CN211226358U - Device for preparing high-purity carbonyl sulfide - Google Patents
Device for preparing high-purity carbonyl sulfide Download PDFInfo
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- CN211226358U CN211226358U CN201922311078.6U CN201922311078U CN211226358U CN 211226358 U CN211226358 U CN 211226358U CN 201922311078 U CN201922311078 U CN 201922311078U CN 211226358 U CN211226358 U CN 211226358U
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- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 238000003860 storage Methods 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 37
- 238000010521 absorption reaction Methods 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000011552 falling film Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- LVVQTPZQNHQLOM-UHFFFAOYSA-N 2,6-dichloro-1,3-benzoxazole Chemical compound C1=C(Cl)C=C2OC(Cl)=NC2=C1 LVVQTPZQNHQLOM-UHFFFAOYSA-N 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 46
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 42
- 239000007788 liquid Substances 0.000 description 18
- 238000000034 method Methods 0.000 description 18
- 230000008569 process Effects 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- HAASPZUBSZGCKU-UHFFFAOYSA-N 6-chloro-3h-1,3-benzoxazole-2-thione Chemical compound ClC1=CC=C2NC(=S)OC2=C1 HAASPZUBSZGCKU-UHFFFAOYSA-N 0.000 description 8
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- UBAZGMLMVVQSCD-UHFFFAOYSA-N carbon dioxide;molecular oxygen Chemical compound O=O.O=C=O UBAZGMLMVVQSCD-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- MTMNJFGEKOYMIV-UHFFFAOYSA-N carbonyl dichloride;toluene Chemical compound ClC(Cl)=O.CC1=CC=CC=C1 MTMNJFGEKOYMIV-UHFFFAOYSA-N 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 2
- 238000009924 canning Methods 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- HCUYBXPSSCRKRF-UHFFFAOYSA-N diphosgene Chemical compound ClC(=O)OC(Cl)(Cl)Cl HCUYBXPSSCRKRF-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- -1 polyethylene Polymers 0.000 description 2
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 2
- 229940116357 potassium thiocyanate Drugs 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
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- 235000014785 Bergenia crassifolia Nutrition 0.000 description 1
- 240000004972 Bergenia crassifolia Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000005603 Prosulfocarb Substances 0.000 description 1
- GNVMUORYQLCPJZ-UHFFFAOYSA-M Thiocarbamate Chemical compound NC([S-])=O GNVMUORYQLCPJZ-UHFFFAOYSA-M 0.000 description 1
- 239000005625 Tri-allate Substances 0.000 description 1
- MWBPRDONLNQCFV-UHFFFAOYSA-N Tri-allate Chemical compound CC(C)N(C(C)C)C(=O)SCC(Cl)=C(Cl)Cl MWBPRDONLNQCFV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 description 1
- 229950004394 ditiocarb Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PQKBPHSEKWERTG-LLVKDONJSA-N ethyl (2r)-2-[4-[(6-chloro-1,3-benzoxazol-2-yl)oxy]phenoxy]propanoate Chemical group C1=CC(O[C@H](C)C(=O)OCC)=CC=C1OC1=NC2=CC=C(Cl)C=C2O1 PQKBPHSEKWERTG-LLVKDONJSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
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- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000002316 fumigant Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- 231100001224 moderate toxicity Toxicity 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- NQLVQOSNDJXLKG-UHFFFAOYSA-N prosulfocarb Chemical compound CCCN(CCC)C(=O)SCC1=CC=CC=C1 NQLVQOSNDJXLKG-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
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- 150000003557 thiazoles Chemical class 0.000 description 1
- UCPYLLCMEDAXFR-UHFFFAOYSA-N triphosgene Chemical compound ClC(Cl)(Cl)OC(=O)OC(Cl)(Cl)Cl UCPYLLCMEDAXFR-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Disclosed is an apparatus for producing high-purity carbonyl sulfide, which includes: a reaction kettle; the condenser is arranged above the reaction kettle and communicated with the reaction kettle, and a water separator is arranged at the bottom of the condenser and communicated with the reaction kettle; the absorption tower is communicated with the top of the condenser, and a water cooler is arranged at the top of the absorption tower; the drying tower is communicated with the water cooler; the buffer tank or the air bag is communicated with the drying tower; the high-efficiency condenser is communicated with the buffer tank or the air bag through a compressor; the crude carbonyl sulfide storage tank is communicated with the high-efficiency condenser; the rectifying tower is communicated with the crude carbonyl sulfide storage tank through a delivery pump, and the top of the rectifying tower is provided with a drain pipe; and the carbonyl sulfur storage tank is communicated with the bottom of the rectifying tower. The device prepares high-purity carbonyl sulfide while solving the problem of tail gas emission in the production of 2, 6-dichlorobenzoxazole.
