CN111268680B - Purification method and purification system of high-purity carbonyl sulfide - Google Patents
Purification method and purification system of high-purity carbonyl sulfide Download PDFInfo
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Abstract
A purification method and a purification system of high-purity carbonyl sulfide are provided, wherein the purification method comprises the following steps: s1, activating an adsorber and then replacing a purification system; s2, removing light components by flash evaporation; s3, freezing the precooler to a temperature between-20 and-40 ℃, and simultaneously precooling the crystallization kettle and the cold trap to a temperature between-150 and-186 ℃; s4, introducing the carbonyl sulfide crude product into a condenser to remove part of heavy components, and then deeply removing the heavy components in a plurality of serially connected adsorbers; s5, allowing carbonyl sulfide gas to enter a crystallization kettle for crystallization; s6, introducing dry normal-temperature nitrogen into the crystallization kettle, and heating; filtering the molten carbonyl sulfide liquid in the crystallization kettle, and then putting the filtered molten carbonyl sulfide liquid into a cold trap; s7, freezing the 4N carbonyl sulfide in the cold trap and collecting the carbonyl sulfide in a product bottle. The purification system comprises a raw material row, a precooler, an adsorber, a crystallization kettle, a cold trap and a collection row; the invention adopts a plurality of purification means such as an adsorption separation method, a flash separation method, a crystallization separation method and the like, effectively removes impurities in the crude product of the carbonyl sulfide at low cost, and obtains the high-purity 4N carbonyl sulfide.
Description
Technical Field
The invention relates to the technical field of purification of high-purity carbonyl sulfide, in particular to a purification method and a purification system of high-purity carbonyl sulfide.
Background
Carbonyl sulfide (chemical formula: COS), also called carbonyl sulfide and carbonyl sulfide, is a colorless gas with a rotten egg smell in a normal state. High purity carbonyl sulfide has been found to have particular utility in integrated circuit chip etching, and the leading integrated circuit manufacturers in the world have established chip etching lines from carbonyl sulfide as a raw material, and the process has a tendency to spread to all integrated circuit manufacturers. Secondly, high purity 4N carbonyl sulfide also has applications in the electronics, photovoltaics and LED industries. Meanwhile, carbonyl sulfide has less influence on the environment than fluohnated gas, and is more and more concerned as raw and auxiliary material gas in the industries of electronic chip manufacturing, photovoltaics, LEDs and the like, and the demand of carbonyl sulfide is expected to rapidly increase in the coming years.
The synthesis process of carbonyl sulfide is more, carbonyl sulfide synthesized by any process has a large amount of impurities, and the carbonyl sulfide can be used in the semiconductor industry after being purified to reach 4N purity, so that the purification method is very important for the production of semiconductor 4N carbonyl sulfide. At present, the purification methods are mostly low-temperature condensation and rectification methods, such as the purification methods mentioned or related to the patent publications CN109231207, CN110862087 and CN107986277, and have the problems of low product purity, low purification efficiency, large investment of a plurality of rectification towers, high production cost of multiple rectification and the like.
In general, the existing carbonyl sulfide purification method has large investment or low efficiency, or the product purity is difficult to reach the quality standard of the electronic industry or the semiconductor industry. Therefore, there is a need for a purification process for high purity 4N carbonyl sulfide that can meet the semiconductor industry.
Disclosure of Invention
The first purpose of the invention is to provide a method for purifying high-purity carbonyl sulfide, which is simple, easy to operate and low in investment, can prepare high-purity 4N carbonyl sulfide, is easy to realize industrial production or can overcome the defects of high investment, low efficiency, low purity and the like to solve the technical problems.
The second objective of the present invention is to provide a purification system for high-purity carbonyl sulfide, which can prepare high-purity 4N carbonyl sulfide, is easy to implement industrial production, and can overcome the disadvantages of large investment, low efficiency, low purity, etc. to solve the above technical problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for purifying high-purity carbonyl sulfide comprises the following steps:
step S1: purging the adsorber and vessel containing the adsorbent in the purification system until the moisture content of said purification system is less than 1ppm, and replacing all the lines and vessels of the purification system with a high purity helium gas evacuation until the nitrogen content in the system is less than 5ppm.
