CN113274880A - Modification process of DTRO (draw texturing yarn) assembly membrane - Google Patents
Modification process of DTRO (draw texturing yarn) assembly membrane Download PDFInfo
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- CN113274880A CN113274880A CN202110706078.5A CN202110706078A CN113274880A CN 113274880 A CN113274880 A CN 113274880A CN 202110706078 A CN202110706078 A CN 202110706078A CN 113274880 A CN113274880 A CN 113274880A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/025—Reverse osmosis; Hyperfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D63/06—Tubular membrane modules
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Abstract
The invention discloses a modification process of a DTRO component membrane, which uses EDC or EDC/NHS as a coupling agent to activate-COOH on the surface of the DTRO component membrane, and then uses the activated-COOH and a membrane containing-NH2The reaction between the hydrophilic compounds leads-OH to the surface of the membrane, so that the DTRO component has stronger hydrophilicity, the water production flux and the pollution resistance of the DTRO component are effectively improved under the condition of not reducing the rejection rate of the DTRO component, meanwhile, the whole modification process directly modifies the DTRO membrane which is made into the component by using a special circulating system, the flow and the scale of the modification process are successfully realized, and the DTRO membrane has the characteristics of rapidness, high efficiency, easy realization and repeatability, and has wider application prospect.
Description
Technical Field
The invention relates to the field of reverse osmosis membrane modification, and particularly relates to a modification process of a DTRO (draw texturing RO) assembly membrane.
Background
The current commercial DTRO (disc tube type reverse osmosis) component has the problems of low pure water flux, poor pollution resistance and the like in engineering application, and greatly restricts the recovery rate and the operation period of equipment in the water treatment process. One of the technologies for improving the pure water flux and the anti-pollution performance of the membrane in the DTRO component is a surface grafting modification technology, namely, the hydrophilic substance or the zwitterionic polymer is coated or grafted on the surface of the membrane to achieve the purpose. However, most of the current modification technologies are still limited to the laboratory scale, and the modification process is relatively complex, the reaction control conditions are harsh, the cost required for modifying the unit membrane area is high, and the scale production is difficult, so that the modification technology is difficult to be applied to the modification of the commercial finished membrane module.
For example: in patent CN 103272498A, ethylene diamine is used as a cross-linking agent to prepare the imidazolidinyl urea grafted and modified aromatic polyamide composite reverse osmosis membrane, so that the biological pollution resistance and chlorine resistance of the reverse osmosis membrane are improved. However, the implementation example is limited to a rectangular reverse osmosis membrane of 13 cm × 11 cm, and industrial application is difficult to realize. In addition, because the membrane used in the DTRO module is a circular ring-shaped membrane, the finished raw membrane material needs to be cut in the preparation process, membrane area of 1/3-1/2 is lost in the process, and if the membrane is modified before the module is manufactured, waste is undoubtedly caused, and extra cost is increased.
In view of the above, the inventors of the present application invented a process for modifying a membrane of a DTRO module.
Disclosure of Invention
The invention aims to provide a modification process of a DTRO component membrane, aiming at improving the water-mixing flux and the pollution resistance of the DTRO component membrane and realizing the process and the scale production of the DTRO component membrane.
In order to achieve the purpose, the invention adopts the following technical scheme: the utility model provides a modified technology of DTRO subassembly diaphragm, adopts following circulation system to modify it, and this circulation system is including the storage tank, defeated material pump, filter, high-pressure pump and the DTRO subassembly that connect gradually, the concentrate output of DTRO subassembly and permeate liquid output are connected with a heat exchanger respectively, the DTRO subassembly is through two the heat exchanger with the storage tank is connected, and modified technology includes following step:
s1: adding an EDC or EDC/NHS coupling agent into the material storage tank, starting the delivery pump to pump the coupling agent into the water inlet end of the DTRO component and circulating the coupling agent in the modification equipment, wherein the pressure of the delivery pump is 5-10bar, the temperature of the coupling agent is controlled to be 4-25 ℃ through a heat exchanger, and the circulation time is 3-24 h;
s2: emptying the coupling agent in the step S1, adding clean water into the storage tank, starting a delivery pump to pump the clean water into the water inlet end of the DTRO component and circulating the clean water in the modification equipment, wherein the pressure of the delivery pump is 10-20bar, the water temperature is controlled to be 20-25 ℃ through a heat exchanger, and the circulation time is 1-2 h;
s3: will contain-NH2Adding the hydrophilic compound solution into the storage tank, and starting a material delivery pump to enable the solution to contain-NH2The hydrophilic compound solution is injected into the water inlet end of the DTRO component and circulates in the modification equipment, wherein the pressure of the material delivery pump is 5-10bar, the temperature of the hydrophilic compound solution is controlled to be 10-60 ℃ through a heat exchanger, and the circulation time is 10-60 min;
s4: and (5) emptying the hydrophilic compound solution in the step (S3), adding clean water into the storage tank, starting a delivery pump to pump the clean water into the water inlet end of the DTRO component, and circulating in modification equipment, wherein the pressure of the delivery pump is 10-20bar, the water temperature is controlled to be 20-25 ℃ through a heat exchanger, and the circulation time is 1-2h, so that the modification of the DTRO component membrane is completed.
