CN107176987A - The method and device of Silk Reeling Waste Liquor recovery purifying sericin - Google Patents
The method and device of Silk Reeling Waste Liquor recovery purifying sericin Download PDFInfo
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- 108010013296 Sericins Proteins 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000002699 waste material Substances 0.000 title claims abstract description 22
- 238000011084 recovery Methods 0.000 title claims description 21
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 239000002351 wastewater Substances 0.000 claims abstract description 23
- 238000000967 suction filtration Methods 0.000 claims abstract description 19
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 150000002500 ions Chemical class 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 230000005684 electric field Effects 0.000 claims description 43
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 239000010405 anode material Substances 0.000 claims description 13
- 238000003860 storage Methods 0.000 claims description 11
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 10
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- 239000000084 colloidal system Substances 0.000 abstract description 2
- 230000005611 electricity Effects 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 108010010803 Gelatin Proteins 0.000 abstract 1
- 229920000159 gelatin Polymers 0.000 abstract 1
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- 235000019322 gelatine Nutrition 0.000 abstract 1
- 235000011852 gelatine desserts Nutrition 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 238000004108 freeze drying Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
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- 238000001556 precipitation Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 description 1
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- 108010022355 Fibroins Proteins 0.000 description 1
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
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- 240000000249 Morus alba Species 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229960004543 anhydrous citric acid Drugs 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
- 235000015523 tannic acid Nutrition 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/43504—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates
- C07K14/43563—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects
- C07K14/43586—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects from silkworms
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- Toxicology (AREA)
- Tropical Medicine & Parasitology (AREA)
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- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Medicinal Chemistry (AREA)
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Abstract
本发明属于废水处理技术领域，具体涉及一种缫丝废液回收纯化丝胶蛋白的方法。本发明缫丝废液回收纯化丝胶蛋白的方法为：缫丝废水经抽滤和超滤除去杂质和无机盐离子；利用Ti/SnO2为阳极材料，铂为阴极材料施加电场，利用电场作用使缫丝废水中丝胶蛋白沉淀，得丝胶蛋白；再将得到的丝胶蛋白经超声清洗后溶于水介质中，再加入无水乙醇，经离心、上清液后得纯化后的丝胶蛋白。本发明的方法在不添加化学试剂的情况下，施加低电量就可以破坏胶体的稳定性，分离得到丝胶蛋白；该方法提取效率可达到68％左右，纯度为90.2％，且操作简单，环境友好，具有工业化应用意义。
The invention belongs to the technical field of wastewater treatment, and in particular relates to a method for recovering and purifying sericin from silk reeling waste liquid. The method for recovering and purifying sericin from silk reeling waste liquid of the present invention is as follows: remove impurities and inorganic salt ions through suction filtration and ultrafiltration of silk reeling waste water ; Precipitate sericin protein in silk reeling wastewater to obtain sericin protein; then dissolve the obtained sericin protein in water medium after ultrasonic cleaning, then add absolute ethanol, centrifuge and supernatant to obtain purified silk gelatin. The method of the present invention can destroy the stability of the colloid and obtain sericin by applying low electricity without adding chemical reagents; the extraction efficiency of the method can reach about 68%, the purity is 90.2%, and the operation is simple and environmentally friendly. Friendly, with industrial application significance.
Description
技术领域technical field
本发明属于废水处理技术领域，具体涉及一种缫丝废液回收纯化丝胶蛋白的方法及装置。The invention belongs to the technical field of wastewater treatment, and in particular relates to a method and a device for recovering and purifying sericin from silk reeling waste liquid.
