CN101623614B - Chlorination reaction device - Google Patents
Chlorination reaction device Download PDFInfo
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- CN101623614B CN101623614B CN2009100130610A CN200910013061A CN101623614B CN 101623614 B CN101623614 B CN 101623614B CN 2009100130610 A CN2009100130610 A CN 2009100130610A CN 200910013061 A CN200910013061 A CN 200910013061A CN 101623614 B CN101623614 B CN 101623614B
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- draft tube
- inner draft
- chlorination reactor
- chlorination
- cylindrical shell
- Prior art date
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- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 15
- 239000000460 chlorine Substances 0.000 claims description 19
- 229910052801 chlorine Inorganic materials 0.000 claims description 16
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 15
- 210000002445 nipple Anatomy 0.000 claims description 6
- 230000002787 reinforcement Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 abstract description 6
- 238000002347 injection Methods 0.000 abstract description 4
- 239000007924 injection Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000003595 mist Substances 0.000 description 9
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 8
- 229910001055 inconels 600 Inorganic materials 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000008246 gaseous mixture Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910000792 Monel Inorganic materials 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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Abstract
The invention relates to a chlorination reaction device adopting the following technical scheme: the chlorination reaction device is composed of an injection mixer, an inner draft tube and a chlorination reactor, wherein the injection mixer is connected with the chlorination reactor, and the inner draft tube is arranged in the chlorination reactor; the injection mixer is characterized in that a material cavity is composed of a chlorination inlet pipe, a flat cover, a cylinder body, a nozzle and a mixed gas inlet pipe, a short section is respectively connected with the cylinder body and a reducer section which is connected with an injecting pipe, and the injecting pipe passes through the chlorination reactor to extend into the inner draft tube; the inner draft tube comprises a tube body, a reinforcing rib, a supporting plate, a lifting lug and a stop block; the inner draft tube is matched with the chlorination reactor by the supporting plate and the stop block; the chlorination reactor is characterized in that an end socket and the cylinder body form a device body, the lower end of the cylinder body is provided with a man hole, a connecting plate and the supporting plate are used for fixing and limiting the inner draft tube, and the cylinder body is provided with a temperature measuring port, a material outlet and a support. The invention has favourable energy saving and loss reduction and obvious environment protection effect, and the production scale of carbon tetrachloride can be controlled from around 40% at present to 2%.
Description
Technical field
The invention relates to chlorination reaction device, is mainly used in monochloro methane and chlorine under catalyst action, reacts in chlorination reaction device, generates the methane chloride mixture that contains hydrogen chloride.
Background technology
The most advanced in the world methane chloride production process technology is the methyl alcohol method.Chlorination reaction device is the nucleus equipment in the methyl alcohol method production link, is the reaction unit of monochloro methane low temperature liquid phase catalytic chlorination in the technological process of production.Only have the fifties with acetaldehyde, fluorocarbon oil to be the production chloroform of raw material and to be the device that raw material is produced carbon tetrachloride with carbon disulfide that production scale is less, technology falls behind.In recent years, domestic enterprise introduces advanced foreign technology and scientific and technological achievement by all means, and 90% adopts introduction methyl alcohol law technology and introduces key equipment, but equipment and materials price height, material reaction efficient is not high, and reaction is not exclusively; Energy consumption is big, and environment protecting is not obvious.
Summary of the invention
In order to address the above problem, the invention provides a kind of reaction to carry out at a lower temperature, and the conversion ratio of chlorine avoided chlorine gathering in reactor almost near 100%, has prevented that effectively blast from taking place; The product ratio can be by regulating CH
3Cl/Cl
2Proportioning and control reaction condition are realized; The device fabrication cost is low, fully production domesticization.
