CN104192803B - A kind of sub-boiling distillation method of high purity hydrochloric acid - Google Patents
A kind of sub-boiling distillation method of high purity hydrochloric acid Download PDFInfo
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- CN104192803B CN104192803B CN201410457895.1A CN201410457895A CN104192803B CN 104192803 B CN104192803 B CN 104192803B CN 201410457895 A CN201410457895 A CN 201410457895A CN 104192803 B CN104192803 B CN 104192803B
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Abstract
The present invention relates to a kind of sub-boiling distillation method of high purity hydrochloric acid, with the hydrochloric acid from fluorine carbon alkane production equipment for raw material, Membrane-distillation operation is carried out in the sub-boiling distillation device of specifying, control the processing parameters such as preheating temperature, Heating temperature, condensing temperature and circular flow, preparation concentration is greater than 35.0%, metal ion content is less than the high purity hydrochloric acid of 1ppb, and the index of its metal ion meets the Semi-C8 standard that semiconductor equipment and material structure (SEMI) propose.The present invention can solve metal ion in high-purity hydrochloric acid and remove this problem, effectively improves distillation rate simultaneously.
Description
Technical field
The present invention relates to a kind of sub-boiling distillation method of high purity hydrochloric acid.
Background technology
Ultra-clean and high pure chemical reagent (ProcessChemicals) is one of key basic chemical industry material in microelectronics industry, particularly super large-scale integration making processes, be mainly used in cleaning and the corrosion of chip, its purity and cleanliness factor have very important impact to the yield rate of unicircuit, electrical property and reliability.High-purity hydrochloric acid is the one that in ultra clean reagents, demand is larger, is the product that a kind of added value is higher.
The purification techniques of ultra-clean and high pure chemical reagent has following several: distillation and rectifying, isothermal distillation, sub-boiling distillation, underpressure distillation, distillation, chemical treatment method, gas absorption techniques, Grain size controlling technology etc.The Con trolling index of high-purity hydrochloric acid relates to multinomial content, comprises concentration, colourity, organic impurity, free chlorine contents, acid ion content, metal ion content, granularity etc.So far, the effect without any a kind of purification techniques can meet numerous index requests simultaneously, and the comprehensive utilization of multiple purification techniques often, can achieve the goal.With regard to the removal of metal ion, generally take the method for sub-boiling distillation.
Traditional sub-boiling distillation device is generally made up of high purity quartz material or fluorine polymeric material, its structure is oblique cutting one prolong in the large silica tube of closed at both ends, be wound with a U-shaped silica tube below, electric stove wire is had as well heater in pipe, well heater is direct heating liquid not, relies on radiation heating fluid surface.Three apertures are arranged at distiller bottom, use respectively as feed, overflow and collection distillate.Its generating surface of the method for this sub-boiling distillation is less, and vaporator rate is comparatively slow, and energy utilization rate is lower.There is bibliographical information, refine nitric acid with traditional sub-boiling distillation device, under the heating power of 150W, ability preparation in 8 hours about 200 milliliters of refining nitric acid; Under the heating power of 400W, within 8 hours, can prepare about 1200 milliliters of high purity waters, this is mainly subject to the restriction of type of heating and evaporation mode.
Other correlation technique as: CN102874757A discloses a kind of preparation method of high purity hydrochloric acid, use technical hydrochloric acid is raw material, by art breading such as evaporation, ultrafiltration, absorption, sub-boiling distillations, preparation meets the high purity hydrochloric acid of HG/T2778-2009 industry standard; The method of Henan chemical industry [2010,27 (7), 61-62] is by carrying out process modification to technical hydrochloric acid preparation facilities, and the technical hydrochloric acid concentration of preparation is greater than 36.0%, Fe and is less than 3mg/L; Shanghai chemical industry for making chlorine and alkali [2006, (1), 13-17] research optimization is carried out to the technique of traditional sub-boiling distillation, the concentration of hydrochloric acid of preparation can reach 36-38%, metal ion content is less than 0.1ppb, reach the Semi-C12 standard that semiconductor equipment and material structure (SEMI) propose, but distillation rate is comparatively slow, can only reach 150-200 ml/hour.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, provides a kind of sub-boiling distillation method of high purity hydrochloric acid.
