substance dissolving, dispersibility in regenerative process, and the more traditional alkali regeneration of regeneration efficiency is high.
Embodiment 3
A kind of micro-filtration, milipore filter regenerative agent and preparation method thereof, the regenerative agent is by K-IAO as chelating agent, hydrogen
Potassium oxide is prepared from as the active alkali without sodium ion, ATMP as water treatment agent, specific preparation side
Method is：
Ionized water 1850g is removed, is added in the container equipped with agitator, add 500g Portugals at the uniform velocity under stirring condition at room temperature
Grape saccharic acid potassium, persistently mixes 15 minutes, after confirmation is completely dissolved, the potassium hydroxide solid that 2250g purity is 98% is added, in 40
DEG C reaction 0.5h, confirmation be completely dissolved after, add 400g ATMPs, be adjusted to deionized water or active alkali
Concentration is 1% regenerative agent aqueous solution pH about 12.5~14.0, controls regenerative agent aqueous solution gross mass about 5000g, obtains finished product
3。
The experiment of the cleaning efficiency of finished product 3 is as follows：
It is 140ppm (with CaCO with the water hardness3Meter) water prepare the aqueous solution containing the concentration of finished product 3 about 2.0% as again
Raw agent, the acetate fiber material NF membrane to filtering amino acid zymotic fluid about 8h carries out pressure flush, and the film water purification leads to before regeneration
Amount drops to the 25% of design flux, and at 45 DEG C, the penetrating amount of solution reaches used during the 85% of design flux for cleaning temperature control
About 110 minutes time.
It is 140ppm (with CaCO with the water hardness3Meter) water prepare contain 45% concentration of sodium hydroxide solution about 2.0%
The aqueous solution carries out pressure flush, regenerates as regenerative agent, the acetate fiber material NF membrane to filtering amino acid zymotic fluid about 8h
The preceding film net water flux drops to the 28% of design flux, and cleaning temperature is controlled at 45 DEG C, and the penetrating amount of solution reaches design flux
85% when about 200 minutes time used.
Two groups of regenerative agents shorten micro-filtration, the trend of milipore filter recovery time as shown in Figure 2, figure it is seen that in temperature
In the case of degree, time, basicity, water hardness all same, in the case that nanofiltration membrane flux is close before regeneration, the embodiment of the present invention 3
The membrane flux that the finished product 3 of preparation regenerates reaches the 75% of design flux, about 80 minutes time, and traditional alkali is needed about 140 minutes；This
The membrane flux of the regeneration of finished product 3 prepared by inventive embodiments 3 reaches about 120 minutes 85% time of design flux, and traditional alkali is needed about
180 minutes, illustrate that the more traditional alkali of the present invention can improve regeneration efficiency, less recovery time.
The better embodiment to this patent is explained in detail above, but this patent is not limited to above-mentioned embodiment party
Formula, in the ken that one skilled in the relevant art possesses, can also be on the premise of this patent objective not be departed from
Make a variety of changes.
Claims (4)
1. a kind of micro-filtration, milipore filter regenerative agent, are raw material preparation by the active alkali without sodium ion, water treatment agent and intercalating agent
Form, it is characterised in that：The active alkali without sodium ion is potassium hydroxide, and intercalating agent is K-IAO, water treatment agent
It is ATMP；Each raw material is respectively according to the proportioning of mass percent：Potassium hydroxide 30%~45%, amino three
Methylene phosphonic acid content 6%~10%, K-IAO 5%~15%, deionized water 30%~59%.
2. micro-filtration according to claim 1, the preparation method of milipore filter regenerative agent, it is characterised in that comprise the following steps：
1) first, by each raw material of formula ratio, add K-IAO in deionized water, stirring cause K-IAO go from
It is completely dissolved in sub- water；
2) secondly, in step 1) potassium hydroxide is added in the gluconic acid aqueous solutions of potassium for preparing, 15min is with up to hydroxide for stirring
Potassium is completely dissolved；
3) last, in step 2) containing of preparing add liquid water treatment agent amino trimethylene in intercalating agent, the aqueous solution of active alkali
Methylphosphonic acid, stirs, and obtains regenerative agent finished product.
3. micro-filtration according to claim 2, the preparation method of milipore filter regenerative agent, it is characterised in that the step 3) in,
Proportion of the regenerative agent finished product being made under the conditions of 20 DEG C is 1.25~1.50g/ml.
4. according to claim 1-3 any described micro-filtration, milipore filter regenerative agent, it is characterised in that add deionized water, dilution
Into the regenerative agent aqueous solution that concentration is 1%, for micro-filtration, ultrafiltration in food industry, petrochemical industry, sewage disposal, steel industry
The cleaning and regeneration of film, concentration is that the pH value of the 1% regenerative agent aqueous solution is 12.5~14.0.
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| CN201710187333.3A CN106861444A (en) | 2017-03-27 | 2017-03-27 | A kind of micro-filtration, milipore filter regenerative agent and preparation method thereof |
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| CN201710187333.3A CN106861444A (en) | 2017-03-27 | 2017-03-27 | A kind of micro-filtration, milipore filter regenerative agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110564516A (en) * | 2019-09-10 | 2019-12-13 | 上海丰信环保科技有限公司 | neutral cleaning agent for cleaning MBR system |
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| CN101039881A (en) * | 2004-02-26 | 2007-09-19 | 汉斯休伯机械制造股份公司 | Installation and method for the treatment of sewage sludge, and membrane unit |
| CN101069817A (en) * | 2007-06-08 | 2007-11-14 | 江南大学 | Micro-filtering or super-filtering film regenerating agent and preparing method |
| CN206027462U (en) * | 2016-08-29 | 2017-03-22 | 天津市华博水务有限公司 | Milipore filter post on -line monitoring chemical cleaning device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1816384A (en) * | 2003-07-04 | 2006-08-09 | 阿克佐诺贝尔股份有限公司 | Cleaning of filtration membranes with peroxides |
| CN101039881A (en) * | 2004-02-26 | 2007-09-19 | 汉斯休伯机械制造股份公司 | Installation and method for the treatment of sewage sludge, and membrane unit |
| CN101069817A (en) * | 2007-06-08 | 2007-11-14 | 江南大学 | Micro-filtering or super-filtering film regenerating agent and preparing method |
| CN206027462U (en) * | 2016-08-29 | 2017-03-22 | 天津市华博水务有限公司 | Milipore filter post on -line monitoring chemical cleaning device |
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| CN110564516A (en) * | 2019-09-10 | 2019-12-13 | 上海丰信环保科技有限公司 | neutral cleaning agent for cleaning MBR system |
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Application publication date: 20170620 |