背景技术Background technique
桑蚕茧丝是一种天然的蛋白质纤维，它主要由70％～80％的丝素，20％～30％的丝胶及少量蜡质和无机物等组成。目前大部分缫丝废水中的丝胶蛋白几乎全部不回收，作为废液全部排除，由于排放污水中蛋白质含量过高，流入河道将会大量消耗水中溶解氧，使水体丧失自净能力，造成大量的环境污染和能源浪费。所以，如果在蚕丝的加工与处理过程中能高效地回收和利用丝胶蛋白以免除对环境的污染，将会产生巨大的经济效益和社会效益。因此，设计出一种能将缫丝废水中丝胶蛋白提取出来的方法是十分有必要的。Mulberry cocoon silk is a natural protein fiber, which is mainly composed of 70% to 80% silk fibroin, 20% to 30% sericin and a small amount of wax and inorganic substances. At present, the sericin protein in most of the silk reeling wastewater is almost not recovered, and it is completely discharged as waste liquid. Because the protein content in the discharged sewage is too high, it will consume a large amount of dissolved oxygen in the water when it flows into the river, causing the water body to lose its self-purification ability, resulting in a large amount of pollution. Environmental pollution and energy waste. Therefore, if sericin can be efficiently recovered and utilized in the process of silk processing and treatment to avoid environmental pollution, huge economic and social benefits will be produced. Therefore, it is very necessary to design a method that can extract sericin in silk reeling wastewater.
丝胶蛋白含大量侧链带亲水基团的氨基酸如丝氨酸、天冬氨酸等，易溶于水中。蚕丝中的杂质主要存于丝胶中。丝胶蛋白含有自由的羧基和氨基，可相互作用而形成双极离子，具有两性性质，在pH值较小的溶液里，丝胶蛋白质以正离子形式存在；在pH值较大的溶液里，丝胶蛋白质以负离子形式存在，丝胶蛋白的等电点是3.8～4.5，当溶液值接近或临界于等电点时，丝胶呈沉淀状而不呈凝胶状。Sericin contains a large number of amino acids with hydrophilic groups in the side chains, such as serine and aspartic acid, and is easily soluble in water. Impurities in silk are mainly stored in sericin. Sericin protein contains free carboxyl groups and amino groups, which can interact to form bipolar ions and have amphoteric properties. In solutions with low pH values, sericin proteins exist in the form of positive ions; in solutions with high pH values, sericin proteins exist in the form of positive ions. Sericin protein exists in the form of negative ions. The isoelectric point of sericin is 3.8-4.5. When the solution value is close to or critical to the isoelectric point, sericin is in the form of precipitation instead of gel.
丝胶蛋白质是一种宝贵的资源，目前缫丝厂制丝生产过程中溶解下来的丝胶蛋白质随生产废水的排放而流失，并成为缫丝生产废水中的主要污染物，会对水环境造成不良影响，缫丝废水中丝胶蛋白质的回收不仅有利于废水的达标排放或循环使用，还可将分离出来的丝胶蛋白质加以利用，开发出高附加值副产品。Sericin protein is a valuable resource. Currently, the sericin protein dissolved in the silk production process of the silk reeling factory is lost with the discharge of production wastewater, and becomes the main pollutant in the silk reeling production wastewater, which will cause harm to the water environment. Adverse effects, the recovery of sericin protein in silk reeling wastewater is not only conducive to the standard discharge or recycling of wastewater, but also the use of the separated sericin protein to develop high value-added by-products.
从废水中提取丝胶的方法有化学提取法和物理提取法两大类。其中化学提取法有化学混凝法、酸析法和有机溶剂沉淀法。物理提取法有离心法、膜分离法、冰冻法和离子交换法几种。There are two methods of extracting sericin from wastewater: chemical extraction and physical extraction. The chemical extraction methods include chemical coagulation, acid analysis and organic solvent precipitation. Physical extraction methods include centrifugation, membrane separation, freezing and ion exchange.
申请号为200710093091.8的专利公开了一种含丝胶蛋白废水的处理方法，它利用丝胶自身与金属发生配位反应而合成丝胶蛋白金属络合物，利用此络合物作为絮凝剂凝聚沉淀丝厂废水中的丝胶，从而对废水进行有效的处理，最后通过稀酸洗涤的方法低成本回收丝胶蛋白。该方法需要加入金属化学试剂，成本高，后续处理复杂。The patent with the application number 200710093091.8 discloses a treatment method for wastewater containing sericin, which uses sericin itself to undergo a coordination reaction with metals to synthesize a sericin metal complex, and uses this complex as a flocculant for coagulation and precipitation Sericin in silk factory wastewater can be effectively treated, and finally sericin protein can be recovered at low cost by dilute acid washing. This method needs to add metal chemical reagents, the cost is high, and the follow-up treatment is complicated.
