CN104548940A - Nanofiltration membrane pretreatment method for eliminating membrane separation oil-water emulsification - Google Patents
Nanofiltration membrane pretreatment method for eliminating membrane separation oil-water emulsification Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 107
- 238000001728 nano-filtration Methods 0.000 title claims abstract description 81
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000926 separation method Methods 0.000 title claims abstract description 16
- 238000002203 pretreatment Methods 0.000 title claims abstract description 15
- 238000004945 emulsification Methods 0.000 title claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 40
- 239000003960 organic solvent Substances 0.000 claims abstract description 37
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 31
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- 150000001875 compounds Chemical class 0.000 claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 230000007423 decrease Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 229950005499 carbon tetrachloride Drugs 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 14
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 18
- 238000005516 engineering process Methods 0.000 description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 12
- 239000003921 oil Substances 0.000 description 12
- 235000019198 oils Nutrition 0.000 description 12
- 239000000203 mixture Substances 0.000 description 7
- 230000004907 flux Effects 0.000 description 6
- 235000019774 Rice Bran oil Nutrition 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 239000008165 rice bran oil Substances 0.000 description 5
- 235000012424 soybean oil Nutrition 0.000 description 5
- 239000003549 soybean oil Substances 0.000 description 5
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
本发明公开了一种消除膜分离油水乳化的纳滤膜预处理方法，所述方法包括：去离子水清洗、复配试剂清洗、与应用所述纳滤膜生产时所使用的有机溶剂相同的有机溶剂清洗3个步骤；本发明所述方法可以有效解决油类物质和纳滤膜中残留的水发生油水乳化的问题。The invention discloses a nanofiltration membrane pretreatment method for eliminating oil-water emulsification in membrane separation, the method comprising three steps: deionized water cleaning, compound reagent cleaning, and organic solvent cleaning which is the same as the organic solvent used in the production of the nanofiltration membrane. The method of the invention can effectively solve the problem of oil-water emulsification between oil substances and residual water in the nanofiltration membrane.
Description
(一)技术领域(1) Technical field
本发明涉及一种纳滤膜预处理方法，特别涉及一种将对油类物质进行有机溶剂纳滤膜分离处理的纳滤膜预处理方法。该预处理方式可以有效解决油和纳滤膜中残留的水发生油水乳化的问题。The invention relates to a nanofiltration membrane pretreatment method, in particular to a nanofiltration membrane pretreatment method for separating and treating oily substances with an organic solvent nanofiltration membrane. This pretreatment method can effectively solve the problem of oil-water emulsification of oil and residual water in the nanofiltration membrane.
(二)背景技术(2) Background technology
膜分离是在20世纪初出现，20世纪60年代后迅速崛起的一门新型分离技术。膜分离技术是一种使用半透膜分离的方法，是在常温下以膜两侧的压力差或电位差为动力，对溶质进行分离和纯化。膜分离技术由于兼有分离、浓缩、纯化和精制的功能，又有高效、节能、环保、可以实现分子级过滤的优点，更有过滤过程简单、易于控制等特征，因此，目前已广泛应用于食品、环保、石油、水处理、化工等领域，产生了巨大的经济效益和社会效益，已成为当今分离科学中最重要的手段之一。Membrane separation is a new separation technology that appeared in the early 20th century and rose rapidly after the 1960s. Membrane separation technology is a method of separation using a semi-permeable membrane, which is driven by the pressure difference or potential difference on both sides of the membrane at room temperature to separate and purify the solute. Membrane separation technology has the functions of separation, concentration, purification and refining, and has the advantages of high efficiency, energy saving, environmental protection, molecular-level filtration, simple filtration process, and easy control. Therefore, it has been widely used at present. Food, environmental protection, petroleum, water treatment, chemical industry and other fields have produced huge economic and social benefits, and have become one of the most important means in today's separation science.
