CN107501152B - A kind of separation method of tert-butyl hydroperoxide - Google Patents
A kind of separation method of tert-butyl hydroperoxide Download PDFInfo
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- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 238000000926 separation method Methods 0.000 title claims abstract description 32
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims abstract description 32
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010992 reflux Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims 2
- 239000000654 additive Substances 0.000 claims 1
- 230000000996 additive effect Effects 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000007792 gaseous phase Substances 0.000 claims 1
- 239000012263 liquid product Substances 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 150000002978 peroxides Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 24
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000010533 azeotropic distillation Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 4
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000001282 iso-butane Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- FXMBBTAYWRVRLJ-UHFFFAOYSA-N OO.C=C(C)C Chemical compound OO.C=C(C)C FXMBBTAYWRVRLJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003592 biomimetic effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- JLRMRTRHBRVQMS-UHFFFAOYSA-N hydrogen peroxide;2-methylpropan-2-ol Chemical compound OO.CC(C)(C)O JLRMRTRHBRVQMS-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
- C07C407/003—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开了一种叔丁基过氧化氢的分离方法。该方法针对叔丁基过氧化氢的合成工艺中存在的二叔丁基过氧化物，通过加入叔丁醇与二叔丁基过氧化物形成共沸物，实现二叔丁基过氧化物的高效分离。经分离提纯后，叔丁基过氧化氢的纯度可达99%以上。本发明的优点是采用共沸精馏方法分离叔丁基过氧化氢和二叔丁基过氧化物，分离效率高，收率高，工艺简单。The invention discloses a method for separating tert-butyl hydroperoxide. The method aims at the di-tert-butyl peroxide existing in the synthesis technique of tert-butyl hydroperoxide, forms azeotrope by adding tert-butanol and di-tert-butyl peroxide, realizes the di-tert-butyl peroxide Efficient separation. After separation and purification, the purity of tert-butyl hydroperoxide can reach more than 99%. The invention has the advantages of adopting the azeotropic distillation method to separate tert-butyl hydroperoxide and di-tert-butyl peroxide, high separation efficiency, high yield and simple process.
Description
技术领域technical field
本发明属于化工分离过程的工艺方法，具体地说，是涉及叔丁基过氧化氢的分离技术。The invention belongs to the technical method of chemical industry separation process, specifically, relates to the separation technology of tert-butyl hydroperoxide.
背景技术Background technique
叔丁基过氧化氢作为活泼的烷烃氢过氧化物，是有机过氧化物中的一个重要分支。目前，合成叔丁基过氧化氢成熟的工艺有：1. 异丁烯双氧水法，此法因原料储存不便且反应条件苛刻等缺点限制了工业生产；2. 异丁烷氧化法，典型的工艺为ACRO和Texaco工艺，这两个工艺的产品附加值高，经济效益好，但反应需要在高温高压下进行，对设备要求高，投资成本大，潜在的危险性大；3. 叔丁醇双氧水法，因投资成本低，是国内工业生产叔丁基过氧化氢的主要方法，但生产过程中会产生大量含酸废水，严重污染环境。专利 CN104262222A报道了一种仿生催化氧化异丁烷制备叔丁基过氧化氢的方法，该反应可以在较为温和、安全的条件下进行，具有极大的产业化价值。As an active alkane hydroperoxide, tert-butyl hydroperoxide is an important branch of organic peroxides. At present, the mature processes for synthesizing tert-butyl hydroperoxide include: 1. Isobutylene hydrogen peroxide method, which limits industrial production due to inconvenient storage of raw materials and harsh reaction conditions; 2. Isobutane oxidation method, the typical process is ACRO and Texaco process, the products of these two processes have high added value and good economic benefits, but the reaction needs to be carried out under high temperature and high pressure, which requires high equipment, large investment costs, and great potential danger; 3. tert-butanol hydrogen peroxide method, Due to the low investment cost, it is the main method for domestic industrial production of tert-butyl hydroperoxide, but a large amount of acid-containing wastewater will be produced during the production process, which seriously pollutes the environment. Patent CN104262222A reports a method for preparing tert-butyl hydroperoxide by biomimetic catalytic oxidation of isobutane. This reaction can be carried out under relatively mild and safe conditions, and has great industrial value.