申请号为201310073594.4，名称为“一种缫丝废水中丝胶蛋白的沉淀方法”的中国专利申请公开了在缫丝废水中依次加入适量的无水柠檬酸和磷酸氢二钠，并通过搅拌器搅拌均匀，再加入适量的鞣酸，再通过加热和静置，从而将缫丝废水中丝胶蛋白的沉淀出来。该方法虽然能够得到丝胶蛋白，但是添加了许多化学试剂，过程也比较复杂。The application number is 201310073594.4, and the Chinese patent application titled "A Method for Precipitating Sericin in Silk Reeling Wastewater" discloses that an appropriate amount of anhydrous citric acid and disodium hydrogen phosphate are sequentially added to the silk reeling wastewater, and passed through a stirrer. Stir evenly, then add an appropriate amount of tannic acid, and then heat and stand still to precipitate the sericin protein in the silk reeling wastewater. Although this method can obtain sericin, many chemical reagents are added, and the process is relatively complicated.
发明内容Contents of the invention
有鉴于此，本发明的目的在于提供一种从缫丝废液回收纯化丝胶蛋白的方法，本方法操作简单，不添加化学试剂，得到的丝胶蛋白提取效率和纯度高。In view of this, the object of the present invention is to provide a method for recovering and purifying sericin from silk reeling waste liquid. The method is simple to operate, does not add chemical reagents, and the obtained sericin has high extraction efficiency and purity.
为实现上述目的，本发明的技术方案为：To achieve the above object, the technical solution of the present invention is:
缫丝废液回收纯化丝胶蛋白的方法，包括以下步骤：The method for recovering and purifying sericin from silk reeling waste liquid comprises the following steps:
1)缫丝废水经抽滤和超滤除去杂质和无机盐离子，得处理液；1) The silk reeling wastewater is removed by suction filtration and ultrafiltration to remove impurities and inorganic salt ions to obtain a treatment solution;
2)利用Ti/SnO2为阳极材料，铂为阴极材料，在步骤1)所述处理液中施加电场，利用电场作用使丝胶蛋白沉淀，得丝胶蛋白；2) using Ti/ SnO2 as the anode material and platinum as the cathode material, applying an electric field in the treatment solution described in step 1), and utilizing the action of the electric field to precipitate sericin to obtain sericin;
3)将步骤2)的丝胶蛋白经超声清洗后溶于水介质中，再加入无水乙醇，经离心、去上清液后得纯化后的丝胶蛋白。3) The sericin protein in step 2) is ultrasonically cleaned and dissolved in water medium, then absolute ethanol is added, and the purified sericin protein is obtained after centrifugation and removal of the supernatant.
本发明分别比较了石墨、钛板电极、Ti/SnO2作为阳极材料可行性，石墨材料在高温环境中会发生溶解，钛板电极价格较高易氧化，Ti/SnO2性能稳定，工作电压小，使用寿命长，因此选择Ti/SnO2作为阳极材料。以高回收率、环保耐用为主要目标，对反应的不同因素进行对比分析，最终得到一套缫丝回收丝胶蛋白的工艺条件。The present invention compares the feasibility of graphite, titanium plate electrode, and Ti/ SnO2 as anode materials respectively. Graphite material will dissolve in high temperature environment, and the price of titanium plate electrode is high and easy to oxidize. Ti/ SnO2 has stable performance and low working voltage , long service life, so choose Ti/SnO 2 as anode material. With the main goal of high recovery rate, environmental protection and durability, the different factors of the reaction were compared and analyzed, and finally a set of process conditions for silk reeling to recover sericin was obtained.
进一步，步骤1)中超滤使用截留量为3～4KDa的超滤装置。Further, the ultrafiltration in step 1) uses an ultrafiltration device with a cutoff of 3-4KDa.
作为一种优选，步骤1)中超滤使用截留量为3.5KDa的超滤装置。As a preference, the ultrafiltration in step 1) uses an ultrafiltration device with a cutoff of 3.5KDa.
