CN109647203B - Improved spinneret plate for parallel channel nanofiltration membrane and preparation method - Google Patents
Improved spinneret plate for parallel channel nanofiltration membrane and preparation method Download PDFInfo
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- CN109647203B CN109647203B CN201811601843.1A CN201811601843A CN109647203B CN 109647203 B CN109647203 B CN 109647203B CN 201811601843 A CN201811601843 A CN 201811601843A CN 109647203 B CN109647203 B CN 109647203B
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- spinneret
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
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Abstract
The invention belongs to the field of membrane preparation of hollow fiber membranes, and particularly relates to an improved spinneret plate for a parallel channel nanofiltration membrane and a preparation method of the improved spinneret plate. An improved spinneret plate for a parallel channel nanofiltration membrane comprises a plurality of spinneret units which are connected with each other; the spinneret unit comprises spinneret orifices and arc spinneret orifices which are arranged on the upper side and the lower side of each spinneret orifice and are symmetrical, and adjacent arc spinneret orifices are connected through straight transition holes. The design of the invention improves the problem that the finally obtained parallel channel base film is seriously deviated from the spinneret orifice due to the expansion of the polymer and the combined action of various factors such as radial stretching, transverse contraction and the like in the preparation process of the base film. The nanofiltration membrane prepared by the parallel channel base membrane formed by the invention has high strength, large flux and extremely low incidence of broken filaments.
Description
Technical Field
The invention belongs to the field of membrane preparation of hollow fiber membranes, and particularly relates to an improved spinneret plate for a parallel channel nanofiltration membrane and a preparation method of the improved spinneret plate.
Background
In the preparation process of the base membrane of the hollow fiber nanofiltration membrane, due to the expansion of the polymer and the comprehensive action of various factors such as radial stretching, transverse contraction and the like, the finally obtained base membrane with parallel channels has serious deviation from spinneret orifices.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides an improved spinneret plate for a parallel channel nanofiltration membrane and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
an improved spinneret plate for a parallel channel nanofiltration membrane comprises a plurality of spinneret units which are connected with each other; the spinneret unit comprises spinneret orifices and arc spinneret orifices which are arranged on the upper side and the lower side of each spinneret orifice and are symmetrical, and adjacent arc spinneret orifices are connected through straight transition holes.
The circular-arc spinneret orifices and the circular spinneret orifices are concentric circles; the arc radiuses of the arc-shaped spinneret holes of the spinneret units at the two ends are larger than the arc radiuses of the arc-shaped spinneret holes of the spinneret unit in the middle.
The axial distance of the straight transition holes of the adjacent spinning units is 0.1-0.2 mm; the radius of the spinneret orifice is 0.25-0.3mm, and the radius of the middle arc spinneret orifice is 0.45-0.5 mm; the radius of the two circular arc spinneret orifices is 0.55-0.6 mm.
The invention also comprises a preparation method of the improved parallel channel nanofiltration membrane, the improved parallel channel nanofiltration membrane is used for spinning the base membrane by using a spinneret plate, the feed liquid conveying pressure is 0.03-0.1MPa, the drafting speed is 16.5-24m/min, the solid content of the feed liquid is 15-35%, and the coagulating bath temperature is 55-85 ℃; obtaining the multi-channel basement membrane.
Compared with the prior art, the invention has the beneficial effects that:
the spinneret plate is optimized as follows: the edge of the spinneret orifice is changed from a linear type to an arc shape, so that the wall thickness of the middle spinneret orifice is reduced by about 10-30%, the wall thickness of the straight transition wall of the adjacent spinneret units is increased by about 10-20%, the channel spacing is increased by 30-50%, the corner is smoothed, and the spinneret orifice of the spinneret plate is increased by 50-100%. The design of the invention improves the problem that the finally obtained parallel channel base film is seriously deviated from the spinneret orifice due to the expansion of the polymer and the combined action of various factors such as radial stretching, transverse contraction and the like in the preparation process of the base film. The nanofiltration membrane prepared by the parallel channel base membrane formed by the invention has high strength, large flux and extremely low incidence of broken filaments.
