CN103113184B - Tetrachloroethylene production device and method - Google Patents
Tetrachloroethylene production device and method Download PDFInfo
- Publication number
- CN103113184B CN103113184B CN201310071626.7A CN201310071626A CN103113184B CN 103113184 B CN103113184 B CN 103113184B CN 201310071626 A CN201310071626 A CN 201310071626A CN 103113184 B CN103113184 B CN 103113184B
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- CN
- China
- Prior art keywords
- chlorination reactor
- chlorine
- zellon
- level
- separation column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 20
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 title abstract 7
- 229950011008 tetrachloroethylene Drugs 0.000 title abstract 7
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 72
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 43
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000460 chlorine Substances 0.000 claims abstract description 37
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 37
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 35
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229960001701 chloroform Drugs 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims description 19
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000470 constituent Substances 0.000 claims description 14
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 13
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 13
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 claims description 7
- 239000002075 main ingredient Substances 0.000 claims description 7
- 238000005194 fractionation Methods 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 230000008569 process Effects 0.000 abstract description 10
- 239000000047 product Substances 0.000 abstract description 8
- 239000006227 byproduct Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a tetrachloroethylene production device and a tetrachloroethylene production method. The tetrachloroethylene production device comprises a first-stage chlorination reactor, a second-stage chlorination reactor, a cooling washing tower, a condenser, a hydrochloric acid absorbing tower, a fractionating tower and a rectifying tower, wherein chlorine and chloride methane material pipelines are arranged on the first-stage chlorination reactor; dichloromethane and trichloromethane material pipelines are arranged on the second-stage chlorination reactor. According to the tetrachloroethylene production device, the second-stage chlorination reactor is arranged additionally; after the dichloromethane and the trichloromethane are filled in the second-stage chlorination reactor, the excess chlorine in the outlet gas of the first-stage chlorination reactor is converted completely; and the rest of dichloromethane and trichloromethane are fractionated to return into the first-stage chlorination reactor to be used. The tetrachloroethylene production device can completely convert the chlorine, so that the processes for recovering the chlorine are reduced, and the investment cost and the operating cost are reduced. When the tetrachloroethylene is produced, the operation of lowering the chlorine ratio or increasing the reaction temperature is not required, so that the product yield is high and the byproduct quantity is low.
Description
Technical field
The present invention relates to a kind of zellon production equipment and method, particularly a kind of thermal chlorination zellon production equipment and method.
Background technology
Domestic existing thermal chlorination zellon production equipment technical process is as shown in Figure 1: chlorine mixes with monochloro methane and adds thinner (trichloromethane or tetracol phenixin) again and mix, enter chlorination reactor, at 570 DEG C of degree left and right temperature, reaction generates zellon and hydrogenchloride, because reaction was chlorine reaction, in chlorination reactor exit gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride and excessive chlorine; Chlorination reactor exit gas through after operation cooling, condensation obtains thick chlorated liquid, the fractionation in separation column of thick chlorated liquid, light constituent returns chlorination reactor, and heavy constituent rectifying in rectifying tower obtains zellon product; The hydrogenchloride be not condensed after condenser condenses and chlorine, then be hydrochloric acid through hydrochloric acid absorption tower by hydrogen chloride absorption, turn back to chlorination reactor after remaining chlorine drying, pressurization.
Because this technique only has one-level chlorination reactor, and be chlorine excessive response, chlorine excessive in chlorination reactor exit gas brings rear operation into, and excessive chlorine is oversize to the operational path reclaimed: one is that equipment material requirement is high, and investment cost is large; Two is that operation easier is larger; Three is that security risk is large; Four is that plant running cost is higher.But all transform than by chlorine if reduce chlorine, zellon turnover ratio can be caused to reduce, product yield reduces; If improve temperature of reaction all to be transformed by chlorine, by-product perchloride can be caused again to increase.
Summary of the invention
In view of this, the invention provides a kind of zellon production equipment and method, chlorine all can be transformed, decrease and reclaim chlorine technical process, and product yield is high, by product is low.
