CN110562923A - Analytical purification process and analytical purification device for diluted hydrochloric acid containing siloxane - Google Patents
Analytical purification process and analytical purification device for diluted hydrochloric acid containing siloxane Download PDFInfo
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- CN110562923A CN110562923A CN201910980724.XA CN201910980724A CN110562923A CN 110562923 A CN110562923 A CN 110562923A CN 201910980724 A CN201910980724 A CN 201910980724A CN 110562923 A CN110562923 A CN 110562923A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 131
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 238000000746 purification Methods 0.000 title claims abstract description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 346
- 238000000605 extraction Methods 0.000 claims abstract description 67
- 239000007789 gas Substances 0.000 claims abstract description 59
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 58
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000005191 phase separation Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 59
- 238000003860 storage Methods 0.000 claims description 55
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 14
- 239000000945 filler Substances 0.000 claims description 11
- 238000003795 desorption Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims 1
- 239000012071 phase Substances 0.000 description 30
- 239000006227 byproduct Substances 0.000 description 16
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000005562 Glyphosate Substances 0.000 description 5
- 229940097068 glyphosate Drugs 0.000 description 5
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000005046 Chlorosilane Substances 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229940050176 methyl chloride Drugs 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- 229960001701 chloroform Drugs 0.000 description 1
- VABRONYHMNKEFB-UHFFFAOYSA-N chloromethane;silicon Chemical compound [Si].ClC VABRONYHMNKEFB-UHFFFAOYSA-N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- FUKUFMFMCZIRNT-UHFFFAOYSA-N hydron;methanol;chloride Chemical compound Cl.OC FUKUFMFMCZIRNT-UHFFFAOYSA-N 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
- C01B17/905—Removal of organic impurities
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention relates to a siloxane-containing dilute hydrochloric acid analysis and purification process and an analysis and purification device, wherein the siloxane-containing dilute hydrochloric acid analysis and purification process comprises the following steps: (1) extracting dilute hydrochloric acid containing siloxane by adopting concentrated sulfuric acid to separate out hydrogen chloride gas, and transferring the siloxane into dilute sulfuric acid; (2) the diluted sulfuric acid containing siloxane is subjected to phase separation to obtain siloxane and diluted sulfuric acid. The analytical purification device for the diluted hydrochloric acid containing the siloxane comprises an extraction tower, a hydrogen chloride condenser and a phase separator. The invention adopts concentrated sulfuric acid to extract diluted hydrochloric acid containing siloxane, so that hydrogen chloride gas is separated out, and the hydrogen chloride can be recycled; the siloxane is transferred to dilute sulfuric acid, and the siloxane and sulfuric acid are easily separated, so that the siloxane and the sulfuric acid can be recycled.
Description
Technical Field
the invention relates to a process and a device for analyzing and purifying dilute hydrochloric acid containing siloxane.
Background
The by-product of siloxane-containing hydrochloric acid from organosilicon plants is mainly derived from:
1. Hydrolyzates of chlorosilane monomers can produce a wide variety of organosilicon polymers, and a large amount of by-product hydrochloric acid is produced during hydrolysis of chlorosilanes, such as: complete hydrolysis of 1 mole of dimethyldichlorosilane can yield 2 moles of hydrogen chloride. The hydrochloric acid, which is a byproduct of the hydrolysis, contains a large amount of silicone-based substances, mainly silanol (linear substances) and cyclosiloxane (cyclic substances), and is hereinafter collectively referred to as "siloxane".
2. the hydrochloric acid which hydrolyzes the monomethylchlorosilane monomer and produces a large amount of hydrogen-containing silicone oil as a byproduct is small in specific gravity difference between the hydrogen-containing silicone oil and the dilute hydrochloric acid, and some hydrogen-containing silicone oils are mutually soluble and extremely difficult to treat.
3. The byproduct hydrochloric acid generated in acid washing in the chlorosilane monomer hydrolysis process and the byproduct acid synthesized by chloromethane contain siloxane.
The threadlike substances in the siloxane in the by-products can be further polymerized to form macromolecules in the reaction device, so that the blockage of an acid conveying pipeline and the blockage of a hydrogen chloride desorption tower are caused, an acid storage container can be formed into a rubber-like siloxane layer, the equipment has to be frequently stopped and disassembled in production, the rubber-like siloxane layer is cleared, the yield of the siloxane is reduced, the starting period is shortened, the labor waste is caused, the siloxane in the hydrogen chloride gas is analyzed, the synthesis quality of the methyl chloride is influenced, the economic benefit of enterprises is directly damaged, and the removal of the siloxane in the by-product hydrochloric acid is a problem to be solved urgently.
