CN110903161A - Preparation method and preparation device of 1, 2, 3-trichloropropane compound - Google Patents
Preparation method and preparation device of 1, 2, 3-trichloropropane compound Download PDFInfo
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- CN110903161A CN110903161A CN201911220963.1A CN201911220963A CN110903161A CN 110903161 A CN110903161 A CN 110903161A CN 201911220963 A CN201911220963 A CN 201911220963A CN 110903161 A CN110903161 A CN 110903161A
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- CFXQEHVMCRXUSD-UHFFFAOYSA-N TCP Natural products ClCC(Cl)CCl CFXQEHVMCRXUSD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- -1 1, 2, 3-trichloropropane compound Chemical class 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 238000010992 reflux Methods 0.000 claims abstract description 111
- AVGQTJUPLKNPQP-UHFFFAOYSA-N 1,1,1-trichloropropane Chemical compound CCC(Cl)(Cl)Cl AVGQTJUPLKNPQP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000005086 pumping Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 230000033228 biological regulation Effects 0.000 claims abstract description 6
- 230000001105 regulatory effect Effects 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 6
- LIPPKMMVZOHCIF-UHFFFAOYSA-N 1,1,2-trichloroprop-1-ene Chemical compound CC(Cl)=C(Cl)Cl LIPPKMMVZOHCIF-UHFFFAOYSA-N 0.000 claims description 5
- XEPXTKKIWBPAEG-UHFFFAOYSA-N 1,1-dichloropropan-1-ol Chemical compound CCC(O)(Cl)Cl XEPXTKKIWBPAEG-UHFFFAOYSA-N 0.000 claims description 5
- ZOKHGHDRKCYWTH-UHFFFAOYSA-N 1,1-dichloropropan-2-ol Chemical compound CC(O)C(Cl)Cl ZOKHGHDRKCYWTH-UHFFFAOYSA-N 0.000 claims description 4
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N 2-propanol Substances CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract 2
- 230000005494 condensation Effects 0.000 abstract 2
- 239000012530 fluid Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 239000000047 product Substances 0.000 description 16
- 239000007789 gas Substances 0.000 description 7
- 238000000605 extraction Methods 0.000 description 6
- 238000010926 purge Methods 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000004302 potassium sorbate Substances 0.000 description 2
- 238000011179 visual inspection Methods 0.000 description 2
- UMGQVBVEWTXECF-UHFFFAOYSA-N 1,1,2,3-tetrachloroprop-1-ene Chemical compound ClCC(Cl)=C(Cl)Cl UMGQVBVEWTXECF-UHFFFAOYSA-N 0.000 description 1
- LFNRXCLLMPFWPP-UHFFFAOYSA-N 1,1-dichloro-3-(3,3-dichloropropoxy)propane Chemical compound ClC(Cl)CCOCCC(Cl)Cl LFNRXCLLMPFWPP-UHFFFAOYSA-N 0.000 description 1
- FALCMQXTWHPRIH-UHFFFAOYSA-N 2,3-dichloroprop-1-ene Chemical compound ClCC(Cl)=C FALCMQXTWHPRIH-UHFFFAOYSA-N 0.000 description 1
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 1
- PWVXXGRKLHYWKM-UHFFFAOYSA-N 5-[2-(benzenesulfonyl)ethyl]-3-[(1-methylpyrrolidin-2-yl)methyl]-1h-indole Chemical compound CN1CCCC1CC(C1=C2)=CNC1=CC=C2CCS(=O)(=O)C1=CC=CC=C1 PWVXXGRKLHYWKM-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 230000002528 anti-freeze Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of chemical product preparation, and discloses a preparation method and a preparation device of a 1, 2, 3-trichloropropane compound.A crude trichloropropane raw material from a tank area enters a lightness-removing column for rectification through flow regulation, and a light component gas phase at the top of the lightness-removing column enters a top condenser for condensation; the condensate of the lightness removing condenser enters a lightness removing reflux tank and is pumped out by a lightness removing reflux pump; pumping out materials at the bottom of the light component removal tower by a light component removal tower bottom pump, feeding the materials into a heavy component removal tower for rectification, and feeding gas phase at the top of the heavy component removal tower into a heavy component removal condenser at the top of the heavy component removal tower for condensation; condensed fluid condensed by the heavy component removal condenser enters a heavy component removal reflux tank and is pumped out by a heavy component removal reflux pump; heavy components at the bottom of the heavy component removal tower are pumped out by a heavy component removal tower bottom pump, and are sent into a tank area after being cooled by a heavy component cooler. The preparation method provided by the invention has simple rectification process and greatly improves the yield.
Description
Technical Field
The invention belongs to the technical field of chemical product preparation, and particularly relates to a preparation method and a preparation device of a 1, 2, 3-trichloropropane compound.
