CN103113184A - Tetrachloroethylene production device and method - Google Patents
Tetrachloroethylene production device and method Download PDFInfo
- Publication number
- CN103113184A CN103113184A CN2013100716267A CN201310071626A CN103113184A CN 103113184 A CN103113184 A CN 103113184A CN 2013100716267 A CN2013100716267 A CN 2013100716267A CN 201310071626 A CN201310071626 A CN 201310071626A CN 103113184 A CN103113184 A CN 103113184A
- Authority
- CN
- China
- Prior art keywords
- chlorination reactor
- zellon
- chlorine
- 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 20
- 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 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
- 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
- 239000000470 constituent Substances 0.000 claims description 17
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 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
- 239000002994 raw material Substances 0.000 claims description 6
- 238000005194 fractionation Methods 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 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
- 238000011084 recovery Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
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- 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) to mix again, enter chlorination reactor, spend reaction generation zellon and hydrogenchloride at the temperature of left and right at 570 ℃, because reaction was the chlorine reaction, in the chlorination reactor exit gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride and excessive chlorine; The chlorination reactor exit gas through after cooling, the condensation of operation obtain thick chlorated liquid, thick chlorated liquid fractionation in separation column, light constituent returns to chlorination reactor, heavy constituent rectifying in rectifying tower obtains the zellon product; The hydrogenchloride that is not condensed after condenser condenses and chlorine, then be hydrochloric acid through hydrochloric acid absorption tower with hydrogen chloride absorption, turn back to chlorination reactor after remaining chlorine drying, pressurization.
Because this technique only has the one-level chlorination reactor, and be the chlorine excessive response, in the chlorination reactor exit gas, excessive chlorine is brought rear operation into, and excessive chlorine is oversize to the operational path that reclaims: the one, and the equipment material requirement is high, and investment cost is large; The 2nd, operation easier is larger; The 3rd, security risk is large; The 4th, device running cost is higher.But, all transform than with chlorine if reduce chlorine, can cause the zellon turnover ratio to reduce, product yield reduces; If improve temperature of reaction, chlorine is all transformed, can cause again the by-product perchloride 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, reduced the technical process of recovery chlorine, and product yield is high, by product is low.
the invention discloses a kind of zellon production equipment, comprise the one-level chlorination reactor, the secondary chlorination reactor, cooling washing tower, condenser, hydrochloric acid absorption tower, separation column and rectifying tower, described one-level chlorination reactor, the secondary chlorination reactor, cooling washing tower and condenser are communicated with successively, described one-level chlorination reactor is provided with chlorine and monochloro methane raw material pipeline, described secondary chlorination reactor is provided with methylene dichloride and trichloromethane raw material pipeline, 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 constituent outlet of described separation column is communicated with the one-level chlorination reactor, the heavy constituent outlet of separation column is communicated with rectifying tower.
The invention also discloses and use above-mentioned zellon production equipment to carry out the method that zellon is produced, the light constituent that chlorine, monochloro methane and separation column return is at one-level chlorination reactor internal reaction, 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 are at secondary chlorination reactor internal reaction, excessive chlorine in one-level chlorination reactor exit gas is all transformed, and in the secondary chlorination reactor outlet gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride, methylene dichloride and trichloromethane; The secondary chlorination reactor outlet gas obtains thick chlorated liquid after cooling, condensation, thick chlorated liquid fractionation in separation column, light constituent returns to the one-level chlorination reactor, and heavy constituent rectifying in rectifying tower obtains the zellon product, and the hydrogenchloride that is 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 ℃.
Further, the temperature of reaction in described secondary chlorination reactor is 350 ~ 450 ℃.
Beneficial effect of the present invention is: the present invention has increased a secondary chlorination reactor, pass into methylene dichloride and trichloromethane in the secondary chlorination reactor, it is all transformed excessive chlorine in one-level chlorination reactor exit gas, and remaining methylene dichloride and trichloromethane return to the utilization of one-level chlorination reactor after by fractionation again; Therefore, the present invention can all transform chlorine, reduced the technical process of recovery chlorine, make technical process simple, easy to operate, safe, cost of investment and running cost have been reduced, and the present invention need not to reduce when producing zellon chlorine than or improve temperature of reaction, make that product yield is high, by product is low.
