CN103724367A - Process for removing and recycling dimethyldichlorosilane from hydrochloric acid gas - Google Patents
Process for removing and recycling dimethyldichlorosilane from hydrochloric acid gas Download PDFInfo
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- CN103724367A CN103724367A CN201410012354.8A CN201410012354A CN103724367A CN 103724367 A CN103724367 A CN 103724367A CN 201410012354 A CN201410012354 A CN 201410012354A CN 103724367 A CN103724367 A CN 103724367A
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Abstract
The invention discloses a process for removing and recycling dimethyldichlorosilane from hydrochloric acid gas. A frozen brine graphite cooler is used. The process is characterized by comprising the following steps: volatilizing liquid CH3Cl to obtain low temperature less than -50 DEG C; absorbing dimethyldichlorosilane by using CH3Cl at low temperature; and separating absorption liquid into gas having more than 99.9% (wt) of CH3Cl in purity and a residue having more than 99.9% (wt) of dimethyldichlorosilane through rectification. According to the process, an original frozen brine graphite cooler can be adopted; cooling capacity can be obtained by using evaporation of the residue in an absorption tower so as to cool the raw material HCl to the temperature less than -20 DEG C; the whole process is performed in closed cycle, thus dimethyldichlorosilane in a gas phase of the raw material HCl can be thoroughly removed, the separated dimethyldichlorosilane can be treated up to the standard and returned to a dimethyldichlorosilane hydrolysis step; and the process has the advantages of simplicity in method, economy and practicability, low operation cost, little pollution and environment friendliness.
Description
Technical field
The present invention relates to chemical field, is a kind of dimethyldichlorosilane(DMCS) technique that removes and reclaim from hydrochloric acid gas.
Background technology
Existing large-scale Organic Silicon Plant hydrolyzing dimethyl dichlorosilane methyl chloride generates siloxanes and pays product hydrochloric acid gas, and hydrochloric acid gas also claims HCl gas.Again by HCl gas and methyl alcohol at saturated ZnCl
2under solution catalyzing, generate methyl chloride, methyl chloride also claims CH
3cl.CH
3cl reacts and generates chlorosilane with Si powder in fluidized-bed.Its main chemical reactions equation is:
n(CH
3)
2SiCl
2＋nH
2O—→〔CH
3)
2SiO〕
n＋2n HCl↑ （1）
Dimethyldichlorosilane(DMCS) siloxanes
2HCl+CH
3OH—→CH
3Cl
3+H
2O （2）
Methyl chloride
2CH
3Cl+Si—→(CH
3)
2SiCl
2 （3）
Dimethyldichlorosilane(DMCS)
Current most economical dimethyldichlorosilane(DMCS) method for hydrolysis is supersaturation Concentraton salt acid system, claims again concentrated hydrochloric acid hydrolysis method.Referring to Fig. 1, dimethyldichlorosilane(DMCS) 1 generates concentrated hydrochloric acids with acid phlegma 2, dimethyldichlorosilane(DMCS) 1 again with concentrated hydrochloric acid in water intense reaction emit the HCl of gaseous state, this is a thermo-negative reaction, can move at normal temperatures.In the HCl gas producing, contain dimethyldichlorosilane(DMCS) <4.31%(mol), siloxanes <0.2%(mol), can be by dimethyldichlorosilane(DMCS) <0.99%(mol in the HCl gas of graphite cooler 501 gas outlet temperature <-10 ℃ through the freezing salt solution of primary amine) be sent to methyl chloride synthesis reactor, as producing CH
3the raw material of Cl.The problem that the dimethyldichlorosilane(DMCS) recovery process of prior art exists is, the dimethyldichlorosilane(DMCS) amount remaining in HCl gas is relevant with cooled outlet temperature, in the time of-10 ℃, dimethyldichlorosilane(DMCS) <0.99%(mol), in the time of-20 ℃, dimethyldichlorosilane(DMCS) <0.5%(mol), salt solution minimum temperature is-25 ℃, lower than the easy crystallization of salt solution of-25 ℃ of temperature, therefore adopt simple fractional condensation method can not thoroughly reclaim the dimethyldichlorosilane(DMCS) in HCl.Dimethyldichlorosilane(DMCS) is brought methyl chloride reactor into HCl, can pollute the catalyzer of blistering reaction.
