CN102515102A - Synthesis method for high-purity hydrogen chloride - Google Patents
Synthesis method for high-purity hydrogen chloride Download PDFInfo
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- CN102515102A CN102515102A CN2011104234160A CN201110423416A CN102515102A CN 102515102 A CN102515102 A CN 102515102A CN 2011104234160 A CN2011104234160 A CN 2011104234160A CN 201110423416 A CN201110423416 A CN 201110423416A CN 102515102 A CN102515102 A CN 102515102A
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Abstract
The invention discloses a synthesis method for high-purity hydrogen chloride, comprising the following steps of: charging the hydrogen and the high-purity chlorine having a weight-volume ratio of 1: 3 purified by a palladium membrane diffuser in a synthesis furnace; combusting in the synthesis furnace at 1000-1500 DEG C to generate HCl (hydrogen chloride); cooling the HCl to a normal temperature in a water cooler; keeping the hydrogen in the charged raw materials 5-10% greater than a stoichiometric number; and installing a dew-point meter in a glass system, simply measuring trace water in the hydrogen chloride, continuously monitoring quality, and bottling after the quality is up to standard. The process is reasonable and simple in production, as well as is the most simple and ideal technology for preparation for hydrogen chloride.
Description
Technical field
The present invention relates to the synthetic technology of a kind of Chemicals, particularly a kind of high-purity hydrogenchloride, be suitable for producing on a large scale high-purity hydrogenchloride
Background technology
hydrogenchloride is the important form that exists of chlorine element, also is very important chemical product and raw material.Be mainly used in and produce PVC, urethane, epoxy resin, organosilicon, viton, fluorochlorohydrocarbon, TiO2 coating and some agrochemicals, material of construction and some pharmaceutical preparations etc.
In the time of
Chemical Manufacture mass consumption chlorine, produce equimolar hydrogen chloride gas usually, so hydrogenchloride is that a kind of common by product is gone up in industry.And HCl is the chemical of a kind of low price, intractable, and the past is normal adopts water absorption method to process that hydrochloric acid is sold or with discharging with the back in the alkali lye.HCl is directly changed into Cl2 be used, realize the recycle of chlorine element in industrial system and the zero release of reaction process, bring huge economic benefit, meet the general requirement of contemporary resource recycling social development.Original technology is to obtain high-purity hydrogenchloride, adopts traditional hydrogen, chlorine synthesis technique, is raw material with High Purity Hydrogen, high-purity chlorine, and impurity is less in the gained synthetic gas, is easy to remove
Summary of the invention
the invention provides a kind of equipment and technology.This technology not only technology is reasonable, and has solved the problem of producing high-purity hydrogenchloride.Adopt this law to enhance productivity greatly.
The technical scheme that the present invention adopts is:
A kind of compound method of high-purity hydrogenchloride is a raw material with High Purity Hydrogen, high-purity chlorine, and integrated continuous production feeds intake and synthesizes high-purity hydrogenchloride, it is characterized in that:
(1) High Purity Hydrogen and the high-purity chlorine that purify through palladium film diffusion instrument get into synthetic furnace respectively, and the weightmeasurement ratio of hydrogen and chlorine is 1:3; In 1000-1500 ℃ of synthetic furnace, burn, generate HCl; In watercooler, be cooled to normal temperature; Wherein advance in the stove raw material hydrogen than the excessive 5%-10% of stoichiometry;
(2) purify and carry out at normal temperatures and pressures, are made up of two portions, and adsorption cleaning and fractional condensation purify; Absorption adopts homemade natural mordenite zeolite under normal temperature, normal pressure, to carry out, and mainly is to remove residual chlorine, water and other trace impurities; Fractional condensation purify be cool off down at-85--100 ℃ temperature condition, condensation; Dew point hygrometer is housed in glass system, has measured the minor amount of water in the hydrogenchloride at any time, the HCl after purifying bottles with liquid.
the present invention specifically discloses a kind of compound method of high-purity hydrogenchloride, is raw material with High Purity Hydrogen, high purity oxygen, directly the novel process of synthetic high-purity hydrogenchloride.