Description of drawings
In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention is described in further detail below in conjunction with accompanying drawing, 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 the one-level chlorination reactor, the secondary chlorination reactor, cooling washing tower, condenser, hydrochloric acid absorption tower, separation column and rectifying tower, described one-level chlorination reactor, the secondary chlorination reactor, cooling washing tower and condenser are communicated with successively, described one-level chlorination reactor is provided with chlorine and monochloro methane raw material pipeline, described secondary chlorination reactor is provided with methylene dichloride and trichloromethane raw material pipeline, 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 constituent outlet of described separation column is communicated with the 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 that chlorine, monochloro methane and separation column return (methylene dichloride, trichloromethane and tetracol phenixin) is at one-level chlorination reactor internal reaction, 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 are at secondary chlorination reactor internal reaction, excessive chlorine in one-level chlorination reactor exit gas is all transformed, and in the secondary chlorination reactor outlet gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride, methylene dichloride and trichloromethane; The secondary chlorination reactor outlet gas obtains thick chlorated liquid after cooling, condensation, thick chlorated liquid fractionation in separation column, light constituent (methylene dichloride, trichloromethane and tetracol phenixin) returns to the one-level chlorination reactor, heavy constituent rectifying in rectifying tower obtains the zellon product, and the hydrogenchloride that is 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 ℃, preferred 570 ℃; Temperature of reaction in described secondary chlorination reactor is 350 ~ 450 ℃, preferred 400 ℃.
The present invention can all transform chlorine, reduced the technical process of recovery chlorine, make technical process simple, easy to operate, safe, cost of investment and running cost have been reduced, and the present invention need not to reduce when producing zellon chlorine than or improve temperature of reaction, make that product yield is high, by product is low.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by invention has been described with reference to the preferred embodiments of the present invention, but those of ordinary skill in the art is to be understood that, can make various changes 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. zellon production equipment, it is characterized in that: comprise the one-level chlorination reactor, the secondary chlorination reactor, cooling washing tower, condenser, hydrochloric acid absorption tower, separation column and rectifying tower, described one-level chlorination reactor, the secondary chlorination reactor, cooling washing tower and condenser are communicated with successively, described one-level chlorination reactor is provided with chlorine and monochloro methane raw material pipeline, described secondary chlorination reactor is provided with methylene dichloride and trichloromethane raw material pipeline, 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 constituent outlet of described separation column is communicated with the one-level chlorination reactor, the heavy constituent outlet of separation column is communicated with rectifying tower.
2. right to use requires 1 described zellon production equipment to carry out the method that zellon is produced, it is characterized in that: the light constituent that chlorine, monochloro methane and separation column return is at one-level chlorination reactor internal reaction, 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 are at secondary chlorination reactor internal reaction, excessive chlorine in one-level chlorination reactor exit gas is all transformed, and in the secondary chlorination reactor outlet gas, main ingredient comprises zellon, tetracol phenixin, hexachloroethane, hydrogenchloride, methylene dichloride and trichloromethane; The secondary chlorination reactor outlet gas obtains thick chlorated liquid after cooling, condensation, thick chlorated liquid fractionation in separation column, light constituent returns to the one-level chlorination reactor, and heavy constituent rectifying in rectifying tower obtains the zellon product, and the hydrogenchloride that is not condensed is absorbed as hydrochloric acid through hydrochloric acid absorption tower.
3. the zellon according to claim 2 method of producing, it is characterized in that: the temperature of reaction in described one-level chlorination reactor is 500 ~ 600 ℃.
4. the zellon according to claim 2 method of producing, it is characterized in that: the temperature of reaction in described secondary chlorination reactor is 350 ~ 450 ℃.
Priority Applications (1)
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CN201310071626.7A CN103113184B (en) | 2013-03-07 | 2013-03-07 | Tetrachloroethylene production device and method |
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CN201310071626.7A CN103113184B (en) | 2013-03-07 | 2013-03-07 | Tetrachloroethylene production device and method |
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CN103113184A true CN103113184A (en) | 2013-05-22 |
CN103113184B CN103113184B (en) | 2014-12-24 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103787823A (en) * | 2014-02-28 | 2014-05-14 | 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 |
CN104587810A (en) * | 2014-12-26 | 2015-05-06 | 浙江林江化工股份有限公司 | Comprehensive utilization method of chlorination tail gas of nitrides |
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 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101503336A (en) * | 2009-03-06 | 2009-08-12 | 刘世刚 | Improved methane chloride production process |
CN101891584A (en) * | 2010-07-20 | 2010-11-24 | 陈开华 | 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 |
-
2013
- 2013-03-07 CN CN201310071626.7A patent/CN103113184B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101503336A (en) * | 2009-03-06 | 2009-08-12 | 刘世刚 | Improved methane chloride production process |
CN101891584A (en) * | 2010-07-20 | 2010-11-24 | 陈开华 | 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 |
Non-Patent Citations (1)
Title |
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张艳梅 等: ""四氯乙烯的生产和应用"", 《中国氯碱》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103787823A (en) * | 2014-02-28 | 2014-05-14 | 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 |
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 |
CN104587810A (en) * | 2014-12-26 | 2015-05-06 | 浙江林江化工股份有限公司 | Comprehensive utilization method of chlorination tail gas of nitrides |
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 |
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CN103113184B (en) | 2014-12-24 |
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Granted publication date: 20141224 |