CN102059053B - Process for absorbing tail gas in process for preparing chlorocyclohexane by cyclohexane method by high-salt wastewater - Google Patents
Process for absorbing tail gas in process for preparing chlorocyclohexane by cyclohexane method by high-salt wastewater Download PDFInfo
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- CN102059053B CN102059053B CN 201010550424 CN201010550424A CN102059053B CN 102059053 B CN102059053 B CN 102059053B CN 201010550424 CN201010550424 CN 201010550424 CN 201010550424 A CN201010550424 A CN 201010550424A CN 102059053 B CN102059053 B CN 102059053B
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- chlorocyclohexane
- tail gas
- sodium chloride
- hydrochloric acid
- cyclohexane
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Abstract
The invention relates to a process for absorbing tail gas in a process for preparing chlorocyclohexane by a cyclohexane method by high-salt wastewater. The process is characterized in that high-concentration sodium chloride industrial wastewater instead of clean water is used as an absorbent. By the process, the tail gas, namely byproduct hydrochloric acid in the process for preparing the chlorocyclohexane by the cyclohexane method can be absorbed, high-concentration sodium chloride industrial wastewater is treated, byproduct industrial sodium chloride is prepared, material selecting difficulty of equipment for treating the high-concentration sodium chloride industrial wastewater is reduced, and the service life of the equipment is prolonged.
Description
Technical field
The invention belongs to field of fine chemical, particularly high-salt wastewater absorbs cyclohexane legal system chlorocyclohexane tail gas process.
Background technology
Chlorocyclohexane is a kind of base stock of organic synthesis, also is a kind of important fine chemical product.It is mainly used in the intermediate of the products such as rubber anti-chark agent CTP, medical artane, agricultural chemicals plictran; Also can be used for polyurethane foaming catalyst N, N-dimethyl cyclohexyl amine, antirust agent etc. synthetic.The preparation method of chlorocyclohexane has cyclohexene hydrogen chloride addition process, cyclohexane Chlorination process and cyclohexanol hydrogen chloride method of substitution etc., wherein the cyclohexane method is take cyclohexane and chlorine as raw material, a hydrogen atom on the chlorine atom substituted cyclohexane ring generates chlorocyclohexane and hydrochloric acid gas.Hydrochloric acid gas and the chlorine that overflows on a small quantity are discharged from as tail gas.Present production technology adopts the clear water absorption tail gas, forms technical hydrochloric acid.
Vulcanization accelerator NS, CBS, the technique waste water sodium chloride-containing that produces in the rubber anti-chark agent CTP production process reaches more than 10%, when sodium chloride concentration surpasses 1%, just can not use biochemical treatment process, so such waste water is a great problem in the wastewater treatment industry.The treatment technology that adopts at present has flocculence, oxidizing process, flocculation-absorption method and evaporation.The best genus evaporation for the treatment of effect wherein, but that the method expends quantity of steam is large, processing cost is high, and the method is at high temperature processed in addition, and high salt hot waste water is strong to the corrosion failure for the treatment of facility, and even if the titanium material, also be no more than 2 years its service life.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of high-salt wastewater to absorb cyclohexane legal system chlorocyclohexane tail gas process, and technical scheme of the present invention is as follows:
Process conditions according to the standby chlorocyclohexane of cyclohexane legal system are produced chlorocyclohexane, and the tail gas of generation absorbs under the little negative pressure of normal temperature with circulating absorption tower, it is characterized in that substituting clear water as absorbent with the sodium chloride industrial wastewater of high concentration.The industrial wastewater of sodium chloride-containing forms saliferous hydrochloric acid after absorbing hydrogen chloride gas, increase along with concentration of hydrochloric acid, sodium chloride can be separated out by mass crystallization, after concentration of hydrochloric acid is greater than 30%, the saliferous hydrochloric acid solution is squeezed into equipment for separating liquid from solid carry out Separation of Solid and Liquid, wherein liquid phase can be used as the technical hydrochloric acid use, and solid phase is crude product sodium chloride and organic impurities, becomes Nacl through further making with extra care.
Used absorbent can be the sodium chloride industrial wastewater of any high concentration among the present invention, such as vulcanization accelerator NS, CBS, and the technique waste water that produces in the rubber anti-chark agent CTP production process.
Circulation of tail gas of the present invention absorption tower operating condition normal temperature refers to 0～30 ℃, preferred 5～10 ℃.
Operating condition little negative pressure in circulation of tail gas of the present invention absorption tower refers to-500～-2000Pa, preferred-900～-1200Pa.
After adopting technique of the present invention, obtained following benefit:
1, absorbed the cyclohexane legal system for the tail gas in the chlorocyclohexane technique, by-product hydrochloric acid;
2, processed the sodium chloride industrial wastewater of high concentration;
3, the industrial sodium chloride of by-product.
4, reduce the selection difficulty of the sodium chloride industrial wastewater treatment device of high concentration, prolonged the service life of equipment.
The specific embodiment
The below elaborates to embodiments of the invention.