Step S2: taking one of the raw material bottles of the raw material row as a flash evaporation collecting bottle, freezing the flash evaporation collecting bottle to-150 to-186 ℃, and carrying out flash evaporation treatment on carbonyl sulfide raw material gas in the raw material row to remove main light component impurities;
and step S3: opening the refrigerant inlet valves of the precooler, the crystallization kettle and the cold trap, introducing refrigerants into the precooler, the crystallization kettle and the cold trap, and adjusting the opening degree of each refrigerant inlet valve, so that the temperature of the precooler is controlled to be between-20 and-40 ℃, and the temperature of the crystallization kettle and the cold trap is controlled to be between-150 and-186 ℃.
And step S4: opening an inlet valve of the precooler to enable the carbonyl sulfur raw material gas to enter the precooler so as to remove part of heavy component impurities in the carbonyl sulfur raw material gas;
opening an inlet valve of the adsorber, and allowing carbonyl sulfide gas to enter the adsorber to deeply remove heavy component impurities;
step S5: opening an inlet valve of the crystallization kettle, and allowing carbonyl sulfide gas to enter the crystallization kettle which reaches a set precooling temperature for crystallization, wherein the precooling temperature is-150 to-186 ℃, and keeping a crystallization state for 10 to 30 minutes;
step S6: and discharging a refrigerant in the jacket of the crystallization kettle, introducing a heating medium into the jacket of the crystallization kettle to slowly melt the carbonyl sulfide, observing the temperature in the crystallization kettle, stopping heating when the temperature of the crystallization kettle reaches-105 ℃, and discharging the liquid carbonyl sulfide into a cold trap which reaches a set precooling temperature after passing through a filter.
Step S7: and freezing the collecting bottles in the collecting row to-150 to-186 ℃, introducing a heating medium into a jacket of the cold trap to heat the cold trap, and introducing gasified carbonyl sulfide into the collecting bottles to obtain qualified 4N carbonyl sulfide gas.
Further, the feeding amount of the carbonyl sulfide gas is not more than 3/4 of the volume of the crystallization kettle.
Further, in the process of collecting the carbonyl gas in the step S7, the gas cylinder discharged by the collection is the gas cylinder frozen to-150 to-186 ℃ until the temperature of the cold trap is recovered to-10 ℃, the collection of the carbonyl sulfide gas is stopped, and after the temperature of the cold trap is continuously raised until the normal temperature, the residual gas in the cold trap is collected by a transfer cylinder.
A purification system using the purification method of the high-purity carbonyl sulfide comprises a raw material discharge, a precooler, an adsorber, a crystallization kettle, a cold trap and a collection discharge;
the output end of the raw material row is communicated to the input end of the precooler;
the output end of the precooler is communicated to the input end of the adsorber;
the output end of the adsorber is communicated to the input end of the crystallization kettle;
the output end of the crystallization kettle is communicated to the input end of the cold trap;
and the output end of the cold trap is communicated to the input end of the collection row.
Further, the gas cylinders of the raw material row and the collecting row are low-temperature-resistant aluminum alloy gas cylinders.
Further, the adsorbent is one or more of a 3A molecular sieve, a 4A molecular sieve, a 5A molecular sieve, a 10X molecular sieve, a 13X molecular sieve, alumina, activated carbon, silica gel and a zeolite molecular sieve.
Furthermore, the precooler, the crystallization kettle and the cold trap are all containers with jackets.
Furthermore, the adsorber is a series combination of a plurality of adsorbers, and each adsorber is filled with a single type of adsorbent or a mixture of a plurality of types of adsorbents.
Further, the bottom of the crystallization kettle is provided with a filter.