Further, the EDC coupling agent is prepared by dissolving EDC in a buffer solution to prepare a uniform and stable solution, wherein the mass concentration of EDC is 0.1-1 wt%.
Further, the EDC/NHS coupling agent is prepared by dissolving EDC/NHS in a buffer solution to prepare a uniform and stable solution, wherein the mass concentration of EDC is 0.1-1wt%, the mass ratio of EDC to NHS > =4:1, EDC is added when the solution is prepared, and NHS is added after the solution reacts for 10-30 min.
Further, the buffer solution contains one or more of borax, sodium citrate, MES or PBS.
Further, the pH of the EDC or EDC/NHS coupling agent is between 4.5 and 6.5.
Further, the group containing-NH2By reacting a solution containing-NH-with a hydrophilic compound2Is dissolved in water to prepare a uniform and stable solution, wherein the solution contains-NH2To make hydrophilicThe compound being a monomer or a polymer, said compound containing-NH2The molecular weight of the hydrophilic compound (2) is 400-1000.
Further, the group containing-NH2The mass concentration of the hydrophilic compound aqueous solution of (2) is 1 to 10 wt%.
Further, the group containing-NH2The hydrophilic compound is polyethylene glycol diamine with a structural formula of (C)2H4O)nC4H12N2O, wherein n is more than or equal to 7 and less than or equal to 20.
Further, the group containing-NH2The hydrophilic compound is amino polyethylene glycol carboxylic acid with the structural formula (C)2H4O)nC5H13NO3Wherein n is more than or equal to 6 and less than or equal to 20.
After the technical scheme is adopted, the invention has the following advantages:
1. the modification process of the DTRO component membrane uses EDC or EDC/NHS as a coupling agent to activate-COOH on the surface of the DTRO component membrane, and then uses the activated-COOH and the membrane containing-NH2the-OH is introduced to the surface of the membrane through the reaction between the hydrophilic compounds, so that the DTRO component has stronger hydrophilicity, and the water production flux and the pollution resistance of the DTRO component are effectively improved under the condition of not reducing the rejection rate of the DTRO component;
2. the modification process of the DTRO component membrane directly modifies the DTRO membrane of the component by using a special circulating system, successfully realizes the flow and scale of the modification process, has the characteristics of rapidness, high efficiency, easy realization and repeatability, and has wider application prospect.
Drawings
FIG. 1 is a schematic diagram of a recycle system for membrane modification of a DTRO module according to the present invention;
FIG. 2 is a schematic diagram of a modification process of a membrane of a DTRO module according to the present invention;
FIG. 3 is a graph showing the results of comparison of anti-contamination performance before and after modification of the DTRO assembly of the present invention.
Description of reference numerals:
1-a material storage tank, 2-a material conveying pump, 3-a filter, 4-a high-pressure pump, 5-a DTRO component and 6-a heat exchanger.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the present invention, it should be noted that the terms "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are all based on the orientation or positional relationship shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the apparatus or element of the present invention must have a specific orientation, and thus, should not be construed as limiting the present invention.
Examples
The invention discloses a process for modifying a membrane of a DTRO (draw texturing yarn) assembly, which is modified by using a circulating system, wherein the circulating system comprises a storage tank, a delivery pump, a filter, a high-pressure pump and the DTRO assembly which are sequentially connected, a concentrated liquid output end and a permeate liquid output end of the DTRO assembly are respectively connected with a heat exchanger, the DTRO assembly is connected with the storage tank through the two heat exchangers, and the circulating system is shown in figure 1.
Concretely, EDC or EDC/NHS is used as a coupling agent in the modification process, -COOH on the surface of the DTRO component membrane is activated, and then the activated-COOH and the activated-NH-containing component membrane are utilized2the-OH is introduced to the surface of the membrane, so that the DTRO component has stronger hydrophilicity, and the water production flux and the pollution resistance of the DTRO component are improved under the condition of not reducing the rejection rate of the DTRO component, and the specific reaction process is shown in figure 2.