近年来，膜分离技术，特别是有机溶剂纳滤技术，作为一种可以实现分子分离的技术而得到极大关注。它的特点是可以通过纳滤膜截留分子量的选择从而分离分子量相近的分子。In recent years, membrane separation technology, especially organic solvent nanofiltration technology, has attracted great attention as a technology that can realize molecular separation. Its characteristic is that it can separate molecules with similar molecular weight through the selection of molecular weight cut-off of nanofiltration membrane.
目前，有机溶剂纳滤技术的使用范围也越来越广，但对油类物质进行有机溶剂纳滤处理时会遇到油水乳化的问题，油与纳滤膜装置中残留的水发生油水乳化，产生乳化层，会造成过膜压力不稳以及膜损坏的问题。At present, the scope of application of organic solvent nanofiltration technology is becoming wider and wider, but when oily substances are treated with organic solvent nanofiltration, the problem of oil-water emulsification will occur. Oil-water emulsification occurs between oil and the water remaining in the nanofiltration membrane device The formation of an emulsified layer will cause problems with unstable pressure across the membrane and damage to the membrane.
目前，解决此问题的方法则是用与生产所需的有机溶剂相同的有机溶剂反复冲洗，但此举不仅导致成本增高，也费时费力。Currently, the solution to this problem is to repeatedly rinse with the same organic solvent used for production, but this is not only costly, but also time-consuming.
(三)发明内容(3) Contents of the invention
本发明涉及一种纳滤膜预处理方法，特别涉及一种将对油类物质进行有机溶剂纳滤膜分离处理的纳滤膜预处理方法。The invention relates to a nanofiltration membrane pretreatment method, in particular to a nanofiltration membrane pretreatment method for separating and treating oily substances with an organic solvent nanofiltration membrane.
本发明采用如下技术方案：The present invention adopts following technical scheme:
一种消除膜分离油水乳化的纳滤膜预处理方法，所述的方法按如下步骤进行：A nanofiltration membrane pretreatment method for eliminating membrane separation oil-water emulsification, said method is carried out as follows:
(1)去离子水清洗：先用去离子水清洗1～2次，所述清洗方法为：首先排空纳滤膜装置中的储存液，加入去离子水，在0.1～1kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10～30分钟后，再以0.1～1kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持1～10分钟，以此为一个周期，循环运转10～30分钟；所述低压状态为1～3kg/cm2，高压状态为4～8kg/cm2；(1) Cleaning with deionized water: first wash with deionized water for 1 to 2 times. The cleaning method is: first empty the storage liquid in the nanofiltration membrane device, add deionized water, At a pulse frequency of min, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, and after maintaining the high pressure state for 10 to 30 minutes, it drops from the high pressure state to the low pressure state at a pulse frequency of 0.1 to 1kg/cm 2 /min , maintaining a low pressure state for 1-10 minutes, taking this as a cycle, and operating in a cycle for 10-30 minutes; the low-pressure state is 1-3kg/cm 2 , and the high-pressure state is 4-8kg/cm 2 ;
(2)复配试剂清洗：然后用复配试剂清洗，重复1～2次，所述清洗方法为：先排空纳滤膜装置中的去离子水，然后加入复配试剂，在0.1～1kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10～30分钟后，再以0.1～1kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持1～10分钟，以此为一个周期，循环运转20～40分钟；所述低压状态为1～5kg/cm2，高压状态为5～10kg/cm2；所述复配试剂选自乙醇、氯仿、甲醇、四氯甲烷、去离子水中的两种或两种以上任意比例的混合溶剂；(2) Compound reagent cleaning: then use the compound reagent to clean, repeat 1-2 times, the cleaning method is: first empty the deionized water in the nanofiltration membrane device, then add the compound reagent, at 