CN100390082C - A kind of treatment and recycling method of dimethyl isophthalate-5-sulfonic acid production wastewater - Google Patents
A kind of treatment and recycling method of dimethyl isophthalate-5-sulfonic acid production wastewater Download PDFInfo
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 title claims abstract description 34
- 239000002351 wastewater Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000004064 recycling Methods 0.000 title description 3
- 238000001179 sorption measurement Methods 0.000 claims abstract description 66
- 229920005989 resin Polymers 0.000 claims abstract description 49
- 239000011347 resin Substances 0.000 claims abstract description 49
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000003795 desorption Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 238000004821 distillation Methods 0.000 claims abstract description 5
- 239000005416 organic matter Substances 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims abstract description 3
- 230000008025 crystallization Effects 0.000 claims abstract description 3
- 229920001429 chelating resin Polymers 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 3
- -1 acrylic ester Chemical class 0.000 claims description 2
- 238000004042 decolorization Methods 0.000 claims description 2
- 125000005396 acrylic acid ester group Chemical group 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- VNGOYPQMJFJDLV-UHFFFAOYSA-N dimethyl benzene-1,3-dicarboxylate Chemical compound COC(=O)C1=CC=CC(C(=O)OC)=C1 VNGOYPQMJFJDLV-UHFFFAOYSA-N 0.000 description 1
- QPGQPZQYAMNOPE-UHFFFAOYSA-N dimethyl benzene-1,3-dicarboxylate;sodium Chemical compound [Na].COC(=O)C1=CC=CC(C(=O)OC)=C1 QPGQPZQYAMNOPE-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开了一种间苯二甲酸二甲酯-5-磺酸生产废水的治理及资源化方法。其步骤为将经过过滤预处理的间苯二甲酸二甲酯-5-磺酸生产废水通过装填有丙烯酸酯类吸附树脂的吸附柱；将吸附出水加碱中和后，经甲醇蒸馏回收和活性炭吸附处理后即可排放；将吸附了间苯二甲酸二甲酯-5-磺酸生产废水中有机物的丙烯酸酯类吸附树脂用热水脱附，脱附液经蒸发浓缩结晶后可回收间苯二甲酸二甲酯-5-磺酸晶体。经本发明公开的方法处理的废水CODCr由180000mg/L降至100mg/L左右，废水中的间苯二甲酸二甲酯-5-磺酸绝大部分可回收为产品，其纯度可达到一级标准。The invention discloses a treatment and resource utilization method for waste water from the production of dimethyl isophthalate-5-sulfonic acid. The steps are to pass the pre-filtered dimethyl isophthalate-5-sulfonic acid production wastewater through an adsorption column filled with acrylate adsorption resin; add alkali to neutralize the adsorbed water, recover it by methanol distillation and use activated carbon It can be discharged after adsorption treatment; the acrylic adsorption resin that has adsorbed the organic matter in the dimethyl isophthalate-5-sulfonic acid production wastewater is desorbed with hot water, and the desorption liquid can be recovered after evaporation, concentration and crystallization. Dimethyl dicarboxylate-5-sulfonic acid crystals. The COD Cr of the waste water treated by the method disclosed in the present invention is reduced from 180000 mg/L to about 100 mg/L, and most of the dimethyl isophthalate-5-sulfonic acid in the waste water can be recovered as products, and its purity can reach one level standard.
Description
一、技术领域 1. Technical field
本发明涉及一种间苯二甲酸二甲酯-5-磺酸生产废水的治理及资源化方法，具体而言，是指采用丙烯酸酯类树脂对间苯二甲酸二甲酯-5-磺酸生产废水吸附及脱附方法。The present invention relates to a treatment and recycling method of waste water from the production of dimethyl isophthalate-5-sulfonic acid. Production wastewater adsorption and desorption method.
