CN203741038U - Continuous production system of high-purity hydrochloric acid - Google Patents
Continuous production system of high-purity hydrochloric acid Download PDFInfo
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- CN203741038U CN203741038U CN201420160523.8U CN201420160523U CN203741038U CN 203741038 U CN203741038 U CN 203741038U CN 201420160523 U CN201420160523 U CN 201420160523U CN 203741038 U CN203741038 U CN 203741038U
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- hydrochloric acid
- online
- under vacuum
- high purity
- rectification under
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 238000010924 continuous production Methods 0.000 title claims abstract description 17
- 238000004821 distillation Methods 0.000 claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 19
- 150000002500 ions Chemical class 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 10
- 239000000460 chlorine Substances 0.000 claims description 10
- 229910052801 chlorine Inorganic materials 0.000 claims description 10
- 238000004587 chromatography analysis Methods 0.000 claims description 9
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000006396 nitration reaction Methods 0.000 claims description 9
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002912 waste gas Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000005388 borosilicate glass Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract 3
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 230000006837 decompression Effects 0.000 abstract 1
- 230000001939 inductive effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 13
- 239000000126 substance Substances 0.000 description 8
- 239000011162 core material Substances 0.000 description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 7
- 238000000746 purification Methods 0.000 description 5
- 241000370738 Chlorion Species 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000195 production control method Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 210000003905 vulva Anatomy 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a continuous production system of high-purity hydrochloric acid, which comprises a technical hydrochloric acid raw material tank, a circular stirring reaction kettle, a first intermediate tank, normal-pressure distillation equipment, a second intermediate tank, circular filter equipment, a third intermediate tank, decompression distillation equipment and a finish product collection tank which are sequentially arranged and communicated via connecting pipelines. The production system further comprises an on-line detection device and an alarm device, wherein the on-line detection device comprises an on-line acid mixer, an on-line chromometer, an on-line particle instrument, an on-line ion chromatograph and an on-line inductive coupling plasma mass spectrograph, and the alarm device gives an alarm when values detected by the on-line detection device exceed corresponding setting ranges.High-purity hydrochloric acid products meeting and even exceeding requirements of the SEMIC12 standard can be obtained by using the device and selecting appropriate technological parameters and conditions.In addition, the device is simple, low in energy consumption and high in efficiency, and the quality of the products produced continuously is stable.
Description
Technical field
The utility model relates to a kind of production equipment of producing the hydrochloric acid that high purity hydrochloric acid uses especially for the IC industry of microfabrication.
Background technology
Super-clean high-pure electronic chemical is the crucial integration starting material that super large-scale integration is manufactured, and its purity, cleanliness factor have very important impact to yield rate, electrical property, reliability etc.Current main-stream semiconductor technology has reached 0.09～0.2 μ m, and tip has reached 22 nanometer levels, and corresponding electronic chemical product has also reached SEMIC12 requirement.High pure electronic chemicals production technology is grasped by a few developed countries such as Germany, Japan and the U.S., and China only can produce elementary and intermediate electronic chemical product at present.High pure electronic purity of chemicals is more and more higher, and value-added content of product is larger.The research and development of ultra-pure electronic chemical product and technology thereof not only have higher strategic value, and also have higher economic worth and social benefit.On July 20th, 2012, State Council printed and distributed " State Council is about the notice of printing and distributing " 12 " national strategy new industry development program ", and high pure electronic chemical just belongs to the electronics key foundation industry in the generation information technical industry in notice.
High purity hydrochloric acid is one of semi-conductor electronic chemical product, is mainly used in the standard RCA cleaning of silicon chip.Be used for cleaning the impurity such as removal silicon chip surface metal and organism.The purity of hydrochloric acid has determined the amount of remained on surface metal, and then has determined the usefulness of semi-conductive yield rate and product.Preparation method about high purity hydrochloric acid has had a lot of relevant reports both at home and abroad, and main technology mode has several as follows:
One, high-purity chlorine, high-purity hydrogen purification techniques, high-purity hydrogen, chlorine reaction are prepared high-purity hydrogen chloride, and high purity water absorbs high-purity hydrogen chloride, prepares the technology of high purity hydrochloric acid.As patent CN97107008.3, adopt high-purity hydrogen, high-purity preparation of chlorine high-purity hydrogen chloride, then absorb and prepare high purity hydrochloric acid, but its to prepare hydrochloric acid be SILVER REAGENT, and do not provide the level of foreign matter content.Patent CN03150469.8, adopts this technique can produce the high purity hydrochloric acid of 20ppb left and right.Technique entirety is complicated, and danger coefficient is higher.