To achieve these goals, the technical scheme of the invention employing is: chlorination reaction device: be made up of jet mixer, inner draft tube and chlorination reactor, jet mixer is connected with chlorination reactor, and inner draft tube places in the chlorination reactor;
Jet mixer: by chlorine inlet pipe, flat cover, cylindrical shell I, nozzle I and combi inlet port pipe component material chamber, the chlorine inlet pipe passes flat cover and inserts in the cylindrical shell I, cylindrical shell I is connected with pipe nipple by flange, pipe nipple is connected with reducer, reducer is provided with temperature-measuring port I, reducer is connected with playpipe, and the playpipe upper end is provided with nozzle II; Playpipe passes chlorination reactor and stretches in the inner draft tube;
Inner draft tube: comprise cylindrical shell II, reinforcement, support plate, hanger and limited block, inner draft tube cooperates with chlorination reactor by support plate and limited block;
Chlorination reactor: end socket and cylindrical shell III connect to form equipment body, cylindrical shell III lower end is provided with manhole, cylindrical shell III inwall is provided with connecting plate and gripper shoe, be used for fixing and spacing inner draft tube, temperature-measuring port II is distributed on the cylindrical shell III, temperature-measuring port III stretches in the inner draft tube, and cylindrical shell III is provided with material outlet and bearing.
The key technical indexes such as the table 1 of the invention.
Table 1 the key technical indexes
| Project | Container |
| Maximum working pressure MPa | 0.74 |
| Design pressure MPa | 2.25 |
| The most high/low operating temperature ℃ | 430 |
| Design temperature ℃ | 480 |
| Name of material | HCl、CH 3OH、CH 3Cl and Cl 2Deng gaseous mixture |
| Material characteristic | Inflammable, highly harm |
| Corrosion allowance mm | 1.5 |
| Hydraulic test pressure MPa | 3.47 |
| Air tight test pressure MPa | 2.25 |
| AB class weld joint efficiency | 1.0 |
| Total volume m 3 | 17.2 |
The beneficial effect of the invention is:
1, the effect of inner draft tube is for mist provides reaction compartment, makes mist can concentrate reaction.In addition, the gap between inner draft tube and chlorination reactor is in order to make mist carry out circular response, to improve reaction efficiency.Originally the shortcoming of the structure of import existence is that reaction compartment is little, and circulation is slow, and efficient is low.In order to solve this difficult problem, adjusted the structure of inner draft tube.Concrete measure is: the length of lengthening inner draft tube and the gap between increasing inner draft tube and chlorination reactor, and the length of inner draft tube is between 4.2～4.5 meters, and the gap between inner draft tube and chlorination reactor is 142～145 millimeters.By the adjustment of these two critical sizes, increased the zone of mixed gas reaction, for gaseous mixture provides sufficient reaction compartment.In addition,, can quicken the inner loop of gaseous mixture, react repeatedly, thereby improved reaction efficiency by strengthening the gap between inner draft tube and chlorination reactor.
2, the outlet side diameter of nozzle is changed, and changes φ 80 into by original φ 70.The shortcoming of original nozzle is that outlet diameter is little, and jet length is far away, and the reaction center regional location that makes reactor causes the mist that does not react completely to enter next system than higher, has influenced the quality of product.Calculate and experimental test through theoretical, nozzle diameter changes φ 80 into and can reduce the reaction center zone, thereby reacting gas is fully mixed, and after the complete reaction, mist just enters next system.
3, equipment and materials is Inconel600, and Inconel600 has desirable intensity, processability, anti-corrosion and heat resistance.Good resistance to high temperature oxidation, burn into cold and hot working performance and cryogenic mechanics performance are arranged.The antioxygenic property of Inconel600 in the oxidation neutral medium is better than pure nickel, and oxidation resistance temperature can be up to 1180 ℃.Contain high nickel and make its reducing resistance medium, no matter in high concentration chloride, still in containing the caustic liquor of OH-, have good anticorrosion stress-resistant performance.The stress corrosion cracking (SCC) of chlorion can not take place in especially anti-chlorine ion stress corrosion, this alloy.The chrome content height also makes it have corrosion resistance in the high temperature oxidation stability medium.Especially anti-dry chlorine gas and hydrogen-chloride etching, temperature can be up to 650 ℃.Thereby the Inconel600 alloy can high temperature resistant chlorine and high-temp chlorination hydrogen, at high temperature has the corrosive nature of anti-caustic alkali and halogen.
By the good product quality that the invention is produced, methane chloride content can bring up to 99.99%, can satisfy the production of organosilicon, Organic fluoride fully; The ratio amplitude of accommodation is big between product, and carrene and chloroform ratio can be adjusted to 80: 20 from 20: 80; Save energy and reduce the cost; Environmental benefit is remarkable, and the carbon tetrachloride proportion of production can be controlled at 2% by present about 40%.The invention can make to be reflected under the lower temperature to be carried out, and the conversion ratio of chlorine avoided chlorine gathering in reactor almost near 100%, has prevented that effectively blast from taking place.