For solving above technical problem, the present invention adopts following technical scheme:
A kind of sub-boiling distillation method of high purity hydrochloric acid, described sub-boiling distillation method is that the hydrochloric acid from fluorine carbon alkane production equipment is entered distiller after preheater preheats, falling film type evaporation is carried out in described distiller, steam after evaporation is collected and is obtained high purity hydrochloric acid in described distiller after condensation, be not pumped in described preheater by the liquid evaporated by recycle pump, wherein, described distiller comprises the kettle with heating jacket, be arranged on the end socket at described kettle top, be arranged on the condenser for steam described in condensation in described kettle, to be arranged in described kettle and the liquid trap be positioned at below described condenser and the film applicator arranged near described kettle inner side-wall, side near described kettle inner side-wall on described film applicator offers multiple discharge hole, the material of described preheater enters in described film applicator, be ejected into described kettle inner side-wall film forming through described discharge hole again to flow down, the concentration of described high purity hydrochloric acid is greater than 35.0%, and in described high purity hydrochloric acid, metal ion content is less than 1ppb, and the preheating temperature of described preheater is 55 ~ 65 DEG C, the Heating temperature of described distiller is 65 ~ 75 DEG C.
Described film applicator be along described kettle circumferential direction around ring pipe, the side of the close described kettle inner side-wall of described ring pipe and the gap of described kettle inner side-wall are 1 ~ 10mm.
Multiple described discharge hole is uniformly distributed along the length direction of described ring pipe on described ring pipe.
Described film applicator is positioned at the top of described heating jacket and arranges near described heating jacket.
Described condenser is connected with described end socket, and the cooling medium inlet pipe of described condenser and outlet pipe all stretch out outside described kettle through described end socket; Described liquid trap is connected with the bottom of described kettle, and the discharge nozzle of described liquid trap stretches out outside described kettle through the bottom of described kettle.
The liquid collection opening of described liquid trap is positioned at immediately below described condenser, and the cross-sectional area of the liquid collection opening of described liquid trap is greater than the cross-sectional area of described condenser.
The cooling temperature of described condenser is 0 ~ 15 DEG C.
The flow of described recycle pump is 0.06 × S ~ 0.3 × S, unit is m
3/ h, wherein, S is the evaporation area of described distiller, unit is m
2.The evaporation area of described distiller is the area of the inner side-wall of described kettle.
In order to ensure the concentration of product and prevent fouling on kettle inner side-wall, require that the described concentration from the hydrochloric acid of fluorine carbon alkane production equipment is greater than 33.0%, be describedly less than 200mg/L from the metal ion content in the hydrochloric acid of fluorine carbon alkane production equipment.
Due to the enforcement of technique scheme, the present invention compared with prior art tool has the following advantages:
In method of the present invention, material evaporates with the form of dynamically formed membrane in distiller, can significantly increase its evaporation area, accelerates the volatilization of its steam, accelerates vaporator rate, collects the feed liquid after evaporation in distiller simultaneously.The concentration of high purity hydrochloric acid adopting the inventive method to prepare is greater than 35.0%, and its metal ion content is less than 1ppb, and the index of metal ion meets the Semi-C8 standard that semiconductor equipment and material structure (SEMI) propose.
Figure of description
Fig. 1 is the process flow sheet of sub-boiling distillation method of the present invention;
Fig. 2 is the part sectioned view of the distiller in sub-boiling distillation method of the present invention;
In figure: 1, preheater; 2, recycle pump; 3, feed-pipe; 4, condenser; 5, end socket; 6, film applicator; 7, kettle; 8, heating jacket; 9, liquid trap; 10, discharge hole.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the present invention is not limited to following examples.
As shown in Fig. 1 ~ 2, the process flow sheet of sub-boiling distillation method of the present invention, material enters distiller after preheater 1 preheating, falling film type evaporation is carried out in distiller, steam after evaporation obtains high purity hydrochloric acid collecting after condensation in distiller, not to be pumped in preheater 1 by recycle pump 2 by the liquid that evaporates and to circulate.
This distiller comprises the kettle 7 with heating jacket 8, the end socket 5 being arranged on kettle 7 top, be arranged on the condenser 4 for condensed steam in kettle 7 and be arranged in kettle 7 and the liquid trap 9 be positioned at below condenser 4, this distiller also comprises the film applicator 6 arranged near kettle 7 inner side-wall, side near kettle 7 inner side-wall on film applicator 6 offers multiple discharge hole 10, the material of preheater 1 enters in film applicator 6, then is ejected into kettle 7 inner side-wall film forming through discharge hole 10 and flows down.Be connected by flange or ground between end socket 5 with kettle 7.