Two, high-purity hydrogen chloride is prepared purification techniques: by technical grade hydrogenchloride purification high-purity hydrogen chloride, then water absorbs.As the in situ preparation of high-purity continuity for the U.S.'s this tower Tyke Wen Qiesi patent CN96194539.7 semiconductor machining, adopt this kind of technology.Utilize this technique to prepare high purity hydrochloric acid, equipment requirements is higher, and danger is larger, and this patent application is in 1996, and Specifications can only reach ppb level, compared with requiring, can not reach production requirement with present SEMI12.Within 2004, Beijing Inst. of Chemical Reagent has also applied for similar patent CN200410091153.8, but regrettably in patent, does not provide corresponding detected result, cannot clearly contrast accordingly.The Japan CN97114388.9 of Tsurumi Soda Co., Ltd. adopts similar technique, provide the result that is less than 30ppt, but patent step is indefinite.Patent CN201110330097.9 adopts similar way, finally makes negatively charged ion and is less than 10ppb, and positively charged ion is less than the product of 50ppt, but does not provide the detailed data of every analysis.
Three, distillation technology boils in Asia: be about to be greater than 21% technical-grade hydrochloric acid and resolve, absorb the technique of resolving preparation of hydrogen chloride high purity hydrochloric acid with ultrapure water.As the patent CN00813864.8 of Merck KGaA, can reach negatively charged ion and be less than 100ppb, positively charged ion is less than the level of 1ppb.Patent CN200410093332.5 adopts this technique, but is only other industrial scale of 0.5kg/h laboratory-scale, and has 20% a large amount of diluted acids to produce, if without corresponding chlor-alkali plant, dilute acid pretreatment will become great problem.
Four, other purification techniquess: air distillation technology, adopt the technology of technical hydrochloric acid air distillation, as patent CN201110132548.8, step temperature difference distillation technology CN201110130302.7, purification by liquid extraction technology etc.These technology special emphasis are had nothing in common with each other, but that the hydrochloric acid obtaining does not all reach is very high-level.
In sum, the existing various high purity hydrochloric acid production technologies of having reported all remain on the level of preparing high purity hydrochloric acid.And vital long-term, extensive to semicon industry, stable, the production control method of low cost high purity hydrochloric acid and device, yet there are no relevant open report.
Summary of the invention
Technical problem to be solved in the utility model is to provide one simple high purity hydrochloric acid continuous process system is set, and utilizes this device can continuously, efficiently, stably obtain the high purity hydrochloric acid product that can be applicable to semicon industry.
For solving above technical problem, the utility model is taked following technical scheme:
A kind of high purity hydrochloric acid continuous process system, it has technical hydrochloric acid opening for feed, exhaust outlet, specifically comprise the technical hydrochloric acid head tank, circulation stirring reactor, the first tundish, atmospheric distillation equipment, the second tundish, circulating filtration equipment, the 3rd tundish, rectification under vacuum equipment, the finished product holding tank that set gradually and be communicated with by connecting tube, described production system is also included in line detector and warning device, and described on-line measuring device comprises:
Online nitration mixture instrument, it is for detecting in real time atmospheric distillation work in-process concentration;
Online colorimeter, it is for detecting in real time atmospheric distillation work in-process colourity and free chlorine content;
Online particle instrument, it is for detecting in real time circulating filtration work in-process granule content;
Online chromatography of ions, it is for detecting in real time finished product anion-content;
Online Inductively coupled plasma mass spectrometry, it is for detecting in real time finished product metal ion content;
When exceeding corresponding setting range, every value that described warning device detects at described on-line measuring device sends warning.
According to further embodiment of the present utility model: described online nitration mixture instrument, online colorimeter are all arranged between the second tundish and circulating filtration equipment; Described online particle instrument is arranged between circulating filtration equipment and the 3rd tundish; Described online chromatography of ions and online Inductively coupled plasma mass spectrometry are arranged between rectification under vacuum equipment and finished product holding tank.