进一步，步骤2)电场的电流密度为1.5～3.5mA/cm2，电场作用的时间为90～120min。Further, in step 2), the current density of the electric field is 1.5-3.5 mA/cm 2 , and the duration of the electric field is 90-120 min.
作为一种优选，步骤2)电场的电流密度为2mA/cm2，电场作用的时间为100min。As a preference, the current density of the electric field in step 2) is 2 mA/cm 2 , and the duration of the electric field is 100 min.
进一步，步骤3)中丝胶蛋白与无水乙醇的体积比为1:3～5。Further, in step 3), the volume ratio of sericin to absolute ethanol is 1:3-5.
作为一种优选，步骤3)中丝胶蛋白与无水乙醇的体积比为1:4。As a preference, the volume ratio of sericin to absolute ethanol in step 3) is 1:4.
进一步，步骤3)所述的离心条件为2500～3500rpm，3～8min。Further, the centrifugation condition described in step 3) is 2500-3500 rpm, 3-8 min.
作为一种优选，步骤3)所述的离心条件为3000rpm，5min。As a preference, the centrifugation condition described in step 3) is 3000rpm, 5min.
进一步，步骤3)中纯化的步骤重复2～4次。作为一种优选，步骤3)中纯化的步骤重复3次。Further, the step of purification in step 3) was repeated 2 to 4 times. As a preference, the step of purification in step 3) is repeated 3 times.
进一步，所述方法还包括步骤：4)将步骤3)得到的丝胶蛋白经冷冻干燥法，冷冻干燥2～4天，得丝胶蛋白产品。Further, the method further includes the step: 4) freeze-drying the sericin obtained in step 3) for 2-4 days to obtain a sericin product.
本发明的目的之二在于提供一种利用缫丝废液回收纯化丝胶蛋白的装置回收纯化丝胶蛋白的方法，所述装置由依次连接的抽滤装置、浓缩装置、超滤装置、储存罐、电场回收装置、分离纯化装置和干燥装置组成；所述储存罐出料口设置有调节阀，所述电场回收装置设置有循环管道，所述循环管道设置有泵，电场回收装置的母液通过循环管道进入到储存罐，所述干燥装置设置有温度控制装置；利用所述装置回收纯化丝胶蛋白的方法，包括以下步骤：The second object of the present invention is to provide a method for recovering and purifying sericin using a device for recovering and purifying sericin from silk reeling waste liquid. , an electric field recovery device, a separation and purification device and a drying device; the outlet of the storage tank is provided with a regulating valve, the electric field recovery device is provided with a circulation pipeline, and the circulation pipeline is provided with a pump, and the mother liquor of the electric field recovery device passes through the circulation The pipeline enters the storage tank, and the drying device is provided with a temperature control device; the method for recovering and purifying sericin by using the device comprises the following steps:
1)缫丝废水进入抽滤装置经抽滤除去杂质，抽滤后的料液在浓缩装置中浓缩后进入截留量为3～4KDa的超滤装置除去无机盐离子，得处理液储存在储存罐中；1) The silk reeling waste water enters the suction filtration device to remove impurities by suction filtration, the feed liquid after suction filtration is concentrated in the concentration device, and then enters the ultrafiltration device with a cutoff of 3-4KDa to remove inorganic salt ions, and the treated liquid is stored in the storage tank middle;
2)通过控制调节阀所述处理液通过管道进入到电场回收装置中，利用电场作用使丝胶蛋白沉淀，得丝胶蛋白；2) The treatment liquid enters the electric field recovery device through the pipeline through the control regulating valve, and the sericin protein is precipitated by the action of the electric field to obtain the sericin protein;
3)步骤2)得到的丝胶蛋白在经过分离纯化装置的2～4次纯化后通过干燥装置干燥2～4天，得丝胶蛋白产品。3) The sericin protein obtained in step 2) is purified by a separation and purification device for 2 to 4 times and then dried by a drying device for 2 to 4 days to obtain a sericin product.