Background
Currently, the closest prior art: 1, 2, 3-trichloropropane, formula: c3H5Cl3Molecular weight: 147.44, respectively; CAS accession number: 96-18-4.
Physical and chemical properties: can be mixed with ethanol, diethyl ether, etc., is toxic, has melting point of-14.7 deg.C, is colorless liquid, and has specific gravity: 1.38 kg/L, the content is more than or equal to 98.5 percent.
The application is as follows: the method is mainly used for producing 2, 3-dichloropropene, organic solvents and tetrachloropropene, and can also be used as a raw material of pesticide chlormequat chloride and the like. The method mainly uses the byproduct of epoxy chloropropane, namely crude trichloropropane (common name epoxy high boiling) as a raw material, and the crude trichloropropane (common name epoxy high boiling) raw material is rectified to separate 1, 2, 3-trichloropropane. However, the existing rectification process of the 1, 2, 3-trichloropropane in the preparation process is complex, the yield is low, and the development of enterprises is influenced.
In summary, the problems of the prior art are as follows: the existing rectification process of the 1, 2, 3-trichloropropane in the preparation process is complex and has low yield.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method and a preparation device of a 1, 2, 3-trichloropropane compound.
The present invention is achieved by a method for producing a 1, 2, 3-trichloropropane compound, the method for producing a 1, 2, 3-trichloropropane compound comprising:
firstly, rectifying a crude trichloropropane raw material from a tank area in a lightness-removing tower through flow regulation, condensing a light component gas phase at the top of the tower in a lightness-removing condenser, pumping a condensate into a lightness-removing reflux tank by a lightness-removing reflux pump, returning a part of the condensate to the top of the tower as a reflux, and extracting a part of the condensate as a light component product to the tank area; pumping the tower bottom material out of the light component removing tower bottom pump and sending the tower bottom material to the heavy component removing tower;
secondly, rectifying the material from the bottom pump of the light component removal tower in a heavy component removal tower, condensing the gas phase at the top of the tower in a heavy component removal condenser, pumping the condensed liquid in a heavy component removal reflux tank by a heavy component removal reflux pump, returning one part of the condensed liquid to the top of the tower as reflux, and taking the other part of the condensed liquid as a trichloropropane product to be extracted out of a tank removal area; heavy components at the bottom of the tower are pumped out by a heavy component removing tower bottom pump, and are sent to a tank field after being cooled by a heavy component cooler.
Further, in the first step, the bottom of the lightness-removing column is heated by steam through a lightness-removing reboiler.
Furthermore, in the first step, the light component is composed of 24.66% of epichlorohydrin, 10.99% of 112 trichloropropane, 54.35% of 123 trichloropropene and 10.00% of 123 trichloropropane by weight percentage.
Further, in the second step, the bottom of the de-heavy tower is heated by steam through a de-heavy reboiler.
Further, the vacuum of the lightness-removing tower in the first step is maintained by a vacuum pump and a vacuum buffer tank for sucking lightness-removing reflux; the vacuum of the de-weighting tower in the second step is maintained by a vacuum pump and a vacuum buffer tank for pumping the de-weighting reflux tank; the pressure of the vacuum buffer tank is-0.08-0.09 MpaG.
Furthermore, in the second step, the heavy component comprises 5.00 percent of 123 trichloropropane, 0.55 percent of 13 dichloro 2 propanol, 51.16 percent of 23 dichloro propanol and 43.28 percent of dichloro propyl ether by weight percentage.
Another object of the present invention is to provide a 1, 2, 3-trichloropropane compound prepared by the method for preparing a 1, 2, 3-trichloropropane compound, wherein the 1, 2, 3-trichloropropane compound comprises, by weight, 0.14% of 123 trichloropropene, 99.50% of 123 trichloropropane, 0.05% of 13 dichloro-2-propanol, and 0.31% of 23 dichloro-propanol.
Another object of the present invention is to provide an apparatus for producing a 1, 2, 3-trichloropropane compound, which performs the process for producing a 1, 2, 3-trichloropropane compound, wherein the apparatus for producing a 1, 2, 3-trichloropropane compound comprises:
the middle upper part of the lightness-removing tower is connected with a feed pump through a pipeline, the lower end of the lightness-removing tower is connected with a dehydrogenation reboiler and a lightness-removing tower bottom pump through pipelines, and the upper end of the lightness-removing tower is connected with a lightness-removing condenser through a pipeline;
the light component removal condenser is connected with the dehydrogenation reflux tank through a pipeline, and the light component removal reflux tank is connected with the vacuum buffer tank and the light component removal reflux pump through a pipeline;
the heavy component removal tower is characterized in that the middle of the heavy component removal tower is connected with the light component removal tower bottom pump through a pipeline, the lower end of the heavy component removal tower is connected with a heavy component removal reboiler and the heavy component removal tower bottom pump through a pipeline, and the upper end of the heavy component removal tower is connected with a heavy component removal condenser through a pipeline.
