CN103387211B - With commercial synthesis hydrogenchloride for the method for electronic grade high-purity hydrogenchloride prepared by raw material - Google Patents
With commercial synthesis hydrogenchloride for the method for electronic grade high-purity hydrogenchloride prepared by raw material Download PDFInfo
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Abstract
The invention discloses a kind of with commercial synthesis hydrogenchloride for the method for electronic grade high-purity hydrogenchloride prepared by raw material, commercial synthesis hydrogenchloride removes through multistage physical dryness, adsorbing and removing carbonic acid gas, compression condensation, rectifying the electronic grade high-purity hydrogenchloride that the low-boiling point gas such as nitrogen, oxygen, hydrogen, carbon monoxide, methane obtain more than 99.999%.This preparation method's cost is low, and income is high, and obtained product purity is high, and product can be widely used in the preparation of opticfiber communication, microelectronics, high temperature superconducting materia.
Description
Technical field
The present invention relates to a kind of preparation method of electronic grade high-purity hydrogenchloride, particularly a kind of with commercial synthesis hydrogenchloride for feed purification prepares the method for electronic grade high-purity hydrogenchloride.
Background technology
Electronic grade high-purity hydrogenchloride is the important materials of the techniques such as silicon chip etching during unicircuit is produced, passivation, extension, gas phase polishing, gettering and clean process, also can be used for Metal smelting, the field such as optical communications and scientific research.Along with the development of large-scale integrated circuit, more and more higher to the requirement of hydrogenchloride purity, except the purity of more than 99.999% should be had, more and more harsher to the content requirement of wherein impurity, especially the content of strict limiting carbon hydrogen compound and hydrocarbon is required, to prevent the formation of C in silicon chip working process.Past, China was mostly from beautiful, Deng state Imported Electronic level hydrogenchloride, but in recent years, the development of the chemical gas needed for China's electronic industry, technically existing many breakthroughs and development.Domestic Ye You unit successfully develops relevant electronic grade hydrogen chloride product, but also far can not meet the need of market.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of with commercial synthesis hydrogenchloride for feed purification prepares the method for electronic grade high-purity hydrogenchloride.
For achieving the above object, the present invention takes following technical proposals to realize:
With commercial synthesis hydrogenchloride for the method for electronic grade high-purity hydrogenchloride prepared by raw material, comprise the following steps:
A., after primary industry hydrogenchloride compresses after filtration, enter bottom the one-level drying tower that siccative is housed, after adsorbing and removing most of moisture from tower top out;
B. enter the secondary drying tower bottom that siccative is housed again, through deep dehydration, to remove after micro-moisture from tower top out, the moisture content removed in post chlorization hydrogen is less than 0.5ppm;
C. then enter bottom the adsorption tower that sorbent material is housed, after absorption, carbon dioxide content is less than 2ppm after adsorbing and removing carbonic acid gas and denier moisture from tower top out;
D. pressurize, enter de-light rectifying tower after condensation, nitrogen, oxygen, hydrogen, carbon monoxide, the low-boiling point gas such as methane are discharged from tower top, form tail gas and reclaim, remove rear a nitrogen content and be less than 2ppm, oxygen content is less than 1ppm, and carbon monoxide content is less than 1ppm, and methane is less than 1ppm;
E. at the bottom of de-light rectifying tower, hydrogen chloride liquid out enters de-heavy rectifying tower again, and vaporization removes the high boiling component heavier than hydrogenchloride;
F. eject from de-heavy rectifying tower the high-purity hydrogen chloride purity come and reach more than 99.999%, compressed bulking system bottling, the high-purity hydrogen chloride after bottling, metal ion total content is less than 0.3ppm.
Further, multistage physical dryness can also be provided with after step b.
Further, the siccative in step a and step b is zeolite molecular sieve.
Preferably, the siccative in step a and step b is 13X zeolite molecular sieve.
Further, the sorbent material in step c is zeolite molecular sieve.
Preferably, the sorbent material in step c is SSZ-13 zeolite molecular sieve.
Preferably, the siccative in step a and step b, the sorbent material in step c is all through 200 DEG C of high-temperature chlorine gas disposals two hours.
Further, after step a Raw commercial synthesis hydrogenchloride compresses after filtration, under the pressure and normal temperature of 0.3-0.6MP, with 1-5M
3the flow of/h enters one-level drying tower.
