CN114685230A - 一种脱氢醋酸生产过程中尾气净化的方法 - Google Patents
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- 239000004287 Dehydroacetic acid Substances 0.000 title claims abstract description 33
- 229940061632 dehydroacetic acid Drugs 0.000 title claims abstract description 33
- 235000019258 dehydroacetic acid Nutrition 0.000 title claims abstract description 33
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- JEQRBTDTEKWZBW-UHFFFAOYSA-N dehydroacetic acid Chemical compound CC(=O)C1=C(O)OC(C)=CC1=O JEQRBTDTEKWZBW-UHFFFAOYSA-N 0.000 title claims abstract 8
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Abstract
本发明公开了一种脱氢醋酸生产过程中尾气净化的方法，包括：(1)将含水、丙酮和甲苯的脱氢醋酸尾气通过喷淋吸收，控制吸收停留时间在1～30s，控制吸收温度在0～40℃，将尾气中水、丙酮完全去除，吸收液蒸馏脱轻，溶剂回用；(2)将步骤(1)脱除水、丙酮后的气体进一步通过膜分离，压力控制在‑0.095～‑0.06MPa，温度控制在20～60℃，回收含量＞99％的甲苯，甲苯回收率＞90％，尾气中有机物含量≤1000mg/m3；(3)上述气体经过氧化裂解，控制裂解停留时间在0.1～60s，裂解温度＜800℃，进行深度净化处理，非烷烃总烃≤70mg/m3，甲苯≤25mg/m3，净化气体达标排放。采用该净化方法，在实现甲苯的回收利用的同时，达到了低能耗、净化气体达标排放的效果。
Description
技术领域
本发明属化工技术领域，具体涉及一种脱氢醋酸生产过程中尾气净化的方法。
背景技术
脱氢醋酸：又称脱氢乙酸，简称DHA；
英文名：Dehydroacetic acid；
外观性质：无色结晶或浅黄色粉末；
溶解性：难溶于水，溶于苯、乙醚、丙酮及热乙醇中；
CAS号：520-45-6；
分子式：C8H8O4；
分子量：168.15；
熔点：109℃；
作用和用途：主要用途是作为低毒、高效、广谱抗菌剂，广泛应用于涂料、油料、皮革制品、食品、饲料、包装材料和化妆品的防霉防腐。
现有技术中脱氢醋酸制备通常由双乙烯酮在含有催化剂的甲苯溶剂中发生二聚制得。一方面，原料双乙烯酮与少量水反应，生成丙酮和二氧化碳，少量丙酮会进入潮品脱氢醋酸中；在潮品脱氢醋酸干燥过程中，尾气中会含有丙酮气体。另一方面，因采用的溶剂为甲苯，潮品脱氢醋酸中会含有2～3％甲苯；在潮品脱氢醋酸干燥过程中，尾气中会含有甲苯气体。
综上，现有工艺中脱氢醋酸潮品干燥过程会产生含甲苯、丙酮、水蒸气等的尾气，进一步污染环境造成排放不达标。现有技术中通常采用的应对方法是：先采用冷凝回收部分甲苯、再采用活性炭吸附去除甲苯，该方法具有能耗高、甲苯回收率低等缺点。
发明内容
本发明所要解决的技术问题在于克服现有技术的上述不足，提供一种可以实现甲苯回收利用的同时，达到低能耗及净化气体达标排放的脱氢醋酸生产过程中尾气净化的方法。