二、背景技术 2. Background technology
间苯二甲酸二甲酯-5-磺酸的商品名为SIPM。该产品可以作为DMT法生产阳离子可染型聚酯的第三单体，俗称三单体。间苯二甲酸二甲酯-5-磺酸钠的生产一般采用“一锅法”，即直接磺化间苯二甲酸后，经甲醇酯化，再与碱反应制得间苯二甲酸二甲酯-5-磺酸钠。采用这一生产工艺，每吨产品将产生强酸性废水约7吨，该废水呈淡黄色，CODcr为180000mg/L左右，主要含有甲醇(CODcr为80000mg/L左右)、间苯二甲酸二甲酯-5-磺酸钠、间苯二甲酸-5-磺酸及其他中间产物(CODcr约为100000mg/L)等有机物，此外还含有7％左右的硫酸钠。由于该类废水盐分和CODcr过高，因此其生产废水的有效治理至今未得解决。The trade name of dimethyl isophthalate-5-sulfonic acid is SIPM. This product can be used as the third monomer in the production of cationic dyeable polyester by DMT method, commonly known as tri-monomer. The production of dimethyl isophthalate-5-sodium sulfonate generally adopts the "one-pot method", that is, after directly sulfonating isophthalic acid, esterification with methanol, and then reacting with alkali to obtain dimethyl isophthalate Sodium ester-5-sulfonate. Using this production process, about 7 tons of strong acid wastewater will be produced per ton of product. The wastewater is light yellow and has a CODcr of about 180,000 mg/L, mainly containing methanol (CODcr is about 80,000 mg/L) and dimethyl isophthalate. -5-sodium sulfonate, isophthalic acid-5-sulfonic acid and other intermediate products (CODcr about 100000mg/L) and other organic substances, in addition to containing about 7% sodium sulfate. Because the salinity and CODcr of this type of wastewater are too high, the effective treatment of its production wastewater has not been solved so far.
丙烯酸酯类吸附树脂既可用于从极性溶剂中吸附非极性溶质，也可用于从非极性溶剂中吸附一定极性的溶质。当从极性溶剂中吸附有机物时，溶质分子的亲水和疏水部分都能被丙烯酸酯类吸附树脂吸附，在吸附过程中，吸附质分子的亲水部分和丙烯酸酯类吸附树脂的表面之间以极性键联(如氢键联)，这种作用力在较高温度下将大幅度减小，故吸附后的丙烯酸酯类吸附树脂可以用热水进行脱附。此类树脂可以克服超高交联树脂只能通过疏水作用吸附分离有机物质的缺点，在一定范围内也可以克服其他小分子有机溶剂对吸附过程的干扰。Acrylate-based adsorption resins can be used to adsorb non-polar solutes from polar solvents, and can also be used to adsorb certain polar solutes from non-polar solvents. When adsorbing organic matter from a polar solvent, both the hydrophilic and hydrophobic parts of the solute molecule can be adsorbed by the acrylate-based adsorption resin. With polar bonding (such as hydrogen bonding), this force will be greatly reduced at higher temperatures, so the adsorbed acrylate resin can be desorbed with hot water. This kind of resin can overcome the shortcomings of ultra-high cross-linked resins that can only adsorb and separate organic substances through hydrophobic interaction, and can also overcome the interference of other small molecule organic solvents on the adsorption process within a certain range.
三、发明内容 3. Contents of the invention
本发明的主要目的是提出一种间苯二甲酸二甲酯-5-磺酸生产废水的治理及资源化方法。利用丙烯酸酯类吸附树脂，既能分离回收绝大部分的间苯二甲酸二甲酯-5-磺酸钠，又能使最终排出的废水减量化、无害化，实现循环经济的目标。Main purpose of the present invention is to propose a kind of treatment and resource utilization method of dimethyl isophthalate-5-sulfonic acid production wastewater. The use of acrylate-based adsorption resins can not only separate and recover most of the dimethyl-5-sodium isophthalate, but also reduce and make the final discharged waste water harmless, so as to achieve the goal of circular economy.
本发明的技术方案如下：Technical scheme of the present invention is as follows:
一种间苯二甲酸二甲酯-5-磺酸生产废水的治理及资源化方法，其包括以下步骤：A treatment and recycling method for dimethyl isophthalate-5-sulfonic acid production wastewater, comprising the following steps:
(1)将经过过滤预处理的间苯二甲酸二甲酯-5-磺酸生产废水于5～40℃以0.5～5BV/h的流量通过装填有丙烯酸酯类吸附树脂的吸附柱；(1) passing the pre-filtered dimethyl isophthalate-5-sulfonic acid production wastewater through an adsorption column filled with acrylate adsorption resin at a flow rate of 0.5 to 5 BV/h at 5 to 40 ° C;
(2)将吸附出水于10～60℃加碱中和至pH＝6～9后，经甲醇蒸馏回收和活性炭吸附处理后即可排放；(2) Add alkali to neutralize the adsorbed effluent at 10-60°C to pH=6-9, and then discharge it after methanol distillation recovery and activated carbon adsorption treatment;
(3)将步骤(1)中吸附了间苯二甲酸二甲酯-5-磺酸生产废水中有机物的丙烯酸酯类吸附树脂用70～90℃的热水脱附，脱附液经蒸发浓缩结晶后可回收间苯二甲酸二甲酯-5-磺酸晶体。(3) Desorb the acrylic ester-based adsorption resin that has adsorbed the organic matter in the waste water from the production of dimethyl isophthalate-5-sulfonic acid in step (1) with hot water at 70 to 90° C., and the desorption solution is evaporated and concentrated Dimethyl isophthalate-5-sulfonic acid crystals can be recovered after crystallization.