Further, the purification system is provided with a sampling port and a pressure gauge.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention does not need to build a rectifying tower, thereby reducing the investment cost and the production cost of equipment;
2. the invention avoids the output of a large amount of waste liquid and waste water in the production stage of carbonyl sulfide crude products, reduces the output of dangerous waste and general solid waste, reduces the production cost and improves the safety benefit of production;
3. aiming at the characteristics of impurities in a carbonyl sulfide crude product, the invention cryogenically cools carbonyl sulfide to remove impurities, then adsorbs the impurities by a molecular sieve, and then enters a crystallization kettle to crystallize and separate other impurities, and the crystallization method has higher efficiency than a rectification method and a cryoseparation method, and can obtain a high-purity 4N carbonyl sulfide product.
4. Compared with the rectification method, the method has the advantages of low investment and high capacity, and can obtain the high-purity 4N carbonyl sulfide product meeting the semiconductor market without complex and expensive equipment and instruments.
Drawings
Fig. 1 is a schematic structural diagram of one embodiment of the present invention.
Wherein: raw material row 1, precooler 2, adsorber 3, crystallization kettle 4, cold trap 5, collection row 6, sampling port 71 and pressure gauge 72.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
A method for purifying high-purity carbonyl sulfide comprises the following steps:
step S1: adsorber 3 is heated to 350 deg.C, adsorber 3 and vessel containing adsorbent in the purification system is purged with dry nitrogen until the moisture content of the purification system is less than 1ppm, and all piping and vessels of the purification system are replaced with high purity 5N helium gas evacuation until the nitrogen content of the system is less than 5ppm.
Step S2: 2 collection bottles were connected to feed line 1 and collection line 6, respectively, and all tubing and vessels of the purification system were replaced with a high purity 5N helium gas pump down until the nitrogen content in the system was less than 5ppm.
Connecting 3 raw material bottles (25 kg per bottle) to the raw material row 1, wherein one raw material bottle is used as a flash evaporation collecting bottle, freezing the flash evaporation collecting bottle to-160 ℃, opening a raw material bottle valve to flash-evaporate carbonyl sulfur raw material gas in the raw material row for multiple times to remove main light component impurities, and enabling the content of the main light component impurities to reach the 4N requirement. Wherein the main light component impurities comprise one or more of N2, H2, O2, ar, CO, total hydrocarbons (calculated as CH 4); the light component reaches the 4N standard, and the main light component has the following impurity contents: nitrogen (N2) is less than or equal to 20ppm; oxygen (O2) is less than or equal to 10ppm; hydrogen (H2) is less than or equal to 10ppm; carbon monoxide (CO) is less than or equal to 10ppm;
for example, the on-line test of this example results in a nitrogen (N2) gas content as the major light component: 12.6PPM; oxygen (O2): 4.5ppm; hydrogen (H2): 1.2ppm; carbon monoxide (CO): 2.4ppm, total hydrocarbons (calculated as CH 4): 4.6ppm, reaching the requirement of 4N.
And step S3: opening the inlet valves of the precooler 2, the crystallization kettle 4 and the cold trap 5, introducing the refrigerants into the precooler 2, the crystallization kettle 4 and the cold trap 5, wherein the refrigerant adopted in the step S3 is liquid nitrogen, and adjusting the opening degree of each refrigerant inlet valve so that the temperature of the precooler 2 is controlled to be between-20 and-40 ℃ (30 ℃) in the embodiment, and the temperatures of the crystallization kettle and the cold trap 5 are controlled to be between-150 and-186 ℃ (170 ℃ in the embodiment).
And step S4: opening an inlet valve of the precooler 2 to enable the carbonyl sulfur raw material gas to enter the precooler 2 so as to remove part of heavy component impurities in the carbonyl sulfur raw material gas; opening an inlet valve of the adsorber 3, and allowing carbonyl sulfide gas to enter the adsorber 3 to deeply remove heavy component impurities such as water, sulfur dioxide, carbon disulfide and the like; in the present embodiment, the adsorbers 3 are arranged in series in multiple stages.