进一步，所述电场回收装置利用Ti/SnO2为阳极材料，铂为阴极材料；所述电场回收装置为间歇式生产。Further, the electric field recovery device uses Ti/SnO 2 as the anode material and platinum as the cathode material; the electric field recovery device is produced intermittently.
进一步，所述缫丝废液回收纯化丝胶蛋白的装置通过程序控制自动化生产。Further, the device for recovering and purifying sericin from silk reeling waste liquid is produced automatically through program control.
本发明的有益效果在于：The beneficial effects of the present invention are:
1)本发明提供的缫丝废液回收纯化丝胶蛋白的方法利用丝胶的胶体性质，在缫丝废水施加以电场，利用电场作用使丝胶蛋白沉淀，该方法在不添加化学试剂的情况下，施加低电量就可以破坏胶体的稳定性，分离得到丝胶蛋白；该方法简单，易操作，环境友好。1) The method for recovering and purifying sericin protein from silk reeling waste liquid provided by the present invention utilizes the colloidal properties of sericin, applies an electric field to the silk reeling wastewater, and utilizes the action of the electric field to precipitate sericin protein. This method does not add chemical reagents Under low power conditions, the stability of the colloid can be destroyed by applying low electricity, and the sericin protein can be separated; the method is simple, easy to operate, and environmentally friendly.
2)本发明的方法母液循环利用，回收纯化的丝胶蛋白为白色粉末，经测试提取效率可达到68％左右，纯度为90.2％。2) According to the method of the present invention, the mother liquor is recycled, and the recovered and purified sericin protein is white powder, and the extraction efficiency can reach about 68% and the purity is 90.2% through testing.
3)本发明提供的缫丝废液回收纯化丝胶蛋白的装置通过程序控制自动化生产，处理流程的运转效率较高，适用于大规模工业化生产，具有工业化应用意义。3) The device for recovering and purifying sericin protein from silk reeling waste liquid provided by the present invention is automatically produced through program control, and the operation efficiency of the treatment process is high. It is suitable for large-scale industrial production and has industrial application significance.
附图说明Description of drawings
图1为本发明缫丝废液回收纯化丝胶蛋白的装置的示意图。Fig. 1 is a schematic diagram of a device for recovering and purifying sericin from silk reeling waste liquid according to the present invention.
具体实施方式detailed description
以下将参照附图，对本发明的优选实施例进行详细描述。优选实施例中未注明具体条件的实验方法，通常按照常规条件，所举实施例是为了更好地对本发明的内容进行说明，但并不是本发明的内容仅限于所举实施例。所以熟悉本领域的技术人员根据上述发明内容对实施方案进行非本质的改进和调整，仍属于本发明的保护范围。Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. The experimental method that does not indicate specific conditions in the preferred embodiment is usually according to conventional conditions, and the examples given are to better illustrate the content of the present invention, but the content of the present invention is not limited to the examples given. Therefore, non-essential improvements and adjustments to the implementation by those skilled in the art based on the content of the invention above still fall within the protection scope of the present invention.
实施例1Example 1
缫丝废液回收纯化丝胶蛋白的方法，包括以下步骤：The method for recovering and purifying sericin from silk reeling waste liquid comprises the following steps:
1)缫丝废水经抽滤除去杂质，抽滤后的料液经截留量为3.5KDa的超滤装置除去杂质和无机盐离子，得处理液；1) the silk reeling wastewater is removed by suction filtration to remove impurities, and the feed liquid after suction filtration is removed by an ultrafiltration device with a cut-off of 3.5KDa to remove impurities and inorganic salt ions to obtain a treatment solution;
2)利用Ti/SnO2为阳极材料，铂为阴极材料，在所述处理液中施加电场，场的电流密度为2mA/cm2，电场作用的时间为100min，利用电场作用使丝胶蛋白沉淀，得丝胶蛋白；2) Using Ti/SnO 2 as the anode material, platinum as the cathode material, applying an electric field in the treatment solution, the current density of the field is 2mA/cm 2 , and the time of the electric field is 100min, and the sericin is precipitated by the electric field , get sericin;
3)将得到的丝胶蛋白经超声清洗后溶于水介质中，再加入丝胶蛋白体积4倍的无水乙醇，经3000rpm，5min离心、去上清液，重复3次，收集沉淀；3) Dissolve the obtained sericin in the water medium after ultrasonic cleaning, then add anhydrous ethanol 4 times the volume of sericin, centrifuge at 3000rpm for 5min, remove the supernatant, repeat 3 times, and collect the precipitate;
4)利用冷冻干燥法，冷冻干燥3天，得到丝胶蛋白产品。4) Utilize freeze-drying method, freeze-dry for 3 days, obtain sericin product.