上述的丙烯酸酯类吸附树脂可选用NDA-7树脂(江苏南大戈德环保科技有限公司生产)、Amberlite XAD-7树脂、Amberlite XAD-8树脂、Diaion HP2MG树脂(Amberlite XAD系列由美国罗门哈斯公司生产，Diaion HPMG系列由日本三菱公司生产)。优先选用NDA-7树脂和XAD-7树脂。The above-mentioned acrylate adsorption resin can be selected from NDA-7 resin (produced by Jiangsu Nanda Gede Environmental Protection Technology Co., Ltd.), Amberlite XAD-7 resin, Amberlite XAD-8 resin, Diaion HP2MG resin (Amberlite XAD series is produced by American Rohm and Haas Produced by the company, Diaion HPMG series is produced by Mitsubishi Corporation of Japan). NDA-7 resin and XAD-7 resin are preferred.
在具体操作步骤中，树脂的吸附可以分两级进行，一级吸附主要为脱色，目的是去除废水淡黄色色素。一级吸附采用双塔串联吸附，单塔脱附的运行方式，即设置I、II、III三个吸附塔，先将I、II塔串联顺流吸附，I塔作为首柱，II塔作为尾柱，当I塔吸附饱和后，切换成II、III塔串联顺流吸附，II塔作为首柱，III塔作为尾柱，同时I塔进行顺流脱附，如此循环操作，可以保证整个装置始终连续运行。二级吸附采用双塔连续移动床操作方式，即吸附塔和脱附塔分别连续运行。一级吸附出水由塔底进入二级吸附塔，树脂由塔顶加入，吸附饱和后的树脂由塔底进入吸附塔贮罐，经真空抽提送入二级脱附塔并使用热水脱附再生，再生后的树脂经脱附塔贮罐被真空抽提补充入二级吸附塔。In the specific operation steps, the adsorption of the resin can be carried out in two stages, and the first stage of adsorption is mainly for decolorization, and the purpose is to remove the light yellow pigment of the wastewater. The first-stage adsorption adopts the operation mode of double-tower series adsorption and single-tower desorption, that is, three adsorption towers I, II, and III are set up, and the I and II towers are connected in series for downstream adsorption, and the I tower is used as the first column, and the II tower is used as the tail column. column, when tower I is saturated, switch to tower II and tower III for downstream adsorption in series, tower II acts as the first column, tower III acts as the tail column, and tower I performs downstream desorption. Such a cycle operation can ensure that the whole device is always continue to operate. The second-stage adsorption adopts the double-tower continuous moving bed operation mode, that is, the adsorption tower and the desorption tower operate continuously respectively. The primary adsorption water enters the secondary adsorption tower from the bottom of the tower, and the resin is added from the top of the tower. The saturated resin enters the storage tank of the adsorption tower from the bottom of the tower, and is sent to the secondary desorption tower by vacuum extraction and desorbed with hot water. Regeneration, the regenerated resin is vacuum extracted through the storage tank of the desorption tower and replenished into the secondary adsorption tower.
有益效果Beneficial effect
本发明与现有技术相比，其显著优点是：(1)经二级吸附后，废水中的间苯二甲酸二甲酯-5-磺酸的含量由100000mg/L降至150mg/L以下。树脂吸附出水经甲醇回收和活性炭吸附工序后，废水的CODCr由180000mg/L降至100mg/L左右，废水中的间苯二甲酸二甲酯-5-磺酸绝大部分可回收为产品，其纯度可达到一级标准；(2)吸附了间苯二甲酸二甲酯-5-磺酸等有机物的丙烯酸系大孔吸附树脂可直接用70～90℃的热水脱附，脱附液中可析出纯度95％以上的间苯二甲酸二甲酯-5-磺酸晶体。即节省了原料，又避免了二次污染。采用本发明方法处理间苯二甲酸二甲酯-5-磺酸生产过程中排放的废水，最终排出的废水符合国家污水排放标准，具有显著的环境、经济和社会效益。Compared with the prior art, the present invention has the remarkable advantages that: (1) after secondary adsorption, the content of dimethyl isophthalate-5-sulfonic acid in the waste water is reduced from 100000mg/L to below 150mg/L . After the resin adsorption effluent undergoes methanol recovery and activated carbon adsorption processes, the COD Cr of the wastewater is reduced from 180,000mg/L to about 100mg/L, and most of the dimethyl isophthalate-5-sulfonic acid in the wastewater can be recovered as products. Its purity can reach the first-class standard; (2) the acrylic macroporous adsorption resin that has adsorbed organic matter such as dimethyl isophthalate-5-sulfonic acid can be directly desorbed with hot water at 70-90 °C, and the desorption solution Dimethyl isophthalate-5-sulfonic acid crystals with a purity of more than 95% can be precipitated in the That is to save raw materials and avoid secondary pollution. By adopting the method of the invention to treat the wastewater discharged during the production process of dimethyl isophthalate-5-sulfonic acid, the finally discharged wastewater complies with the national sewage discharge standard and has remarkable environmental, economic and social benefits.