Summary of the invention
Technical problem to be solved by this invention is, can thoroughly eliminate the dimethyldichlorosilane(DMCS) in raw material HCl gas phase, and the dimethyldichlorosilane(DMCS) separating can be processed to the qualified dimethyldichlorosilane(DMCS) hydrolyzing process that all turns back to, there is method simple, economical and practical, running cost is low removes and reclaims dimethyldichlorosilane(DMCS) technique from hydrochloric acid gas.
Solving one of technical scheme that its technical problem adopts is: a kind ofly from hydrochloric acid gas, remove and reclaim dimethyldichlorosilane(DMCS) technique, it comprises dimethyldichlorosilane(DMCS) hydrolyzing process 400 and chilled brine graphite cooler 501, it is characterized in that, further comprising the steps of:
1) one-level HCl cold-exchange 507-1 is set in the downstream of chilled brine graphite cooler 501, gas phase is containing dimethyldichlorosilane(DMCS) < 0.99%(mol) HCl gas 4 be cooled to temperature <-20 ℃, make dimethyldichlorosilane(DMCS) < 0.5%(mol) dry HCl5 enter glass wool filter 502, through glass wool filter 502 dehydrations, by the >90%(wt being suspended in HCl gas phase) concentrated acid droplet and the filtering of the little liquid pearl of dimethyldichlorosilane(DMCS), and be gathered in the receiving tank of glass wool filter 502 bottoms that large drop is slipped to by gravity, filtered dimethyldichlorosilane(DMCS) < 0.5%(mol) in dry HCl5, contain H
2o < 100ppm(wt), this dry HCl all can not cause corrosion to subsequent handling carbon steel equipment, pipeline etc.,
2) dry HCl5 dimethyldichlorosilane(DMCS) < 0.5%(mol) enters dimethyldichlorosilane(DMCS) absorption tower 504 built-in metal screen waviness packings, the liquid CH after mistake is cold
3cl and dry HCl are at corrugated wire gauze packing surface counter current contact, liquid CH
3cl constantly volatilizees, and temperature reduces rapidly thereupon, liquid CH
3the volatilization of Cl provides a large amount of cold temperature, make exhaust gas HCl body temperature be down to <-35 ℃, absorption agent temperature <-50 ℃, dimethyldichlorosilane(DMCS) is dissolved in absorption agent absorption liquid temperature is raise, be accompanied by dimethyldichlorosilane(DMCS) and be absorbed unnecessary heat, make a part of liquid CH
3cl is evaporated in gas phase, and the dry HCl6 removing after dimethyldichlorosilane(DMCS) contains CH
3cl < 2.3%(mol), dimethyldichlorosilane(DMCS) < 0.01～0.02%(mol) after one-level HCl cold-exchange 507-1 and secondary HCl cold-exchange 507-2 heat exchange, deliver to CH
3cl synthesis reaction vessel, secondary HCl cold-exchange 507-2 can alleviate the load of chilled brine graphite cooler 501 a part of chilled brines;
3) 504 tower reactor liquid effluents and level liquid CH from dimethyldichlorosilane(DMCS) absorption tower
3cl supercooler 509-1 changes the stage casing that enters rectifying tower 505 after cold, and the stage casing of rectifying tower 505 is provided with upper and lower two sections of fillers, and epimere filler sprays fresh liquid CH
3cl8, by dimethyldichlorosilane(DMCS) < 0.1%(wt) by rectifying tower, work off one's feeling vent one's spleen and 11 send into circulation CH
3cl compressor, absorption liquid makes rectifying tower 505 contain dimethyldichlorosilane(DMCS) >99.9%(wt by hypomere filling extract rectification), CH
3cl < 0.1%(wt) still liquid, after water-cooled, returns to pump 503 by dimethyldichlorosilane(DMCS) and is sent to dimethyldichlorosilane(DMCS) hydrolyzing process 400.