Preferably, described production system is totally-enclosed super clean production system, and other parts except technical hydrochloric acid opening for feed are all in air-tight state, and described tundish, exhaust outlet are all the time with high pure nitrogen tonifying Qi sealing.
Further, described atmospheric distillation equipment comprises tower reactor, rectifying tower, steam heater and condenser, and the material of tower reactor is high purity graphite, and the material of rectifying tower and condenser is borosilicate glass.
Further, described rectification under vacuum equipment comprises rectification under vacuum tower reactor, rectification under vacuum king-post, rectification under vacuum condenser, counter flow controller, finished product water cooler, vacuum system, oil bath heating unit, described rectification under vacuum tower reactor, rectification under vacuum king-post, the material of rectification under vacuum condenser is pure quartz glass.
Further, described circulating filtration equipment comprises circulation tube that both ends are communicated with the second tundish, is successively set on pumping and multi-stage filter core on circulation tube.The material of circulation tube is PFA.Filter core material is PFA, and aperture is 0.1 μ m.
Preferably, described connecting tube adopts the high-purity tetrafluoroethylene of steel lining.
Preferably, described high purity hydrochloric acid continuous process system also comprises waste gas treatment equipment and waste liquor treatment equipment
Preferably, described atmospheric distillation holding tank adopts the sleeping tank of steel lining tetrafluoro plastics, and atmospheric distillation tower tower reactor adopts liner ptfe plastic tower reactor.
Utilize a concrete grammar of the utility model production high purity hydrochloric acid as follows:
(1) chemistry dechlorination: technical-grade hydrochloric acid and reducing substance such as tin protochloride, ferrous sulfate, oxalic acid etc. are joined in circulation stirring reactor, and circulation stirring reaction 1.5-2h, is reduced to the content of technical hydrochloric acid free chlorine below 300ppb;
(2) atmospheric distillation: enter atmospheric distillation equipment through the hydrochloric acid of step (1) and carry out atmospheric distillation, control vapor pressure 0.25 ± 0.05Mpa, flow 450 ± 50L/H, reflux ratio 1:1.2 ~ 2, condensate temperature is less than 4 ~ 8 DEG C.The content of every negatively charged ion except chlorion is reduced to below 800ppb, and every cation concn is reduced to below 2ppb.
(3) circulating filtration: by the hydrochloric acid after atmospheric distillation through filter core circulating filtration, to the concentration that is greater than 0.1 μ m granule density be down to 15/below ml;
(4) rectification under vacuum: by the hydrochloric acid rectification under vacuum after circulating filtration, control rectification temperature 60-80 DEG C, air pressure 20 ± 5Kpa, reflux ratio 1:1.8 ~ 2.5,0 ~ 5 DEG C of temperature of cooling water.Cation concn control is less than to 50ppt, except chlorion vulva ionic concn is less than 50ppb.
(5) setting of on-line measuring device:
The concentration setting range of a, online nitration mixture instrument is 36% ~ 37.5%, and the colourity setting range of online colorimeter is 10 once black for being less than, and free chlorine is less than 300ppb;
The particle setting range of b, online particle instrument is >0.1 μ m particle <15/ml.
Negatively charged ion (except the chlorion) setting range of c, online chromatography of ions is <50ppb;
The setting range of the metal ion of d, online Inductively coupled plasma mass spectrometry is <50ppt.
Due to the enforcement of above technical scheme, the utility model compared with prior art tool has the following advantages:
Utilize the utility model device, and select suitable processing parameter and condition, can obtain and meet the high purity hydrochloric acid product that even exceedes SEMI C12 standard-required.In addition, the utility model device is simple, energy consumption is low, and efficiency is high, continuously production constant product quality.
Brief description of the drawings
Below in conjunction with accompanying drawing and specific embodiment, the utility model is described in more detail:
Fig. 1 is according to the structural representation of high purity hydrochloric acid continuous process system of the present utility model;
Wherein: 1, technical hydrochloric acid head tank; 2, circulation stirring reactor; 3, the first tundish; 4, rectifying tower reactor; 5, atmospheric distillation tower; 6, conventional rectifying condenser; 7, atmospheric distillation holding tank; 8,0.2 μ m filter core; 9,0.1 μ m filter core; 10, the second tundish; 11, rectification under vacuum tower reactor; 12, rectification under vacuum king-post; 13, rectification under vacuum condenser; 14, counter flow controller; 15, finished product water cooler; 16, finished product holding tank; 17, finished product packing bucket; 18, vacuum system; 19, online nitration mixture instrument; 20, online colorimeter; 21, online particle instrument; 22, online chromatography of ions; 23, online Inductively coupled plasma mass spectrometry; 24, waste liquor treatment equipment; 25, waste gas treatment equipment.
