CN104689688A - A process of dehydrating composite gas - Google Patents
A process of dehydrating composite gas Download PDFInfo
- Publication number
- CN104689688A CN104689688A CN201310656547.2A CN201310656547A CN104689688A CN 104689688 A CN104689688 A CN 104689688A CN 201310656547 A CN201310656547 A CN 201310656547A CN 104689688 A CN104689688 A CN 104689688A
- Authority
- CN
- China
- Prior art keywords
- gas
- acetylene
- hydrogen chloride
- temperature
- moisture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of chemical purification, and relates to a method of deeply dehydrating mixed gas of acetylene and hydrogen chloride. The method includes following three steps: a step of washing with a solvent, a step of mixing at a low temperature and a step of performing centrifugal collection. The method includes: washing and collecting water molecules in acetylene gas in a washing tower by utilization of a washing solvent with low saturated vapor pressure and a low freezing point, subjecting the washing solvent and the acetylene gas to gas liquid separation, separating water from the washing solvent, circulating the washing solvent after indirect cooling and heat exchange, indirectly cooling hydrogen chloride gas by chilled brine, rapidly fully mixing the hydrogen chloride gas and the acetylene gas, and further separating hydrogen chloride liquid drops residue in the mixed gas by a centrifugal collector. The water content in the prepared mixed gas of the acetylene and the hydrogen chloride is less than 0.01% by mass. The method is reasonable in process design, simple and easily controllable in operation conditions, high in dehydration efficiency, low in investment, and suitable for deep dehydration occasions of the mixed gas of the acetylene and the hydrogen chloride.
Description
Technical field:
The invention belongs to chemical purification technical field, relate to the method for moisture in a kind of deep removal acetylene and chlorine hydride mixed gas.
Background technology:
VCM manufactures Corvic, the raw material of the copolymer resinses such as vinyl chloride, vinylidene chloride and vinyl acetate, vinyl chloride resin (being called for short PVC) annual production occupies first of global various plastics variety at present, and the production method of VCM mainly contains with the ethylene process of petroleum path with the acetylene method of calcium carbide route.At present, external most of producer adopts ethylene process, and the ethylene process technological process of production is long, severe reaction conditions; Due to acetylene method production technology relative maturity, the technological process of production is short, so China adopts the producer of acetylene method more than the producer of employing ethylene process, the ratio of the PVC output that the PVC output adopting acetylene method to produce is produced with ethylene process is about 7:3.In China in recent ten years, the acetylene method preparing chloroethylene monomer list covering device production scale of building constantly expands, and the production technology research and development of single covering device of large-scale relatively lag behind, the dehydration problem of acetylene and chlorine hydride mixed gas still continues to use traditional technology, therefore the harm that in gaseous mixture, remaining moisture causes reaction system and relevant device and corrosion are still very serious, become and affect one of bottleneck that device normally produces; About the dewatering of acetylene and chlorine hydride mixed gas, once had in history and remove the moisture in hydrogen chloride gas with the concentrated sulfuric acid and remove the method for the moisture in acetylene gas with solid caustic soda, this method needs consume a large amount of caustic soda and produce a large amount of refuses.The beginning of this century, the VCM process units of Dutch John Brown & Co. that China introduces, wherein acetylene gas adopts two mole sieve driers to hocket, another regeneration of drying, regeneration gas be hot nitrogen, after dry, in acetylene gas, the mass fraction of water is 3 × 10
-6, hydrogen chloride gas adopts indirect cooler refrigerated separation hydrochloric acid mist, and in dry afterchlorinate hydrogen, the mass fraction of water is 10 × 10
-6, right latter two gas and vapor permeation sends into next workshop section, and the public work equipment of this technique device dehydration needed for workshop section is many, and investment cost is high, and operating procedure is complicated, is unwell to popularity, the dehydration technology that current domestic VCM manufacturing enterprise generally adopts be the later stage sixties in last century China research and develop voluntarily, concrete mode is: refining acetylene gas and hydrogen chloride gas enter blender after passing through to regulate mol ratio carries out normal temperature and mix, be indirectly cooled through the graphite condenser of two-stage series connection again and condense to about-14 DEG C, the hydrochloric acid liquid of the hydrochloric acid mist part that steam in gaseous mixture and hydrogen chloride are formed with more than 40% bottom graphite condenser is discharged, all the other are then less easily entrained by and enter acid mist filter, mineral wool layer trap filter through being soaked with fluorosilicon oil is separated, part hydrochloric acid mist is filtered layer to be stopped, be condensed into hydrochloric acid drop to be trapped, be not filtered layer to trap the hydrochloric acid mist be retained down and then after preheater preheats, deliver to next workshop section with gaseous mixture, above-mentioned flow process is generally summarised as two kinds of gases, and " normal temperature mixes, cryogenic condensation, filtration retains " flow process (being called for short " dry method dehydration " flow process), the technological deficiency that this flow and method exists is: when part hydrochloric acid mist is aerosol state, mineral wool filter course can not make the whole isolated by filtration of hydrochloric acid mist particulate of aerosol state, and this is that aerocolloidal particle gravity and extension balance characteristics determined.Usually, dry method dewatering process flow impossible be removed by water in gaseous mixture thoroughly, and mill practices data for many years show, " dry method dehydration " be acetylene and the water content more than high ten times of remaining actual water content in chlorine hydride mixed gas than theory calculate afterwards.