Further, the upper part of the vacuum buffer tank is connected with a vacuum pump through a pipeline, and the lightness removing reflux pump is connected with the upper part of the lightness removing tower and the tank area through a pipeline;
the lightness-removing reboiler is connected with the lightness-removing tower through a pipeline and forms a circulating pipeline with the lightness-removing tower.
Further, the heavy component removal condenser is connected with a heavy component removal reflux tank through a pipeline, the heavy component removal reflux tank is connected with a vacuum buffer pump and a heavy component removal reflux pump through a pipeline, the heavy component removal reflux pump is connected with the upper part of a heavy component removal tower and a tank area through a pipeline, the heavy component removal reboiler is connected with the heavy component removal tower through a pipeline, a circulation pipeline is formed by the light component removal tower, and a bottom pump of the heavy component removal tower is connected with the tank area through a pipeline.
Further, a feeding regulating valve and a feeding flowmeter are arranged between the feeding pump and the light component removal tower;
a regulating valve is arranged between the dehydrogenation reboiler and the light component removal tower;
a reflux regulating valve is arranged between the light component removing reflux pump and the tank area, and a heating regulating valve and a reflux regulating valve are arranged between the light component removing reflux pump and the light component removing tower;
a heating regulating valve is arranged between the heavy component removal reboiler and the heavy component removal tower;
and a regulating valve and a heating regulating valve are arranged between the heavy component removal reflux pump and the heavy component removal tower, and a regulating valve is arranged between the heavy component removal reflux pump and the tank field.
In summary, the advantages and positive effects of the invention are: the preparation method provided by the invention has simple rectification process and greatly improves the yield.
The 1, 2, 3-trichloropropane compound prepared by the preparation method of the 1, 2, 3-trichloropropane compound comprises, by weight, 0.14% of 123 trichloropropene, 99.50% of 123 trichloropropane, 0.05% of 13 dichloro-2-propanol and 0.31% of 23 dichloro-propanol.
Drawings
FIG. 1 is a flow chart of a process for preparing a 1, 2, 3-trichloropropane compound according to an embodiment of the present invention.
FIG. 2 is a diagram showing an apparatus for producing a 1, 2, 3-trichloropropane compound according to an embodiment of the present invention.
In the figure: 1. a light component removal tower; 2. a feed pump; 3. a light component removal reboiler; 4. a light component removal tower bottom pump; 5. a light component removal condenser; 6. a light component removal reflux tank; 7. a vacuum buffer tank; 8. a light component removal reflux pump; 9. a vacuum pump; 10. a de-weighting tower; 11. a de-heavy reboiler; 12. a de-weighting column bottom pump; 13. a de-weighting condenser; 14. a de-weighting reflux tank; 15. a heavy-load removal reflux pump.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, the preparation method of a 1, 2, 3-trichloropropane compound provided by the embodiment of the present invention includes:
s101, rectifying a crude trichloropropane raw material from a tank area into a lightness-removing tower through flow regulation, condensing a light component gas phase at the top of the tower into a lightness-removing condenser at the top of the tower, pumping a condensate into a lightness-removing reflux tank, pumping out the condensate by a lightness-removing reflux pump, returning a part of the condensate to the top of the tower as a reflux, and extracting a part of the condensate as a light component product to the tank area; the material at the bottom of the tower is pumped out by a light component removal tower bottom pump and sent to a heavy component removal tower.
S102, rectifying the material from the bottom pump of the light component removal tower in a heavy component removal tower, condensing the gas phase at the top of the tower in a heavy component removal condenser, pumping the condensed liquid in a heavy component removal reflux tank by a heavy component removal reflux pump, returning one part of the condensed liquid to the top of the tower as reflux, and taking the other part of the condensed liquid as a trichloropropane product to be extracted out of a tank removal area; heavy components at the bottom of the tower are pumped out by a heavy component removing tower bottom pump, and are sent to a tank field after being cooled by a heavy component cooler.
In the embodiment of the invention, the heating at the bottom of the light component removal tower is realized by steam through a light component removal reboiler, and the heating at the bottom of the heavy component removal tower is realized by steam through a heavy component removal reboiler.
In the embodiment of the invention, the vacuum environments of the light component removal tower and the heavy component removal tower are respectively maintained by pumping respective reflux tanks through a vacuum pump and a vacuum buffer tank, and the pressure of the vacuum buffer tank is-0.08-0.09 MpaG.
In the embodiment of the invention, part of condensate pumped by the light component removal reflux pump is used as reflux and pumped back to the top of the light component removal tower, and part of condensate is used as a light component product and is extracted to a tank area.