Further, in steps d hydrogenchloride from adsorption tower out after, be compressed to 1.5-2.5MP, be cooled to-15 DEG C--25 DEG C.
Preferably, in steps d hydrogenchloride from adsorption tower out after, be compressed to 2.0MP, be cooled to-20 DEG C.
The present invention has following technique effect: remove the low-boiling point gas such as nitrogen, oxygen, hydrogen, carbon monoxide, methane and the micro-high boiling material heavier than hydrogenchloride, the electronic grade high-purity hydrogenchloride of obtained more than 99.999% by commercial synthesis hydrogenchloride through multistage physical dryness, adsorbing and removing carbonic acid gas, compression condensation, rectifying.This preparation method's cost is low, and income is high, and obtained product purity is high, and product can be widely used in multiple public good in unicircuit production, also may be used for Metal smelting, other field of scientific studies such as optical communications.
Further, according to water content and the product purity requirement of different material product, multistage physical dryness can be set, fully remove the moisture in raw material.
Further, siccative of the present invention can use the model zeolite molecular sieves such as 3A, 5A, 13X, preferred 13X molecular sieve desiccant, this siccative does not react with hydrogenchloride, and water-retaining capacity is large, and possesses enough intensity, and metal ion and dust can not be brought into hydrogen chloride gas, easily regenerate.
Further, sorbent material can adopt the sorbent materials such as 5A, 13X, SSZ-13 zeolite molecular sieve, and preferred SSZ-13 zeolite molecular sieve, SSZ-13 is functional to carbon dioxide adsorption, easily regenerates.
Further, siccative used in the present invention and sorbent material are all through 200 DEG C of high-temperature chlorine gas disposals 2 hours, and after process, dust rate reduces, intensity enhancing, can meet dry and adsorption entails.
Accompanying drawing explanation
Fig. 1 is process flow sheet in the embodiment of the present invention 1.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be described in detail.
Embodiment 1:
Fig. 1 is the process flow sheet of preparation method of the present invention.As shown in Figure 1, preparation method of the present invention comprises the following steps:
A. primary industry hydrogenchloride removes mechanical impurity more after compression after filtration, with 1M under the pressure and normal temperature of 0.4MP
3the flow of/h from be equipped with numbering DH05 13X type zeolite molecular sieve one-level drying tower 1 bottom enter, after adsorbing and removing most of moisture from tower top out;
B. enter the secondary drying tower bottom of the 13X type zeolite molecular sieve that numbering DH06 is housed again, through deep dehydration, to remove after micro-moisture from tower top out, the moisture content removed in post chlorization hydrogen is less than 0.5ppm;
C. then enter bottom the adsorption tower that SSZ-13 zeolite molecular sieve is housed, after absorption, carbon dioxide content is less than 2ppm after adsorbing and removing carbonic acid gas and denier moisture from tower top out;
D. 2.2MP is forced into, de-light rectifying tower is entered, nitrogen, oxygen after being condensed to-18 DEG C, hydrogen, carbon monoxide, the low-boiling point gas such as methane are discharged from tower top, form tail gas and reclaim, remove rear a nitrogen content and be less than 2ppm, oxygen content is less than 1ppm, and carbon monoxide content is less than 1ppm, and methane is less than 1ppm;
E. at the bottom of de-light rectifying tower, hydrogen chloride liquid out enters de-heavy rectifying tower again, and vaporization removes the high boiling component heavier than hydrogenchloride;
F. eject from de-heavy rectifying tower the high-purity hydrogen chloride purity come and reach more than 99.999%, compressed bulking system bottling, high-purity hydrogen chloride after bottling, metal ion total content is less than 0.3ppm, wherein metal ion removes a part by sorbent material, removes remainder additionally by de-heavy rectifying tower.
The present invention adopts commercial synthesis hydrogenchloride as raw material, major cause is: in petrochemical complex by-product hydrogen chloride, organic impurity is many, particularly C2 hydro carbons not easily and HCl separation, and the organic impurity of synthesising hydrogen wants much less relatively, compares petrochemical complex by-product hydrogen chloride easily purifying.Whole nation by-product hydrogen chloride is a lot, and be used for synthetic hydrochloric acid at present, the price of hydrochloric acid is lower, and profit is not high, and electronic grade hydrogen chloride is expensive, can be enterprise and brings benefit.