Solving two of technical scheme that its technical problem adopts is: a kind ofly from hydrochloric acid gas, remove and reclaim dimethyldichlorosilane(DMCS) technique, it comprises dimethyldichlorosilane(DMCS) hydrolyzing process 400, it is characterized in that, further comprising the steps of:
A) will be from dimethyldichlorosilane(DMCS) hydrolyzing process 400 containing dimethyldichlorosilane(DMCS) >4.31%(mol) HCl gas 3 enter secondary HCl cold-exchange 507-2, again through absorbing tower bottoms vaporizer 510 and tri-grades of coolings of one-level HCl cold-exchange 507-1, be cooled to temperature <-20 ℃ and enter glass wool filter 502, through glass wool filter 502 dehydrations, by the >90%(wt being suspended in HCl gas phase) concentrated acid droplet and the filtering of the little liquid pearl of dimethyldichlorosilane(DMCS), and be gathered in the receiving tank of glass wool filter 502 bottoms that large drop is slipped to by gravity, filtered dimethyldichlorosilane(DMCS) < 0.5%(mol) in dry HCl5, contain H
2o < 100ppm(wt) enter dimethyldichlorosilane(DMCS) absorption tower 504, the housing of dimethyldichlorosilane(DMCS) absorption tower 504 packing section is that stainless steel or copper are made, low temperature that can resistance to-70 ℃, this dry HCl all can not cause corrosion to subsequent handling carbon steel equipment, pipeline etc.,
B) fresh liquid CH
3cl8 or circulating liquid CH
3cl9 is at level liquid CH
3cl supercooler 509-1 with absorb tower bottoms 7 change cold after, then through secondary liquid CH
3cl supercooler 509-2 liquid CH
3cl evaporation generation cycle CH
3cl gas 10, fresh liquid CH
3cl8 or circulating liquid CH
3cl9 be cooled to temperature <-20 ℃ equably sprinkle on the built-in corrugated wire gauze packing in dimethyldichlorosilane(DMCS) absorption tower 504, liquid CH
3cl is in the volatilization of corrugated wire gauze packing surface, and temperature reduces rapidly thereupon, liquid CH
3the volatilization of Cl provides a large amount of cold temperature, makes exhaust gas HCl body temperature be down to <-35 ℃; Absorption agent CH
3cl temperature <-50 ℃; All dimethyldichlorosilane(DMCS) is absorbed into liquid phase, and the absorption heat of dimethyldichlorosilane(DMCS) makes absorption temperature be elevated to-20 ℃, and unnecessary absorption heat makes a part of liquid CH
3cl gasification enters the dry HCl6 removing after dimethyldichlorosilane(DMCS), contains CH
3cl < 2.3%(mol), dimethyldichlorosilane(DMCS) < 0.01～0.02%(mol) after one-level HCl cold-exchange 507-1 and secondary HCl cold-exchange 507-2 re-heat, deliver to CH
3cl synthesis reaction vessel;
C) absorb tower bottoms 7 at level liquid CH
3in Cl supercooler 509-1, change cold after, enter and absorb tower bottoms vaporizer 510, the gas phase of evaporation is sent to the stage casing of rectifying tower 505, as gas-phase feed, remaining liquid phase is spread across through being evenly distributed on the hypomere filler of rectifying tower 505, by dimethyldichlorosilane(DMCS) < 0.1%(wt) by rectifying tower, work off one's feeling vent one's spleen and 11 send into circulation CH
3cl compressor, hot dimethyldichlorosilane(DMCS) and silicone liquid 12, after water-cooled, are returned to pump 503 by dimethyldichlorosilane(DMCS) and are sent to dimethyldichlorosilane(DMCS) hydrolyzing process 400.
The present invention adopt freezing add to absorb from hydrochloric acid gas, remove and reclaim dimethyldichlorosilane(DMCS) technique, the advantage having is:
(a) by fractional condensation 78～80% dimethyldichlorosilane(DMCS) HCl again with dimethyldichlorosilane(DMCS) < 0.5%(mol) dry HCl change and be as cold as-20 ℃, fractional condensation obtains 88～90% dimethyldichlorosilane(DMCS), through glass wool filter dehydration, by the >90%(wt being suspended in HCl gas phase) concentrated acid droplet and the filtering of the little liquid pearl of dimethyldichlorosilane(DMCS), and be gathered in the receiving tank of the glass wool filter bottom that large drop is slipped to by gravity, filtered dimethyldichlorosilane(DMCS) < 0.5%(mol) in dry HCl, contain H
2o < 100ppm(wt), this dry HCl all can not cause corrosion to subsequent handling carbon steel equipment, pipeline etc.