Film applicator 6 be along kettle 7 circumferential direction around ring pipe, the side of close kettle 7 inner side-wall of ring pipe and the gap of kettle 7 inner side-wall are 1-10mm.Multiple discharge hole 10 on ring pipe annularly the length direction of pipe be uniformly distributed.The size of discharge hole 10 and distribution meet the requirement of even cloth film.The setting of film applicator 6 is positioned at the top of heating jacket 8 and arranges near heating jacket 8.
Condenser 4 is connected with end socket 5, and the cooling medium inlet pipe of condenser 4 and outlet pipe all stretch out through end socket outside kettle 7, and particularly, condenser 4 can duplex coiled tube condenser; Liquid trap 9 is connected with the bottom of kettle 7, and the discharge nozzle of liquid trap 9 stretches out outside kettle 7 through the bottom of kettle 7, and particularly, liquid trap 9 can be triangular funnel form.
Particularly, liquid trap 9 is positioned at immediately below condenser 4, and the cross-sectional area of the liquid collection opening of liquid trap 9 is greater than the cross-sectional area of condenser 4.
Below by specific embodiment, sub-boiling distillation method of the present invention is described further.
Embodiment 1 ~ 7
Raw material hydrochloric acid adopts the hydrochloric acid from fluorine carbon alkane production equipment, and the kettle 7 internal diameter D=500mm of the distiller of employing, the height H=800mm of heating jacket 8, the surface-area of kettle 7 inner side-wall is S=1.256m
2, the surface-area of kettle 7 inner side-wall is evaporation area.Control related process parameters, after having cut extraction, the collection liquid of first 2 hours is collected separately, afterwards as formal product.Relevant implementation data sees the following form 1:
Table 1
Data as can be seen from upper table, Heating temperature, condensing temperature, internal circulating load all have considerable influence for the quality of product hydrochloric acid and flow, operate within implementing process parameter of the present invention, can meet concentration of hydrochloric acid be greater than 35.0% and metal ion be less than the requirement of 1ppb.
Sub-boiling distillation method of the present invention can solve the contradiction of boiling between middle production quality control and velocity of evaporation Asia simultaneously, as:
(1) by accurately controlling preheating temperature and the Heating temperature of material, meet the high product quality of sub-boiling distillation, wherein, the heat source temperature that the heat source temperature that preheating temperature is preheater 1, Heating temperature are heating jacket 8, concrete control, the temperature of preheater 1 endogenous pyrogen is less than the temperature of the thermal source in heating jacket 8, and the fluctuation of control of heat source temperature is no more than 0.5 DEG C.
(2) by increasing film applicator in the kettle that condenser and liquid trap are housed, material being evaporated with the form of dynamically formed membrane in kettle, can significantly increase its evaporation area, accelerate the volatilization of its steam, accelerate vaporator rate.
(3) by design and the coolant temperature control of the duplex coil pipe of condenser 4, significantly increase condensation area, accelerate its vapor condensation, increase condensing rate, the fluctuation of controlled cooling model medium temperature is no more than 0.5 DEG C.
(4) by increasing the circulation being arranged so that material of recycle pump 2, save the energy, improve efficiency of energy utilization, the flow of recycle pump 2 should be accurate, and can be adjusted according to concrete applicable cases.
Above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; and the invention is not restricted to the embodiments described; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed within protection scope of the present invention.
Claims (8)
1. the sub-boiling distillation method of a high purity hydrochloric acid, it is characterized in that: described sub-boiling distillation method is that the hydrochloric acid from fluorine carbon alkane production equipment is entered distiller after preheater preheats, falling film type evaporation is carried out in described distiller, steam after evaporation is collected and is obtained high purity hydrochloric acid in described distiller after condensation, be not pumped in described preheater by the liquid evaporated by recycle pump, wherein, described distiller comprises the kettle with heating jacket, be arranged on the end socket at described kettle top, be arranged on the condenser for steam described in condensation in described kettle, to be arranged in described kettle and the liquid trap be positioned at below described condenser and the film applicator arranged near described kettle inner side-wall, side near described kettle inner side-wall on described film applicator offers multiple discharge hole, the material of described preheater enters in described film applicator, be ejected into described kettle inner side-wall film forming through described discharge hole again to flow down, the concentration of described high purity hydrochloric acid is greater than 35.0%, and in described high purity hydrochloric acid, metal ion content is less than 1ppb, and the preheating temperature of described preheater is 55 ~ 65 DEG C, the Heating temperature of described distiller is 65 ~ 75 DEG C, and the concentration of the described hydrochloric acid from fluorine carbon alkane production equipment is greater than 33.0%, is describedly less than 200mg/L from the metal ion content in the hydrochloric acid of fluorine carbon alkane production equipment.