The invention discloses a kind of zellon production equipment, comprise one-level chlorination reactor, secondary chlorination reactor, cooling washing tower, condenser, hydrochloric acid absorption tower, separation column and rectifying tower, described one-level chlorination reactor, secondary chlorination reactor, cooling washing tower is communicated with successively with condenser, described one-level chlorination reactor is provided with chlorine and monochloro methane feed conduit, described secondary chlorination reactor is provided with methylene dichloride and trichloromethane feed conduit, the pneumatic outlet of described condenser is communicated with hydrochloric acid absorption tower, the liquid exit of condenser is communicated with separation column, the light fraction outlet of described separation column is communicated with one-level chlorination reactor, the heavy constituent outlet of separation column is communicated with rectifying tower.
The invention also discloses the method using above-mentioned zellon production equipment to carry out zellon production, the light constituent that chlorine, monochloro methane and separation column return reacts in one-level chlorination reactor, and in one-level chlorination reactor exit gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride and excessive chlorine; One-level chlorination reactor exit gas, methylene dichloride and trichloromethane react in secondary chlorination reactor, all transformed by excessive chlorine in one-level chlorination reactor exit gas, in secondary chlorination reactor outlet gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride, methylene dichloride and trichloromethane; Secondary chlorination reactor outlet gas obtains thick chlorated liquid after cooling, condensation, the fractionation in separation column of thick chlorated liquid, light constituent returns one-level chlorination reactor, and heavy constituent rectifying in rectifying tower obtains zellon product, and the hydrogenchloride be not condensed is absorbed as hydrochloric acid through hydrochloric acid absorption tower.
Further, the temperature of reaction in described one-level chlorination reactor is 500 ~ 600 DEG C.
Further, the temperature of reaction in described secondary chlorination reactor is 350 ~ 450 DEG C.
Beneficial effect of the present invention is: invention increases a secondary chlorination reactor, methylene dichloride and trichloromethane is passed in secondary chlorination reactor, make it all be transformed by excessive chlorine in one-level chlorination reactor exit gas, and remaining methylene dichloride and trichloromethane utilize by returning one-level chlorination reactor after fractionation again; Therefore, chlorine can all transform by the present invention, decrease and reclaim chlorine technical process, make that technical process is simple, easy to operate, security is high, decrease cost of investment and running cost, and the present invention without the need to reducing chlorine ratio or improving temperature of reaction, makes that product yield is high, by product is low when producing zellon.
Accompanying drawing explanation
In order to make the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the present invention is described in further detail, wherein:
Fig. 1 is the process flow sheet of existing zellon production equipment;
Fig. 2 is the process flow sheet of zellon production equipment of the present invention.
Embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.
Fig. 2 is the process flow sheet of zellon production equipment of the present invention, as shown in the figure, zellon production equipment of the present invention, comprise one-level chlorination reactor, secondary chlorination reactor, cooling washing tower, condenser, hydrochloric acid absorption tower, separation column and rectifying tower, described one-level chlorination reactor, secondary chlorination reactor, cooling washing tower is communicated with successively with condenser, described one-level chlorination reactor is provided with chlorine and monochloro methane feed conduit, described secondary chlorination reactor is provided with methylene dichloride and trichloromethane feed conduit, the pneumatic outlet of described condenser is communicated with hydrochloric acid absorption tower, the liquid exit of condenser is communicated with separation column, the light fraction outlet of described separation column is communicated with one-level chlorination reactor, the heavy constituent outlet of separation column is communicated with rectifying tower.
Zellon production method of the present invention, the light constituent (methylene dichloride, trichloromethane and tetracol phenixin) that chlorine, monochloro methane and separation column return reacts in one-level chlorination reactor, and in one-level chlorination reactor exit gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride and excessive chlorine; One-level chlorination reactor exit gas, methylene dichloride and trichloromethane react in secondary chlorination reactor, all transformed by excessive chlorine in one-level chlorination reactor exit gas, in secondary chlorination reactor outlet gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride, methylene dichloride and trichloromethane; Secondary chlorination reactor outlet gas obtains thick chlorated liquid after cooling, condensation, the fractionation in separation column of thick chlorated liquid, light constituent (methylene dichloride, trichloromethane and tetracol phenixin) returns one-level chlorination reactor, heavy constituent rectifying in rectifying tower obtains zellon product, and the hydrogenchloride be not condensed is absorbed as hydrochloric acid through hydrochloric acid absorption tower.