Summary of the invention:
The object of the invention is to overcome the shortcoming existed in prior art, on the basis of existing industry " dry method dehydration " technology development provide a kind of technological process simple, save hydrogen chloride consumption, cryogenic energy utilization is reasonable, SR is little, the method of moisture in the deep removal acetylene that dewatering efficiency is high and chlorine hydride mixed gas, VCM is prepared through catalytic action further again, for preparing the purposes such as Corvic after making residual moisture in gaseous mixture reach lower content.
To achieve these goals, the present invention adopts solvent wash method first to remove most moisture in acetylene gas, form aerosol form liquid particle when avoiding the moisture in acetylene gas to mix with hydrogen chloride to be difficult to be separated, improve gaseous mixture dewatering efficiency, its main technique feature comprises solvent wash, low-temperature mixed and centrifugal trapping three processes, namely first force down with saturated vapor, surface tension is little, freezing point is low and hydrone large for surface tension in acetylene gas is washed trapping by the cleaning solvent of low temperature in scrubbing tower, again by cleaning solvent and acetylene gas through gas-liquid separation and cleaning solvent separates moisture, by indirectly lowering the temperature, heat exchange Posterior circle uses, by hydrogen chloride gas by even with acetylene gas rapid mixing after the indirect cooling down of chilled brine, go out the hydrochloric acid drop that left behind in mist again through centrifugal trapping separator for further separation, the acetylene that obtained dehydrating effect is good and chlorine hydride mixed gas body for subsequent use.The present invention makes " dry method dehydration ", and technological process there occurs the change of matter, in order to distinguish with it, referred to as " wet method dehydration " flow process.
Particular content of the present invention is: taken out the acetylene gas containing normal temperature saturation water through surge tank by acetylene gas steel cylinder, send into the bottom of glass scrubbing tower, spray at top of tower the cleaning solvent tetrachloroethanes that temperature is 0-2 DEG C simultaneously, to make in acetylene gas contained saturated vapor because of cooling and surface tension effects by tetrachloroethanes droplet capture, acetylene gas overflows from tower top through after scrubber overhead gas-liquid separator, and portion gas is collected and is retained in surge flask for subsequent use; Collect at the bottom of scrubbing tower and obtain moisture tetrachloroethanes liquid, use through lowering the temperature and regenerating the Posterior circle that dewaters; Taken out the hydrogen chloride gas allocated into containing a certain amount of moisture again by hydrogen chloride gas steel cylinder through surge tank, send in dividing wall type glass cold traps, with-35 DEG C of chilled brines indirect heat exchange with it, make hydrogen chloride gas be cooled to-14 DEG C; Then the hydrogen chloride gas of low temperature and acetylene gas is made tangentially to enter rapid mixing in jacket type low-temperature mixed device even, adopt-35 DEG C of chilled brines to carry out indirect heat exchange with it simultaneously, mixture temperature is made to be down to-14 DEG C, gaseous mixture is made to enter in the centrifugal collector of jacket type low-temperature mixed device bottom again, remaining hydrochloric acid mist in trapping gaseous mixture; Finally, separate the acetylene of liquid hydrochloric acid and chlorine hydride mixed gas body portion collection and be kept in surge flask for subsequent use.