叔丁基过氧化氢合成工艺中存在一定量的二叔丁基过氧化物，目前的分离方法有化学萃取法和减压精馏法，化学萃取法分离效果不佳，会引入新的杂质，且产生大量的废液。由于两个组分的沸点十分接近，故采用减压精馏法也难以完全实现两者的分离。There is a certain amount of di-tert-butyl peroxide in the synthesis process of tert-butyl hydroperoxide. The current separation methods include chemical extraction and vacuum distillation. The separation effect of chemical extraction is not good, and new impurities will be introduced. And produce a large amount of waste liquid. Since the boiling points of the two components are very close, it is difficult to completely separate them by vacuum distillation.
为实现叔丁基过氧化氢合成工艺中叔丁基过氧化氢和二叔丁基过氧化物的完全分离，开发一种共沸分离叔丁基过氧化氢和二叔丁基过氧化物的精馏方法，其对于实现叔丁基过氧化氢产业化具有重要的意义。In order to realize the complete separation of tert-butyl hydroperoxide and di-tert-butyl peroxide in the synthesis process of tert-butyl hydroperoxide, a kind of azeotropic separation of tert-butyl hydroperoxide and di-tert-butyl peroxide was developed The rectification method is of great significance for realizing the industrialization of tert-butyl hydroperoxide.
发明内容Contents of the invention
本发明的目的在于克服现有技术的不足，提供一种分离效率高，纯度高的叔丁基过氧化氢的分离方法。The object of the invention is to overcome the deficiencies in the prior art, and a kind of separation efficiency is high, the separation method of the high-purity tert-butyl hydroperoxide is provided.
为实现上述目的，本发明采用的技术方案是：In order to achieve the above object, the technical scheme adopted in the present invention is:
一种叔丁基过氧化氢的分离方法，在叔丁基过氧化氢和二叔丁基过氧化物的混合液中加入共沸剂，该共沸剂能与二叔丁基过氧化物形成共沸物，再通过精馏实现叔丁基过氧化氢和二叔丁基过氧化物的完全分离。A method for separating tert-butyl hydroperoxide, adding an entrainer to the mixture of tert-butyl hydroperoxide and di-tert-butyl peroxide, the entrainer can form di-tert-butyl peroxide Azeotrope, and then complete separation of tert-butyl hydroperoxide and di-tert-butyl peroxide through rectification.
在上述的分离方法中，作为优选的，包括如下步骤：将叔丁基过氧化氢和二叔丁基过氧化物的混合液与共沸剂混合，先预热后通过进料口进入精馏塔，通过精馏分离后，塔顶气相产物经过冷凝器冷凝得二叔丁基过氧化物和共沸剂形成的共沸物，其中一部分经过回流返回塔顶，另一部分从精馏塔的出料口采出；塔釜液相产物为叔丁基过氧化氢产品，其中一部分经过再沸器返回塔釜，另一部分从精馏塔的出料口采出。In the above-mentioned separation method, preferably, the following steps are included: mixing the mixed solution of tert-butyl hydroperoxide and di-tert-butyl peroxide with an entrainer, preheating and then entering the rectification tower through the feed port , after being separated by rectification, the gas phase product at the top of the tower is condensed by a condenser to obtain an azeotrope formed by di-tert-butyl peroxide and an entrainer, a part of which is returned to the top of the tower through reflux, and the other part is discharged from the rectification tower The liquid phase product of the tower still is a tert-butyl hydroperoxide product, a part of which returns to the tower still through a reboiler, and another part is taken out from the outlet of the rectifying tower.
在上述的分离方法中，作为优选的，所述的共沸剂为叔丁醇，添加量为32~38 kg/h。In the above separation method, preferably, the entrainer is tert-butanol, and the addition amount is 32-38 kg/h.