In the embodiment of the invention, part of the condensate pumped by the heavy component removal reflux pump is used as reflux and pumped back to the tower top, and part of the condensate is used as a trichloropropane product and is extracted from a tank removal area.
As shown in fig. 2, an apparatus for preparing a 1, 2, 3-trichloropropane compound according to an embodiment of the present invention includes a light component removal column 1, a feed pump 2, a light component removal reboiler 3, a light component removal column bottom pump 4, a light component removal condenser 5, a light component removal reflux tank 6, a vacuum buffer tank 7, a light component removal reflux pump 8, a vacuum pump 9, a heavy component removal column 10, a heavy component removal reboiler 11, a heavy component removal column bottom pump 12, a heavy component removal condenser 13, a heavy component removal reflux tank 14, and a heavy component removal reflux pump 15.
The middle part of the light component removal tower 1 is connected with a feed pump 2 through a pipeline, the upper part of the light component removal tower is connected with a light component removal condenser through a pipeline, and the lower part of the light component removal tower is connected with a light component removal reboiler 3 and a light component removal tower bottom pump 4 through pipelines.
The light component removal condenser 5 is connected with the middle part of the heavy component removal tower through a pipeline, the light component removal reboiler is connected with the middle lower part of the light component removal tower, and the bottom pump of the light component removal tower is connected with the tank field through a pipeline.
The upper part of the heavy component removal tower 10 is connected with a heavy component removal condenser 13 through a pipeline, and the lower part of the heavy component removal tower is connected with a heavy component removal reboiler 11 and a heavy component removal tower bottom pump 12 through pipelines.
The heavy component removal condenser 13 is connected with a heavy component removal reflux tank 14 through a pipeline, the heavy component removal reflux tank is connected with a vacuum buffer tank and a heavy component removal reflux pump 15 through a pipeline, the heavy component removal reflux pump is connected with the upper part of the heavy component removal tower and the middle part of the light component removal tower through a pipeline, and the heavy component removal reboiler is connected with the middle lower part of the heavy component removal tower through a pipeline;
the upper part of the light component removal tower is connected with a light component removal condenser 5 through a pipeline, the lower part of the light component removal tower is connected with a light component removal reboiler and a light component removal tower bottom pump through a pipeline, the light component removal condenser is connected with a light component removal reflux tank through a pipeline, and the light component removal reflux tank 6 is connected with a vacuum buffer tank 7 and a light component removal reflux pump 8 through a pipeline.
The light component removal reflux pump 8 is connected with the upper part of the light component removal tower and the tank area through pipelines, the light component removal reboiler is connected with the light component removal tower through a pipeline, and the bottom pump of the light component removal tower is connected with the middle part of the heavy component removal tower through a pipeline.
The vacuum buffer tank is connected with a vacuum pump 9 through a pipeline.
In a preferred embodiment, the middle upper part of the lightness-removing column is connected with a feed pump through a pipeline, the lower end of the lightness-removing column is connected with a dehydrogenation reboiler and a lightness-removing column bottom pump through pipelines, and the upper end of the lightness-removing column is connected with a lightness-removing condenser through a pipeline.
The light component removal condenser is connected with the dehydrogenation reflux tank through a pipeline, and the light component removal reflux tank is connected with the vacuum buffer tank and the light component removal reflux pump through a pipeline.
In the embodiment of the invention, the upper part of the vacuum buffer tank is connected with a vacuum pump through a pipeline, and the lightness removing reflux pump is connected with the upper part of the lightness removing tower and the tank area through a pipeline.
The lightness-removing reboiler is connected with the lightness-removing tower through a pipeline and forms a circulating pipeline with the lightness-removing tower.
In the embodiment of the invention, the trichloropropane preparation device also comprises a heavy component removal tower, the middle part of the heavy component removal tower is connected with the light component removal tower bottom pump through a pipeline, the lower end of the heavy component removal tower is connected with a heavy component removal reboiler and a heavy component removal tower bottom pump through pipelines, and the upper end of the heavy component removal tower is connected with a heavy component removal condenser through a pipeline.
In the embodiment of the invention, the heavy component removal condenser is connected with a heavy component removal reflux tank through a pipeline, the heavy component removal reflux tank is connected with a vacuum buffer pump and a heavy component removal reflux pump through a pipeline, the heavy component removal reflux pump is connected with the upper part of a heavy component removal tower and a tank area through a pipeline, the heavy component removal reboiler is connected with the heavy component removal tower through a pipeline to form a circulation pipeline with the light component removal tower, and the bottom pump of the heavy component removal tower is connected with the tank area through a pipeline.
In the embodiment of the invention, a feed regulating valve and a feed flow meter are arranged between the feed pump and the light component removal tower.
And a regulating valve is arranged between the dehydrogenation reboiler and the light component removal tower.