The cleaning solvent that acetylene gas washing process of the present invention uses is organic chlorohydrocarbon or inorganic acid liquid, comprises tetrachloroethanes, trichloroethanes, dichloroethanes, vinyl chloride, hydrochloric acid, sulfuric acid, nitric acid and mixed acid liquid; After solvent wash acetylene gas, cleaning solvent is easy to carry out sufficient gas-liquid separation, and the cleaning solvent mass fraction taken out of with acetylene gas is 0 ~ 30%, and preferably 0 ~ 10%; The cleaning solvent of circulation or the temperature range of chilled brine are between normal temperature is to-35 DEG C; By the acetylene gas of the direct wash cooling of cleaning solvent and the temperature range of hydrogen chloride gas that is indirectly cooled between normal temperature is to-20 DEG C, preferably between-10 ~-14 DEG C; When acetylene gas and hydrogen chloride gas two kinds of gas and vapor permeation, first acetylene gas and hydrogen chloride gas are divided into after some equal portions respectively and carry out mixing of small size, gather the two kinds of gas and vapor permeation carrying out overall size again, after the even process of low temperature rapid mixing in addition centrifugal trapping hydrochloric acid mist process, water content mass fraction remaining in gaseous mixture is less than 0.01%.
Compared with prior art, its technical flow design is reasonable, and operating condition is simple and easy to control, and wet method dewatering efficiency is high in the present invention, and this technology is applied to the deep dehydration occasion of acetylene and chlorine hydride mixed gas by the enterprise being applicable to producing VCM.Specific implementation method is as follows, but does not therefore limit this method.
Detailed description of the invention:
Embodiment 1:
The acetylene gas of 10mol/h containing normal temperature saturation water is taken out through surge tank by acetylene gas steel cylinder, send into the bottom of glass scrubbing tower, spray into cleaning solvent 550g/h tetrachloroethanes at top of tower simultaneously, tetrachloroethanes fluid temperature remains within the scope of 0-2 DEG C, to make in acetylene gas contained saturated vapor because of cooling and surface tension effects by tetrachloroethanes droplet capture, acetylene gas overflows from tower top through after tower overhead gas liquid/gas separator, and portion gas is collected and is retained in surge flask, applies for analytical control; Collect at the bottom of scrubbing tower and obtain moisture tetrachloroethanes liquid, tetrachloroethanes liquid uses through lowering the temperature and regenerating the Posterior circle that dewaters; Take out through surge tank the hydrogen chloride gas that 10.5mol/h allocates a certain amount of moisture into by hydrogen chloride gas steel cylinder again, send in dividing wall type glass cold traps, with-35 DEG C of chilled brines indirect heat exchange with it, make hydrogen chloride gas be cooled to-14 DEG C by normal temperature; Then the hydrogen chloride gas of low temperature and acetylene gas is made tangentially to enter in jacket type low-temperature mixed device, rapid mixing is even at low temperatures, adopt-35 DEG C of chilled brines to carry out indirect heat exchange with it simultaneously, mixture temperature is made to be down to-14 DEG C, gaseous mixture is made to enter in the centrifugal collector of jacket type low-temperature mixed device bottom again, remaining hydrochloric acid mist in trapping gaseous mixture, finally, the acetylene separating liquid hydrochloric acid and chlorine hydride mixed gas body divide to collect and be retained in confession analytical control in surge flask to be applied; Another part gas can through in alkali liquor absorption and after discharge; The analytical control of each stock gas dewatering the results are shown in subordinate list 1.
Embodiment 2:
The acetylene gas of 10mol/h containing normal temperature saturation water is taken out through surge tank by acetylene gas steel cylinder, send into the bottom of glass scrubbing tower, spray into cleaning solvent 500g/h1 at top of tower simultaneously, 1,1-trichloroethanes, 1,1,1-trichloroethanes fluid temperature remains within the scope of 0-2 DEG C, to make in acetylene gas contained saturated vapor because of cooling and surface tension effects by 1,1,1-trichloroethanes droplet capture, acetylene gas overflows from tower top through after tower overhead gas liquid/gas separator, and portion gas is collected and is retained in surge flask, applies for analytical control; Obtain 1,1,1-moisture trichloroethanes at the bottom of scrubbing tower, 1,1,1-trichloroethanes liquid uses through lowering the temperature and regenerating the Posterior circle that dewaters; Take out through surge tank the hydrogen chloride gas that 10.5mol/h allocates a certain amount of moisture into by hydrogen chloride gas steel cylinder, send in dividing wall type glass cold traps, with-35 DEG C of chilled brines indirect heat exchange with it, make hydrogen chloride gas be cooled to-14 DEG C by normal temperature; The hydrogen chloride gas of low temperature and acetylene gas tangentially enter in jacket type low-temperature mixed device, rapid mixing is even at low temperatures, adopt-35 DEG C of chilled brines to carry out indirect heat exchange with it simultaneously, mixture temperature is made to be down to-14 DEG C, gaseous mixture is made to enter in the centrifugal collector of jacket type low-temperature mixed device bottom again, remaining hydrochloric acid mist in trapping gaseous mixture, finally, separate the acetylene of liquid hydrochloric acid and chlorine hydride mixed gas body portion collection and be retained in surge flask, applying for analytical control; Another part gas can through in alkali liquor absorption and after discharge, the analytical control of each stock gas dewatering the results are shown in subordinate list 1.