2. the sub-boiling distillation method of high purity hydrochloric acid according to claim 1, it is characterized in that: described film applicator be along described kettle circumferential direction around ring pipe, the side of the close described kettle inner side-wall of described ring pipe and the gap of described kettle inner side-wall are 1 ~ 10mm.
3. the sub-boiling distillation method of high purity hydrochloric acid according to claim 2, is characterized in that: multiple described discharge hole is uniformly distributed along the length direction of described ring pipe on described ring pipe.
4. the sub-boiling distillation method of high purity hydrochloric acid according to claim 1, is characterized in that: described film applicator is positioned at the top of described heating jacket and arranges near described heating jacket.
5. the sub-boiling distillation method of high purity hydrochloric acid according to claim 1, is characterized in that: described condenser is connected with described end socket, and the cooling medium inlet pipe of described condenser and outlet pipe all stretch out outside described kettle through described end socket; Described liquid trap is connected with the bottom of described kettle, and the discharge nozzle of described liquid trap stretches out outside described kettle through the bottom of described kettle.
6. the sub-boiling distillation method of high purity hydrochloric acid according to claim 1, is characterized in that: the liquid collection opening of described liquid trap is positioned at immediately below described condenser, and the cross-sectional area of the liquid collection opening of described liquid trap is greater than the cross-sectional area of described condenser.
7. the sub-boiling distillation method of high purity hydrochloric acid according to claim 1, is characterized in that: the cooling temperature of described condenser is 0 ~ 15 DEG C.
8. the sub-boiling distillation method of high purity hydrochloric acid according to claim 1, is characterized in that: the flow of described recycle pump is 0.06 × S ~ 0.3 × S, unit is m
3/ h, wherein, S is the evaporation area of described distiller, unit is m
2.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105174219B (en) * | 2015-10-19 | 2017-07-04 | 湖州森诺膜技术工程有限公司 | The system that a kind of use vacuum type Membrane Materials system concentrates watery hydrochloric acid |
| CN106044712A (en) * | 2016-08-12 | 2016-10-26 | 韶关高科祥高新材料有限公司 | Production method for high-purity hydrochloric acid |
| CN107515148A (en) * | 2017-08-07 | 2017-12-26 | 袁洪林 | A kind of sub-boiling distillation device equipment |
| CN107441750B (en) * | 2017-09-26 | 2020-05-01 | 天津科技大学 | Sub-boiling distillation device and application thereof |
| CN109592656A (en) * | 2019-01-31 | 2019-04-09 | 内蒙古通威高纯晶硅有限公司 | A kind of preparation method of impurity analysis acid |
| CN110589784B (en) * | 2019-10-08 | 2021-11-23 | 中国计量科学研究院 | Fine series purification system and purification method for laboratory-grade ultrapure nitric acid |
| CN113908571B (en) * | 2021-11-22 | 2023-08-15 | 南京浦世环境科技发展有限公司 | Laboratory acid purification device |
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| CN1669616A (en) * | 2004-12-22 | 2005-09-21 | 上海氯碱化工股份有限公司 | Process for producing super clean and high-purity reagent by low temperature evaporation and cooling |
| CN102874757A (en) * | 2012-10-29 | 2013-01-16 | 国药集团化学试剂有限公司 | Preparation method of high-purity hydrochloric acid |
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| CN1669616A (en) * | 2004-12-22 | 2005-09-21 | 上海氯碱化工股份有限公司 | Process for producing super clean and high-purity reagent by low temperature evaporation and cooling |
| CN102874757A (en) * | 2012-10-29 | 2013-01-16 | 国药集团化学试剂有限公司 | Preparation method of high-purity hydrochloric acid |
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