Wherein the requirements for deeply removing water, sulfur dioxide and carbon disulfide heavy component impurities are as follows: sulfur dioxide (SO 2) is less than or equal to 5ppm; the water content (H2O) is less than or equal to 5ppm; carbon disulfide (CS 2) is less than or equal to 5ppm;
the content of the main heavy components obtained by the online test of the embodiment is water: 4.6ppm; sulfur dioxide (SO 2): 2.6ppm; carbon disulfide (CS 2): 1.8ppm, reaching the requirement of 4N.
Step S5: and opening an inlet valve of the crystallization kettle 4, introducing the carbonyl sulfide gas into the crystallization kettle 4 (the volume is 40L, and the precooling temperature of the crystallization kettle 4 is-150 to-186 ℃) which reaches the set precooling temperature, crystallizing, and keeping the crystallization state for 25 minutes. It is particularly noted that the feeding amount of the carbonyl sulfide gas should not exceed 3/4 of the volume of the crystallization vessel.
Step S6: discharging a refrigerant (liquid nitrogen in the embodiment) in the jacket of the crystallization kettle 4, introducing a heating medium into the jacket of the crystallization kettle 4 to slowly melt carbonyl sulfide, observing the temperature in the crystallization kettle, and when the temperature of the crystallization kettle 4 reaches-105 ℃, hydrogen sulfide and carbon dioxide are solid; stopping heating, discharging the liquid carbonyl sulfide into a cold trap 5 at 186 ℃ after passing through a filter.
Step S7: freezing the collecting bottle in the collecting row 6, introducing dry normal-temperature nitrogen into a jacket of the cold trap 5 to heat the cold trap, and introducing gasified carbonyl sulfide into the collecting bottle to obtain qualified 4N carbonyl sulfide gas, wherein the purity of 4N is 99.99%.
The test of the finished product of the embodiment obtains the content of carbon dioxide and hydrogen sulfide as carbon dioxide (CO 2): 15.5ppm; hydrogen sulfide (H2S): 4.56PPM, and the requirement of 4N is met.
Therefore, the invention does not need to build a rectifying tower, thereby reducing the equipment investment cost and the production cost;
the invention has no carbonyl sulfide crude product production stage, avoids the output of a large amount of waste liquid and waste water, reduces the output of dangerous waste and general solid waste, reduces the production cost and improves the safety benefit of production;
aiming at the characteristics of impurities in a carbonyl sulfide crude product, the invention cryogenically cools carbonyl sulfide to remove impurities, then adsorbs the impurities by a molecular sieve, and then enters a crystallization kettle to crystallize and separate other impurities, and the crystallization method has higher efficiency than a rectification method and a cryoseparation method, and can obtain a high-purity 4N carbonyl sulfide product.
Compared with the rectification efficiency, the invention has the advantages of low investment and high productivity, and can obtain the high-purity 4N carbonyl sulfide product meeting the semiconductor market without complex and expensive equipment and instruments.
The purification process has the advantages of simple steps, easy operation, less investment, capability of preparing high-purity 4N carbonyl sulfide, easiness in realizing industrial production, capability of overcoming the defects of high investment, low efficiency, low purity and the like.
Further, the feeding amount of the carbonyl sulfide gas is not more than 3/4 of the volume of the crystallization kettle 4, and the feeding amount needs to be accurately calculated, namely, the fed raw materials need to be continuously metered.
Further, in the process of collecting the carbonyl gas in the step S7, the gas cylinder of the collecting exhaust 6 is frozen, the freezing temperature is between-150 ℃ and-186 ℃, the carbonyl sulfide gas collection is stopped until the temperature of the cold trap 5 is recovered to-10 ℃, and after the temperature of the cold trap 5 is continuously increased until the temperature reaches the normal temperature, the residual gas in the cold trap 5 is collected by a transfer cylinder.