其所要解决的技术问题可以通过以下技术方案来实施。
一种脱氢醋酸生产过程中尾气净化的方法，其特点为，包括如下步骤：
(1)将含水、丙酮和甲苯的脱氢醋酸尾气通过喷淋吸收，控制吸收停留时间在1～30s，控制吸收温度在0～40℃，将尾气中水、丙酮完全去除，吸收液蒸馏脱轻，溶剂回用；
(2)将步骤(1)脱除水、丙酮后的气体进一步通过膜分离，压力控制在-0.095～-0.06MPa，温度控制在20～60℃，回收含量＞99％的甲苯，甲苯回收率＞90％，尾气中有机物含量≤1000mg/m3；
(3)上述气体经过氧化裂解，控制裂解停留时间在0.1～60s，裂解温度＜800℃，进行深度净化处理，非烷烃总烃≤70mg/m3，甲苯≤25mg/m3，净化气体达标排放。
作为本技术方案的进一步改进，步骤(1)中，喷淋吸收采用的吸收剂为高沸点极性溶剂。
作为本技术方案的更进一步改进，所述高沸点极性溶剂为醇类或酮类。
作为本发明的优选实施例，所述醇类为乙二醇、丙二醇、丁二醇或碳原子数＞4的醇。
也作为本发明的优选实施例，所述酮类选自NMP或DMI。
采用上述技术方案的脱氢醋酸生产过程中尾气净化的方法，脱氢醋酸尾气(含水、丙酮、甲苯等)首先通过喷淋吸收，吸收剂为高沸点极性溶剂，控制吸收停留时间和吸收温度，将尾气中水、丙酮完全去除，吸收液蒸馏，脱轻后的吸收剂回用；脱除水、丙酮后的气体进一步通过膜分离，回收甲苯，尾气中有机物含量≤1000mg/m3；上述气体最后经过氧化裂解，控制裂解停留时间和裂解温度，进行深度净化处理，甲苯≤25mg/m3，净化气体达标排放。
采用该净化方法，在实现甲苯的回收利用的同时，达到了低能耗、净化气体达标排放的效果。
附图说明
图1为本发明脱氢醋酸生产过程中尾气净化方法的流程图
具体实施方式
下面结合附图对本发明的具体实施方式进行进一步的详细说明。
参照图1，本发明主要针对脱氢醋酸生产过程中含有水、丙酮、甲苯等的尾气，提供一种脱氢醋酸生产过程中尾气净化的方法。脱氢醋酸尾气(含水、丙酮、甲苯等)首先采用高沸点极性溶剂进行喷淋吸收，将尾气中水、丙酮完全去除，吸收液蒸馏脱轻，溶剂回用；然后将脱除水、丙酮后的气体进一步通过膜分离技术，回收甲苯；最后上述气体经过氧化裂解技术，进行深度净化处理，净化气体达标排放。
具体工艺步骤如下：
(1)脱氢醋酸尾气(含水、丙酮、甲苯等)通过喷淋吸收，控制吸收停留时间t＝1～30s，吸收温度T＝0～40℃，将尾气中水、丙酮完全去除，吸收液蒸馏脱轻，溶剂回用；
(2)脱除水、丙酮后的气体进一步通过膜分离，压力-0.095～-0.06MPa，温度20～60℃，回收含量＞99％的甲苯，甲苯回收率＞90％，尾气中有机物含量≤1000mg/m3；
(3)上述气体经过氧化裂解，控制裂解停留时间t＝0.1～60s，裂解温度T＜800℃，进行深度净化处理，非烷烃总烃≤70mg/m3，甲苯≤25mg/m3，净化气体达标排放；
进一步的，喷淋吸收采用的吸收剂为高沸点极性溶剂，包括醇类(乙二醇、丙二醇、丁二醇和碳原子数＞4的醇)、酮类(NMP、DMI等酮类)；
以下为更具体的实施例。
实施例1：
脱氢醋酸尾气(含水、丙酮、甲苯等)首先采用吸附剂为乙二醇进行喷淋吸收，控制吸收停留时间2s，吸收温度0℃，尾气中丙酮含量5ppm、水50ppm；脱除水、丙酮后的气体然后通过膜分离，压力-0.08MPa、温度30℃，回收含量99.5％的甲苯，甲苯回收率93.8％，尾气中有机物含量880mg/m3；上述气体经过氧化裂解，控制裂解停留时间t＝10s，裂解温度780℃，进行深度净化处理，非烷烃总烃42mg/m3，甲苯10mg/m3，净化气体达标排放。
实施例2：