Drawings
Fig. 1 is a schematic view of the overall structure of a spinneret plate for an improved parallel channel nanofiltration membrane according to the present invention;
fig. 2 is a schematic view of the overall structure of a spinneret plate in the prior art;
fig. 3 is an SEM photograph of a nanofiltration membrane obtained by a spinneret in the prior art;
fig. 4 is an SEM photograph of the nanofiltration membrane obtained by the spinneret plate for the improved parallel channel nanofiltration membrane of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
FIG. 1 shows an improved spinneret for parallel channel nanofiltration membranes, comprising a plurality of spinning units connected to each other; the spinneret unit comprises spinneret orifices and arc spinneret orifices (1 and 2) which are arranged symmetrically on the upper side and the lower side of each spinneret orifice, and adjacent arc spinneret orifices are connected through straight transition holes (4).
The circular-arc spinneret orifices and the circular spinneret orifices 3 are concentric circles; the arc radius of the arc-shaped spinneret holes 1 of the spinneret units at the two ends is larger than that of the arc-shaped spinneret holes 2 of the spinneret unit in the middle.
Example 1: the axial distance of the straight transition holes of the adjacent spinning units is 0.1 mm; the radius of each spinneret orifice is 0.25mm, and the radius of the middle arc spinneret orifice is 0.45 mm; the radius of the circular arc spinneret orifices at the two ends is 0.55 mm. The base film is spun by using the improved spinneret plate in the embodiment 1, the feed liquid conveying pressure is 0.03MPa, the drafting speed is 16.5m/min, the solid content of the feed liquid is 15 percent, and the coagulating bath temperature is 55 ℃; obtaining the multi-channel basement membrane.
Example 2: the axial distance of the straight transition holes of the adjacent spinning units is 0.2 mm; the radius of each spinneret orifice is 0.3mm, and the radius of the middle arc spinneret orifice is 0.5 mm; the radius of the circular arc spinneret orifices at the two ends is 0.6 mm. The base film is spun by using the improved spinneret plate of the embodiment 2, the feed liquid conveying pressure is 0.1MPa, the drafting speed is 24m/min, the solid content of the feed liquid is 35 percent, and the coagulating bath temperature is 85 ℃; obtaining the multi-channel basement membrane.
Example 3: the axial distance of the straight transition holes of the adjacent spinning units is 0.15 mm; the radius of each spinneret orifice is 0.28mm, and the radius of the middle arc spinneret orifice is 0.48 mm; the radius of the circular arc spinneret orifices at the two ends is 0.58 mm. The base film is spun by using the improved spinneret plate of the embodiment 3, the feed liquid conveying pressure is 0.05MPa, the drafting speed is 21.5m/min, the solid content of the feed liquid is 16 percent, and the coagulating bath temperature is 75 ℃. And immersing the obtained multichannel base film in deionized water to be detected.
Comparative example 1: the same procedure as in example 3 was repeated except that a single passage was used (the arc radius of the arc-shaped orifices 1 of the orifice units at both ends was equal to the arc radius of the arc-shaped orifice 2 of the orifice unit in the middle).
Comparative example 2: the feed liquid conveying pressure is 0.22MPa, the drawing speed is 13.8m/min, the solid content of the feed liquid is 28 percent, and the temperature of the coagulation bath is 55 ℃. And immersing the obtained multichannel base film in deionized water to be detected. The rest is the same as in example 3.
Comparative example 3: the base film was prepared using prior art multiple passes (inner layer orifices having a diameter of 0.6mm, outer layer orifices having a distance (width) perpendicular to the axial direction of 0.3mm, and adjacent inner layer orifices having a distance of 0.6 mm.
The base films obtained in examples 1 to 3 and comparative examples 1 to 3 were used for functional layer coating to obtain examples 4 to 6; comparative examples 4 to 6; aqueous solution 2 parts (mass parts not specified) of piperazine, 0.1 part of sodium hydroxide, and 100 parts of deionized water. 0.1 part of trimesoyl chloride and 100 parts of normal hexane are taken as organic phase solution. And (3) interfacial polymerization process: the base membrane was immersed in phase A for 10s and purged with high velocity air for 4 min. And immersing the product in the B phase for 40s, and treating the product for 40s by using low-speed hot air at the temperature of 80-100 ℃ to obtain the product, wherein the product is immersed in deionized water to be detected. Figure 3 shows an SEM photograph of the nanofiltration membrane prepared in comparative example 6. Figure 4 shows an SEM photograph of the nanofiltration membrane prepared in example 6.
The multi-channel membrane rupture strength test method comprises the steps of taking 10.0cm multi-channel membrane filaments to test in a rupture strength tester, and recording results in the following table 1.