Siccative used in the present invention and sorbent material are all through 200 DEG C of high-temperature chlorine gas disposals 2 hours, and after process, dust rate reduces, intensity enhancing, can meet dry and adsorption entails.
In order to repeatedly reuse siccative and sorbent material in the present invention, use constant-pressure and high-temperature reclaiming process to make it regeneration, the siccative after regeneration and sorbent material can meet this processing requirement.
Realizing continuous prodution for enhancing productivity, can arrange and organize dry adsorption unit more, after one group of device adsorptive power declines, only need be switched to another group adsorption unit, need not stop, one group under being switched enters step for regeneration and regenerates rear for subsequent use simultaneously.
In this technique, all pipeline equipments are all through de-oiling and slagging-off primary treatment, polishing, passivation and dehydration special processing and the precision process before filling, ensure the isolation of system and air in filling process, make bottled product each component content and online product content measured value basically identical.
Embodiment 2:
Preparation method of the present invention comprises the following steps:
A. after primary industry hydrogenchloride compresses after filtration, with 1.5M under the pressure and normal temperature of 0.3MP
3the flow of/h from be equipped with numbering DH05 13X type zeolite molecular sieve one-level drying tower 1 bottom enter, after adsorbing and removing most of moisture from tower top out;
B. enter the secondary drying tower bottom of the 13X type zeolite molecular sieve that numbering DH06 is housed again, through deep dehydration, to remove after micro-moisture from tower top out, the moisture content removed in post chlorization hydrogen is less than 0.5ppm;
C. then enter bottom the adsorption tower that SSZ-13 zeolite molecular sieve is housed, after absorption, carbon dioxide content is less than 2ppm after adsorbing and removing carbonic acid gas and denier moisture from tower top out;
D. 2.0MP is forced into, de-light rectifying tower is entered, nitrogen, oxygen after being condensed to-20 DEG C, hydrogen, carbon monoxide, the low-boiling point gas such as methane are discharged from tower top, form tail gas and reclaim, remove rear a nitrogen content and be less than 2ppm, oxygen content is less than 1ppm, and carbon monoxide content is less than 1ppm, and methane is less than 1ppm;
E. at the bottom of de-light rectifying tower, hydrogen chloride liquid out enters de-heavy rectifying tower again, and vaporization removes the high boiling component heavier than hydrogenchloride;
F. eject from de-heavy rectifying tower the high-purity hydrogen chloride purity come and reach more than 99.999%, compressed bulking system bottling, the high-purity hydrogen chloride after bottling, metal ion total content is less than 0.3ppm.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; the Method and Technology content of above-mentioned announcement can be utilized to make possible variation and amendment to technical solution of the present invention; therefore; every content not departing from technical solution of the present invention; according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification, all belong to the protection of technical solution of the present invention.
Claims (10)
1. with commercial synthesis hydrogenchloride for the method for electronic grade high-purity hydrogenchloride prepared by raw material, it is characterized in that, comprise the following steps:
A., after primary industry hydrogenchloride compresses after filtration, enter bottom the one-level drying tower that siccative is housed, after adsorbing and removing most of moisture from tower top out;
B. enter the secondary drying tower bottom that siccative is housed again, through deep dehydration, to remove after micro-moisture from tower top out, the moisture content removed in post chlorization hydrogen is less than 0.5ppm;
C. then enter bottom the adsorption tower that sorbent material is housed, after absorption, carbon dioxide content is less than 2ppm after adsorbing and removing carbonic acid gas and denier moisture from tower top out;
D. pressurize, enter de-light rectifying tower after condensation, nitrogen, oxygen, hydrogen, carbon monoxide, methane low-boiling point gas is discharged from tower top, form tail gas and reclaim, remove rear a nitrogen content and be less than 2ppm, oxygen content is less than 1ppm, and carbon monoxide content is less than 1ppm, methane is less than 1ppm, and hydrogen content is less than 0.2ppm;
E. at the bottom of de-light rectifying tower, hydrogen chloride liquid out enters de-heavy rectifying tower again, and vaporization removes the high boiling component heavier than hydrogenchloride and most of metal ion;
F. eject from de-heavy rectifying tower the high-purity hydrogen chloride purity come and reach more than 99.999%, compressed bulking system bottling, the high-purity hydrogen chloride after bottling, metal ion total content is less than 0.3ppm.