四、具体实施方式 4. Specific implementation
以下通过实施例进一步说明本发明。The present invention is further illustrated by the following examples.
实施例1：将100mL的NDA-7树脂装入带夹套的玻璃吸附柱中(Φ30×250mm)。取200mL的淡黄色废水进行过滤预处理，废水的CODCr为180000mg/L，其中间苯二甲酸二甲酯-5-磺酸的CODCr为100000mg/L。吸附温度为室温，将废水以1BV/h的流量首先通过NDA-7树脂床层，处理量为2000mL/批。吸附出水为无色，CODCr降至50000mg/L，间苯二甲酸二甲酯-5-磺酸含量降至150mg/L以下。将吸附出水经甲醇蒸馏回收和活性炭吸附后检测，出水CODCr降至100mg/L，间苯二甲酸二甲酯-5-磺酸未检出。Example 1: 100 mL of NDA-7 resin was loaded into a jacketed glass adsorption column (Φ30×250 mm). Take 200mL of light yellow waste water for filtration pretreatment, the COD Cr of waste water is 180000mg/L, wherein the COD Cr of dimethyl isophthalate-5-sulfonic acid is 100000mg/L. The adsorption temperature is room temperature, and the waste water is first passed through the NDA-7 resin bed at a flow rate of 1BV/h, and the treatment capacity is 2000mL/batch. The adsorbed water is colorless, the COD Cr is reduced to 50000mg/L, and the content of dimethyl isophthalate-5-sulfonic acid is reduced to below 150mg/L. The adsorbed effluent was recovered by methanol distillation and detected after activated carbon adsorption. The COD Cr of the effluent was reduced to 100 mg/L, and dimethyl isophthalate-5-sulfonic acid was not detected.
经吸附后的NDA-7树脂用350mL的热水进行洗脱再生，热水的温度为80℃，热水流量为1BV/h。脱附液经蒸馏结晶后可析出纯度95％以上的间苯二甲酸二甲酯-5-磺酸晶体，树脂经脱附再生后可恢复吸附能力。The adsorbed NDA-7 resin was eluted and regenerated with 350mL of hot water, the temperature of the hot water was 80°C, and the flow rate of the hot water was 1BV/h. After the desorption liquid is distilled and crystallized, dimethyl isophthalate-5-sulfonic acid crystals with a purity of more than 95% can be precipitated, and the resin can recover its adsorption capacity after desorption and regeneration.
实施例2：将实施例1中的NDA-7树脂分别以Amberlite XAD-7树脂、Amberlite XAD-8树脂、Diaion HP2MG树脂代替，其他操作条件保持不变，每批处理量和出水水质均明显逊于实施例1中处理效果。Embodiment 2: NDA-7 resin among the embodiment 1 is replaced with Amberlite XAD-7 resin, Amberlite XAD-8 resin, Diaion HP2MG resin respectively, other operating conditions remain unchanged, each batch capacity and effluent water quality are all obviously inferior In embodiment 1 processing effect.
实施例3：将实施例1中的吸附温度用玻璃夹套控制为45±1℃，其他操作条件保持不变，每批处理量和出水水质均明显逊于实施例1。Example 3: The adsorption temperature in Example 1 is controlled to 45±1° C. with a glass jacket, and other operating conditions remain unchanged, and the treatment capacity and effluent quality of each batch are obviously inferior to those of Example 1.
实施例4：将实施例1中的吸附流量以3BV/h替代，洗脱再生时热水的温度为90℃，其他操作条件保持不变，每批处理量和出水水质与实施例1类似。Example 4: The adsorption flow rate in Example 1 was replaced by 3BV/h, the temperature of hot water during elution and regeneration was 90°C, and other operating conditions remained unchanged. The treatment capacity and effluent quality of each batch were similar to those in Example 1.