(b) select liquid CH
3cl is as absorption agent:
1) HCl after absorption is as CH
3the synthesis material of Cl, at this moment only contains CH in raw material HCl
3cl < 2.3%(mol), it for the purity of sintetics without impact;
2) standby fresh liquid CH each other
3cl and circulating liquid CH
3cl is all not moisture, the cleanliness that removes dimethyldichlorosilane(DMCS) in the dry HCl after dimethyldichlorosilane(DMCS) after two kinds of absorption agent washings is respectively dimethyldichlorosilane(DMCS) < 0.01%(wt), or dimethyldichlorosilane(DMCS) < 0.02%(wt), therefore alleviated CH
3synthetic the sending out of Cl answers the siloxanes of still to pollute;
3) the liquid CH of temperature <-20 ℃
3cl is in dimethyldichlorosilane(DMCS) absorption tower filling surface and gas phase HCl counter current contact, along with HCl, constantly blows over surface liquid CH
3the continuous volatilization temperature of Cl is down to rapidly-50 ℃ thereupon, system total working pressure P
1>=0.4MPa, CH
3the dividing potential drop P of Cl
2< 0.01MPa, corresponding CH
3the temperature of saturation of Cl is-69.5 ℃.
Table 1 is CH under differing temps
3cl and dimethyldichlorosilane(DMCS) saturated vapour pressure and relative volatility
| Temperature ℃ | 20 | -10 | -20 | -30 | -35 |
| P 3mmHg | 3327 | 1335 | 898.1 | 584.8 | 465 |
| P 4mmHg | 114 | 26.2 | 14.7 | 7.9 | 5.7 |
| αP 3/P 4 | 32.7 | 51.0 | 61.1 | 74.0 | 81.7 |
Wherein: P
3for CH
3cl saturated vapour pressure; P
4for dimethyldichlorosilane(DMCS) saturated vapour pressure; α is relative volatility
Be shown in Table 1, the lower dimethyldichlorosilane(DMCS) saturated vapour pressure of temperature is lower, CH
3the relative volatility of Cl is higher, and dimethyldichlorosilane(DMCS) more easily proceeds to liquid phase and is absorbed.
(C) absorb tower bottoms and be sent to rectifying tower, rectifying tower top obtains dimethyldichlorosilane(DMCS) < 0.1%(wt) CH
3cl works off one's feeling vent one's spleen and is sent to fluidized-bed and reacts with Si powder and generate dimethyldichlorosilane(DMCS), the CH obtaining at rectifying tower through rectifying tower
3cl < 0.1%(wt) hot dimethyldichlorosilane(DMCS) and silicone liquid are returned and are pumped into toward the recycle of dimethyldichlorosilane(DMCS) hydrolyzing process to dimethyldichlorosilane(DMCS) after still liquid water cooler water-cooled.
Of the present inventionly from hydrochloric acid gas, remove and reclaim dimethyldichlorosilane(DMCS) technique, can thoroughly eliminate the dimethyldichlorosilane(DMCS) in raw material HCl gas phase, and the dimethyldichlorosilane(DMCS) separating can be processed to the qualified dimethyldichlorosilane(DMCS) hydrolyzing process that all turns back to, there is method simple, economical and practical, running cost is low, pollutes less, is beneficial to the advantages such as environmental protection.
Accompanying drawing explanation
Fig. 1 is the dimethyldichlorosilane(DMCS) recovery process schematic flow sheet of prior art.
Fig. 2 is a kind of dimethyldichlorosilane(DMCS) process flow diagram that removes and reclaim from hydrochloric acid gas of the present invention.
Fig. 3 is that another kind of the present invention removes and reclaim dimethyldichlorosilane(DMCS) process flow diagram from hydrochloric acid gas.