Description
Technical Field
The disclosure relates to the technical field of chemical equipment, in particular to a device for preparing high-purity carbonyl sulfide.
Background
Carbonyl sulfide (chemical formula: COS), also known as carbonyl sulfide, was first synthesized by KarolyThanz, a scientist of Hungary in 1867, and first realized large-scale industrial production by the chemical industry company of Ihara, Japan in 1970, is an important intermediate for synthesizing thiocarbamate pesticides and medicines, and can be used for synthesizing thioacid, substituted thiazole, pesticide badan, herbicide triallate, thiocarb, prosulfocarb, and the like; meanwhile, the carbonyl sulfide has moderate toxicity, can be degraded and converted, and can be used as a grain fumigant and a petrochemical standard gas raw material instead of methyl bromide and phosphine. In recent years, it has been found that high purity carbonyl sulfide can be used as an etching gas for integrated circuit fabrication to replace fluoride etching gases that are difficult to degrade and have a greenhouse effect. With the increasing attention of governments on environmental protection, carbonyl sulfide, which is a gas having less environmental impact than fluoride, is more and more concerned as a raw material gas in the industries of electronic chip manufacturing, photovoltaics, LEDs and the like, and the demand of carbonyl sulfide is expected to be in a rapid growth trend in the coming years.
The carbonyl sulfide synthesizing process includes carbon monoxide process, potassium thiocyanate or ammonium thiocyanate process. Among them, the carbon monoxide method has simple process flow and high yield, and the industrial production generally adopts the process from the consideration of cost and raw material source, but the reaction speed is slow, and more carbon monoxide methods are usedImpurities of (e.g. H)2S、CS2、CO2Etc., affecting the purity of the product. The process of potassium thiocyanate or ammonium thiocyanate has the features of small apparatus, easy operation, etc. during the reaction, partial carbonyl sulfide is decomposed into impurity H2S and CO2The purification difficulty is increased, and the method can produce a large amount of inorganic salt as a byproduct, and is not suitable for industrial mass preparation.
2, 6-dichlorobenzoxazole is an important organic synthesis intermediate, and is widely used for synthesis of pesticides, medicines and the like, such as synthesis of oryzanol and fenoxaprop-p-ethyl. At present, the domestic industrial method for synthesizing 2, 6-dichlorobenzoxazole is mainly obtained by taking 2-mercapto-6-chlorobenzoxazole and solid phosgene as raw materials and N, N-dimethylformamide as a catalyst and reacting in a toluene system to release hydrogen chloride and carbonyl sulfide gases with equal moles without H2S、CS2、SO2And the like.
At present, the tail gas discharged by the reaction is mainly treated by a liquid alkali absorption method in industry, but new waste water and waste salt are generated while the waste gas is treated, and the problem of three wastes cannot be fundamentally solved.
SUMMERY OF THE UTILITY MODEL
The present disclosure relates to another apparatus for preparing high-purity carbonyl sulfide, which includes:
a reaction kettle;
the condenser is arranged above the reaction kettle and communicated with the reaction kettle, and a water separator is arranged at the bottom of the condenser and communicated with the reaction kettle;
the absorption tower is communicated with the top of the condenser, and a water cooler is arranged at the top of the absorption tower;
the drying tower is communicated with the water cooler;
the buffer tank or the air bag is communicated with the drying tower;
the high-efficiency condenser is communicated with the buffer tank or the air bag through a compressor;
the crude carbonyl sulfide storage tank is communicated with the high-efficiency condenser;
the rectifying tower is communicated with the crude carbonyl sulfide storage tank through a delivery pump, and the top of the rectifying tower is provided with a drain pipe;
and the carbonyl sulfur storage tank is communicated with the bottom of the rectifying tower.
Drawings
FIG. 1 shows a schematic configuration diagram of an apparatus for producing high-purity carbonyl sulfide according to an embodiment of the present disclosure;
fig. 2 shows a gas chromatogram for producing high purity carbonyl sulfide in an embodiment of the present disclosure.
Detailed description of the invention
In the following description, certain specific details are included to provide a thorough understanding of various disclosed embodiments. One skilled in the relevant art will recognize, however, that the embodiments can be practiced without one or more of the specific details, or with other methods, components, materials, and so forth.