In conclusion, in the obtained diluted hydrochloric acid containing siloxane, the siloxane and the diluted hydrochloric acid have small specific gravity difference and are mutually soluble, so that the siloxane and the diluted hydrochloric acid are extremely difficult to separate, and great pressure is generated for environmental protection.
in addition, in the production process of organic silicon chloromethane or methane chloride, concentrated sulfuric acid is needed to be adopted to wash and purify harmful substances in chloromethane gas, dichloromethane gas or trichloromethane gas: dimethyl ether, methanol, water vapor and siloxane, thereby obtaining a byproduct of dilute sulfuric acid containing organic matters. China is a world production country of methane chloride, organic silicon and glyphosate with the largest capacity, methyl chloride is produced by adopting a methanol-hydrogen chloride method in the production process of the methane chloride and the organic silicon, and the methyl chloride is a byproduct in the synthesis of dimethyl phosphite serving as a raw material of the glyphosate, so dilute sulfuric acid containing organic matters is produced in the production process of the methane chloride, the organic silicon and the glyphosate. According to incomplete statistics, 80-90% of dilute sulfuric acid as a byproduct in China is about 30 ten thousand tons, and the problem that the dilute sulfuric acid as the byproduct with high organic content is difficult to treat is increasingly prominent in 2017 under the background of continuously enhanced environment-friendly finishing force.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the dilute sulfuric acid vacuum concentration device and the dilute sulfuric acid vacuum concentration method which are low in cost, low in energy consumption, good in treatment effect, high in reliability and stable in operation.
A process for the analytical purification of dilute hydrochloric acid containing siloxane, characterized in that it comprises the following steps:
(1) Extracting dilute hydrochloric acid containing siloxane by adopting concentrated sulfuric acid to separate out hydrogen chloride gas, and transferring the siloxane into dilute sulfuric acid;
(2) The diluted sulfuric acid containing siloxane is subjected to phase separation to obtain siloxane and diluted sulfuric acid.
Preferably, in the diluted siloxane-containing hydrochloric acid in the step (1), the mass concentration of siloxane is 0.01-5%, and the mass concentration of hydrochloric acid is 3-31%.
Preferably, the concentrated sulfuric acid is organic matter-containing concentrated sulfuric acid. The invention can adopt pure concentrated sulfuric acid and also can adopt byproducts of organic silicon factories. As mentioned in the background art, dilute sulfuric acid (waste sulfuric acid) containing organic matters is produced as a byproduct in the production process of methane chloride, organic silicon and glyphosate, and the dilute sulfuric acid is concentrated into concentrated sulfuric acid which can be used as an extractant in the step (1), so that the dilute sulfuric acid as the byproduct is utilized to the maximum extent.
preferably, the method further comprises the step (3): and (3) concentrating the dilute sulfuric acid to obtain concentrated sulfuric acid, and returning the concentrated sulfuric acid to the step (1) for extraction.
In order to increase the concentration of the concentrated sulfuric acid, one-stage or multi-stage vacuum concentration devices can be adopted for concentration. Preferably, the dilute sulfuric acid in the step (2) is subjected to two-stage vacuum concentration to obtain concentrated sulfuric acid with the mass concentration of more than 80%. A general recommendation is 80-97%.
Preferably, hydrogen peroxide is added into the concentrated sulfuric acid after concentration, the addition amount of the hydrogen peroxide in the hydrogen peroxide accounts for 0.03-20% of the mass of the concentrated sulfuric acid, siloxane in the hydrogen peroxide is oxidized into white carbon black, the white carbon black is removed by filtration, and the concentrated sulfuric acid is returned to the step (1) for use.
a desorption and purification device for siloxane-containing dilute hydrochloric acid comprises an extraction tower, a hydrogen chloride condenser and a phase separator, wherein the top of the extraction tower is provided with a gas outlet, the upper part of the extraction tower is provided with a concentrated sulfuric acid inlet, the lower part of the extraction tower is provided with a siloxane-containing dilute hydrochloric acid inlet, and the bottom of the extraction tower is provided with a dilute sulfuric acid outlet; a dilute sulfuric acid outlet at the bottom of the extraction tower is communicated with a liquid inlet of the phase separator, and the phase separator is also provided with a dilute sulfuric acid outlet and a siloxane outlet; the gas outlet at the top of the extraction tower is communicated with the gas inlet of a hydrogen chloride condenser, and the hydrogen chloride condenser is also provided with a hydrogen chloride outlet and a condensed water outlet.
preferably, three layers of fillers are arranged in the extraction tower from top to bottom, a liquid distributor is arranged above each layer of fillers, the concentrated sulfuric acid inlet is arranged at the uppermost layer of liquid distributor, and the siloxane-containing dilute hydrochloric acid inlet is arranged at the lowermost layer of liquid distributor; and a circulating sulfuric acid inlet is also arranged at the liquid distribution layer of the middle layer and is communicated with the first sulfuric acid storage tank and the condensed water outlet of the hydrogen chloride condenser.