Embodiment
Referring to Fig. 1, high purity hydrochloric acid continuous process system comprises technical hydrochloric acid head tank 1, circulation stirring reactor 2, the first tundish 3, atmospheric distillation equipment, the second tundish 7, circulating filtration equipment, the 3rd tundish 10, rectification under vacuum equipment, finished product holding tank 16, finished product packing bucket 17, waste liquor treatment equipment 24, waste gas treatment equipment 25, on-line measuring device and warning device.
Atmospheric distillation equipment mainly comprises heating unit (not shown) and the rectifying tower reactor 4 being connected successively, atmospheric distillation tower 5, atmospheric distillation condenser 6, atmospheric distillation holding tank (work in-process tank) 7.The material of rectifying tower reactor 4 is high purity graphite.The material of atmospheric distillation tower 5 and atmospheric distillation condenser 6 is borosilicate glass.
Circulating filtration equipment mainly comprises PFA corrugated tube, the pumping setting gradually on PFA corrugated tube, 0.2 μ m the filter core 8 and 0.1 μ m filter core 9 that both ends are communicated with atmospheric distillation holding tank 7 respectively.
Rectification under vacuum equipment mainly comprises rectification under vacuum tower reactor 11, rectification under vacuum king-post 12, rectification under vacuum condenser 13, counter flow controller 14, finished product water cooler 15, vacuum system 18.Rectification under vacuum tower reactor 11, rectification under vacuum king-post 12, the material of rectification under vacuum condenser 13 is pure quartz glass.
On-line measuring device comprises the online nitration mixture instrument 19 that is arranged between the second tundish 7 and circulating filtration equipment and online colorimeter 20, be arranged on online particle instrument 21 between circulating filtration equipment and the 3rd tundish 10, be arranged on online chromatography of ions 22 between rectification under vacuum equipment and finished product holding tank 16 and Inductively coupled plasma mass spectrometry 23 online.Online nitration mixture instrument 19 is for detecting in real time atmospheric distillation work in-process concentration; Online colorimeter 20 is for detecting in real time atmospheric distillation work in-process colourity and free chlorine content; Online particle instrument 21 is for detecting in real time circulating filtration work in-process granule content; Online chromatography of ions 22 is for detecting in real time finished product anion-content; Online Inductively coupled plasma mass spectrometry 23 is for detecting in real time finished product metal ion content.The concentration setting range of online nitration mixture instrument is 36% ~ 37.5%, and the colourity setting range of online colorimeter is 10 once black for being less than, and free chlorine is less than 300ppb; The particle setting range of online particle instrument is >0.1 μ m particle <15/ml.Negatively charged ion (except the chlorion) setting range of online chromatography of ions is <50ppb; The setting range of the metal ion of online Inductively coupled plasma mass spectrometry is <50ppt.
When exceeding corresponding setting range, every value that warning device detects at on-line measuring device sends warning.
Adopt production system of the present utility model to produce continuously a specific embodiment of high purity hydrochloric acid as follows.
(1) technical hydrochloric acid is passed in circulation stirring reactor, add weight is 0.8% ferrous sulfate of technical hydrochloric acid weight simultaneously, and circulation stirring reacts approximately 1.5 hours;
(2) hydrochloric acid of processing through step (1) passes into atmospheric distillation equipment with the flow of 500L/H, and control heating steam pressure is 0.25 ± 0.05Mpa, reflux ratio 1:1.2, and 4 ~ 8 DEG C of condensate temperatures, carry out rectifying, obtain atmospheric distillation work in-process;
(3) enter into circulating filtration equipment through the work in-process of step (2) and filter 2 hours, detect that the concentration that is wherein greater than 0.1 μ m granule density is less than 15/ml;
(4) enter into rectification under vacuum equipment through the work in-process of step (3) and carry out rectification under vacuum, feed rate 500L/H, controlling rectification under vacuum still internal pressure is 80KPa, reflux ratio is 1:2.5, obtain hydrochloric acid finished product, sampling detects data and shows, the content of metal ion is all below 5ppt, it is 10 once black that finished product colourity is less than, and free chlorine content is less than 300ppb.