(1) unstripped gas
are synthetic to be that the plant hydrogen that brine electrolysis makes obtains through the purification of palladium film diffusion instrument with hydrogen, and hydrogen purity can reach 6N.Chlorine is to adopt high-purity chlorine, and its purity is 4.8N.
(2) technology point
get into synthetic furnace respectively through hydrogen and the high-purity chlorine that palladium film diffusion instrument purifies.In synthetic furnace, burn, generate HCl.Flame temperature is cooled to normal temperature more than 1000 ℃ in watercooler.For the content that makes chlorine in the synthetic gas is low as far as possible, advance in the stove raw material hydrogen than the excessive 5%-10% of stoichiometry.Because the purity of the virgin gas that adopts is high, foreign matter content is low, and except that HCl, major impurity is unreacted excessive hydrogen in the synthetic gas; Though chlorine is easier to reaction with the hydrogen ratio, still has the residual chlorine of traces of unreacted in the product, also has trace impurity and other reaction product of being brought into by virgin gas.
chilled synthetic gas gets into cleaning section.Purify and carry out at normal temperatures and pressures, be made up of two portions, adsorption cleaning and fractional condensation purify.The homemade natural mordenite zeolite of absorption employing etc. carries out under normal temperature, normal pressure.Mainly be to remove residual chlorine, water and other trace impurities; Fractional condensation purify be cool off down at-85--100 ℃ temperature condition, condensation.Constantly discharge residual excessive hydrogen and some noncondensable gases in condenser overhead.
HCl after purifying bottles with liquid.Dew point hygrometer is housed in glass system, has measured the minor amount of water in the hydrogenchloride fairly simplely.
The working method that the present invention is concrete:
The outlet of
palladium film diffusion instrument connects the inlet one of synthetic furnace through pipeline; The outlet two of chlorine purification device is through the inlet two of pipeline connection synthetic furnace, and the outlet of synthetic furnace is through the inlet of pipeline connection watercooler, and the outlet one of the outlet of watercooler, chlorine purification device connects the inlet of vent gas treatment tower through pipeline; The outlet of watercooler connects the inlet of HCI gas purifier through pipeline, and the outlet one of HCI gas purifier is through pipeline be linked in sequence glass threeway, vacuum pump; The outlet two of HCI gas purifier is through the inlet of pipeline connection steel cylinder, and the outlet of steel cylinder connects the inlet of vent gas treatment tower through pipeline; The outlet three of HCI gas purifier connects the inlet of vent gas treatment tower through pipeline.Adopting hydrogen, chlorine synthesis technique, is raw material with High Purity Hydrogen, high-purity chlorine, and impurity is less in the gained synthetic gas, is easy to remove, and enhances productivity greatly.
palladium film diffusion instrument is provided with the outlet 102 of the inlet 101 and the palladium film diffusion instrument of palladium film diffusion instrument, and the outlet of palladium film diffusion instrument connects the inlet 1 of synthetic furnace through pipeline; The chlorine purification device is provided with the inlet 1 of chlorine purification device, the inlet 2 402 of chlorine purification device, the outlet 1 of chlorine purification device, the outlet 2 404 of chlorine purification device; The outlet two of chlorine purification device connects the inlet 2 202 of synthetic furnace through pipeline; The outlet 203 of synthetic furnace is through the inlet 301 of pipeline connection watercooler, and the outlet 302 of watercooler, the outlet of chlorine purification device 1 connect the inlet 901 of vent gas treatment tower through pipeline; The outlet 302 of watercooler is through the inlet 501 of pipeline connection HCI gas purifier, and the outlet 1 of HCI gas purifier connects glass threeway 6 through pipeline, and the glass threeway connects vacuum pump 7 through pipeline; The outlet 2 503 of HCI gas purifier is through the inlet 801 of pipeline connection steel cylinder, and the outlet 802 of steel cylinder connects the inlet 901 of vent gas treatment tower through pipeline; The outlet 3 504 of HCI gas purifier is through the inlet 901 of pipeline connection vent gas treatment tower, and the vent gas treatment tower is provided with vent gas treatment tower outlet 902.