0.1-1kg At a pulse frequency of 0.1kg/cm 2 /min, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure. Decrease to a low pressure state, maintain the low pressure state for 1 to 10 minutes, take this as a cycle, and cycle for 20 to 40 minutes; the low pressure state is 1 to 5kg/cm 2 , and the high pressure state is 5 to 10kg/cm 2 ; Said composite reagent is selected from ethanol, chloroform, methanol, tetrachloromethane, two or more mixed solvents in any proportion in deionized water;
(3)与应用所述纳滤膜生产时所使用的有机溶剂相同的有机溶剂清洗：最后用与生产时所使用的有机溶剂相同的有机溶剂清洗，所述清洗方法为：先排空纳滤膜装置中的复配试剂，加入与生产时所使用的有机溶剂相同的有机溶剂，在0.1～2kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10～30分钟后，再以0.1～2kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持1～10分钟，以此为一个周期，循环运转10～30分钟；所述低压状态为1～10kg/cm2，高压状态为15～25kg/cm2。(3) cleaning with the same organic solvent as the organic solvent used in the production of the nanofiltration membrane: finally cleaning with the same organic solvent as the organic solvent used in the production, the cleaning method is: first empty the nanofiltration The compound reagent in the membrane device is added with the same organic solvent as the organic solvent used in production, and at a pulse frequency of 0.1-2kg/cm 2 /min, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, After maintaining the high pressure state for 10 to 30 minutes, then drop from the high pressure state to the low pressure state at a pulse frequency of 0.1 to 2kg/cm 2 /min, and maintain the low pressure state for 1 to 10 minutes, taking this as a cycle, and cycle for 10 to 10 minutes. 30 minutes; the low-pressure state is 1-10 kg/cm 2 , and the high-pressure state is 15-25 kg/cm 2 .
本发明所述的纳滤膜预处理方法，步骤(2)中，优选所述的复配试剂为乙醇、甲醇和去离子水体积比85：5：10的复配溶液。In the nanofiltration membrane pretreatment method of the present invention, in step (2), the compounded reagent is preferably a compounded solution with a volume ratio of ethanol, methanol and deionized water of 85:5:10.
步骤(3)中，应用所述纳滤膜生产时所使用的有机溶剂是指：在食品、环保、石油、水处理、化工等领域的具体生产过程中所采用的有机溶剂，根据具体生产过程中不同油类物质的需要所选取。本发明在步骤(1)、(2)的清洗基础上，步骤(3)采用与生产时所使用的有机溶剂相同的有机溶剂对纳滤膜进行最后的清洗，与现有纳滤膜的预处理方法——用与生产时所使用的有机溶剂相同的有机溶剂反复冲洗相比，降低了成本，简单高效。In step (3), the organic solvent used when applying the nanofiltration membrane to produce refers to: the organic solvent used in the specific production process in the fields of food, environmental protection, petroleum, water treatment, chemical industry, etc., according to the specific production process Selected according to the needs of different oil substances. The present invention is based on the cleaning of steps (1) and (2), and step (3) adopts the same organic solvent as the organic solvent used in production to carry out the final cleaning of the nanofiltration membrane, which is different from the pre-treatment of the existing nanofiltration membrane. Treatment method - Compared with repeated washing with the same organic solvent used in production, the cost is reduced, simple and efficient.
本发明所述纳滤膜预处理方法可以有效解决油类物质和纳滤膜中残留的水发生油水乳化的问题。The nanofiltration membrane pretreatment method of the invention can effectively solve the problem of oil-water emulsification of oily substances and residual water in the nanofiltration membrane.