Above the utility model is described in detail; its object is to allow the personage who is familiar with this art can understand content of the present utility model and be implemented; can not limit protection domain of the present utility model with this; all equivalences of doing according to spirit of the present utility model change or modify, and all should be encompassed in protection domain of the present utility model.
Claims (8)
1. a high purity hydrochloric acid continuous process system, it is characterized in that: described production system has technical hydrochloric acid opening for feed, exhaust outlet, specifically comprise the technical hydrochloric acid head tank, circulation stirring reactor, the first tundish, atmospheric distillation equipment, the second tundish, circulating filtration equipment, the 3rd tundish, rectification under vacuum equipment, the finished product holding tank that set gradually and be communicated with by connecting tube, described production system is also included in line detector and warning device, and described on-line measuring device comprises:
Online nitration mixture instrument, it is for detecting in real time atmospheric distillation work in-process concentration;
Online colorimeter, it is for detecting in real time atmospheric distillation work in-process colourity and free chlorine content;
Online particle instrument, it is for detecting in real time circulating filtration work in-process granule content;
Online chromatography of ions, it is for detecting in real time finished product anion-content;
Online Inductively coupled plasma mass spectrometry, it is for detecting in real time finished product metal ion content;
When exceeding corresponding setting range, every value that described warning device detects at described on-line measuring device sends warning.
2. high purity hydrochloric acid continuous process system according to claim 1, is characterized in that: described online nitration mixture instrument, online colorimeter are all arranged between described the second tundish and described circulating filtration equipment; Described online particle instrument is arranged between described circulating filtration equipment and described the 3rd tundish; Described online chromatography of ions and online Inductively coupled plasma mass spectrometry are arranged between described rectification under vacuum equipment and described finished product holding tank.
3. high purity hydrochloric acid continuous process system according to claim 1, it is characterized in that: described production system is totally-enclosed super clean production system, other parts except described technical hydrochloric acid opening for feed are all in air-tight state, and described tundish, exhaust outlet are all the time with high pure nitrogen tonifying Qi sealing.
4. high purity hydrochloric acid continuous process system according to claim 1, it is characterized in that: described atmospheric distillation equipment comprises tower reactor, rectifying tower, steam heater and condenser, the material of described tower reactor is high purity graphite, and the material of described rectifying tower and condenser is borosilicate glass.
5. high purity hydrochloric acid continuous process system according to claim 1, it is characterized in that: described rectification under vacuum equipment comprises rectification under vacuum tower reactor, rectification under vacuum king-post, rectification under vacuum condenser, counter flow controller, finished product water cooler, vacuum system, oil bath heating unit, described rectification under vacuum tower reactor, rectification under vacuum king-post, the material of rectification under vacuum condenser is pure quartz glass.
6. high purity hydrochloric acid continuous process system according to claim 1, it is characterized in that: described circulating filtration equipment comprises circulation tube that both ends are communicated with the second described tundish, is successively set on pumping and multi-stage filter core on described circulation tube, and the material of described circulation tube is PFA.
7. high purity hydrochloric acid continuous process system according to claim 1, is characterized in that: described connecting tube adopts the high-purity tetrafluoroethylene of steel lining.
8. high purity hydrochloric acid continuous process system according to claim 1, is characterized in that: described high purity hydrochloric acid continuous process system also comprises waste gas treatment equipment and waste liquor treatment equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420160523.8U CN203741038U (en) | 2014-04-03 | 2014-04-03 | Continuous production system of high-purity hydrochloric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420160523.8U CN203741038U (en) | 2014-04-03 | 2014-04-03 | Continuous production system of high-purity hydrochloric acid |
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| Publication Number | Publication Date |
|---|---|
| CN203741038U true CN203741038U (en) | 2014-07-30 |
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| CN201420160523.8U Expired - Lifetime CN203741038U (en) | 2014-04-03 | 2014-04-03 | Continuous production system of high-purity hydrochloric acid |
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| Country | Link |
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| CN (1) | CN203741038U (en) |
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2014
- 2014-04-03 CN CN201420160523.8U patent/CN203741038U/en not_active Expired - Lifetime
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