In the present invention, the temperature of reaction in described one-level chlorination reactor is 500 ~ 600 DEG C, preferably 570 DEG C; Temperature of reaction in described secondary chlorination reactor is 350 ~ 450 DEG C, preferably 400 DEG C.
Chlorine can all transform by the present invention, decrease and reclaim chlorine technical process, make that technical process is simple, easy to operate, security is high, decrease cost of investment and running cost, and the present invention without the need to reducing chlorine ratio or improving temperature of reaction, makes that product yield is high, by product is low when producing zellon.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by referring to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, various change can be made to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (4)
1. a zellon production equipment, it is characterized in that: comprise one-level chlorination reactor, secondary chlorination reactor, cooling washing tower, condenser, hydrochloric acid absorption tower, separation column and rectifying tower, described one-level chlorination reactor, secondary chlorination reactor, cooling washing tower is communicated with successively with condenser, described one-level chlorination reactor is provided with chlorine and monochloro methane feed conduit, described secondary chlorination reactor is provided with methylene dichloride and trichloromethane feed conduit, the pneumatic outlet of described condenser is communicated with hydrochloric acid absorption tower, the liquid exit of condenser is communicated with separation column, the light fraction outlet of described separation column is communicated with one-level chlorination reactor, the heavy constituent outlet of separation column is communicated with rectifying tower.
2. use the zellon production equipment described in claim 1 to carry out the method for zellon production, it is characterized in that: the light constituent that chlorine, monochloro methane and separation column return reacts in one-level chlorination reactor, in one-level chlorination reactor exit gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride and excessive chlorine; One-level chlorination reactor exit gas, methylene dichloride and trichloromethane react in secondary chlorination reactor, all transformed by excessive chlorine in one-level chlorination reactor exit gas, in secondary chlorination reactor outlet gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride, methylene dichloride and trichloromethane; Secondary chlorination reactor outlet gas obtains thick chlorated liquid after cooling, condensation, the fractionation in separation column of thick chlorated liquid, light constituent returns one-level chlorination reactor, and heavy constituent rectifying in rectifying tower obtains zellon product, and the hydrogenchloride be not condensed is absorbed as hydrochloric acid through hydrochloric acid absorption tower.
3. the method for zellon production according to claim 2, is characterized in that: the temperature of reaction in described one-level chlorination reactor is 500 ~ 600 DEG C.
4. the method for zellon production according to claim 2, is characterized in that: the temperature of reaction in described secondary chlorination reactor is 350 ~ 450 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310071626.7A CN103113184B (en) | 2013-03-07 | 2013-03-07 | Tetrachloroethylene production device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310071626.7A CN103113184B (en) | 2013-03-07 | 2013-03-07 | Tetrachloroethylene production device and method |
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| Publication Number | Publication Date |
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| CN103113184A CN103113184A (en) | 2013-05-22 |
| CN103113184B true CN103113184B (en) | 2014-12-24 |
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| CN201310071626.7A Expired - Fee Related CN103113184B (en) | 2013-03-07 | 2013-03-07 | Tetrachloroethylene production device and method |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787823B (en) * | 2014-02-28 | 2015-04-08 | 重庆海洲化学品有限公司 | Method for recovering organic chloride from rectification residues of methane chloride or/and tetrachloroethylene |
| CN104587810B (en) * | 2014-12-26 | 2017-06-20 | 浙江林江化工股份有限公司 | A kind of method of comprehensive utilization of the chlorination tail gas of itrated compound |
| CN117776860A (en) * | 2024-02-28 | 2024-03-29 | 山东新龙科技股份有限公司 | Method and device for co-producing trichloroethylene and tetrachloroethylene |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503336B (en) * | 2009-03-06 | 2013-03-13 | 刘世刚 | Improved methane chloride production process |
| CN101891584B (en) * | 2010-07-20 | 2013-06-05 | 自贡鸿鹤化工股份有限公司 | Preparation method of tetrachloroethylene |
| CN102816046A (en) * | 2012-08-13 | 2012-12-12 | 自贡鸿鹤化工股份有限公司 | Industrial preparation method for tetrachloroethylene |
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| CN103113184A (en) | 2013-05-22 |
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Granted publication date: 20141224 |