(四)附图说明(4) Description of drawings
图1：实施例1无/经过预处理的利用有机溶剂-纳滤技术富集米糠油中的谷维素的生产过程中的过膜压力变化；Fig. 1: the change of transmembrane pressure in the production process of the oryzanol enriched in rice bran oil utilizing organic solvent-nanofiltration technology without/through pretreatment in embodiment 1;
图2：实施例1无/经过预处理的利用有机溶剂-纳滤技术富集米糠油中的谷维素的生产过程中的膜通量变化；Fig. 2: the change of membrane flux in the production process of oryzanol enriched in rice bran oil utilizing organic solvent-nanofiltration technology without/after pretreatment in embodiment 1;
图3：实施例2无/经过预处理的利用有机溶剂-纳滤技术脱除大豆油中的有害物质的生产过程中的过膜压力变化；Fig. 3: the change of membrane pressure in the production process of embodiment 2 without/through pretreatment utilizing organic solvent-nanofiltration technology to remove harmful substances in soybean oil;
图4：实施例2无/经过预处理的利用有机溶剂-纳滤技术脱除大豆油中的有害物质的生产过程中的膜通量变化；Fig. 4: the change of membrane flux in the production process of utilizing organic solvent-nanofiltration technology to remove harmful substances in soybean oil without/through pretreatment in embodiment 2;
图5：实施例3无/经过预处理的利用有机溶剂-纳滤技术脱除金枪鱼油中的有害物质的生产过程中的过膜压力变化；Fig. 5: the change of membrane pressure in the production process of embodiment 3 without/after pretreatment utilizing organic solvent-nanofiltration technology to remove harmful substances in tuna oil;
图6：实施例3无/经过预处理的利用有机溶剂-纳滤技术脱除金枪鱼油中的有害物质的生产过程中的膜通量变化。Figure 6: Changes in membrane flux during the production process of removing harmful substances in tuna oil using organic solvent-nanofiltration technology in Example 3 without/with pretreatment.
(五)具体实施方式(5) Specific implementation methods
下面结合实例对本发明做进一步的阐述，但是本发明不仅限于此。The present invention will be further elaborated below in conjunction with examples, but the present invention is not limited thereto.
实施例1：Example 1:
利用有机溶剂-纳滤技术富集米糠油中的谷维素，所用有机试剂为丙酮，米糠油和丙酮的混合物用纳滤膜分离处理之前，对纳滤膜进行预处理，其预处理方法为：Use organic solvent-nanofiltration technology to enrich oryzanol in rice bran oil. The organic reagent used is acetone. Before the mixture of rice bran oil and acetone is separated and treated by nanofiltration membrane, the nanofiltration membrane is pretreated. The pretreatment method is as follows:
(1)去离子水清洗：先用去离子水清洗2次，所述清洗方法为：首先排空纳滤膜装置中的储存液，加入去离子水，在0.1kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10分钟后，再以0.1kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持2分钟，以此为一个周期，循环运转15分钟；所述低压状态为1kg/cm2，高压状态为5kg/cm2；(1) Cleaning with deionized water: first wash twice with deionized water, the cleaning method is: first empty the storage liquid in the nanofiltration membrane device, add deionized water, and pulse at 0.1kg/cm 2 /min Under the frequency, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, and after maintaining the high pressure state for 10 minutes, then drops from the high pressure state to the low pressure state at a pulse frequency of 0.1kg/cm 2 /min, and maintains the low pressure state for 2 Minutes, take this as a cycle, and cycle for 15 minutes; the low-pressure state is 1kg/cm 2 , and the high-pressure state is 5kg/cm 2 ;
(2)复配试剂清洗：然后用复配试剂清洗，所述复配试剂选自乙醇和去离子水的混合溶剂，混合体积比例为85：15，重复1次，所述清洗方法为：先排空纳滤膜装置中的去离子水，然后加入复配试剂，在0.3kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10分钟后，再以0.3kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持3分钟，以此为一个周期，循环运转20分钟；所述低压状态为2kg/cm2，高压状态为10kg/cm2；(2) Compound reagent cleaning: then clean with compound reagent, described compound reagent is selected from the mixed solvent of ethanol and deionized water, the mixing volume ratio is 85:15, repeat 1 time, described cleaning method is: first Empty the deionized water in the nanofiltration membrane device, and then add the compound reagent. Under the pulse frequency of 0.3kg/cm 2 /min, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, and maintains 10 Minutes later, drop from the high pressure state to the low pressure state at a pulse frequency of 0.3kg/cm 2 /min, and maintain the low pressure state for 3 minutes, taking this as a cycle, and cycle for 20 minutes; the low pressure state is 2kg/cm 2 , the high pressure state is 10kg/cm 2 ;
(3)与应用所述纳滤膜生产时所使用的有机溶剂相同的有机溶剂丙酮清洗：最后用与生产时所使用的有机溶剂相同的有机溶剂丙酮清洗，所述清洗方法为：先排空纳滤膜装置中的复配试剂，加入丙酮，在0.1kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10分钟后，再以0.1kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持2分钟，以此为一个周期，循环运转10分钟；所述低压状态为3kg/cm2，高压状态为15kg/cm2。(3) cleaning with the same organic solvent acetone as the organic solvent used in the production of the nanofiltration membrane: finally cleaning with the same organic solvent acetone as the organic solvent used in the production, the cleaning method is: first emptying Add acetone to the compound reagent in the nanofiltration membrane device, and at a pulse frequency of 0.1kg/cm 2 /min, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, and after maintaining the high pressure state for 10 minutes, then The pulse frequency of 0.1kg/cm 2 /min is reduced from the high pressure state to the low pressure state, and the low pressure state is maintained for 2 minutes, which is taken as a cycle, and the cycle is run for 10 minutes; the low pressure state is 3kg/cm 2 , and the high pressure state is 15kg /cm 2 .