In figure: 1 dimethyldichlorosilane(DMCS), 2 acid phlegmas, 3 containing dimethyldichlorosilane(DMCS) < 4.3%(mol) HCl gas, 4 gas phases are containing dimethyldichlorosilane(DMCS) < 0.99%(mol) HCl gas, 5 dimethyldichlorosilane(DMCS) < 0.5%(mol) dry HCl, 6 remove the dry HCl after dimethyldichlorosilane(DMCS), and 7 absorb tower bottoms, 8 fresh liquid CH
3cl, 9 circulating liquid CH
3cl, 10 circulation CH
3cl gas, 11 rectifying tower are worked off one's feeling vent one's spleen, 12 hot dimethyldichlorosilane(DMCS) and silicone liquid, the dimethyldichlorosilane(DMCS) of 13 freezing recovery and siloxanes, 400 dimethyldichlorosilane(DMCS) hydrolyzing process, 501 chilled brine graphite coolers, 502 glass wool filters, 503 dimethyldichlorosilane(DMCS)s return to pump, 504 dimethyldichlorosilane(DMCS) absorption towers, 505 rectifying tower, 506 reboilers, 507-1 one-level HCl cold-exchange, 507-2 secondary HCl cold-exchange, 508 still liquid water coolers, 509-1 level liquid CH
3cl supercooler, 509-2 secondary liquid CH
3cl supercooler, 510 absorb tower bottoms vaporizer.
Embodiment
The invention will be further described to utilize two embodiment shown in Fig. 2 and Fig. 3 below.
With reference to Fig. 2, embodiment 1 a kind of removes and reclaims dimethyldichlorosilane(DMCS) technique from hydrochloric acid gas, that one-level HCl cold-exchange 507-1 is set in the downstream of existing chilled brine graphite cooler 501, gas phase is containing dimethyldichlorosilane(DMCS) < 0.99%(mol) HCl gas 4 be cooled to temperature <-20 ℃, make dimethyldichlorosilane(DMCS) < 0.5%(mol) dry HCl5 carry out glass wool filter 502, through glass wool filter 502 dehydrations, by the >90%(wt being suspended in HCl gas phase) concentrated acid droplet and the filtering of the little liquid pearl of dimethyldichlorosilane(DMCS), and be gathered in the receiving tank of glass wool filter 502 bottoms that large drop is slipped to by gravity, filtered dimethyldichlorosilane(DMCS) < 0.5%(mol) in dry HCl5, contain H
2o < 100ppm(wt), this dry HCl all can not cause corrosion to subsequent handling carbon steel equipment, pipeline etc., dimethyldichlorosilane(DMCS) < 0.5%(mol) dry HCl5 carries out dimethyldichlorosilane(DMCS) absorption tower 504 built-in metal screen waviness packings, the liquid CH after mistake is cold
3cl and dry HCl are at corrugated wire gauze packing surface counter current contact, liquid CH
3cl constantly volatilizees, and temperature is down to rapidly the limit-70 ℃, liquid CH thereupon
3the volatilization of Cl provides a large amount of cold temperature, make exhaust gas HCl body temperature be down to <-35 ℃, absorption agent temperature <-50 ℃, dimethyldichlorosilane(DMCS) is dissolved in absorption agent absorption liquid temperature is raise, be accompanied by dimethyldichlorosilane(DMCS) and be absorbed unnecessary heat, make a part of liquid CH
3cl is evaporated in gas phase, and the dry HCl6 removing after dimethyldichlorosilane(DMCS) contains CH
3cl < 2.3%(mol), dimethyldichlorosilane(DMCS) < 0.01～0.02%(mol) after one-level HCl cold-exchange 507-1 and secondary HCl cold-exchange 507-2 heat exchange, deliver to CH
3cl synthesis reaction vessel, secondary HCl cold-exchange 507-2 can alleviate the load of chilled brine graphite cooler 501 a part of chilled brines.
504 tower reactor liquid effluents and level liquid CH from dimethyldichlorosilane(DMCS) absorption tower
3cl supercooler 509-1 changes the stage casing that enters rectifying tower 505 after cold, and the stage casing of rectifying tower 505 is provided with upper and lower two sections of fillers, and epimere filler sprays fresh liquid CH
3cl8, by dimethyldichlorosilane(DMCS) < 0.1%(wt) by rectifying tower, work off one's feeling vent one's spleen and 11 send into circulation CH
3cl compressor, absorption liquid makes rectifying tower 505 contain dimethyldichlorosilane(DMCS) >99.9%(wt by hypomere filling extract rectification), CH
3cl < 0.1%(wt) still liquid, after water-cooled, returns to pump 503 by dimethyldichlorosilane(DMCS) and is sent to dimethyldichlorosilane(DMCS) hydrolyzing process 400.