TABLE 1
| Breaking strength, N | |
| Example 1 | 52.7 |
| Example 2 | 60.2 |
| Example 3 | 54.1 |
| Comparative example 1 | 5.2 |
| Comparative example 2 | 39.6 |
| Comparative example 3 | 62.9 |
The multi-channel membrane separation performance test method comprises the following steps:
testing liquid: with 2000mg/L magnesium sulfate (MgSO)4) And (4) testing the solution.
The operation parameters are as follows: the test was carried out using a multichannel membrane evaluation apparatus, the pressure was 0.5MPa, the pH was 7.0 at 25 ℃, and the recovery rate was 15%.
Calculating the formula:
retention rate R ═ CI-CO)/CI100% of CIFor water conductivity, COConducting for water outlet;
flux F ═ V/(a × T), where V is the water production volume, a is the membrane area, and T is the measurement time. Table 2 is a comparison table of separation performance of nanofiltration membrane
TABLE 2
| Flux (LMH) | MgSO4(％) | |
| Example 4 | 38 | 96 |
| Example 5 | 30 | 97 |
| Example 6 | 35 | 95 |
| Comparative example 4 | 45 | 97 |
| Comparative example 5 | 17 | 95 |
| Comparative example 6 | 11 | 93 |
And (4) conclusion: the base film spun by the improved spinneret orifice has higher breaking strength and higher flux.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (2)
1. The improved spinneret plate for the parallel channel nanofiltration membrane is characterized by comprising a plurality of spinneret units which are connected with each other, wherein each spinneret unit comprises a circular spinneret hole and arc spinneret holes which are symmetrically arranged at the upper side and the lower side of the circular spinneret hole, and adjacent arc spinneret holes are connected through straight transition holes;
the circular-arc spinneret orifices and the circular spinneret orifices are concentric circles; the arc radiuses of the arc-shaped spinneret holes of the spinneret units at the two ends are larger than the arc radiuses of the arc-shaped spinneret holes of the spinneret units in the middle;
the axial distance of the straight transition holes of the adjacent spinning units is 0.1-0.2 mm; the radius of the circular spinneret orifice is 0.25-0.3mm, and the radius of the middle circular arc spinneret orifice is 0.45-0.5 mm; the radius of the two circular arc spinneret orifices is 0.55-0.6 mm.
2. The preparation method of the improved parallel channel nanofiltration membrane is characterized in that the improved parallel channel nanofiltration membrane of claim 1 is used for spinning a base membrane by using a spinneret plate, the feed liquid conveying pressure is 0.03-0.1MPa, the drafting speed is 16.5-24m/min, the solid content of the feed liquid is 15-35%, and the coagulation bath temperature is 55-85 ℃; obtaining the multi-channel basement membrane.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1177022A (en) * | 1996-12-26 | 1998-03-25 | 上海德全化纤设备厂 | Method for mfg. multiple hellow shaped spinning plate |
| CN201648583U (en) * | 2010-03-30 | 2010-11-24 | 常州纺兴精密机械有限公司 | Duplex hollow spinneret |
| CN106256933A (en) * | 2016-08-28 | 2016-12-28 | 义乌华鼎锦纶股份有限公司 | A kind of moisture absorbing and sweat releasing delustering fibre and preparation method thereof |
| CN107653501A (en) * | 2017-10-12 | 2018-02-02 | 天津膜天膜科技股份有限公司 | The spinneret of more endoporus runners and its application |
| CN108014645A (en) * | 2017-12-15 | 2018-05-11 | 天津膜天膜科技股份有限公司 | A kind of parallel channels film and its membrane module |
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- 2018-12-26 CN CN201811601843.1A patent/CN109647203B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1177022A (en) * | 1996-12-26 | 1998-03-25 | 上海德全化纤设备厂 | Method for mfg. multiple hellow shaped spinning plate |
| CN201648583U (en) * | 2010-03-30 | 2010-11-24 | 常州纺兴精密机械有限公司 | Duplex hollow spinneret |
| CN106256933A (en) * | 2016-08-28 | 2016-12-28 | 义乌华鼎锦纶股份有限公司 | A kind of moisture absorbing and sweat releasing delustering fibre and preparation method thereof |
| CN107653501A (en) * | 2017-10-12 | 2018-02-02 | 天津膜天膜科技股份有限公司 | The spinneret of more endoporus runners and its application |
| CN108014645A (en) * | 2017-12-15 | 2018-05-11 | 天津膜天膜科技股份有限公司 | A kind of parallel channels film and its membrane module |
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