表1米糠油和丙酮的混合物分别用无/经过预处理的纳滤膜分离处理之后的外观描述Table 1 The appearance description of the mixture of rice bran oil and acetone after separation with no/pretreated nanofiltration membrane
并且，由图1、图2可知，经预处理后，过膜压力稳定且膜通量下降速度明显下降，表明有效避免了油与纳滤膜装置中残留的水发生油水乳化。Moreover, it can be seen from Figures 1 and 2 that after pretreatment, the pressure across the membrane is stable and the rate of decline in the membrane flux is significantly reduced, indicating that oil-water emulsification between oil and residual water in the nanofiltration membrane device is effectively avoided.
实施例2：Example 2:
利用有机溶剂-纳滤技术脱除大豆油中的有害物质，所用有机试剂为正己烷，大豆油和正己烷的混合物用纳滤膜分离处理之前，对纳滤膜进行预处理，其预处理方法为：Use organic solvent-nanofiltration technology to remove harmful substances in soybean oil. The organic reagent used is n-hexane. Before the mixture of soybean oil and n-hexane is separated and treated by nanofiltration membrane, the nanofiltration membrane is pretreated. The pretreatment method for:
(1)去离子水清洗：先用去离子水清洗2次，所述清洗方法为：首先排空纳滤膜装置中的储存液，加入去离子水，在0.1kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10分钟后，再以0.1kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持2分钟，以此为一个周期，循环运转15分钟；所述低压状态为1kg/cm2，高压状态为5kg/cm2；(1) Cleaning with deionized water: first wash twice with deionized water, the cleaning method is: first empty the storage liquid in the nanofiltration membrane device, add deionized water, and pulse at 0.1kg/cm 2 /min Under the frequency, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, and after maintaining the high pressure state for 10 minutes, then drops from the high pressure state to the low pressure state at a pulse frequency of 0.1kg/cm 2 /min, and maintains the low pressure state for 2 Minutes, take this as a cycle, and cycle for 15 minutes; the low-pressure state is 1kg/cm 2 , and the high-pressure state is 5kg/cm 2 ;
(2)复配试剂清洗：然后用复配试剂清洗，所述复配试剂选自乙醇和去离子水的混合溶剂，混合体积比例为90：10，重复1次，所述清洗方法为：先排空纳滤膜装置中的去离子水，然后加入复配试剂，在0.3kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10分钟后，再以0.3kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持3分钟，以此为一个周期，循环运转20分钟；所述低压状态为2kg/cm2，高压状态为10kg/cm2；(2) Compound reagent cleaning: then clean with compound reagent, described compound reagent is selected from the mixed solvent of ethanol and deionized water, the mixing volume ratio is 90:10, repeat 1 time, described cleaning method is: first Empty the deionized water in the nanofiltration membrane device, and then add the compound reagent. Under the pulse frequency of 0.3kg/cm 2 /min, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, and maintains 10 Minutes later, drop from the high pressure state to the low pressure state at a pulse frequency of 0.3kg/cm 2 /min, and maintain the low pressure state for 3 minutes, taking this as a cycle, and cycle for 20 minutes; the low pressure state is 2kg/cm 2 , the high pressure state is 10kg/cm 2 ;