The specific modification process comprises the following steps:
s1: adding an EDC or EDC/NHS coupling agent into the material storage tank, starting the delivery pump to pump the coupling agent into the water inlet end of the DTRO component and circulating the coupling agent in the modification equipment, wherein the pressure of the delivery pump is 5-10bar, the temperature of the coupling agent is controlled to be 4-25 ℃ through a heat exchanger, and the circulation time is 3-24 h;
s2: emptying the coupling agent in the step S1, adding clean water into the storage tank, starting a delivery pump to pump the clean water into the water inlet end of the DTRO component and circulating the clean water in the modification equipment, wherein the pressure of the delivery pump is 10-20bar, the water temperature is controlled to be 20-25 ℃ through a heat exchanger, and the circulation time is 1-2 h;
s3: will contain-NH2Adding the hydrophilic compound solution into the storage tank, and starting a material delivery pump to enable the solution to contain-NH2The hydrophilic compound solution is injected into the water inlet end of the DTRO component and circulates in the modification equipment, wherein the pressure of the material delivery pump is 5-10bar, the temperature of the hydrophilic compound solution is controlled to be 10-60 ℃ through a heat exchanger, and the circulation time is 10-60 min;
s4: and (5) emptying the hydrophilic compound solution in the step (S3), adding clean water into the storage tank, starting a delivery pump to pump the clean water into the water inlet end of the DTRO component, and circulating in modification equipment, wherein the pressure of the delivery pump is 10-20bar, the water temperature is controlled to be 20-25 ℃ through a heat exchanger, and the circulation time is 1-2h, so that the modification of the DTRO component membrane is completed.
Specifically, the pH value of the EDC or EDC/NHS coupling agent is 4.5-6.5, wherein the EDC coupling agent is prepared by dissolving EDC (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) water-soluble carbodiimide in a buffer solution to prepare a uniform and stable solution, wherein the mass concentration of EDC is 0.1-1wt%, and the buffer solution contains one or more of borax, sodium citrate, MES (2-morpholinoethanesulfonic acid) or PBS (polybutylene succinate).
The EDC/NHS coupling agent is prepared by dissolving EDC (1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride)/NHS (N-hydroxysuccinimide) in a buffer solution to prepare a uniform and stable solution, wherein the buffer solution is one or more of borax, sodium citrate, MES or PBS, the mass concentration of EDC is 0.1-1wt%, the mass ratio of EDC to NHS > =4:1, EDC is firstly added during the preparation of the solution, and NHS is added after the reaction is carried out for 10-30 min.
Specifically, the compound contains-NH2Mass concentration of the hydrophilic compound aqueous solution1 to 10wt%, said-NH-containing2By reacting a solution containing-NH-with a hydrophilic compound2Is dissolved in water to prepare a uniform and stable solution, wherein the solution contains-NH2Is a monomer or a polymer, said hydrophilic compound containing-NH2The molecular weight of the hydrophilic compound is 400-1000, so that the water yield of the DTRO component can be ensured to be improved while the retention performance of the DTRO component is not reduced.
Preferably, said group containing-NH2The hydrophilic compound is polyethylene glycol diamine with a structural formula of (C)2H4O)nC4H12N2O, wherein n is more than or equal to 7 and less than or equal to 20; or amino polyethylene glycol carboxylic acid with the structural formula (C)2H4O)nC5H13NO3Wherein n is more than or equal to 6 and less than or equal to 20, the molecular weight of the hydrophilic compound can be changed from a sawtooth structure into a zigzag structure in an aqueous solution, and the hydrophilicity-O-is distributed on the surface of a chain to enable a polymer to be easily combined with water molecules, so that the modified diaphragm has high flux and strong anti-pollution capacity.
Experiment 1: flux comparison before and after modification of the DTRO module:
the test conditions are shown in table 1, and the test results are shown in table 2. As can be seen from Table 2, compared with the unmodified DTRO component, the pure water flux of the modified DTRO component is improved by about 45% under the same conditions, and the rejection rate is not obviously reduced, which indicates that the pure water flux of the DTRO component can be effectively improved after the modified DTRO component is modified by adopting the process.