实施例5：Example 5:
(1)一级吸附：选用三只吸附塔，每塔内径为600mm，塔高5500mm，每塔填装NDA-7树脂600kg。将CODCr为180000mg/L，其中间苯二甲酸二甲酯-5-磺酸的CODCr为100000mg/L的淡黄色废水经过滤后打入吸附塔，吸附采用I、II号双塔串联顺流吸附的办法，吸附流量为1.6m3/h，每批处理量为12m3，吸附出水为无色。(1) Primary adsorption: Three adsorption towers are selected, each tower has an inner diameter of 600mm, a tower height of 5500mm, and each tower is filled with 600kg of NDA-7 resin. The COD Cr is 180000mg/L, wherein the COD Cr of dimethyl isophthalate-5-sulfonic acid is 100000mg/L light yellow waste water is put into the adsorption tower after filtering, and the adsorption adopts No. Flow adsorption method, the adsorption flow rate is 1.6m 3 /h, the treatment capacity of each batch is 12m 3 , and the adsorbed water is colorless.
(2)二级吸附：二级吸附采用双塔连续移动床操作方式，即吸附塔和脱附塔分别连续运行。每塔内径为1400mm，塔高11060mm，每塔填装NDA-7树脂1000kg。一级吸附出水由塔底进入二级吸附塔，废水流量为1.2m3/h，树脂由塔顶加入，每小时装填树脂一次。吸附饱和后的树脂由塔底进入吸附塔贮罐，每小时卸载树脂一次，经真空抽提送入二级脱附塔并使用热水脱附再生，再生后的树脂经脱附塔贮罐被真空抽提补充入二级吸附塔。CODCr降至55000mg/L，间苯二甲酸二甲酯-5-磺酸含量降至100mg/L以下。将吸附出水经甲醇蒸馏回收和活性炭吸附后检测，出水CODCr降至150mg/L，间苯二甲酸二甲酯-5-磺酸未检出。(2) Secondary adsorption: Secondary adsorption adopts the double-tower continuous moving bed operation mode, that is, the adsorption tower and the desorption tower operate continuously respectively. The inner diameter of each tower is 1400mm, the tower height is 11060mm, and each tower is filled with 1000kg of NDA-7 resin. The primary adsorption effluent enters the secondary adsorption tower from the bottom of the tower, the waste water flow rate is 1.2m 3 /h, and the resin is added from the top of the tower, and the resin is filled once per hour. The saturated resin enters the storage tank of the adsorption tower from the bottom of the tower, and the resin is unloaded once an hour, and then sent to the secondary desorption tower through vacuum extraction and desorbed and regenerated with hot water. Vacuum extraction supplements into the secondary adsorption tower. COD Cr is reduced to 55000mg/L, and the content of dimethyl isophthalate-5-sulfonic acid is reduced to below 100mg/L. The adsorbed effluent was recovered by methanol distillation and detected after activated carbon adsorption. The COD Cr of the effluent was reduced to 150mg/L, and dimethyl isophthalate-5-sulfonic acid was not detected.
(3)热脱附：经吸附后的NDA-7树脂用热水进行洗脱再生，热水的温度为83℃，热水流量为1.2m3/h。脱附液经蒸馏结晶后可析出纯度95％以上的间苯二甲酸二甲酯-5-磺酸晶体，树脂经脱附再生后可恢复吸附能力。(3) Thermal desorption: The adsorbed NDA-7 resin is eluted and regenerated with hot water, the temperature of the hot water is 83°C, and the flow rate of the hot water is 1.2m 3 /h. After the desorption liquid is distilled and crystallized, dimethyl isophthalate-5-sulfonic acid crystals with a purity of more than 95% can be precipitated, and the resin can recover its adsorption capacity after desorption and regeneration.
实施例6：将实施例1中的吸附流量以0.5BV/h替代，吸附温度用玻璃夹套控制为5±1℃，其他操作条件保持不变，每批处理量和出水水质均略逊于实施例1。Example 6: The adsorption flow rate in Example 1 was replaced by 0.5BV/h, the adsorption temperature was controlled to 5±1°C with a glass jacket, and other operating conditions remained unchanged. Example 1.
实施例7：将实施例1中的吸附流量以5BV/h替代，脱附温度以70℃替代，其他操作条件保持不变，每批处理量和出水水质均略逊于实施例1。Example 7: The adsorption flow rate in Example 1 was replaced by 5BV/h, the desorption temperature was replaced by 70°C, and other operating conditions remained unchanged, and the treatment capacity and effluent quality of each batch were slightly inferior to those in Example 1.
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