(3)与应用所述纳滤膜生产时所使用的有机溶剂相同的有机溶剂正己烷清洗：最后用与生产时所使用的有机溶剂相同的有机溶剂正己烷清洗，所述清洗方法为：先排空纳滤膜装置中的复配试剂，加入正己烷，在0.1kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10分钟后，再以0.1kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持2分钟，以此为一个周期，循环运转10分钟；所述低压状态为3kg/cm2，高压状态为15kg/cm2。(3) cleaning with the same organic solvent n-hexane as the organic solvent used in the production of the nanofiltration membrane: finally cleaning with the same organic solvent n-hexane as the organic solvent used in production, the cleaning method is: first Empty the compound reagent in the nanofiltration membrane device, add n-hexane, and at a pulse frequency of 0.1kg/cm 2 /min, the membrane pressure of the nanofiltration membrane device will rise from low pressure to high pressure, and after maintaining the high pressure state for 10 minutes , and then drop from the high pressure state to the low pressure state at a pulse frequency of 0.1kg/cm 2 /min, maintain the low pressure state for 2 minutes, take this as a cycle, and cycle for 10 minutes; the low pressure state is 3kg/cm 2 , the high pressure state The state is 15kg/cm 2 .
表2大豆油和正己烷的混合物分别用无/经过预处理的纳滤膜分离处理之后的外观描述Table 2 The appearance description of the mixture of soybean oil and n-hexane after separation and treatment by nanofiltration membrane without/with pretreatment
并且，由图3、图4可知，经预处理后，过膜压力稳定且膜通量下降速度明显下降，表明有效避免了油与纳滤膜装置中残留的水发生油水乳化。Moreover, it can be seen from Figure 3 and Figure 4 that after pretreatment, the pressure across the membrane is stable and the rate of decline in membrane flux is significantly reduced, indicating that oil-water emulsification between oil and residual water in the nanofiltration membrane device is effectively avoided.
实施例3：Example 3:
利用有机溶剂-纳滤技术脱除金枪鱼油中的有害物质，所用有机试剂为正庚烷，金枪鱼油和正庚烷的混合物用纳滤膜分离处理之前，对纳滤膜进行预处理，其预处理方法为：Use organic solvent-nanofiltration technology to remove harmful substances in tuna oil. The organic reagent used is n-heptane. Before the mixture of tuna oil and n-heptane is separated and treated by nanofiltration membrane, the nanofiltration membrane is pretreated. The method is:
(1)去离子水清洗：先用去离子水清洗2次，所述清洗方法为：首先排空纳滤膜装置中的储存液，加入去离子水，在0.2kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持8分钟后，再以0.2kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持2分钟，以此为一个周期，循环运转12分钟；所述低压状态为1kg/cm2，高压状态为5kg/cm2；(1) Cleaning with deionized water: first wash with deionized water for 2 times, the cleaning method is: first empty the storage liquid in the nanofiltration membrane device, add deionized water, pulse at 0.2kg/cm 2 /min Under the frequency, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure. After maintaining the high pressure state for 8 minutes, it drops from the high pressure state to the low pressure state at a pulse frequency of 0.2kg/cm 2 /min, and maintains the low pressure state for 2 minutes. Minutes, take this as a cycle, and cycle for 12 minutes; the low-pressure state is 1kg/cm 2 , and the high-pressure state is 5kg/cm 2 ;
(2)复配试剂清洗：然后用复配试剂清洗，所述复配试剂选自乙醇和去离子水的混合溶剂，混合体积比例为90：10，重复1次，所述清洗方法为：先排空纳滤膜装置中的去离子水，然后加入复配试剂，在0.3kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10分钟后，再以0.3kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持3分钟，以此为一个周期，循环运转20分钟；所述低压状态为2kg/cm2，高压状态为10kg/cm2；(2) Compound reagent cleaning: then clean with compound reagent, described compound reagent is selected from the mixed solvent of ethanol and deionized water, the mixing volume ratio is 90:10, repeat 1 time, described cleaning method is: first Empty the deionized water in the nanofiltration membrane device, and then add the compound reagent. Under the pulse frequency of 0.3kg/cm 2 /min, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, and maintains 10 Minutes later, drop from the high pressure state to the low pressure state at a pulse frequency of 0.3kg/cm 2 /min, and maintain the low pressure state for 3 minutes, taking this as a cycle, and cycle for 20 minutes; the low pressure state is 2kg/cm 2 , the high pressure state is 10kg/cm 2 ;