And a reflux regulating valve is arranged between the light component removing reflux pump and the tank area, and a heating regulating valve and a reflux regulating valve are arranged between the light component removing reflux pump and the light component removing tower.
And a heating regulating valve is arranged between the heavy component removal reboiler and the heavy component removal tower.
And a regulating valve and a heating regulating valve are arranged between the heavy component removal reflux pump and the heavy component removal tower, and a regulating valve is arranged between the heavy component removal reflux pump and the tank field.
The embodiments of the present invention will be further described with reference to the following embodiments.
Raw materials and product specification
1.3. By-product composition
Second, preparation before trial run and driving
2.1. System purge
And after the equipment and the pipeline are installed, the whole system is required to be purged so as to remove residual welding slag and iron rust in the pipeline of the equipment. Before purging, equipment, instruments and pipeline accessories which cannot participate in purging are isolated, and the device mainly comprises a flow meter, a regulating valve, a liquid level meter and the like and is detached before purging. And after the purging is finished, the flow meter, the regulating valve, the liquid level meter and the like which are detached are recovered, and the tower internals and the filling filler can be installed.
2.2. General provisions for systematic testing
(1) After the pipeline is installed, the pipeline system is tested for strength, tightness and the like according to design rules so as to check the engineering quality of the pipeline system and each connecting part. The test items of the device are as follows: the test method comprises a strength test, a hydraulic test, an air pressure test, a leakage test and a vacuum test.
(2) The strength test and tightness test of the pipeline system are generally carried out by adopting hydraulic pressure. If the hydraulic strength test is difficult due to the design structure or other reasons, the pneumatic test can be used instead, but effective safety measures must be taken and the test pressure must not exceed relevant regulations.
(3) The following conditions should be provided before the pipeline system test:
the pipeline system is constructed and meets the design requirements and relevant regulations;
finishing the installation of the supporting and hanging bracket;
after the welding work is finished, the welding line and other parts to be checked are checked to be qualified, and the welding line and other parts to be checked are not painted and insulated;
the temporary reinforcement measures for the test are checked and confirmed to be safe and reliable;
the pressure gauge for the test is qualified;
with a well-established and approved protocol.
(4) Before the pipeline system test, an isolation blind plate is arranged between the pipeline system and the running pipeline.
(5) Before the test, systems, equipment, instruments and pipes which cannot participate in the test are isolated, and the parts added with the blind plates should be marked and recorded obviously.
(6) If leakage occurs in the test process, the pressure repair is not needed. After the defect is eliminated, it should be retested.
(7) After the system is tested to be qualified, the test medium is preferably discharged at an appropriate outdoor place, and safety is paid attention.
(8) After the test is finished, all temporary blind plates should be removed in time, the record is checked, and the test record of the pipeline system is filled.
2.3. Hydraulic test
(1) Clean water is used as the water for the hydraulic test, the content of chloride ions in the water is not more than 25ppm, and the air is exhausted after the water is injected into the system.
(2) Hydraulic test pressure: the strength test pressure of the vacuum pipeline is 0.2Mpa, and the tightness test pressure is 0.1 Mpa; the strength test pressure of other middle and low pressure pipelines is 1.25 times of the working pressure, and the tightness test pressure is the working pressure.
(3) The hydraulic test is preferably carried out at an ambient temperature of more than 5 ℃ or else antifreeze measures are required.
(4) For a pipeline system with a large position difference, the static pressure influence of the test medium is considered. The liquid pipeline is subject to the highest point pressure, but the lowest point pressure does not exceed the bearing capacity of the valve and the pipe fittings.
(5) In the hydraulic strength test, the pressure rise should be slow. And stopping pressing for ten minutes after the test pressure is reached, and taking the condition of no leakage and no deformation by visual inspection as a qualified condition.
(6) The hydraulic tightness test is generally carried out after the strength test is qualified, and the hydraulic tightness test is comprehensively checked to be qualified as no leakage.
2.4. Air pressure test
(1) The pneumatic test medium is generally carried out with air or an inert gas.
(2) The air pressure tightness test should be carried out after the hydraulic strength test is qualified.
(3) The pressure of the air pressure strength test is 1.15 times of the working pressure, and the vacuum pipeline is 0.2 Mpa; the pressure of the tightness test is working pressure, but the vacuum pipeline is not less than 0.1 Mpa.
(4) During the air pressure strength test, the pressure rise should be slow step by step. The pressure is increased to 50% of the test pressure, and the pressure is checked, if no leakage or abnormality exists, and the pressure is increased step by step according to 10% of the test pressure until the test pressure is strengthened. And each stage of pressure stabilization is carried out for three minutes, and five minutes after the test pressure is reached, the product is qualified as no leakage, no deformation by visual inspection.