With reference to Fig. 3, the another kind of embodiment 2 removes and reclaims dimethyldichlorosilane(DMCS) technique from hydrochloric acid gas, to contain dimethyldichlorosilane(DMCS) >4.31%(mol from dimethyldichlorosilane(DMCS) hydrolyzing process 400), siloxanes < 0.2%(mol) HCl gas enters secondary HCl cold-exchange 507-2, again through absorbing tower bottoms vaporizer 510 and tri-grades of coolings of one-level HCl cold-exchange 507-1, be cooled to temperature <-20 ℃ and enter glass wool filter 502, through glass wool filter 502 dehydrations, by the >90%(wt being suspended in HCl gas phase) concentrated acid droplet and the filtering of the little liquid pearl of dimethyldichlorosilane(DMCS), and be gathered in the receiving tank of glass wool filter 502 bottoms that large drop is slipped to by gravity, filtered dimethyldichlorosilane(DMCS) < 0.5%(mol) in dry HCl5, contain H
2o < 100ppm(wt) enter dimethyldichlorosilane(DMCS) absorption tower 504, the housing of dimethyldichlorosilane(DMCS) absorption tower 504 packing section is that stainless steel or copper are made, low temperature that can resistance to-70 ℃, this dry HCl all can not cause corrosion to subsequent handling carbon steel equipment, pipeline etc., fresh liquid CH
3cl8 and circulating liquid CH
3cl9 is at level liquid CH
3cl supercooler 509-1 with absorb tower bottoms 7 change cold after, then through secondary liquid CH
3cl supercooler 509-2 evaporation generation cycle CH
3cl gas 10, fresh liquid CH
3cl8 and circulating liquid CH
3cl9 be cooled to temperature <-20 ℃ equably sprinkle on the built-in corrugated wire gauze packing in dimethyldichlorosilane(DMCS) absorption tower 504, liquid CH
3cl is in the volatilization of corrugated wire gauze packing surface, and temperature is down to rapidly the limit-70 ℃, liquid CH thereupon
3the volatilization of Cl provides a large amount of cold temperature, makes exhaust gas HCl body temperature be down to <-35 ℃, absorption agent CH
3cl temperature <-50 ℃, all dimethyldichlorosilane(DMCS) is absorbed into liquid phase.Absorption heat after dimethyldichlorosilane(DMCS) makes absorption temperature be elevated to-20 ℃, and unnecessary absorption heat makes a part of liquid CH
3cl gasification enters the dry HCl6 removing after dimethyldichlorosilane(DMCS), contains CH
3cl < 2.3%(mol), dimethyldichlorosilane(DMCS) < 0.01～0.02%(mol) after one-level HCl cold-exchange 507-1 and secondary HCl cold-exchange 507-2 heat exchange, deliver to CH
3cl synthesis reaction vessel.
The present invention removes and reclaims the related frock of dimethyldichlorosilane(DMCS) technique and all adopts this area mature technology product from hydrochloric acid gas.
Claims (2)
1. from hydrochloric acid gas, remove and reclaim a dimethyldichlorosilane(DMCS) technique, it comprises dimethyldichlorosilane(DMCS) hydrolyzing process (400) and chilled brine graphite cooler (501), it is characterized in that, further comprising the steps of:
1) in the downstream of chilled brine graphite cooler (501), one-level HCl cold-exchange (507-1) is set, gas phase is containing dimethyldichlorosilane(DMCS) < 0.99%(mol) HCl gas (4) be cooled to temperature <-20 ℃, make dimethyldichlorosilane(DMCS) < 0.5%(mol) dry HCl(5) enter glass wool filter (502), through glass wool filter (502) dehydration, by the >90%(wt being suspended in HCl gas phase) concentrated acid droplet and the filtering of the little liquid pearl of dimethyldichlorosilane(DMCS), and be gathered in the receiving tank of glass wool filter (502) bottom that large drop is slipped to by gravity, obtain after filtration dimethyldichlorosilane(DMCS) < 0.5%(mol) dry HCl(5) in containing H
2o < 100ppm(wt),
2) dry HCl(5 dimethyldichlorosilane(DMCS) < 0.5%(mol)) enter dimethyldichlorosilane(DMCS) absorption tower (504) built-in metal screen waviness packings, the liquid CH after mistake is cold
3cl and dry HCl are at corrugated wire gauze packing surface counter current contact, liquid CH
3cl constantly volatilizees, and temperature reduces rapidly thereupon, liquid CH
3the volatilization of Cl provides a large amount of cold temperature, make exhaust gas HCl body temperature be down to <-35 ℃, absorption agent temperature <-50 ℃, dimethyldichlorosilane(DMCS) is dissolved in absorption agent absorption liquid temperature is raise, be accompanied by dimethyldichlorosilane(DMCS) and be absorbed unnecessary heat, make a part of liquid CH