Unless otherwise required by the disclosure, throughout the specification and the appended claims, the words "comprise", "comprising", and "have" are to be construed in an open, inclusive sense, i.e., "including but not limited to".
Reference throughout the specification to "one embodiment," "an embodiment," "in another embodiment," or "in certain embodiments" means that a particular reference element, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" or "in another embodiment" or "in certain embodiments" in various places throughout this specification are not necessarily all referring to the same embodiment, and furthermore, particular elements, structures, or features may be combined in any suitable manner in one or more embodiments.
Definition of
In the present disclosure, the term "solid phosgene" refers to bis (trichloromethyl) carbonate, which has similar reactivity to phosgene and diphosgene, can react with various compounds such as alcohol, aldehyde, amine, amide, carboxylic acid, phenol, hydroxylamine, etc., and can also be cyclized and condensed to prepare heterocyclic compounds. In the present disclosure, phosgene solids may also be replaced with phosgene, diphosgene. In the present disclosure, the term "reaction vessel" refers to a vessel having physical or chemical reaction, and the structural design and parameter configuration of the vessel are used to realize the heating, evaporation, cooling and low-speed mixing functions required by the process.
In the present disclosure, the term "reflux water separator" refers to a device that continuously separates water from a reaction system in a reaction kettle by using an azeotrope formed by an organic solvent and water in a certain proportion at a certain temperature.
In the present disclosure, the term "condenser" refers to a component of a refrigeration system, belonging to a type of heat exchanger, which is capable of converting a gas or vapor into a liquid, and transferring the heat in the tubes to a refrigerant in contact with the tubes in a rapid manner.
In the present disclosure, the term "surge tank" refers to an important accessory device of the compressor, which is mainly used to balance the pressure fluctuation of the compression system, so that the system works more smoothly. In the present disclosure, the term "compressor" refers to a body in a source device, which is a device that converts mechanical energy of a prime mover (typically an electric motor) into gas pressure energy, and is a gas pressure generating device that compresses gas.
In the present disclosure, the term "storage tank" refers to a storage container for storing refined chemicals such as acid and alkali, organic solvents, gases, liquids, etc. The materials of the storage tank are polyethylene storage tank, polypropylene storage tank, glass fiber reinforced plastic storage tank, ceramic storage tank, rubber storage tank, stainless steel storage tank, etc.
In the present disclosure, the term "transfer pump" means a transfer apparatus for continuously transferring a material in accordance with a transfer condition to a desired place through a horizontally or vertically laid pipe.
In the present disclosure, the term "rectification column" refers to a column vapor-liquid contacting device that performs rectification. By utilizing the property that each component in the mixture has different volatility, namely the vapor pressure of each component is different at the same temperature, the light component (low-boiling-point substance) in the liquid phase is transferred into the gas phase, and the heavy component (high-boiling-point substance) in the gas phase is transferred into the liquid phase, thereby realizing the purpose of separation.
In the present disclosure, the term "evacuation pipe" refers to a member provided to discharge an impurity gas such as nitrogen, oxygen, carbon dioxide, etc. from a container, a pipe, etc.
Detailed Description
The present disclosure relates to another apparatus for preparing high-purity carbonyl sulfide, which includes:
a reaction kettle;
the condenser is arranged above the reaction kettle and communicated with the reaction kettle, and a water separator is arranged at the bottom of the condenser and communicated with the reaction kettle;
the absorption tower is communicated with the top of the condenser, and a water cooler is arranged at the top of the absorption tower;
the drying tower is communicated with the water cooler;
the buffer tank or the air bag is communicated with the drying tower;
the high-efficiency condenser is communicated with the buffer tank or the air bag through a compressor;
the crude carbonyl sulfide storage tank is communicated with the high-efficiency condenser;
the rectifying tower is communicated with the crude carbonyl sulfide storage tank through a delivery pump, and the top of the rectifying tower is provided with a drain pipe;
and the carbonyl sulfur storage tank is communicated with the bottom of the rectifying tower.
In certain embodiments, the absorber column is a falling film absorber column.
In certain embodiments, the absorption tower comprises a first absorption tower and a second absorption tower, the first absorption tower is communicated with the top of the condenser, the second absorption tower is communicated with the first absorption tower, the top of the second absorption tower is provided with a water cooler, the drying tower comprises a first drying tower and a second drying tower, the first drying tower is communicated with the water cooler, the second drying tower is communicated with the first drying tower, and the second drying tower is communicated with the buffer tank or the air bag.