(5) And after the strength test is qualified, reducing the pressure to working pressure, and detecting the leakage by using soapy water. If no leakage exists, the pressure is stabilized for thirty minutes, and the pressure is not reduced, the tightness test is qualified.
2.5. Other tests
(1) After the tests are finished, single machine test and water combined transportation of the mobile equipment can be carried out, after the water combined transportation, the whole system discharges water, the system is blown clean by compressed air, then the air is replaced by nitrogen, and the oxygen content is analyzed by sampling the system gas until the system gas is qualified.
(2) After the tightness test of the vacuum system is qualified, during linkage test operation, a vacuum degree test is carried out at a design pressure, the time is 24 hours, and the pressurization rate is not more than 5 percent.
(3) The leakage test is carried out after the system is flushed and qualified, and the pressure measurement and temperature measurement points in the test are representative. The leakage test pressure is working pressure, the time is 24 hours, and the average leakage rate per hour is not more than 0.5 percent, so the product is qualified.
Third, test run, driving
Firstly, analyzing raw materials and determining operation parameters for standby. During production, if the raw materials have different compositions, the operation parameters need to be recalculated and determined. The following operating parameters are based on the raw material composition during the design of the second and middle process packs, and the process operating parameters are as follows:
light component removal tower T-201:
pressure at the top of the column: -80kPaG
The tower top temperature: 88.2 deg.C
Bottom pressure: -77kPaG
Temperature at the bottom of the column: 114.2 deg.C
The reflux ratio of the tower top is as follows: r is 48.5
The tower top reflux amount: 1280kg/h (1.3 m)3/h)
The tower feeding amount: 1000kg/h (0.75 m)3/h)
The extraction amount at the top of the tower is as follows: 26kg/h (0.028 m)3/h)
The extraction amount at the bottom of the tower is as follows: 974kg/h (0.79 m)3/h)
Reboiler heat duty at the bottom of the column: 17.1 ten thousand calories per hour
Amount of circulating cooling water at the top of the tower: 15 ton/h
A heavy component removal tower T-202:
pressure at the top of the column: -80kPaG
The tower top temperature: 104.3 deg.C
Bottom pressure: -77kPaG
Temperature at the bottom of the column: 130-140.6 deg.C
The reflux ratio of the tower top is as follows: r is 0.45
The tower top reflux amount: 323kg/h (0.241 m)3/h)
The tower feeding amount: 974kg/h (0.79 m)3/h)
The extraction amount at the top of the tower is as follows: 716kg/h (0.525 m)3/h)
The extraction amount at the bottom of the tower is as follows: 257kg/h (0.24 m)3/h)
Reboiler heat duty at the bottom of the column: 7.7 ten thousand calories per hour
Amount of circulating cooling water at the top of the tower: 9 tons/hour.
3.1. Starting circulating water system
(1) And (3) filling water into the circulating water pump, discharging air from the suction pipe and the pump head, starting a power supply of the circulating water pump, monitoring the reading of a pressure gauge at the outlet of the pump, and confirming that the circulating water is circulated normally.
(2) Opening a circulating water inlet and outlet valve of the condenser, opening a high-point emptying valve of the water return pipe, emptying air, and closing the high-point emptying valve.
3.2. Starting a vacuum system
(1) And filling water into the vacuum pump water tank, opening the inlet and outlet valves of the pump, and starting the power supply.
(2) After the water is completely circulated, the water tank is properly supplemented with water.
(3) And observing the reading of the vacuum gauge of the vacuum buffer tank to be about-0.08-0.09 MpaG, and ensuring the long-time stability. And according to the situation, if the vacuum is higher than-0.09 MpaG to 0.095MpaG, adjusting the opening of the vacuum breaking valve.
3.3. T-201 system for opening light component removal tower
(1) And opening an inlet and outlet valve of the feeding pump and opening a power supply of the feeding pump.
(2) The feed regulating valve FV-201 is set to manual, the reading of the feed flowmeter FIC-201 is observed, and the feed regulating valve FV-201 is adjusted to make the reading of the feed flowmeter FIC-201 equal0.75m3/h。
(3) A reboiler E-202 at the bottom of the tower is adjusted by a valve TV-202 manually, the liquid level LIC-201 of the tower bottom is observed, and the reboiler E-202 is adjusted by the valve TV-202 when the liquid level appears.
(4) Observing the liquid level LIC-202 of the reflux tank, starting a reflux pump P-201 when the liquid level reaches 50% -60%, manually setting a reflux adjusting valve FV-202, adjusting the valve position FV-202 to ensure that the liquid level LIC-202 of the reflux tank is basically unchanged, and adjusting the opening of a heating adjusting valve TV-202 until the reflux amount FIC-202 at the top of the tower is stabilized to be equal to1.33m3H is used as the reference value. During the period, the tower kettle is prevented from being evaporated to dryness and the liquid level of the tower kettle cannot be seen; if the reflux does not reach the specified value and the liquid level in the tower kettle rises too fast, the feeding flow of the tower can be properly reduced; and (4) observing whether the reading of the vacuum gauge of the vacuum buffer tank is stable or not, and if the vacuum drops, properly closing the opening of the vacuum breaking valve.