The character of the hydrogenchloride of the present invention's preparation:
Very easily water-soluble (1:500), the aqueous solution is colourless transparent liquid;
specific density (d154) 1.20 (39.11%), 1.15 (29.57%), 1.10 (20%), 1.05 (10.17%).
The compound method of high-purity hydrogenchloride disclosed by the invention compared with prior art has the following advantages:
(1) present method can continous-stable production hydrogenchloride, solved feed intake original intermittence can not stably manufactured drawback.
(2) integrated continuous production feeds intake
, the technology of rectifying, purification can better utilised cold and heat, makes production cost lower.
Steady quality behind
(3) continuous production can large-scale industrial production.
Description of drawings:
Fig. 1 is the technical process of the high-purity hydrogenchloride of preparation; Wherein 1, palladium film diffusion instrument; 101, the inlet of palladium film diffusion instrument; 102, the outlet of palladium film diffusion instrument; 2, synthetic furnace; 201, the inlet one of synthetic furnace; 202, the inlet two of synthetic furnace; 203, the outlet of synthetic furnace; 3, watercooler; 301, the inlet of watercooler; 302, the outlet of watercooler; 4, chlorine purification device; 401, the inlet one of chlorine purification device; 402, the inlet two of chlorine purification device; 403, the outlet one of chlorine purification device; 404, the outlet two of chlorine purification device; 5, HCI gas purifier; 501, the inlet of HCI gas purifier; 502, the outlet one of HCI gas purifier; 503, the outlet two of HCI gas purifier; 504, the outlet three of HCI gas purifier; 6, glass threeway; 7, vacuum pump; 8, steel cylinder; 801, the inlet of steel cylinder; 9, vent gas treatment tower; 901, the inlet of vent gas treatment tower; 902, the outlet of vent gas treatment tower.
Embodiment:
The present invention is explained below in conjunction with embodiment in
; The scheme of embodiment described here; Do not limit the present invention; One of skill in the art can make improvements and change according to spirit of the present invention, and described these improvement and variation all should be regarded as within the scope of the invention, and scope of the present invention and essence are limited claim.
Embodiment 1
(1) integrated continuous production feeds intake syntheticly, and the hydrogen and the high-purity chlorine that purify through palladium film diffusion instrument get into synthetic furnace respectively, and the weightmeasurement ratio of hydrogen and fluorine chlorine is 1:3; In 1000 ℃ of synthetic furnaces, burn, generate HCl; In watercooler, be cooled to normal temperature; Advance in the stove raw material hydrogen than stoichiometry excessive 5%%;
(2) purify and carry out at normal temperatures and pressures, are made up of two portions, and adsorption cleaning and fractional condensation purify; Absorption adopts homemade natural mordenite zeolite under normal temperature, normal pressure, to carry out, and mainly is to remove residual chlorine, water and other trace impurities; It is cooling, condensation under-85 ℃ temperature condition that fractional condensation purifies; Dew point hygrometer is housed in glass system, has measured the minor amount of water in the hydrogenchloride at any time, the HCl after purifying bottles with liquid.Fig. 1 is seen in technical process.