The method for preparing the high-purity carbonyl sulfide based on the device comprises the following steps:
step 1: mixing toluene, 2-mercapto-6-chlorobenzoxazole and DMF, heating to 84-86 ℃, refluxing and dividing water until the water content in the toluene solution is less than 100ppm, the molar ratio of solid phosgene to toluene in the solid phosgene toluene solution is 1: 3-1: 5, and the molar ratio of 2-mercapto-6-chlorobenzoxazole to toluene is 1: 2-1: 5;
step 2: cooling to 55-60 ℃, dropwise adding a solid phosgene toluene solution for 5-8 h, maintaining the temperature at 55-60 ℃ in the dropwise adding process, and keeping the temperature until the content of the 2-mercapto-6-chlorobenzoxazole is detected to be less than 0.1%;
and step 3: and (3) removing impurities from the gas evaporated in the step (2) and separating to obtain the high-purity carbonyl sulfide.
Wherein the impurity removal and separation step comprises the following steps:
and (3) condensing the gas evaporated in the step (2) to remove toluene, washing with water to remove HCl gas, condensing the gas to a compressed gas or liquid fluid or a mixed state thereof through compression, and rectifying the compressed gas or liquid fluid or the mixed state thereof to obtain a gas-phase component and a liquid-phase component, wherein the liquid-phase component is high-purity carbonyl sulfide.
Hereinafter, the present disclosure will be explained in detail by the following examples in order to better understand various aspects of the present application and advantages thereof. It should be understood, however, that the following examples are not limiting and are merely illustrative of certain embodiments of the present disclosure.
Examples
Example 1
As shown in fig. 1, an apparatus for preparing high-purity carbonyl sulfide, comprising:
an apparatus for producing high purity carbonyl sulfide, comprising:
a reaction kettle 1;
the condenser 3 is arranged above the reaction kettle 1 and communicated with the reaction kettle 1, a water separator 2 is arranged at the bottom of the condenser 3, and the water separator 2 is communicated with the reaction kettle 1;
the absorption tower 4 is communicated with the top of the condenser 3, and a water cooler 5 is arranged at the top of the absorption tower 4;
a drying tower 6, wherein the drying tower 6 is communicated with the water cooler 5;
a buffer tank or air bag 7, wherein the buffer tank or air bag 7 is communicated with the drying tower 6;
the high-efficiency condenser 9 is communicated with the buffer tank or the air bag 7 through a compressor 8;
a crude carbonyl sulfide storage tank 10, wherein the crude carbonyl sulfide storage tank 10 is communicated with the high-efficiency condenser 9;
the rectifying tower 12 is communicated with the crude carbonyl sulfide storage tank 10 through a delivery pump 11, and the top of the rectifying tower 12 is provided with an emptying pipe 13;
and the carbonyl sulfide storage tank 14 is communicated with the bottom of the rectifying tower 12.
385kg of toluene and 413kg of solid phosgene (99%) are added into a 1500L reaction kettle, and the mixture is stirred for 0.5h at room temperature, so that the system is fully dissolved and then transferred into an elevated tank. Adding 802kg of toluene, 800kg of 2-mercapto-6-chlorobenzoxazole and 12.6 kg of DMF into a 5000L reaction kettle, stirring and mixing, heating to 84-86 ℃, refluxing and water separating until the water content of the toluene solution in the kettle is less than 100 ppm. And (3) reducing the temperature to 55 ℃, starting to drip the solid phosgene toluene solution in the upper tank, controlling the temperature to be between 55 and 60 ℃ in the dripping process, keeping the temperature for 6 hours at the range of 60 ℃ after dripping is finished, carrying out sampling tracking analysis, and finishing the reaction after the content of the 2-mercapto-6-chlorobenzoxazole is detected to be less than 0.1%. In the dropping process, after toluene in the gas discharged by the reaction is removed by a condenser, tail gas is absorbed and separated by HCl through a falling film absorption tower, enters a drying tower through a water cooler for drying, then enters a compressor for compression to 1.25Mpa after passing through a storage tank or an air bag, the compressed tail gas enters a high-efficiency condenser for condensation to a compressed gas or a liquid or a mixed state thereof, and the temperature is about-4 ℃. The liquid is conveyed to a crude carbonyl sulfide storage tank for temporary storage through a pipeline. When the product carbonyl sulfide storage tank reaches a certain liquid level, a delivery pump is started to deliver compressed gas or liquid or a mixed state of the compressed gas or the liquid to a rectifying tower for rectification, a gas phase part in a kettle is lifted to a condenser of the rectifying tower through a rectifying column, the lifted gas phase mainly comprises light impurity gases such as nitrogen, oxygen, carbon dioxide and the like and carbonyl sulfide, the gas phase part is cooled to-60 to-50 ℃ in the condenser, most of the carbonyl sulfide gas is liquefied to be changed into descending liquid to flow back to the rectifying kettle, the light impurities such as nitrogen, oxygen, carbon dioxide and the like cannot be liquefied, and the impurities are evacuated by a vacuum unit, discharged into a waste gas treatment system through an emptying pipe, treated and discharged after reaching the standard. And (3) pressurizing and canning carbonyl sulfide at the bottom of the rectifying still to a carbonyl sulfide storage tank to obtain 248kg of carbonyl sulfide, and carrying out gas chromatography analysis on gas in the storage tank.