Pressure and the speed of chlorine according to process stipulation is passed in the reactor that cyclohexane is housed, reaction generates chlorocyclohexane and hydrochloric acid gas, hydrochloric acid gas and the chlorine that overflows are on a small quantity discharged reactor by exhaust port, by circulating absorption tower 5～10 ℃ temperature and-900～-pressure of 1200Pa absorbs, substitute clear water with the sodium chloride industrial wastewater of high concentration and make absorbent.The industrial wastewater of sodium chloride-containing forms saliferous hydrochloric acid after absorbing hydrogen chloride gas, increase along with concentration of hydrochloric acid, sodium chloride can be separated out by mass crystallization, after concentration of hydrochloric acid is greater than 30%, the saliferous hydrochloric acid solution is squeezed into equipment for separating liquid from solid carry out Separation of Solid and Liquid, wherein liquid phase can be used as the technical hydrochloric acid use, and solid phase is crude product sodium chloride, becomes Nacl through further making with extra care.
Be dissolved with a certain amount of sodium chloride in the hydrochloric acid that produces in above-described embodiment, the content of sodium chloride is different with the difference of concentration of hydrochloric acid, when concentration of hydrochloric acid is 30%, and the amount of sodium chloride-containing about 6.5%, when concentration of hydrochloric acid was 36%, sodium chloride content was almost nil.Therefore this hydrochloric acid can be used for salt or the alkali that titration contains sodium, such as titration Na
2S solution is produced H
2S gas carries out neutralization reaction etc. with NaOH solution.
Claims (4)
1. a high-salt wastewater absorbs cyclohexane legal system chlorocyclohexane tail gas process, process conditions according to the standby chlorocyclohexane of cyclohexane legal system are produced chlorocyclohexane, the tail gas that produces absorbs under the little negative pressure of normal temperature with circulating absorption tower, it is characterized in that substituting clear water as absorbent with the sodium chloride industrial wastewater of high concentration; The operating temperature of circulating absorption tower is controlled at 0～30 ℃; The operating pressure of circulating absorption tower is-500～-2000Pa; The industrial wastewater of sodium chloride-containing forms saliferous hydrochloric acid after absorbing hydrogen chloride gas, increase along with concentration of hydrochloric acid, sodium chloride can be separated out by mass crystallization, after concentration of hydrochloric acid is greater than 30%, the saliferous hydrochloric acid solution is squeezed into equipment for separating liquid from solid carry out Separation of Solid and Liquid, wherein liquid phase can be used as the technical hydrochloric acid use, and solid phase is crude product sodium chloride and organic impurities, becomes Nacl through further making with extra care.
2. high-salt wastewater according to claim 1 absorbs cyclohexane legal system chlorocyclohexane tail gas process, it is characterized in that used absorbent is the technique waste water that produces in vulcanization accelerator NS, CBS, the rubber anti-chark agent CTP production process.
3. high-salt wastewater according to claim 1 absorbs cyclohexane legal system chlorocyclohexane tail gas process, it is characterized in that the operating temperature of circulating absorption tower is controlled at 5～10 ℃.
4. high-salt wastewater according to claim 1 absorbs cyclohexane legal system chlorocyclohexane tail gas process, and the operating pressure that it is characterized in that circulating absorption tower is-900～-1200Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010550424 CN102059053B (en) | 2010-11-19 | 2010-11-19 | Process for absorbing tail gas in process for preparing chlorocyclohexane by cyclohexane method by high-salt wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010550424 CN102059053B (en) | 2010-11-19 | 2010-11-19 | Process for absorbing tail gas in process for preparing chlorocyclohexane by cyclohexane method by high-salt wastewater |
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| Publication Number | Publication Date |
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| CN102059053A CN102059053A (en) | 2011-05-18 |
| CN102059053B true CN102059053B (en) | 2013-02-13 |
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| CN 201010550424 Active CN102059053B (en) | 2010-11-19 | 2010-11-19 | Process for absorbing tail gas in process for preparing chlorocyclohexane by cyclohexane method by high-salt wastewater |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105506669B (en) * | 2016-01-05 | 2017-07-11 | 西南石油大学 | A kind of preparation method of chlorocyclohexane |
| CN110075669A (en) * | 2019-05-29 | 2019-08-02 | 湖南长宏新能源材料有限责任公司 | A kind of purification treatment of nonferrous smelting HCl exhaust gas and recycle technique |
| CN113582203A (en) * | 2021-08-23 | 2021-11-02 | 内蒙古东孚精细化学品有限公司 | Desalting device and method by using hydrochloric acid |
| CN115608135B (en) * | 2022-10-08 | 2023-05-12 | 湖北泰盛化工有限公司 | Self-consistent recycling treatment method for salt-containing wastewater and hydrochloric acid-containing waste gas |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1151968A (en) * | 1995-12-13 | 1997-06-18 | 广东省制盐工业设计研究所 | Crystallization technology for producing sodium chloride |
| CN101648104A (en) * | 2008-08-13 | 2010-02-17 | 北京格瑞华阳科技发展有限公司 | Technology for reclaiming hydrogen chloride tail gas in chemical production |
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- 2010-11-19 CN CN 201010550424 patent/CN102059053B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1151968A (en) * | 1995-12-13 | 1997-06-18 | 广东省制盐工业设计研究所 | Crystallization technology for producing sodium chloride |
| CN101648104A (en) * | 2008-08-13 | 2010-02-17 | 北京格瑞华阳科技发展有限公司 | Technology for reclaiming hydrogen chloride tail gas in chemical production |
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| CN102059053A (en) | 2011-05-18 |
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