Embodiment 2
(1) integrated continuous production feeds intake syntheticly, and the hydrogen and the high-purity chlorine that purify through palladium film diffusion instrument get into synthetic furnace respectively, and the weightmeasurement ratio of hydrogen and fluorine chlorine is 1:3; In 1500 ℃ of synthetic furnaces, burn, generate HCl; In watercooler, be cooled to normal temperature; Advance in the stove raw material hydrogen than stoichiometry excessive 10%;
(2) purify and carry out at normal temperatures and pressures, are made up of two portions, and adsorption cleaning and fractional condensation purify; Absorption adopts homemade natural mordenite zeolite under normal temperature, normal pressure, to carry out, and mainly is to remove residual chlorine, water and other trace impurities; It is cooling, condensation under-100 ℃ temperature condition that fractional condensation purifies; Dew point hygrometer is housed in glass system, has measured the minor amount of water in the hydrogenchloride at any time, the HCl after purifying bottles with liquid.Fig. 1 is seen in technical process.
Embodiment 3
(1) integrated continuous production feeds intake syntheticly, and the hydrogen and the high-purity chlorine that purify through palladium film diffusion instrument get into synthetic furnace respectively, and the weightmeasurement ratio of hydrogen and fluorine chlorine is 1:3; In 1350 ℃ of synthetic furnaces, burn, generate HCl; In watercooler, be cooled to normal temperature; Advance in the stove raw material hydrogen than stoichiometry excessive 10%;
(2) purify and carry out at normal temperatures and pressures, are made up of two portions, and adsorption cleaning and fractional condensation purify; Absorption adopts homemade natural mordenite zeolite under normal temperature, normal pressure, to carry out, and mainly is to remove residual chlorine, water and other trace impurities; It is cooling, condensation under-100 ℃ temperature condition that fractional condensation purifies; Dew point hygrometer is housed in glass system, has measured the minor amount of water in the hydrogenchloride at any time, the HCl after purifying bottles with liquid.
Palladium film diffusion instrument is provided with the outlet 102 of the inlet 101 and the palladium film diffusion instrument of palladium film diffusion instrument, and the outlet of palladium film diffusion instrument connects the inlet 1 of synthetic furnace through pipeline; The chlorine purification device is provided with the inlet 1 of chlorine purification device, the inlet 2 402 of chlorine purification device, the outlet 1 of chlorine purification device, the outlet 2 404 of chlorine purification device; The outlet two of chlorine purification device connects the inlet 2 202 of synthetic furnace through pipeline; The outlet 203 of synthetic furnace is through the inlet 301 of pipeline connection watercooler, and the outlet 302 of watercooler, the outlet of chlorine purification device 1 connect the inlet 901 of vent gas treatment tower through pipeline; The outlet 302 of watercooler is through the inlet 501 of pipeline connection HCI gas purifier, and the outlet 1 of HCI gas purifier connects glass threeway 6 through pipeline, and the glass threeway connects vacuum pump 7 through pipeline; The outlet 2 503 of HCI gas purifier is through the inlet 801 of pipeline connection steel cylinder, and the outlet 802 of steel cylinder connects the inlet 901 of vent gas treatment tower through pipeline; The outlet 3 504 of HCI gas purifier is through the inlet 901 of pipeline connection vent gas treatment tower, and the vent gas treatment tower is provided with vent gas treatment tower outlet 902, and Fig. 1 is seen in technical process
Claims (2)
1. the compound method of high-purity hydrogenchloride is a raw material with High Purity Hydrogen, high-purity chlorine, and integrated continuous production feeds intake and synthesizes high-purity hydrogenchloride, it is characterized in that:
(1) High Purity Hydrogen and the high-purity chlorine that purify through palladium film diffusion instrument get into synthetic furnace respectively, and the weightmeasurement ratio of hydrogen and chlorine is 1:3; In 1000-1500 ℃ of synthetic furnace, burn, generate HCl; In watercooler, be cooled to normal temperature; Wherein advance in the stove raw material hydrogen than the excessive 5%-10% of stoichiometry;
(2) purification is carried out at normal temperatures and pressures, is made up of two portions, and adsorption cleaning and fractional condensation purify; Absorption adopts homemade natural mordenite zeolite under normal temperature, normal pressure, to carry out, and mainly is to remove residual chlorine, water and other trace impurities; Fractional condensation purify be cool off down at-85--100 ℃ temperature condition, condensation; Dew point hygrometer is housed in glass system, has measured the minor amount of water in the hydrogenchloride at any time, the HCl after purifying bottles with liquid.