The results of the gas chromatography are shown in FIG. 2, in which:
table 1: results of chromatographic analysis
| Peak number | Name of peak | Retention time | Peak height | Peak area | Content (wt.) |
| 1 | 0.752 | 607.397 | 2001.350 | 0.0599 | |
| 2 | 2.437 | 102932.961 | 3338880.500 | 99.9401 | |
| Total of | 103540.358 | 3340881.850 | 100.00 |
The content of carbonyl sulfide was 99.9401, i.e. 99.9% by area normalization.
Example 2
As shown in fig. 1, an apparatus for preparing high-purity carbonyl sulfide, comprising:
an apparatus for producing high purity carbonyl sulfide, comprising:
a reaction kettle 1;
the condenser 3 is arranged above the reaction kettle 1 and communicated with the reaction kettle 1, a water separator 2 is arranged at the bottom of the condenser 3, and the water separator 2 is communicated with the reaction kettle 1;
the absorption tower 4 comprises a first absorption tower and a second absorption tower, the first absorption tower is communicated with the top of the condenser 3, the second absorption tower is communicated with the first absorption tower, and a water cooler 5 is arranged at the top of the second absorption tower;
a drying tower 6, wherein the drying tower 6 comprises a first drying tower and a second drying tower, the first drying tower is communicated with the water cooler 5, and the second drying tower is communicated with the first drying tower;
a buffer tank or air bag 7, wherein the buffer tank or air bag 7 is communicated with the second drying tower;
the high-efficiency condenser 9 is communicated with the buffer tank or the air bag 7 through a compressor 8;
a crude carbonyl sulfide storage tank 10, wherein the crude carbonyl sulfide storage tank 10 is communicated with the high-efficiency condenser 9;
the rectifying tower 12 is communicated with the crude carbonyl sulfide storage tank 10 through a delivery pump 11, and the top of the rectifying tower 12 is provided with an emptying pipe 13;
and the carbonyl sulfide storage tank 14 is communicated with the bottom of the rectifying tower 12.
641kg of toluene and 413kg of solid phosgene (99%) are added into a 1500L reaction kettle, and the mixture is stirred at room temperature for 0.5h to ensure that the system is fully dissolved and then transferred into a head tank. 2007kg of toluene, 800kg of 2-mercapto-6-chlorobenzoxazole and 28.5kg of DMF are added into a 5000L reaction kettle, stirred and mixed, and heated to 84-86 ℃ for reflux water diversion until the water content of the toluene solution in the kettle is less than 100 ppm. And (3) reducing the temperature to 55 ℃, starting to drip the solid phosgene toluene solution in the upper tank, controlling the temperature to be between 55 and 60 ℃ in the dripping process, keeping the temperature for 6 hours at the range of 60 ℃ after dripping is finished, carrying out sampling tracking analysis, and finishing the reaction after the content of the 2-mercapto-6-chlorobenzoxazole is detected to be less than 0.1%. In the dropping process, after toluene in the gas discharged by the reaction is removed by a condenser, tail gas is absorbed and separated by HCl through a falling film absorption tower, enters a drying tower through a water cooler for drying, then enters a compressor for compression to 1.25Mpa after passing through a storage tank or an air bag, the compressed tail gas enters a high-efficiency condenser for condensation to a compressed gas or a liquid or a mixed state thereof, and the temperature is about-4 ℃. Compressed gas or liquid or a mixed state thereof is conveyed to a crude carbonyl sulfide storage tank for temporary storage through a pipeline. After the crude carbonyl sulfide storage tank reaches a certain liquid level, a delivery pump is started to deliver compressed gas or liquid or a mixed state of the compressed gas or the liquid to a rectifying tower for rectification, a gas phase part in a kettle is lifted to a condenser of the rectifying tower through a rectifying column, the lifted gas phase mainly comprises light impurity gases such as nitrogen, oxygen, carbon dioxide and the like and carbonyl sulfide, the gas phase part is cooled to-60 to-50 ℃ in the condenser, most of the carbonyl sulfide gas is liquefied to be changed into descending liquid to flow back to the rectifying kettle, the light impurities such as nitrogen, oxygen, carbon dioxide and the like cannot be liquefied, and the impurities are evacuated by a vacuum unit, discharged into a waste gas treatment system through an emptying pipe, treated and discharged after reaching the standard. And (3) pressurizing and canning the carbonyl sulfide at the bottom of the rectifying still to a carbonyl sulfide storage tank to obtain 248kg of carbonyl sulfide with the purity of 99.9 percent.