Embodiment 3:
The acetylene gas of 10mol/h containing normal temperature saturation water is taken out through surge tank by acetylene gas steel cylinder, send into the bottom of glass scrubbing tower, spray into cleaning solvent 450g/h1 at top of tower simultaneously, 1-dichloroethanes, 1,1-dichloroethanes fluid temperature remains within the scope of 0-2 DEG C, to make in acetylene gas contained saturated vapor because of cooling and surface tension effects by 1,1-dichloroethanes droplet capture, acetylene gas overflows from tower top through after tower overhead gas liquid/gas separator, portion gas is collected and is retained in surge flask, applies for analytical control; 1,1-moisture dichloroethanes liquid is obtained at the bottom of scrubbing tower.1,1-dichloroethanes liquid uses through lowering the temperature and regenerating the Posterior circle that dewaters.Take out through surge tank the hydrogen chloride gas that 10.5mol/h allocates a certain amount of moisture content into by hydrogen chloride gas steel cylinder, send in dividing wall type glass cold traps, with-35 DEG C of chilled brines indirect heat exchange with it, make hydrogen chloride gas be down to-14 DEG C by normal temperature.The hydrogen chloride gas of above-mentioned low temperature and acetylene gas tangentially enter in jacket type low-temperature mixed device, rapid mixing is even at low temperatures, adopt-35 DEG C of chilled brines to carry out indirect heat exchange with it simultaneously, mixture temperature is made to be down to-14 DEG C, gaseous mixture is made to enter in the centrifugal collector of jacket type low-temperature mixed device bottom again, remaining hydrochloric acid mist in trapping gaseous mixture; Finally, separate the acetylene of liquid hydrochloric acid and chlorine hydride mixed gas body to divide to collect and be retained in surge flask and apply for analytical control; Another part gas can through in alkali liquor absorption and after discharge; The analytical control of each stock gas dewatering the results are shown in subordinate list 1.
The analytical control result of each step gas dewatering of table 1
Claims (5)
1. the removing process of moisture in a composite gas, it is characterized in that taking out by acetylene gas steel cylinder the acetylene gas containing normal temperature saturation water through surge tank, send into the bottom of glass scrubbing tower, spray at top of tower the cleaning solvent tetrachloroethanes that temperature is 0-2 DEG C simultaneously, to make in acetylene gas contained saturated vapor because of cooling and surface tension effects by tetrachloroethanes droplet capture, acetylene gas overflows from tower top through after scrubber overhead gas-liquid separator, and portion gas is collected and is retained in surge flask for subsequent use; Collect at the bottom of scrubbing tower and obtain moisture tetrachloroethanes liquid, use through indirectly lowering the temperature and regenerating the Posterior circle that dewaters; Taken out the hydrogen chloride gas allocated into containing a certain amount of moisture again by hydrogen chloride gas steel cylinder through surge tank, send in dividing wall type glass cold traps, with-35 DEG C of chilled brines indirect heat exchange with it, make hydrogen chloride gas be cooled to-14 DEG C; Then the hydrogen chloride gas of low temperature and acetylene gas is made tangentially to enter rapid mixing in jacket type low-temperature mixed device even, adopt-35 DEG C of chilled brines to carry out indirect heat exchange with it simultaneously, mixture temperature is made to be down to-14 DEG C, gaseous mixture is made to enter in the centrifugal collector of jacket type low-temperature mixed device bottom again, remaining hydrochloric acid mist in trapping gaseous mixture; Finally, the acetylene and the chlorine hydride mixed gas body that separate liquid hydrochloric acid are collected and are kept in surge flask for subsequent use.
2. the removing process of moisture in composite gas according to claim 1, it is characterized in that the cleaning solvent that acetylene gas washing process uses is organic chlorohydrocarbon or inorganic acid liquid, comprise tetrachloroethanes, trichloroethanes, dichloroethanes, vinyl chloride, hydrochloric acid, sulfuric acid, nitric acid and mixed acid liquid.
3. the removing process of moisture in composite gas according to claim 1, after it is characterized in that solvent wash acetylene gas, cleaning solvent carries out sufficient gas-liquid separation, and the cleaning solvent mass fraction taken out of with acetylene gas is 0 ~ 30%.
4. the removing process of moisture in composite gas according to claim 1, is characterized in that the temperature range of cleaning solvent or the chilled brine circulated is between normal temperature is to-35 DEG C; By the acetylene gas of the direct wash cooling of cleaning solvent and the temperature range of hydrogen chloride gas that is indirectly cooled between normal temperature is to-20 DEG C.