在上述的分离方法中，作为优选的，所述的预热是指预热到温度为25~30℃。In the above separation method, preferably, the preheating refers to preheating to a temperature of 25-30°C.
在上述的分离方法中，作为优选的，所述的精馏塔的理论塔板数为30~50块，进料口所在的进料板位置为第7~12块。In the above separation method, preferably, the number of theoretical plates of the rectification column is 30-50, and the position of the feed plate where the feed inlet is located is the 7th-12th plate.
在上述的分离方法中，作为优选的，所述的塔釜温度38.3~58.6℃，塔釜压力为6~18 KPa。In the above separation method, preferably, the temperature of the tower bottom is 38.3-58.6° C., and the pressure of the tower bottom is 6-18 KPa.
在上述的分离方法中，作为优选的，所述的回流的摩尔比为1.9~2.7：1。In the above separation method, preferably, the molar ratio of the reflux is 1.9-2.7:1.
与现有技术相比，本发明具有如下有益效果：本发明采用共沸精馏方法分离叔丁基过氧化氢和二叔丁基过氧化物，经分离提纯后，叔丁基过氧化氢的纯度可达99%以上；分离效率高，收率高，工艺简单。Compared with the prior art, the present invention has the following beneficial effects: the present invention adopts azeotropic distillation method to separate tert-butyl hydroperoxide and di-tert-butyl peroxide, after separation and purification, the tert-butyl hydroperoxide The purity can reach more than 99%; the separation efficiency is high, the yield is high, and the process is simple.
具体实施方式Detailed ways
本发明用以下实施例说明，但本发明并不限于下述实施例。通过三个实施例，对本发明所提供的方法进行进一步说明。The present invention is illustrated by the following examples, but the invention is not limited to the following examples. Through three examples, the method provided by the present invention is further described.
实施例1Example 1
将本发明方法用于叔丁基过氧化氢和二叔丁基过氧化物的分离过程。混合液的处理量为50 kg/h，其中叔丁基过氧化氢的质量分数为60%，二叔丁基过氧化物的质量分数为40%。添加叔丁醇35 kg/h，将叔丁基过氧化氢和二叔丁基过氧化物的混合液与共沸剂叔丁醇混合，先预热后通过进料口进入精馏塔，通过精馏分离后，塔顶气相产物经过冷凝器冷凝得二叔丁基过氧化物和共沸剂形成的共沸物，其中一部分经过回流返回塔顶，另一部分从精馏塔的出料口采出；塔釜液相产物为叔丁基过氧化氢产品，其中一部分经过再沸器返回塔釜，另一部分从精馏塔的出料口采出。其中进料温度为30℃，进料压力为18 KPa，进料口的进料板位置为第7块，控制回流比为1.9，控制塔釜温度50.3℃，塔釜压力为11 KPa，塔釜采出产叔丁基过氧化氢品中二叔丁基过氧化物的含量为58 ppm，叔丁基过氧化氢的收率为100%。The method of the present invention is used for the separation process of tert-butyl hydroperoxide and di-tert-butyl peroxide. The treatment capacity of the mixed liquid is 50 kg/h, the mass fraction of tert-butyl hydroperoxide is 60%, and the mass fraction of di-tert-butyl peroxide is 40%. Add 35 kg/h of tert-butyl alcohol, mix the mixed solution of tert-butyl hydroperoxide and di-tert-butyl peroxide with the entrainer tert-butanol, preheat and then enter the rectification tower through the feed port, pass through the rectifying After separation by distillation, the gas phase product at the top of the tower is condensed by a condenser to obtain an azeotrope formed by di-tert-butyl peroxide and an entrainer, part of which is returned to the top of the tower through reflux, and the other part is extracted from the outlet of the rectification tower ; The liquid phase product of the tower still is the tert-butyl hydroperoxide product, wherein a part returns to the tower still through the reboiler, and another part is extracted from the outlet of the rectifying tower. Among them, the feed temperature is 30°C, the feed pressure is 18 KPa, the position of the feed plate of the feed inlet is the seventh block, the reflux ratio is controlled to be 1.9, the temperature of the tower kettle is controlled to be 50.3°C, and the pressure of the tower kettle is 11 KPa. The content of di-tert-butyl peroxide in the produced tert-butyl hydroperoxide product is 58 ppm, and the yield of tert-butyl hydroperoxide is 100%.