A purification system using the purification method of the high-purity carbonyl sulfide comprises a raw material row 1, a precooler 2, an absorber 3, a crystallization kettle 4, a cold trap 5 and a collection row 6;
the output end of the raw material row 1 is communicated to the input end of the precooler 2;
the output end of the precooler 2 is communicated to the input end of the adsorber 3;
the output end of the absorber 3 is communicated to the input end of the crystallization kettle 4;
the output end of the crystallization kettle 4 is communicated to the input end of the cold trap 5;
the output end of the cold trap 5 is communicated to the input end of the collection row 6.
The purification system can realize the purification method of the high-purity carbonyl sulfide; therefore, the purification system can prepare high-purity 4N carbonyl sulfide, is easy to realize industrial production, and can overcome the defects of large investment, low efficiency, low purity and the like.
Further, the gas cylinders of the raw material row 1 and the collection row 6 are both low-temperature-resistant aluminum alloy gas cylinders, wherein the raw material row 1 is provided with a plurality of raw material cylinders, and the collection row 6 is provided with a plurality of raw material cylinders
Further, the adsorbent is one or more of a 3A molecular sieve, a 4A molecular sieve, a 5A molecular sieve, a 10X molecular sieve, a 13X molecular sieve, alumina, activated carbon, silica gel and a zeolite molecular sieve.
Furthermore, the precooler 2, the crystallization kettle 4 and the cold trap 5 are all jacketed vessels. The jacket is filled with refrigerant, and the refrigerant mainly is low-temperature liquid including but not limited to alcohol, glycol, silicone oil, liquid nitrogen, etc.
Furthermore, the adsorbers 3 are arranged in a multistage series, that is, a plurality of adsorbers 3 are used in a series combination, and each adsorber 3 is filled with a single type of adsorbent or a mixture of a plurality of adsorbents.
Further, the filter is installed to crystallization kettle 4's bottom, the filter fineness of filter is 0.1um, the filter plays the solid-liquid separation effect.
Further, the purification system is provided with a sampling port 71 and a pressure gauge 72; the number of the sampling ports 71 and the pressure gauges 72 can be set according to actual conditions; the gas in the purification system can be sampled through a sampling port 71, and the pressure of each pipeline in the purification system can be observed through a pressure gauge 72.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (9)
1. The method for purifying the high-purity carbonyl sulfide is characterized by comprising the following steps of:
step S1: purging the adsorber and the container containing the adsorbent in the purification system until the moisture content of the purification system is less than 1ppm, and performing evacuation replacement on all pipelines and containers of the purification system by using high-purity helium gas until the nitrogen content in the system is less than 5ppm;
step S2: taking one raw material bottle of the raw material row as a flash evaporation collecting bottle, freezing the flash evaporation collecting bottle to-150 to-186 ℃, and carrying out flash evaporation treatment on carbonyl sulfide raw material gas in the raw material row to remove main light component impurities;
and step S3: opening refrigerant inlet valves of a precooler, a crystallization kettle and a cold trap, introducing refrigerants into the precooler, the crystallization kettle and the cold trap, and adjusting the opening degree of each refrigerant inlet valve so that the temperature of the precooler is controlled to be between-20 and-40 ℃, and the temperature of the crystallization kettle and the temperature of the cold trap are controlled to be between-150 and-186 ℃;
and step S4: opening an inlet valve of the precooler to enable the carbonyl sulfur raw material gas to enter the precooler so as to remove part of heavy component impurities in the carbonyl sulfur raw material gas;
opening an inlet valve of the adsorber, and allowing carbonyl sulfide gas to enter the adsorber to deeply remove heavy component impurities;
step S5: opening an inlet valve of the crystallization kettle, and allowing carbonyl sulfide gas to enter the crystallization kettle which reaches a set precooling temperature for crystallization, wherein the precooling temperature is-150 to-186 ℃, and keeping a crystallization state for 10 to 30 minutes;
step S6: discharging a refrigerant in the jacket of the crystallization kettle, introducing a heating medium into the jacket of the crystallization kettle to slowly melt carbonyl sulfide, observing the temperature in the crystallization kettle, stopping heating when the temperature of the crystallization kettle reaches-105 ℃, and discharging liquid carbonyl sulfide into a cold trap which reaches a set precooling temperature after passing through a filter;
step S7: freezing the collecting bottles in the collecting row to-150 to-186 ℃, introducing a heating medium into a jacket of the cold trap to heat the cold trap, and introducing gasified carbonyl sulfide into the collecting bottles to obtain qualified 4N carbonyl sulfide gas;
in the process of collecting the carbonyl gas in the step S7, the gas cylinder of the collecting and discharging is the gas cylinder which is frozen to-150 to-186 ℃ until the temperature of the cold trap is recovered to-10 ℃, the carbonyl sulfide gas collection is stopped, and after the temperature of the cold trap is continuously raised to normal temperature, the residual gas in the cold trap is collected by a transfer cylinder.