实施例2Example 2
缫丝废液回收纯化丝胶蛋白的方法，包括以下步骤：The method for recovering and purifying sericin from silk reeling waste liquid comprises the following steps:
1)缫丝废水经抽滤除去杂质，抽滤后的料液经截留量为4KDa的超滤装置除去杂质和无机盐离子，得处理液；1) The silk reeling wastewater is removed by suction filtration to remove impurities, and the feed liquid after suction filtration is removed by an ultrafiltration device with a cut-off of 4KDa to remove impurities and inorganic salt ions to obtain a treatment solution;
2)利用Ti/SnO2为阳极材料，铂为阴极材料，在所述处理液中施加电场，场的电流密度为2mA/cm2，电场作用的时间为100min，利用电场作用使丝胶蛋白沉淀，得丝胶蛋白；2) Using Ti/SnO 2 as the anode material, platinum as the cathode material, applying an electric field in the treatment solution, the current density of the field is 2mA/cm 2 , and the time of the electric field is 100min, and the sericin is precipitated by the electric field , get sericin;
3)将得到的丝胶蛋白经超声清洗后溶于水介质中，再加入丝胶蛋白体积4.5倍的无水乙醇，经3000rpm，5min离心、去上清液，重复3次，收集沉淀；3) Dissolve the obtained sericin in the water medium after ultrasonic cleaning, then add absolute ethanol with 4.5 times the volume of sericin, centrifuge at 3000rpm for 5min, remove the supernatant, repeat 3 times, and collect the precipitate;
4)利用冷冻干燥法，冷冻干燥3天，得到丝胶蛋白产品。4) Utilize freeze-drying method, freeze-dry for 3 days, obtain sericin product.
实施例3Example 3
缫丝废液回收纯化丝胶蛋白的方法，包括以下步骤：The method for recovering and purifying sericin from silk reeling waste liquid comprises the following steps:
1)缫丝废水经抽滤除去杂质，抽滤后的料液经截留量为3.5KDa的超滤装置除去杂质和无机盐离子，得处理液；1) the silk reeling wastewater is removed by suction filtration to remove impurities, and the feed liquid after suction filtration is removed by an ultrafiltration device with a cut-off of 3.5KDa to remove impurities and inorganic salt ions to obtain a treatment solution;
2)利用Ti/SnO2为阳极材料，铂为阴极材料，在所述处理液中施加电场，场的电流密度为2mA/cm2，电场作用的时间为100min，利用电场作用使丝胶蛋白沉淀，得丝胶蛋白；2) Using Ti/SnO 2 as the anode material, platinum as the cathode material, applying an electric field in the treatment solution, the current density of the field is 2mA/cm 2 , and the time of the electric field is 100min, and the sericin is precipitated by the electric field , get sericin;
3)将得到的丝胶蛋白经超声清洗后溶于水介质中，再加入丝胶蛋白体积3.5倍的无水乙醇，经3200rpm，5min离心、去上清液，重复3次，收集沉淀；3) Dissolve the obtained sericin in the water medium after ultrasonic cleaning, then add absolute ethanol 3.5 times the volume of sericin, centrifuge at 3200rpm for 5min, remove the supernatant, repeat 3 times, and collect the precipitate;
4)利用冷冻干燥法，冷冻干燥3天，得到丝胶蛋白产品。4) Utilize freeze-drying method, freeze-dry for 3 days, obtain sericin product.
对比实施例4Comparative Example 4
施加电场的阳极材料为石墨或钛板电极，其他条件同实施例1。The anode material for applying the electric field is graphite or titanium plate electrode, and other conditions are the same as in Example 1.