TABLE 1 test conditions
| Test items | Raw material liquid | Test temperature (. degree. C.) | Test pressure (bar) | Feed flow (L/min) |
| Pure water flux | Tap water | 28±1 | 22.5 | 18-20 |
| Retention rate | 48ms/cm NaCl solution | 35±1 | 55.0 | 18-20 |
TABLE 2 test results
| Pure water flux (LMH) | Retention (%) | |
| Pre-modification DTRO (draw texturing yarn) component | 31.2 | 99.47 |
| Modified DTRO component | 45.5 | 99.55 |
Experiment 2: and (3) comparing the pollution resistance before and after the modification of the DTRO component:
as shown in fig. 3, it can be seen from fig. 3 that the operating pressure of the modified DTRO module is significantly reduced with the increase rate of the operating time under the same water inlet condition, and the chemical washing period is prolonged from 80h to over 220 h. The pollution resistance of the DTRO component can be effectively enhanced after the modification by the process.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A modification process of a DTRO component membrane is characterized in that: adopt following circulation system to modify it, this circulation system is including the storage tank, defeated material pump, filter, high-pressure pump and the DTRO subassembly that connect gradually, the concentrate output and the permeate liquid output of DTRO subassembly are connected with a heat exchanger respectively, the DTRO subassembly is through two the heat exchanger with the storage tank is connected, and modification process includes following step:
s1: adding an EDC or EDC/NHS coupling agent into the material storage tank, starting the delivery pump to pump the coupling agent into the water inlet end of the DTRO component and circulating the coupling agent in the modification equipment, wherein the pressure of the delivery pump is 5-10bar, the temperature of the coupling agent is controlled to be 4-25 ℃ through a heat exchanger, and the circulation time is 3-24 h;
s2: emptying the coupling agent in the step S1, adding clean water into the storage tank, starting a delivery pump to pump the clean water into the water inlet end of the DTRO component and circulating the clean water in the modification equipment, wherein the pressure of the delivery pump is 10-20bar, the water temperature is controlled to be 20-25 ℃ through a heat exchanger, and the circulation time is 1-2 h;
s3: will contain-NH2Adding the hydrophilic compound solution into the storage tank, and starting a material delivery pump to enable the solution to contain-NH2The hydrophilic compound solution is injected into the water inlet end of the DTRO component and circulates in the modification equipment, wherein the pressure of the material delivery pump is 5-10bar, the temperature of the hydrophilic compound solution is controlled to be 10-60 ℃ through a heat exchanger, and the circulation time is 10-60 min;
s4: and (5) emptying the hydrophilic compound solution in the step (S3), adding clean water into the storage tank, starting a delivery pump to pump the clean water into the water inlet end of the DTRO component, and circulating in modification equipment, wherein the pressure of the delivery pump is 10-20bar, the water temperature is controlled to be 20-25 ℃ through a heat exchanger, and the circulation time is 1-2h, so that the modification of the DTRO component membrane is completed.
2. The process of claim 1, wherein the step of modifying the membrane of the DTRO module comprises: the EDC coupling agent is prepared by dissolving EDC in a buffer solution to prepare a uniform and stable solution, wherein the mass concentration of EDC is 0.1-1 wt%.
3. The process of claim 1, wherein the step of modifying the membrane of the DTRO module comprises: the EDC/NHS coupling agent is prepared by dissolving EDC/NHS in a buffer solution to prepare a uniform and stable solution, wherein the mass concentration of EDC is 0.1-1wt%, the mass ratio of EDC to NHS > =4:1, EDC is firstly added when the solution is prepared, and NHS is added after the reaction is carried out for 10-30 min.
4. A process for modifying a membrane of a DTRO module according to claim 2 or 3, wherein: the buffer solution contains one or more of borax, sodium citrate, MES or PBS.
5. The process of claim 1, wherein the step of modifying the membrane of the DTRO module comprises: the EDC or EDC/NHS coupling agent has a pH of between 4.5 and 6.5.
6. The DTRO module membrane of claim 1, wherein the DTRO module membrane comprises a membrane having a membrane opening and a membrane openingThe process is characterized by comprising the following steps: said group containing-NH2By reacting a solution containing-NH-with a hydrophilic compound2Is dissolved in water to prepare a uniform and stable solution, wherein the solution contains-NH2Is a monomer or a polymer, said hydrophilic compound containing-NH2The molecular weight of the hydrophilic compound (2) is 400-1000.
7. The process of claim 1, wherein the step of modifying the membrane of the DTRO module comprises: said group containing-NH2The mass concentration of the hydrophilic compound aqueous solution of (2) is 1 to 10 wt%.
8. The process of claim 1 or 6, wherein the step of modifying the membrane of the DTRO module comprises: said group containing-NH2The hydrophilic compound is polyethylene glycol diamine with a structural formula of (C)2H4O)nC4H12N2O, wherein n is more than or equal to 7 and less than or equal to 20.
9. The process of claim 1 or 6, wherein the step of modifying the membrane of the DTRO module comprises: said group containing-NH2The hydrophilic compound is amino polyethylene glycol carboxylic acid with the structural formula (C)2H4O)nC5H13NO3Wherein n is more than or equal to 6 and less than or equal to 20.
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2021
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