实施例2Example 2
将本发明方法用于叔丁基过氧化氢和二叔丁基过氧化物的分离过程。混合液的处理量为50 kg/h，其中叔丁基过氧化氢的质量分数为70%，二叔丁基过氧化物的质量分数为30%。添加叔丁醇32 kg/h，将叔丁基过氧化氢和二叔丁基过氧化物的混合液与共沸剂叔丁醇混合，先预热后通过进料口进入精馏塔，通过精馏分离后，塔顶气相产物经过冷凝器冷凝得二叔丁基过氧化物和共沸剂形成的共沸物，其中一部分经过回流返回塔顶，另一部分从精馏塔的出料口采出；塔釜液相产物为叔丁基过氧化氢产品，其中一部分经过再沸器返回塔釜，另一部分从精馏塔的出料口采出。其中进料温度为25℃，进料压力为6 KPa，进料口的进料板位置为第8块，控制回流比为2.2，控制塔釜温度38.3℃，塔釜压力为6 KPa，塔釜采出产叔丁基过氧化氢品中二叔丁基过氧化物的含量为38 ppm，叔丁基过氧化氢的收率为100%。The method of the present invention is used for the separation process of tert-butyl hydroperoxide and di-tert-butyl peroxide. The treatment capacity of the mixed liquid is 50 kg/h, the mass fraction of tert-butyl hydroperoxide is 70%, and the mass fraction of di-tert-butyl peroxide is 30%. Add 32 kg/h of tert-butyl alcohol, mix the mixed solution of tert-butyl hydroperoxide and di-tert-butyl peroxide with the entrainer tert-butanol, enter the rectification tower through the feed port after preheating first, pass through the rectifying After separation by distillation, the gas phase product at the top of the tower is condensed by a condenser to obtain an azeotrope formed by di-tert-butyl peroxide and an entrainer, part of which is returned to the top of the tower through reflux, and the other part is extracted from the outlet of the rectification tower ; The liquid phase product of the tower still is the tert-butyl hydroperoxide product, wherein a part returns to the tower still through the reboiler, and another part is extracted from the outlet of the rectifying tower. Among them, the feed temperature is 25°C, the feed pressure is 6 KPa, the position of the feed plate of the feed inlet is the 8th block, the reflux ratio is controlled to be 2.2, the temperature of the tower kettle is controlled to be 38.3°C, the pressure of the tower kettle is 6 KPa, the tower kettle The content of di-tert-butyl peroxide in the produced tert-butyl hydroperoxide product is 38 ppm, and the yield of tert-butyl hydroperoxide is 100%.
实施例3Example 3
将本发明方法用于叔丁基过氧化氢和二叔丁基过氧化物的分离过程。混合液的处理量为50 kg/h，其中叔丁基过氧化氢的质量分数为80%，二叔丁基过氧化物的质量分数为20%。添加叔丁醇38 kg/h，叔丁基过氧化氢和二叔丁基过氧化物的混合液与共沸剂叔丁醇混合，先预热后通过进料口进入精馏塔，通过精馏分离后，塔顶气相产物经过冷凝器冷凝得二叔丁基过氧化物和共沸剂形成的共沸物，其中一部分经过回流返回塔顶，另一部分从精馏塔的出料口采出；塔釜液相产物为叔丁基过氧化氢产品，其中一部分经过再沸器返回塔釜，另一部分从精馏塔的出料口采出。其中进料温度为30℃，进料压力为18 KPa，进料口的进料板位置为第12块，控制回流比为2.7，控制塔釜温度58.6℃，塔釜压力为18 KPa，塔釜采出产叔丁基过氧化氢品中二叔丁基过氧化物的含量为25 ppm，叔丁基过氧化氢的收率为100%。The method of the present invention is used for the separation process of tert-butyl hydroperoxide and di-tert-butyl peroxide. The treatment capacity of the mixed liquid is 50 kg/h, the mass fraction of tert-butyl hydroperoxide is 80%, and the mass fraction of di-tert-butyl peroxide is 20%. Add 38 kg/h of tert-butyl alcohol, mix the mixture of tert-butyl hydroperoxide and di-tert-butyl peroxide with the entrainer tert-butanol, preheat and then enter the rectification tower through the feed port, and pass through the rectification After separation, the gas phase product at the top of the tower is condensed by a condenser to obtain an azeotrope formed by di-tert-butyl peroxide and an entrainer, a part of which is returned to the top of the tower through reflux, and the other part is extracted from the