(5) Sampling and analyzing the reflux liquid at the tower top, and taking the trichloropropane content of 123 not more than 10 percent as qualified. Note that sampling is taking a live sample.
(6) Blending of products extracted from tower topThe throttle valve LV-202 is set to be manual, the opening of the throttle valve is adjusted, and the produced flow FI-203 is read as0.03m3H is used as the reference value. The reflux quantity FIC-202 at the top of the tower is reduced and stabilized to1.3m3In this case, the reflux ratio R was 48.5.
(7) Adjusting valve LV-201 to manual operation, observing tower kettle liquid level LIC-201, opening inlet and outlet valves of tower bottom pump P-202 when liquid level reaches 50% -60%, starting pump power supply, adjusting valve position of LV-202 to make tower bottom produced flow FI-204 read0.79m3/h。
(8) The operation is stable for more than half an hour, and the regulating valves can be set to be automatic.
3.4. Open heavy tower T-202 system that takes off
(1) The material enters the T-102 tower from the T-201 through the P-202
(2) The tower bottom reboiler E-204 heating regulating valve TV-204 is set to be manual, the liquid level LIC-203 of the tower bottom is observed, and the tower reboiler E-204 regulating valve TV-204 is opened when the liquid level appears.
(3) Observing the liquid level LIC-204 of the reflux tank, starting a reflux pump P-203 when the liquid level reaches 50% -60%, manually setting a reflux adjusting valve FV-205, adjusting the valve position FV-205 to ensure that the liquid level LIC-204 of the reflux tank is basically unchanged, and adjusting the opening of a heating adjusting valve TV-204 until the reflux amount FIC-205 at the top of the tower is stabilized to be equal to0.77m3/h。
(4) Sampling and analyzing the reflux liquid at the tower top, and determining that the content of the 123 trichloropropane exceeds 99 percent.
(5) The regulating valve LV-204 of the product extracted from the tower top is set to be manual, and the opening degree of the regulating valve is regulated to ensure that the extraction flow FI-206 is read as0.525m3H is used as the reference value. The reflux quantity FIC-205 at the top of the tower is reduced and stabilized to0.24m3In this case, the reflux ratio R was 0.45.
(6) And (3) manually setting an adjusting valve LV-203, observing the liquid level LIC-203 of the tower bottom, starting an inlet and outlet valve of a tower bottom pump P-204 when the liquid level reaches 50% -60%, starting a pump power supply, and adjusting the valve position of the LV-203 to keep the liquid level at the bottom of the tower basically unchanged.
(7) The operation is stable for more than half an hour, and the regulating valves can be set to be automatic.
Fourthly, stopping and overhauling
1. The feed pump was turned off.
2. The reboiler steam inlet valve was closed.
3. And closing the liquid phase extraction at the tower top, and carrying out total reflux and temperature reduction.
4. The bottom pump was turned off.
5. It was confirmed that the temperature at the column top and the column bottom was decreased to 40 ℃ or lower.
6. The circulating water system is closed.
7. The vacuum system was turned off.
8. And opening an emptying valve of the vacuum system, and emptying the vacuum system.
9. And opening the tower bottom pump to empty the tower kettle.
10. The product pump is turned on to empty the product tank.
11. And (5) purging the pipeline.
12. And continuously emptying the tower kettle and the tank.
13. Induce and drain the stranguria.
14. And (5) replacing nitrogen in the system.
15. And (5) sampling and analyzing the system gas. And after the product is qualified, the product can be overhauled.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (11)
1. A method for producing a 1, 2, 3-trichloropropane compound, comprising:
firstly, rectifying a crude trichloropropane raw material from a tank area in a lightness-removing tower through flow regulation, condensing a light component gas phase at the top of the tower in a lightness-removing condenser, pumping a condensate into a lightness-removing reflux tank by a lightness-removing reflux pump, returning a part of the condensate to the top of the tower as a reflux, and extracting a part of the condensate as a light component product to the tank area; pumping the tower bottom material out of the light component removing tower bottom pump and sending the tower bottom material to the heavy component removing tower;
secondly, rectifying the material from the bottom pump of the light component removal tower in a heavy component removal tower, condensing the gas phase at the top of the tower in a heavy component removal condenser, pumping the condensed liquid in a heavy component removal reflux tank by a heavy component removal reflux pump, returning one part of the condensed liquid to the top of the tower as reflux, and taking the other part of the condensed liquid as a trichloropropane product to be extracted out of a tank removal area; heavy components at the bottom of the tower are pumped out by a heavy component removing tower bottom pump, and are sent to a tank field after being cooled by a heavy component cooler.