2. The method for purifying carbonyl sulfide as claimed in claim 1, wherein: the feeding amount of the carbonyl sulfide gas is not more than 3/4 of the volume of the crystallization kettle.
3. A purification system using the purification method of high-purity carbonyl sulfide according to any one of claims 1 to 2, characterized in that: comprises a raw material row, a precooler, an adsorber, a crystallization kettle, a cold trap and a collection row;
the output end of the raw material row is communicated to the input end of the precooler;
the output end of the precooler is communicated to the input end of the adsorber;
the output end of the adsorber is communicated to the input end of the crystallization kettle;
the output end of the crystallization kettle is communicated to the input end of the cold trap;
and the output end of the cold trap is communicated to the input end of the collection row.
4. The purification system of the purification process of high purity carbonyl sulfide as claimed in claim 3, wherein: the gas cylinders of the raw material row and the collecting row are low-temperature-resistant aluminum alloy gas cylinders.
5. The purification system of the purification process of high purity carbonyl sulfide as claimed in claim 3, wherein: the adsorbent is one or more of 3A molecular sieve, 4A molecular sieve, 5A molecular sieve, 10X molecular sieve, 13X molecular sieve, alumina, activated carbon and silica gel.
6. The purification system of a purification process of high purity carbonyl sulfide as claimed in claim 3, wherein: the precooler, the crystallization kettle and the cold trap are all containers with jackets.
7. The purification system of the purification process of high purity carbonyl sulfide as claimed in claim 3, wherein: the adsorber is a series combination of a plurality of adsorbers, and each adsorber is filled with a single type of adsorbent or a mixture of a plurality of adsorbents.
8. The purification system of a purification process of high purity carbonyl sulfide as claimed in claim 3, wherein: and a filter is arranged at the bottom of the crystallization kettle.
9. The purification system of the purification process of high purity carbonyl sulfide as claimed in claim 3, wherein: the purification system is provided with a sampling port and a pressure gauge.
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| US4098684A (en) * | 1976-11-29 | 1978-07-04 | Gulf Research & Development Company | Purification of liquid n-paraffins containing carbonyl sulfide and other sulfur compounds |
| KR20120008534A (en) * | 2009-05-07 | 2012-01-30 | 레르 리키드 쏘시에떼 아노님 뿌르 레？드 에렉스뿔라따시옹 데 프로세데 조르즈 클로드 | COS Purification Method |
| CN103328379B (en) * | 2011-04-18 | 2015-04-08 | 昭和电工株式会社 | Process for producing carbonyl sulfide |
| JP2013212950A (en) * | 2012-04-02 | 2013-10-17 | Toagosei Co Ltd | Method for producing high purity carbonyl sulfide |
| CN108786665B (en) * | 2018-05-25 | 2024-09-17 | 福建久策气体股份有限公司 | Carbonyl sulfide preparation device and application method |
| CN208667111U (en) * | 2018-08-21 | 2019-03-29 | 江西华特电子化学品有限公司 | A kind of purification system of carbonyl sulfur |
| CN109231207A (en) * | 2018-10-24 | 2019-01-18 | 欧中汇智电子材料研究院(重庆)有限公司 | Carbonyl sulphur preparing process and preparation facilities |
| 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 |
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