3cl is evaporated in gas phase, removes the dry HCl(6 after dimethyldichlorosilane(DMCS)) contain CH
3cl < 2.3%(mol), dimethyldichlorosilane(DMCS) < 0.01～0.02%(mol) after one-level HCl cold-exchange (507-1) and secondary HCl cold-exchange (507-2) heat exchange, deliver to CH
3cl synthesis reaction vessel;
3) from dimethyldichlorosilane(DMCS) absorption tower (504) tower reactor liquid effluent and level liquid CH
3cl supercooler (509-1) changes the stage casing that enters rectifying tower (505) after cold, and rectifying tower (505) is provided with upper and lower two sections of fillers, and epimere filler sprays fresh liquid CH
3cl(8), by dimethyldichlorosilane(DMCS) < 0.1%(wt) by rectifying tower work off one's feeling vent one's spleen (11) send into circulation CH
3cl compressor, absorption liquid makes rectifying tower (505) contain dimethyldichlorosilane(DMCS) >99.9%(wt by hypomere filling extract rectification), CH
3cl < 0.1%(wt) still liquid, after water-cooled, returns to pump (503) by dimethyldichlorosilane(DMCS) and is sent to dimethyldichlorosilane(DMCS) hydrolyzing process (400).
2. from hydrochloric acid gas, remove and reclaim a dimethyldichlorosilane(DMCS) technique, it comprises dimethyldichlorosilane(DMCS) hydrolyzing process (400), it is characterized in that, further comprising the steps of:
A) will be from dimethyldichlorosilane(DMCS) hydrolyzing process (400) containing dimethyldichlorosilane(DMCS) >4.31%(mol) HCl gas (3) enter secondary HCl cold-exchange (507-2), again through absorbing tower bottoms vaporizer (510) and three grades of coolings of one-level HCl cold-exchange (507-1), be cooled to temperature <-20 ℃ and enter glass wool filter (502), through glass wool filter (502) dehydration, by the >90%(wt being suspended in HCl gas phase) concentrated acid droplet and the filtering of the little liquid pearl of dimethyldichlorosilane(DMCS), and be gathered in the receiving tank of glass wool filter (502) bottom that large drop is slipped to by gravity, filtered dimethyldichlorosilane(DMCS) < 0.5%(mol) dry HCl(5), contain H
2o < 100ppm(wt) enter dimethyldichlorosilane(DMCS) absorption tower (504),
B) fresh liquid CH
3cl(8) or circulating liquid CH
3cl(9) at level liquid CH
3cl supercooler (509-1) with absorb tower bottoms (7) change cold after, then through secondary liquid CH
3cl supercooler (509-2) liquid CH
3cl evaporation generation cycle CH
3cl gas (10), fresh liquid CH
3cl(8) or circulating liquid CH
3cl(9) be cooled to temperature <-20 ℃ equably sprinkle on dimethyldichlorosilane(DMCS) absorption tower (504) built-in corrugated wire gauze packing, liquid CH
3cl is in the volatilization of corrugated wire gauze packing surface, and temperature reduces rapidly thereupon, liquid CH
3the volatilization of Cl provides a large amount of cold temperature, makes exhaust gas HCl body temperature be down to <-35 ℃; Absorption agent CH
3cl temperature <-50 ℃; All dimethyldichlorosilane(DMCS) is absorbed into liquid phase, and the absorption heat of dimethyldichlorosilane(DMCS) makes absorption temperature be elevated to-20 ℃, and unnecessary absorption heat makes a part of liquid CH
3cl gasification enters the dry HCl(6 removing after dimethyldichlorosilane(DMCS)), contain CH
3cl < 2.3%(mol), dimethyldichlorosilane(DMCS) < 0.01～0.02%(mol) after one-level HCl cold-exchange (507-1) and secondary HCl cold-exchange (507-2) re-heat, deliver to CH
3cl synthesis reaction vessel;
C) absorb tower bottoms (7) at level liquid CH
3in Cl supercooler (509-1), change cold after, enter and absorb tower bottoms vaporizer (510), the gas phase of evaporation is sent to the stage casing of rectifying tower (505), as gas-phase feed, remaining liquid phase is spread across through being evenly distributed on the hypomere filler of rectifying tower (505), by dimethyldichlorosilane(DMCS) < 0.1%(wt) by rectifying tower work off one's feeling vent one's spleen (11) send into circulation CH
3cl compressor, hot dimethyldichlorosilane(DMCS) and silicone liquid (12), after water-cooled, are returned to pump (503) by dimethyldichlorosilane(DMCS) and are sent to dimethyldichlorosilane(DMCS) hydrolyzing process (400).