5. the removing process of moisture in composite gas according to claim 1, it is characterized in that acetylene gas and hydrogen chloride gas mixed feeding mol ratio are 1:1.05 ~ 1.10, after acetylene gas and hydrogen chloride gas are divided into some equal portions respectively, first carry out two kinds of gas and vapor permeation of small size, gather the two kinds of gas and vapor permeation carrying out overall size again, after the even process of low temperature rapid mixing in addition centrifugal trapping hydrochloric acid mist process, water content mass fraction remaining in gaseous mixture is less than 0.01%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310656547.2A CN104689688A (en) | 2013-12-06 | 2013-12-06 | A process of dehydrating composite gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310656547.2A CN104689688A (en) | 2013-12-06 | 2013-12-06 | A process of dehydrating composite gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104689688A true CN104689688A (en) | 2015-06-10 |
Family
ID=53337466
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310656547.2A Pending CN104689688A (en) | 2013-12-06 | 2013-12-06 | A process of dehydrating composite gas |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104689688A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293469A (en) * | 2018-10-10 | 2019-02-01 | 青岛科技大学 | A kind of method of toluene di-isocyanate(TDI) by-product hydrogen chloride gas and the dehydration of acetylene gas mixed freezing |
| CN112569737A (en) * | 2020-11-27 | 2021-03-30 | 天能化工有限公司 | System and method for freeze dehydration in vinyl chloride production |
-
2013
- 2013-12-06 CN CN201310656547.2A patent/CN104689688A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293469A (en) * | 2018-10-10 | 2019-02-01 | 青岛科技大学 | A kind of method of toluene di-isocyanate(TDI) by-product hydrogen chloride gas and the dehydration of acetylene gas mixed freezing |
| CN109293469B (en) * | 2018-10-10 | 2021-06-08 | 青岛科技大学 | Method for mixing, freezing and dehydrating toluene diisocyanate byproduct hydrogen chloride gas and acetylene gas |
| CN112569737A (en) * | 2020-11-27 | 2021-03-30 | 天能化工有限公司 | System and method for freeze dehydration in vinyl chloride production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2600348C2 (en) | Method for trapping carbon dioxide from flue gas of power plant and device for implementation thereof | |
| CN109126392B (en) | Method for carrying out CO (carbon monoxide) in flue gas by adopting ionic liquid2Trapping device and process | |
| CN203060888U (en) | Methylal deep dehydration purifying device | |
| CN109999618B (en) | System and method for separating carbon dioxide from medium-high pressure gas source | |
| CN104449880B (en) | A kind of raw gas purifying method and device | |
| CN104031692B (en) | The device and method of a kind of coking raw gas high temperature direct chilling reparation technology heat medium water | |
| CN103589462A (en) | Technological method for purifying coal oven gas and recovering chemical products | |
| CN103318850A (en) | Low-temperature waste heat recovery system for pyrite and metallurgical off-gas acid making device | |
| CN102267868B (en) | Industrial production apparatus for trichloroethylene | |
| CN104876792A (en) | Method for producing high-purity chloropropene | |
| CN102327726B (en) | Method for dewatering desorption gas for flue gas desulfurization and recycling condensate | |
| CN101544530B (en) | Method for deep removal of water in ethyne and chlorine hydride mixed gas | |
| CN104436998A (en) | Method for removing acid gas by adopting methanol as absorbent | |
| CN100447120C (en) | Technological process for refining trimethylolpropane | |
| CN104860789A (en) | Method for recovering propylene in preparation process of chloropropene | |
| CN104689688A (en) | A process of dehydrating composite gas | |
| CN103708993B (en) | A kind of vinylidene is thick cracking gas alkali cleaning and dehydrating process in producing | |
| CN102247743B (en) | Dehydration method for desorption gas used in desulphurization of flue gas | |
| CN205269356U (en) | Device is washed to methyl alcohol for low temperature | |
| CN107998825B (en) | HCl tail gas purification device and HCl tail gas purification process | |
| CN202238069U (en) | Treatment system for burnt gas produced during continuous reforming catalyst regeneration | |
| CN108635895A (en) | A kind of rectifying column, distillation system and rectificating method | |
| CN102775267B (en) | Method and system for recycling cyclohexane solvent in SBS (styrene-butadiene-styrene) production | |
| CN108854456B (en) | System and method for recycling heat energy of desorption tower | |
| CN207012812U (en) | MDEA regenerative device of solution during a kind of caustic wash desulfuration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150610 |