2. The process for producing a 1, 2, 3-trichloropropane compound as claimed in claim 1, wherein in the first step, the bottom of the lightness-removing column is heated by steam through a lightness-removing reboiler.
3. The process for producing a 1, 2, 3-trichloropropane compound as claimed in claim 1, wherein in the first step, the light component is composed of, by weight, 24.66% of epichlorohydrin, 10.99% of 112 trichloropropane, 54.35% of 123 trichloropropene and 10.00% of 123 trichloropropane.
4. The process for producing a 1, 2, 3-trichloropropane compound as claimed in claim 1, wherein in the second step, the bottom of the de-heaving column is heated with steam by passing through a de-heaving reboiler.
5. The process for producing a 1, 2, 3-trichloropropane compound as claimed in claim 1, wherein the vacuum of the lightness-removing column in the first step is maintained by a vacuum pump, a vacuum buffer tank and a lightness-removing reflux tank; the vacuum of the de-weighting tower in the second step is maintained by a vacuum pump and a vacuum buffer tank for pumping the de-weighting reflux tank; the pressure of the vacuum buffer tank is-0.08-0.09 MpaG.
6. The process for preparing a 1, 2, 3-trichloropropane compound as claimed in claim 1, wherein in the second step the heavy components consist of, by weight, 123-trichloropropane 5.00%, 13-dichloro-2-propanol 0.55%, 23-dichloropropanol 51.16 and 43.28% dichloropropanol.
7. A 1, 2, 3-trichloropropane compound prepared by the process of claim 1, 2, 3-trichloropropane compound, wherein the 1, 2, 3-trichloropropane compound comprises, by weight, 0.14% of 123 trichloropropene, 99.50% of 123 trichloropropane, 0.05% of 13 dichloro-2-propanol, and 0.31% of 23 dichloro-propanol.
8. An apparatus for producing a 1, 2, 3-trichloropropane compound, which carries out the process for producing a 1, 2, 3-trichloropropane compound according to any one of claims 1 to 6, wherein the apparatus for producing a 1, 2, 3-trichloropropane compound comprises:
the middle upper part of the lightness-removing tower is connected with a feed pump through a pipeline, the lower end of the lightness-removing tower is connected with a dehydrogenation reboiler and a lightness-removing tower bottom pump through pipelines, and the upper end of the lightness-removing tower is connected with a lightness-removing condenser through a pipeline;
the light component removal condenser is connected with the dehydrogenation reflux tank through a pipeline, and the light component removal reflux tank is connected with the vacuum buffer tank and the light component removal reflux pump through a pipeline;
the heavy component removal tower is characterized in that the middle of the heavy component removal tower is connected with the light component removal tower bottom pump through a pipeline, the lower end of the heavy component removal tower is connected with a heavy component removal reboiler and the heavy component removal tower bottom pump through a pipeline, and the upper end of the heavy component removal tower is connected with a heavy component removal condenser through a pipeline.
9. The apparatus for producing a 1, 2, 3-trichloropropane compound according to claim 8, wherein the vacuum buffer tank is connected at an upper portion thereof to a vacuum pump through a pipe, and the lightness-removing reflux pump is connected to the lightness-removing column and the tank section through a pipe;
the lightness-removing reboiler is connected with the lightness-removing tower through a pipeline and forms a circulating pipeline with the lightness-removing tower.
10. The apparatus for producing a 1, 2, 3-trichloropropane compound according to claim 8, wherein the de-heavy condenser is connected to a de-heavy reflux drum via a pipe, the de-heavy reflux drum is connected to a vacuum buffer pump and a de-heavy reflux pump via a pipe, the de-heavy reflux pump is connected to an upper part of the de-heavy tower and the drum region via a pipe, the de-heavy reboiler is connected to the de-heavy tower via a pipe, and forms a circulation line with the de-light tower, and the de-heavy tower bottom pump is connected to the drum region via a pipe.
11. The apparatus for producing a 1, 2, 3-trichloropropane compound according to claim 8, wherein a feed regulating valve and a feed flow meter are provided between the feed pump and the lightness-removing column;
a regulating valve is arranged between the dehydrogenation reboiler and the light component removal tower;
a reflux regulating valve is arranged between the light component removing reflux pump and the tank area, and a heating regulating valve and a reflux regulating valve are arranged between the light component removing reflux pump and the light component removing tower;
a heating regulating valve is arranged between the heavy component removal reboiler and the heavy component removal tower;
and a regulating valve and a heating regulating valve are arranged between the heavy component removal reflux pump and the heavy component removal tower, and a regulating valve is arranged between the heavy component removal reflux pump and the tank field.
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