outlet of the rectifying tower; The liquid phase product in the tower bottom is a tert-butyl hydroperoxide product, a part of which is returned to the tower bottom through a reboiler, and the other part is extracted from the outlet of the rectifying tower. Among them, the feed temperature is 30°C, the feed pressure is 18 KPa, the position of the feed plate of the feed inlet is the 12th block, the reflux ratio is controlled to be 2.7, the temperature of the tower kettle is controlled to be 58.6°C, and the pressure of the tower kettle is 18 KPa. The content of di-tert-butyl peroxide in the produced tert-butyl hydroperoxide product is 25 ppm, and the yield of tert-butyl hydroperoxide is 100%.
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| FR3091280B1 (en) * | 2018-12-26 | 2021-06-25 | Arkema France | PURIFICATION OF ALKYL HYDROPEROXIDE BY EXTRACTIVE DISTILLATION |
| FR3091283B1 (en) * | 2018-12-26 | 2021-06-25 | Arkema France | PURIFICATION OF ALKYL HYDROPEROXIDE BY DISTILLATION IN THE PRESENCE OF METHANOL AND WATER |
| CN112300044A (en) * | 2019-12-06 | 2021-02-02 | 广东中准新材料科技有限公司 | Synthesis and purification method of high-purity tert-butyl peroxy-2-ethylhexyl carbonate |
| CN112300045A (en) * | 2019-12-06 | 2021-02-02 | 广东中准新材料科技有限公司 | Synthesis and purification method of high-purity tert-amyl peroxy-2-ethylhexyl carbonate |
| CN112159343A (en) * | 2020-10-26 | 2021-01-01 | 北京水木滨华科技有限公司 | Purification method of tert-butyl hydroperoxide |
| CN112300046A (en) * | 2020-11-27 | 2021-02-02 | 信汇科技有限公司 | Purification method of tert-butyl hydroperoxide and recycling method of tert-butyl alcohol |
| CN112375025A (en) * | 2020-11-27 | 2021-02-19 | 信汇科技有限公司 | Purification method of tert-butyl hydroperoxide |
| CN115850143A (en) * | 2022-12-26 | 2023-03-28 | 兰州助剂厂有限责任公司 | A method for removing light components from tert-butyl hydroperoxide |
| CN118271221A (en) * | 2024-06-04 | 2024-07-02 | 优耐德引发剂(淮北)有限公司 | Process method for constant boiling rectification and purification of tert-butyl hydroperoxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105523982A (en) * | 2014-10-23 | 2016-04-27 | 茅海强 | Method for preparing tert-butyl hydroperoxide |
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| CN105523982A (en) * | 2014-10-23 | 2016-04-27 | 茅海强 | Method for preparing tert-butyl hydroperoxide |
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| Title |
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| New method for preparation of 9,10-phenanthrenequinone;Saito, Yoshinori等;《Aromatikkusu》;19871031;第202页 * |
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Effective date of registration: 20250219 Address after: Zuohukou District, Zhenjiang City, Jiangsu Province, 2016 Patentee after: JIANGSU ZHONGJIANG MATERIALS TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. Country or region after: China Address before: 516081 room 205, building a, R & D building, No.5, Keji Road, science and Technology Innovation Park, Dayawan West District, Huizhou City, Guangdong Province Patentee before: HUIZHOU RESEARCH INSTITUTE, SUN YAT-SEN University Country or region before: China |