The device of the embodiment of the disclosure prepares high-purity carbonyl sulfide while solving the problem of exhaust emission in the production of 2, 6-dichlorobenzoxazole.
In the present disclosure, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions.
From the foregoing it will be appreciated that, although specific embodiments of the disclosure have been described herein for purposes of illustration, various modifications or improvements may be made by those skilled in the art without departing from the spirit and scope of the disclosure, and that such modifications or improvements are intended to be within the scope of the appended claims.
Claims (3)
1. An apparatus for producing high-purity carbonyl sulfide, comprising:
a reaction kettle;
the condenser is arranged above the reaction kettle and communicated with the reaction kettle, and a water separator is arranged at the bottom of the condenser and communicated with the reaction kettle;
the absorption tower is communicated with the top of the condenser, and a water cooler is arranged at the top of the absorption tower;
the drying tower is communicated with the water cooler;
the buffer tank or the air bag is communicated with the drying tower;
the high-efficiency condenser is communicated with the buffer tank or the air bag through a compressor;
the crude carbonyl sulfide storage tank is communicated with the high-efficiency condenser;
the rectifying tower is communicated with the crude carbonyl sulfide storage tank through a delivery pump, and the top of the rectifying tower is provided with a drain pipe;
and the carbonyl sulfur storage tank is communicated with the bottom of the rectifying tower.
2. The apparatus according to claim 1, wherein the absorption column is a falling film absorption column.
3. The apparatus according to claim 1, wherein the absorption tower comprises a first absorption tower and a second absorption tower, the first absorption tower is communicated with the top of the condenser, the second absorption tower is communicated with the first absorption tower, a water cooler is arranged at the top of the second absorption tower, the drying tower comprises a first drying tower and a second drying tower, the first drying tower is communicated with the water cooler, the second drying tower is communicated with the first drying tower, and the second drying tower is communicated with the buffer tank or the air bag.
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| CN201922311078.6U CN211226358U (en) | 2019-12-20 | 2019-12-20 | Device for preparing high-purity carbonyl sulfide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862087A (en) * | 2019-12-20 | 2020-03-06 | 顺毅南通化工有限公司 | Method and device for preparing high-purity carbonyl sulfide |
| CN112645330A (en) * | 2020-12-17 | 2021-04-13 | 浙江省天正设计工程有限公司 | Device and process for recovering carbonyl sulfide in chlorination process tail gas |
| CN114602201A (en) * | 2022-01-17 | 2022-06-10 | 福建久策气体股份有限公司 | Carbonyl sulfide purification device and purification method thereof |
-
2019
- 2019-12-20 CN CN201922311078.6U patent/CN211226358U/en not_active Withdrawn - After Issue
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862087A (en) * | 2019-12-20 | 2020-03-06 | 顺毅南通化工有限公司 | Method and device for preparing high-purity carbonyl sulfide |
| CN110862087B (en) * | 2019-12-20 | 2024-02-13 | 顺毅南通化工有限公司 | Method and device for preparing high-purity carbonyl sulfide |
| CN112645330A (en) * | 2020-12-17 | 2021-04-13 | 浙江省天正设计工程有限公司 | Device and process for recovering carbonyl sulfide in chlorination process tail gas |
| CN114602201A (en) * | 2022-01-17 | 2022-06-10 | 福建久策气体股份有限公司 | Carbonyl sulfide purification device and purification method thereof |
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