2. method according to claim 1, is characterized in that, is also provided with multistage physical dryness after step b.
3. method according to claim 1, is characterized in that, the siccative in step a and step b is zeolite molecular sieve.
4. method according to claim 2, is characterized in that, the siccative in step a and step b is 13X zeolite molecular sieve.
5. method according to claim 1, is characterized in that, the sorbent material in step c is zeolite molecular sieve.
6. method according to claim 4, is characterized in that, the sorbent material in step c is SSZ-13 zeolite molecular sieve.
7. the method according to claim 1-6 any one, is characterized in that, the siccative in step a and step b, and the sorbent material in step c is all through 200 DEG C of high-temperature chlorine gas disposals two hours.
8. method according to claim 7, is characterized in that, after step a Raw commercial synthesis hydrogenchloride compresses after filtration, under the pressure and normal temperature of 0.3-0.6MPa, with 1-5M
3the flow of/h enters one-level drying tower.
9. method according to claim 7, is characterized in that, in steps d hydrogenchloride from adsorption tower out after, be compressed to 1.5-2.5MPa, be cooled to-15 DEG C--25 DEG C.
10. method according to claim 9, is characterized in that, in steps d hydrogenchloride from adsorption tower out after, be compressed to 2.0MPa, be cooled to-20 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399053B (en) * | 2015-12-07 | 2018-01-30 | 南通山剑石墨设备有限公司 | Hydrogen chloride drying system |
| CN105502294B (en) * | 2015-12-28 | 2018-11-20 | 青岛科技大学 | A kind of electronic grade high-purity hydrogen chloride high pressure method for preparing |
| CN106276796B (en) * | 2016-07-19 | 2019-06-14 | 浙江博瑞电子科技有限公司 | A method of preparing high-purity hydrogen chloride |
| CN107746040B (en) * | 2017-10-17 | 2021-04-13 | 山东新龙科技股份有限公司 | Process and equipment for refining hydrogen chloride by using byproduct gas from production of trichloroethylene |
| CN107840307A (en) * | 2017-11-30 | 2018-03-27 | 南通星球石墨设备有限公司 | A kind of HCl gas synthesis driving system |
| CN108557766B (en) * | 2018-02-11 | 2019-12-27 | 浙江博瑞电子科技有限公司 | Refining method of hydrogen chloride |
| CN109368593B (en) * | 2018-11-26 | 2020-04-10 | 浙江博瑞电子科技有限公司 | Method for preparing electronic grade hydrogen chloride gas containing ppbv grade moisture impurities |
| CN110508105B (en) * | 2019-08-28 | 2021-08-10 | 山东康宝生化科技有限公司 | Device and method for separating carbon dioxide and hydrogen chloride from sucralose tail gas |
| KR20230058221A (en) | 2021-10-22 | 2023-05-03 | 효성화학 주식회사 | Methode for preparing high-purity hydrogen chloride |
| CN113816338A (en) * | 2021-11-09 | 2021-12-21 | 湖北和远气体股份有限公司 | Preparation device and process of ultra-high-purity hydrogen chloride gas for semiconductor |
| CN114634163B (en) * | 2022-05-18 | 2022-08-05 | 北京化工大学 | Production device and method for manufacturing electronic grade hydrogen chloride |
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| CN1644487A (en) * | 2004-12-21 | 2005-07-27 | 上海氯碱化工股份有限公司 | Apparatus and method for preparing high-purity hydrochloric acid by low-temperature evaporation |
| CN101200286A (en) * | 2007-12-05 | 2008-06-18 | 南京大学 | Method for refining byproduct hydrogen chloride during production process of organochlorine products |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644487A (en) * | 2004-12-21 | 2005-07-27 | 上海氯碱化工股份有限公司 | Apparatus and method for preparing high-purity hydrochloric acid by low-temperature evaporation |
| CN101200286A (en) * | 2007-12-05 | 2008-06-18 | 南京大学 | Method for refining byproduct hydrogen chloride during production process of organochlorine products |
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