Description of drawings
Fig. 1: the overall structure schematic diagram of the invention;
Fig. 2: jet mixer structural representation;
Fig. 3: inner draft tube structural representation;
Fig. 4: be among Fig. 3 A to view;
Fig. 5: the vertical view that is Fig. 3;
Fig. 6: chlorination reactor structural representation;
Fig. 7: nozzle arrangements schematic diagram;
Fig. 8: the vertical view that is Fig. 7.
The specific embodiment
As shown in Figure 1, chlorination reaction device is made up of jet mixer 1, inner draft tube 2, chlorination reactor 3, and jet mixer 1 is fixedlyed connected by vessel flange 109 with chlorination reactor 3, and inner draft tube 2 places in the chlorination reactor 3.
As shown in Figure 2, jet mixer 1: by chlorine inlet pipe 101, flat cover 102, cylindrical shell I 103, nozzle I 104 and combi inlet port pipe 113 component material chambeies, chlorine inlet pipe 101 passes flat cover 102 and inserts in the cylindrical shell I 103, the outlet side diameter of nozzle I 104 is φ 80, cylindrical shell I 103 is connected with pipe nipple 106 by flange 105, pipe nipple 106 is connected with reducer 107, reducer 107 is provided with temperature-measuring port I 112, reducer 107 is connected by flange 108 with playpipe 110, playpipe 110 upper ends are provided with nozzle II 111, and nozzle II 111 outlet side diameters are φ 80; Playpipe 110 passes chlorination reactor 3 and stretches in the inner draft tube 2.Chlorine is by chlorine inlet pipe 101, and mists such as monochloro methane enter in the material cavity by blender inlet tube 113, tentatively mixes in material cavity, via reducer 107, by playpipe 110, is entered in the inner draft tube 2 by nozzle II 111 injections.In jet mixer 1, material can also further mix by in the process of reducer 107, sprayed by nozzle II 111 to enter in the inner draft tube 2, thereby material can reach excellent contact again, makes the reaction can be abundant.Detect mixture temperature in the reducer 107 by temperature-measuring port I 112, for chlorination reactor 3 external heat provide the prerequisite parameter.
As Fig. 3～shown in Figure 5, inner draft tube 2: comprise cylindrical shell II 201, reinforcement 202, support plate 203, hanger 204 and limited block 205; Inner draft tube 2 cooperates with chlorination reactor 3 by support plate 203 and limited block 205.The length of inner draft tube 2 is set to 4.5 meters in the present embodiment, and the gap between inner draft tube and chlorination reactor inner core is set to 145 millimeters.Inner draft tube 2 makes mist can concentrate reaction for mist provides reaction compartment.Gap between the inner core of inner draft tube 2 and chlorination reactor 3 is in order to make mist carry out circular response, to improve reaction efficiency.
As shown in Figure 6, chlorination reactor 3: end socket 306 connects to form equipment body with cylindrical shell III 308 by vessel flange 305, and cylindrical shell III 308 length are 10 meters, and the length of cylindrical shell III 308 can be controlled the gaseous mixture reaction indirectly, reacts fully; Cylindrical shell III 308 lower ends are provided with manhole 301, and manhole 301 is held concurrently and is connected with jet mixer 1, and can overhaul and change equipment part.Cylindrical shell III 308 inwalls are provided with connecting plate 302 and gripper shoe 303, are used for fixing and spacing inner draft tube 2, with support plate 203 in the inner draft tube 2 and limited block 205 matched in clearance, for mist provides reaction compartment.Temperature-measuring port II 304 is distributed on the cylindrical shell II308, and temperature-measuring port III 310 stretches in the inner draft tube 2, measures and control temperature of charge everywhere by temperature-measuring port, for the temperature of material reaction provides underlying parameter.Cylindrical shell III 308 is provided with material outlet 307 and bearing 309.The final finished material is gone out by material outlet 307.Entire reaction course can guarantee stable reaction and complete by temperature-measuring port II 304 monitoring everywhere.