(3)与应用所述纳滤膜生产时所使用的有机溶剂相同的有机溶剂正庚烷清洗：最后用与生产时所使用的有机溶剂相同的有机溶剂正庚烷清洗，所述清洗方法为：先排空纳滤膜装置中的复配试剂，加入正庚烷，在0.1kg/cm2/min的脉冲频率下，纳滤膜装置的过膜压力从低压升至高压，在高压状态维持10分钟后，再以0.1kg/cm2/min的脉冲频率从高压状态降至低压状态，在低压状态维持2分钟，以此为一个周期，循环运转10分钟；所述低压状态为3kg/cm2，高压状态为15kg/cm2。(3) cleaning with the same organic solvent n-heptane of the organic solvent used in the production of the nanofiltration membrane: finally cleaning with the same organic solvent n-heptane of the organic solvent used in production, the cleaning method is : First empty the compound reagent in the nanofiltration membrane device, add n-heptane, and at a pulse frequency of 0.1kg/cm 2 /min, the membrane pressure of the nanofiltration membrane device rises from low pressure to high pressure, and maintains at high pressure After 10 minutes, drop from the high pressure state to the low pressure state with a pulse frequency of 0.1kg/cm 2 /min, and maintain the low pressure state for 2 minutes, taking this as a cycle, and cycle for 10 minutes; the low pressure state is 3kg/cm 2 , the high pressure state is 15kg/cm 2 .
表3金枪鱼油和正庚烷的混合物分别用无/经过预处理的纳滤膜分离处理之后的外观描述Table 3 The appearance description of the mixture of tuna oil and n-heptane after separation with no/pretreated nanofiltration membrane
并且，由图5、图6可知，经预处理后，过膜压力稳定且膜通量下降速度明显下降，表明有效避免了油与纳滤膜装置中残留的水发生油水乳化。Moreover, it can be seen from Figures 5 and 6 that after pretreatment, the pressure across the membrane is stable and the rate of decline in the membrane flux is significantly reduced, indicating that oil-water emulsification between oil and residual water in the nanofiltration membrane device is effectively avoided.
最后，还需要注意的是，以上列举的仅是本发明的若干个具体实施例。显然，本发明不限于以上实施例，还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形，均应认为是本发明的保护范围。Finally, it should be noted that the above examples are only some specific embodiments of the present invention. Obviously, the present invention is not limited to the above embodiments, and many variations are possible. All deformations that can be directly derived or associated by those skilled in the art from the content disclosed in the present invention should be considered as the protection scope of the present invention.
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| CN115491224A (en) * | 2021-06-17 | 2022-12-20 | 中国石油化工股份有限公司 | Method for recovering dewaxing solvent in light lubricating oil base oil filtrate |
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| CN115491226A (en) * | 2021-06-17 | 2022-12-20 | 中国石油化工股份有限公司 | Method for recovering dewaxing solvent in heavy lubricant base oil filtrate |
| CN115491224A (en) * | 2021-06-17 | 2022-12-20 | 中国石油化工股份有限公司 | Method for recovering dewaxing solvent in light lubricating oil base oil filtrate |
| CN115491226B (en) * | 2021-06-17 | 2024-03-26 | 中国石油化工股份有限公司 | Method for recovering dewaxing solvent in heavy lubricating oil base oil filtrate |
| CN115491224B (en) * | 2021-06-17 | 2024-03-26 | 中国石油化工股份有限公司 | Method for recovering dewaxing solvent in light lubricating oil base oil filtrate |
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