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| CN201410012354.8A CN103724367B (en) | 2014-01-11 | 2014-01-11 | Remove from HCl gas and reclaim dimethyldichlorosilane(DMCS) technique |
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| CN201410012354.8A CN103724367B (en) | 2014-01-11 | 2014-01-11 | Remove from HCl gas and reclaim dimethyldichlorosilane(DMCS) technique |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105597508A (en) * | 2015-12-21 | 2016-05-25 | 浙江衢州正邦有机硅有限公司 | Absorption and utilization method of polymethyl triethoxy silane reaction exhaust |
| DE102015201446A1 (en) | 2015-01-28 | 2016-07-28 | Wacker Chemie Ag | Process for the purification of contaminated gaseous hydrogen chloride |
| CN110003263A (en) * | 2019-03-12 | 2019-07-12 | 余家骧 | One kind removes from HCl and recycles dimethyldichlorosilane technique completely |
| CN110845734A (en) * | 2019-10-15 | 2020-02-28 | 中国化学赛鼎宁波工程有限公司 | System and method for hydrolyzing organochlorosilane and refining hydrochloric acid |
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| CN101423193A (en) * | 2008-12-04 | 2009-05-06 | 浙江恒业成有机硅有限公司 | Technique for reducing impurity content in gas phase hydrogenchloride from hydrolysis of dimethyldichlorosilane |
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| US4935220A (en) * | 1988-05-17 | 1990-06-19 | Wacker-Chemie Gmbh | Process for purifying crude gaseous hydrogen chloride |
| CN101423193A (en) * | 2008-12-04 | 2009-05-06 | 浙江恒业成有机硅有限公司 | Technique for reducing impurity content in gas phase hydrogenchloride from hydrolysis of dimethyldichlorosilane |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102015201446A1 (en) | 2015-01-28 | 2016-07-28 | Wacker Chemie Ag | Process for the purification of contaminated gaseous hydrogen chloride |
| WO2016120288A1 (en) | 2015-01-28 | 2016-08-04 | Wacker Chemie Ag | Method for purifying contaminated gaseous hydrogen chloride |
| JP2018502810A (en) * | 2015-01-28 | 2018-02-01 | ワッカー ケミー アクチエンゲゼルシャフトＷａｃｋｅｒ Ｃｈｅｍｉｅ ＡＧ | Method for purifying contaminated gaseous hydrogen chloride |
| US10179735B2 (en) | 2015-01-28 | 2019-01-15 | Wacker Chemie Ag | Method for purifying contaminated gaseous hydrogen chloride |
| CN105597508A (en) * | 2015-12-21 | 2016-05-25 | 浙江衢州正邦有机硅有限公司 | Absorption and utilization method of polymethyl triethoxy silane reaction exhaust |
| CN105597508B (en) * | 2015-12-21 | 2018-10-26 | 浙江衢州正邦有机硅有限公司 | Method is absorbed and utilized in a kind of poly- methyltriethoxysilane reaction end gas |
| CN110003263A (en) * | 2019-03-12 | 2019-07-12 | 余家骧 | One kind removes from HCl and recycles dimethyldichlorosilane technique completely |
| CN110845734A (en) * | 2019-10-15 | 2020-02-28 | 中国化学赛鼎宁波工程有限公司 | System and method for hydrolyzing organochlorosilane and refining hydrochloric acid |
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