Used material
The chlorination reaction apparatus adopts the Inconel600 material, and flange adopts the Inconel600 forging, and nozzle adopts the Monel material.
The operation principle of the invention is: medium tentatively mixes in material cavity by chlorine inlet pipe and blender inlet tube respectively, in reducer, further mix, via reducer, pass through playpipe, enter in the inner draft tube by nozzle ejection, electrical heating is carried out in the chlorination reactor outside, by temperature-measuring port control temperature, when reaching the medium reaction temperature, fully react in inner draft tube, the chlorination reactor interruption is provided with temperature-measuring port, with temperature in control and the adjusting chlorination reactor, make medium continue to react at the chlorination reactor inner chamber, the end product material is gone out by material outlet, finishes the circulatory system and monochloro methane low temperature liquid phase catalytic chlorination system.
Claims (2)
1. chlorination reaction device, it is characterized in that: be made up of jet mixer (1), inner draft tube (2) and chlorination reactor (3), jet mixer (1) is connected with chlorination reactor (3), and inner draft tube (2) places in the chlorination reactor (3);
Jet mixer (1): by chlorine inlet pipe (101), flat cover (102), cylindrical shell I (103), nozzle I (104) and combi inlet port pipe (113) component material chamber, chlorine inlet pipe (101) passes flat cover (102) and inserts in the cylindrical shell I (103), cylindrical shell I (103) is connected with pipe nipple (106) by flange (105), pipe nipple (106) is connected with reducer (107), reducer (107) is provided with thermometric I (112), reducer (107) is connected with playpipe (110), and playpipe (110) upper end is provided with nozzle II (111); Playpipe (110) passes chlorination reactor (3) and stretches in the inner draft tube (2);
Inner draft tube (2): comprise cylindrical shell II (201), reinforcement (202), support plate (203), hanger (204) and limited block (205), inner draft tube (2) cooperates with chlorination reactor (3) by support plate (203) and limited block (205);
Chlorination reactor (3): end socket (306) connects to form equipment body with cylindrical shell III (308), cylindrical shell III (308) lower end is provided with manhole (301), cylindrical shell III (308) inwall is provided with connecting plate (302) and gripper shoe (303), be used for fixing and spacing inner draft tube (2), temperature-measuring port II (304) is distributed on the cylindrical shell III (308), temperature-measuring port III (310) stretches in the inner draft tube (2), and cylindrical shell III (308) is provided with material outlet (307) and bearing (309).
2. according to the described chlorination reaction device of claim 1, the length that it is characterized in that described inner draft tube (2) is 4.2～4.5 meters, and the gap between inner draft tube (2) and chlorination reactor (3) is 142～145 millimeters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100130610A CN101623614B (en) | 2009-08-11 | 2009-08-11 | Chlorination reaction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100130610A CN101623614B (en) | 2009-08-11 | 2009-08-11 | Chlorination reaction device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101623614A CN101623614A (en) | 2010-01-13 |
| CN101623614B true CN101623614B (en) | 2011-11-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100130610A Active CN101623614B (en) | 2009-08-11 | 2009-08-11 | Chlorination reaction device |
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| Country | Link |
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| CN (1) | CN101623614B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295959B (en) * | 2011-07-25 | 2013-09-11 | 安徽淮化股份有限公司 | Gas-washing device for gas producer |
| CN105170057A (en) * | 2015-09-02 | 2015-12-23 | 南通市天时化工有限公司 | Chlorination method capable of controlling reaction process, and special apparatus thereof |
| CN109647321A (en) * | 2019-01-18 | 2019-04-19 | 江苏海企技术工程股份有限公司 | A kind of energy saving thermal chlorination reaction unit for methane chloride |
| CN111389321A (en) * | 2020-03-23 | 2020-07-10 | 山东凯泰科技股份有限公司 | Reactor for producing chloropropene |
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| Publication number | Publication date |
|---|---|
| CN101623614A (en) | 2010-01-13 |
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Address after: 110000 Liaoning Province, Shenyang Hunnan New District Nanping Road No. 2 Patentee after: Shenyang Orient Titanium Industry Co., Ltd. Address before: South Street in Dongling District of Shenyang city of Liaoning Province, No. 137 110016 Patentee before: Shenyang Orient Titanium Industry Co., Ltd. |