脱氢醋酸尾气(含水、丙酮、甲苯等)首先采用吸附剂为丙二醇进行喷淋吸收，控制吸收停留时间5s，吸收温度10℃，尾气中丙酮含量10ppm、水80ppm；脱除水、丙酮后的气体然后通过膜分离，压力-0.06MPa、温度20℃，回收含量99.6％的甲苯，甲苯回收率93.6％，尾气中有机物含量800mg/m3；上述气体经过氧化裂解，控制裂解停留时间t＝5s，裂解温度700℃，进行深度净化处理，非烷烃总烃50mg/m3，甲苯15mg/m3，净化气体达标排放。
实施例3：
脱氢醋酸尾气(含水、丙酮、甲苯等)首先采用吸附剂为丁二醇进行喷淋吸收，控制吸收停留时间30s，吸收温度40℃，尾气中丙酮含量12ppm、水75ppm；脱除水、丙酮后的气体然后通过膜分离，压力-0.095MPa、温度60℃，回收含量99.7％的甲苯，甲苯回收率93.2％，尾气中有机物含量750mg/m3；上述气体经过氧化裂解，控制裂解停留时间t＝50s，裂解温度550℃，进行深度净化处理，非烷烃总烃45mg/m3，甲苯20mg/m3，净化气体达标排放。
实施例4：
脱氢醋酸尾气(含水、丙酮、甲苯等)首先采用吸附剂为NMP进行喷淋吸收，控制吸收停留时间15s，吸收温度20℃，尾气中丙酮含量8ppm、水55ppm；脱除水、丙酮后的气体然后通过膜分离，压力-0.075MPa、温度40℃，回收含量99.7％的甲苯，甲苯回收率92.8％，尾气中有机物含量650mg/m3；上述气体经过氧化裂解，控制裂解停留时间t＝30s，裂解温度650℃，进行深度净化处理，非烷烃总烃50mg/m3，甲苯15mg/m3，净化气体达标排放。
实施例5：
脱氢醋酸尾气(含水、丙酮、甲苯等)首先采用吸附剂为DMI进行喷淋吸收，控制吸收停留时间20s，吸收温度30℃，尾气中丙酮含量10ppm、水60ppm；脱除水、丙酮后的气体然后通过膜分离，压力-0.075MPa、温度35℃，回收含量99.8％的甲苯，甲苯回收率94.1％，尾气中有机物含量680mg/m3；上述气体经过氧化裂解，控制裂解停留时间t＝40s，裂解温度680℃，进行深度净化处理，非烷烃总烃55mg/m3，甲苯20mg/m3，净化气体达标排放。
以上已以较佳实施例公开了本发明，然其并非用以限制本发明，凡采用等同替换或者等效变换方式所获得的技术方案，均落在本发明的保护范围之内。
Claims (5)
1.一种脱氢醋酸生产过程中尾气净化的方法，其特征在于，包括如下步骤：
(1)将含水、丙酮和甲苯的脱氢醋酸尾气通过喷淋吸收，控制吸收停留时间在1～30s，控制吸收温度在0～40℃，将尾气中水、丙酮完全去除，吸收液蒸馏脱轻，溶剂回用；
(2)将步骤(1)脱除水、丙酮后的气体进一步通过膜分离，压力控制在-0.095～-0.06MPa，温度控制在20～60℃，回收含量＞99％的甲苯，甲苯回收率＞90％，尾气中有机物含量≤1000mg/m3；
(3)上述气体经过氧化裂解，控制裂解停留时间在0.1～60s，裂解温度＜800℃，进行深度净化处理，非烷烃总烃≤70mg/m3，甲苯≤25mg/m3，净化气体达标排放。
2.根据权利要求1所述的脱氢醋酸生产过程中尾气净化的方法，其特征在于，步骤(1)中，喷淋吸收采用的吸收剂为高沸点极性溶剂。
3.根据权利要求2所述的脱氢醋酸生产过程中尾气净化的方法，其特征在于，所述高沸点极性溶剂为醇类或酮类。
4.根据权利要求3所述的脱氢醋酸生产过程中尾气净化的方法，其特征在于，所述醇类为乙二醇、丙二醇、丁二醇或碳原子数＞4的醇。
5.根据权利要求3所述的脱氢醋酸生产过程中尾气净化的方法，其特征在于，所述酮类选自NMP或DMI。
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