2. the described method of claim 1, wherein the outlet of palladium film diffusion instrument connects the inlet one of synthetic furnace through pipeline; The outlet two of chlorine purification device is through the inlet two of pipeline connection synthetic furnace, and the outlet of synthetic furnace is through the inlet of pipeline connection watercooler, and the outlet one of the outlet of watercooler, chlorine purification device connects the inlet of vent gas treatment tower through pipeline; The outlet of watercooler connects the inlet of HCI gas purifier through pipeline, and the outlet one of HCI gas purifier is through pipeline be linked in sequence glass threeway, vacuum pump; The outlet two of HCI gas purifier is through the inlet of pipeline connection steel cylinder, and the outlet of steel cylinder connects the inlet of vent gas treatment tower through pipeline; The outlet three of HCI gas purifier connects the inlet of vent gas treatment tower through pipeline.
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| CN2011104234160A CN102515102A (en) | 2011-12-16 | 2011-12-16 | Synthesis method for high-purity hydrogen chloride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502295A (en) * | 2015-12-31 | 2016-04-20 | 上海正帆科技股份有限公司 | Electronic grade hydrogen chloride purification method |
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| CN1488570A (en) * | 2003-08-21 | 2004-04-14 | 上海氯碱化工股份有限公司 | Apparatus and method for industrialize production for superclear high-pure chlorhydric acid |
| US6793905B1 (en) * | 1999-10-07 | 2004-09-21 | Merck Patent Gmbh | Method for producing high-purity hydrochloric acid |
| 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 |
| CN101007622A (en) * | 2006-01-26 | 2007-08-01 | 山东恒通化工股份有限公司 | Device for tail chlorine degassing and absorption for preparing hydrochloride gas and its preparation method |
| CN101823693A (en) * | 2009-03-02 | 2010-09-08 | 张天德 | Method for preparing ultrapure hydrogen chloride gas from chloroacetic acid tail gas by sulfur catalyst method |
| CN101823694A (en) * | 2010-05-06 | 2010-09-08 | 杭州四面体科技有限公司 | Processing method for purifying sulfur-containing chlorine hydride |
| CN101948095A (en) * | 2010-10-18 | 2011-01-19 | 天津市泰亨气体有限公司 | Technique for preparing hydrogen chloride and recovering steam by using synthesis method |
-
2011
- 2011-12-16 CN CN2011104234160A patent/CN102515102A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6793905B1 (en) * | 1999-10-07 | 2004-09-21 | Merck Patent Gmbh | Method for producing high-purity hydrochloric acid |
| CN1488570A (en) * | 2003-08-21 | 2004-04-14 | 上海氯碱化工股份有限公司 | Apparatus and method for industrialize production for superclear high-pure chlorhydric acid |
| 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 |
| CN101007622A (en) * | 2006-01-26 | 2007-08-01 | 山东恒通化工股份有限公司 | Device for tail chlorine degassing and absorption for preparing hydrochloride gas and its preparation method |
| CN101823693A (en) * | 2009-03-02 | 2010-09-08 | 张天德 | Method for preparing ultrapure hydrogen chloride gas from chloroacetic acid tail gas by sulfur catalyst method |
| CN101823694A (en) * | 2010-05-06 | 2010-09-08 | 杭州四面体科技有限公司 | Processing method for purifying sulfur-containing chlorine hydride |
| CN101948095A (en) * | 2010-10-18 | 2011-01-19 | 天津市泰亨气体有限公司 | Technique for preparing hydrogen chloride and recovering steam by using synthesis method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105502295A (en) * | 2015-12-31 | 2016-04-20 | 上海正帆科技股份有限公司 | Electronic grade hydrogen chloride purification method |
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Application publication date: 20120627 |