分别比较了石墨、钛板电极、Ti/SnO2作为为阳极材料可行性，使用一段时间发现石墨材料在高温环境中会发生溶解，钛板电极价格较高易氧化，Ti/SnO2性能稳定，工作电压小，使用寿命长，因此选择Ti/SnO2作为阳极材料。The feasibility of graphite, titanium plate electrode, and Ti/SnO 2 as anode materials were compared respectively. After using for a period of time, it was found that graphite material would dissolve in high temperature environment, titanium plate electrode was more expensive and easy to oxidize, and Ti/SnO 2 had stable performance. The working voltage is small and the service life is long, so Ti/SnO 2 is selected as the anode material.
实施例5Example 5
参见图1所示，缫丝废液回收纯化丝胶蛋白的装置：所述装置由依次连接的抽滤装置1、浓缩装置2、超滤装置3、储存罐4、电场回收装置5、分离纯化装置6和干燥装置7组成；所述储存罐4出料口设置有调节阀8，所述电场回收装置设置有循环管道9，所述循环管道9设置有泵10，电场回收装置5的母液通过循环管道9进入到储存罐4，所述干燥装置7设置有温度控制装置；Referring to Figure 1, the device for recovering and purifying sericin from silk reeling waste liquid: the device consists of a suction filtration device 1, a concentration device 2, an ultrafiltration device 3, a storage tank 4, an electric field recovery device 5, a separation and purification device connected in sequence The device 6 and the drying device 7 are composed; the outlet of the storage tank 4 is provided with a regulating valve 8, the electric field recovery device is provided with a circulation pipeline 9, and the circulation pipeline 9 is provided with a pump 10, and the mother liquor of the electric field recovery device 5 passes through The circulation pipeline 9 enters the storage tank 4, and the drying device 7 is provided with a temperature control device;
所述电场回收装置5利用Ti/SnO2为阳极材料，铂为阴极材料；所述电场回收装置为间歇式生产，所述缫丝废液回收纯化丝胶蛋白的装置通过程序控制自动化生产。The electric field recovery device 5 utilizes Ti/SnO 2 as the anode material and platinum as the cathode material; the electric field recovery device is produced intermittently, and the device for recovering and purifying sericin from the silk reeling waste liquid is automatically produced through program control.
实施例6Example 6
利用缫丝废液回收纯化丝胶蛋白的装置回收纯化丝胶蛋白的方法，包括以下步骤：The method for recovering and purifying sericin by using a device for recovering and purifying sericin from silk reeling waste liquid comprises the following steps:
1)缫丝废水进入抽滤装置1经抽滤除去杂质，抽滤后的料液在浓缩装置2中浓缩后进入截留量为3～4KDa的超滤装置3除去无机盐离子，得处理液储存在储存罐4中；1) Silk reeling waste water enters the suction filtration device 1 to remove impurities through suction filtration, and the feed liquid after suction filtration is concentrated in the concentration device 2 and then enters the ultrafiltration device 3 with a cutoff of 3-4KDa to remove inorganic salt ions, and the treated liquid is stored In storage tank 4;
2)通过控制调节阀8所述处理液通过管道进入到电场回收装置5中，利用电场作用使丝胶蛋白沉淀，得丝胶蛋白；2) by controlling the regulating valve 8, the treatment liquid enters the electric field recovery device 5 through the pipeline, and the sericin is precipitated by the action of the electric field to obtain the sericin;
3)步骤2)得到的丝胶蛋白在经过分离纯化装置6的2～4次纯化后通过干燥装置7干燥2～4天，得丝胶蛋白产品。3) The sericin protein obtained in step 2) is purified by the separation and purification device 6 for 2 to 4 times and then dried by the drying device 7 for 2 to 4 days to obtain a sericin product.
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。Finally, it is noted that the above embodiments are only used to illustrate the technical solutions of the present invention without limitation. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be carried out Modifications or equivalent replacements without departing from the spirit and scope of the technical solution of the present invention shall be covered by the claims of the present invention.
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