Preferably, the device further comprises a dilute sulfuric acid concentration device, wherein the dilute sulfuric acid concentration device comprises a first-stage vacuum concentration kettle and a second-stage vacuum concentration kettle, a dilute sulfuric acid outlet of the phase separator is communicated with a liquid inlet of the first-stage vacuum concentration kettle, a liquid outlet of the first-stage vacuum concentration kettle is communicated with a liquid inlet of the second-stage vacuum concentration kettle, and a liquid outlet of the second-stage vacuum concentration kettle is communicated with a concentrated sulfuric acid inlet of the extraction tower.
Preferably, the primary vacuum concentration kettle is provided with a primary heater and a primary condenser, the primary heater adopts 0.6-2.0 Mpa saturated steam as a heat source, a gas inlet of the primary condenser is communicated with a gas outlet of the primary vacuum concentration kettle, a gas outlet of the primary condenser is communicated with vacuum, and a liquid outlet of the primary condenser is communicated with a condensed water storage tank;
The second-stage vacuum concentration kettle is provided with a second-stage heater and a second-stage condenser, the second-stage heater adopts 1.0-2.0 Mpa saturated steam as a heat source, a gas inlet of the second-stage condenser is communicated with a gas outlet of the second-stage vacuum concentration kettle, a gas outlet of the second-stage condenser is communicated with vacuum, and a liquid outlet of the second-stage condenser is communicated with a condensed water storage tank.
Preferably, the device further comprises an oxidation and filtration device, the oxidation and filtration device comprises a cooler, a fourth sulfuric acid storage tank, a filter, a fifth sulfuric acid storage tank and a hydrogen peroxide storage tank, a liquid outlet of the second-stage vacuum concentration kettle is communicated with a concentrated sulfuric acid inlet of the desorption tower through the cooler, the fourth sulfuric acid storage tank, the filter and the fifth sulfuric acid storage tank in sequence, and the fourth sulfuric acid storage tank is communicated with the hydrogen peroxide storage tank.
Preferably, the hydrogen chloride condenser comprises a first condenser and a second condenser, a gas outlet at the top of the extraction tower is communicated with a gas inlet of the first condenser, a gas outlet of the first condenser is communicated with a gas inlet of the second condenser, the second condenser is provided with a hydrogen chloride discharge port, and liquid outlets of the first condenser and the second condenser are respectively communicated with a circulating sulfuric acid inlet.
Preferably, a dilute sulfuric acid outlet at the bottom of the desorption tower is communicated with a liquid inlet of the phase separator through a second sulfuric acid storage tank, and a dilute sulfuric acid outlet of the phase separator is communicated with a liquid inlet of the first-stage vacuum concentration kettle through a third sulfuric acid storage tank.
The dilute sulfuric acid concentration device of the invention can refer to the dilute sulfuric acid vacuum concentration device and method disclosed in Chinese patent CN 108358176A.
It should be noted that the various vessels/tanks/kettles/vessels of the present invention are generally connected by pipes, and pumps and valves may be provided on the pipes to control the flow rate and direction of the fluid, which are well known to those skilled in the art and will not be described in detail.
The invention has the beneficial effects that:
1. Extracting dilute hydrochloric acid containing siloxane by adopting concentrated sulfuric acid to separate out hydrogen chloride gas, wherein the hydrogen chloride gas can be recycled;
2. The siloxane is transferred into dilute sulfuric acid, and the siloxane and the sulfuric acid are easily separated, so that the siloxane and the sulfuric acid can be recycled;
3. concentrating dilute sulfuric acid obtained after phase separation to obtain concentrated sulfuric acid with high concentration, which can be used as an extracting agent and can also be used for other purposes;
4. Dilute sulfuric acid containing organic matters can be concentrated into concentrated sulfuric acid to be used as an extracting agent, so that the concentrated sulfuric acid which is a byproduct in the production process of methane chloride, organic silicon and glyphosate is maximally utilized;
5. the extraction tower with three layers of fillers and a liquid distributor is adopted, so that the liquid mass transfer efficiency is improved;
6. The concentrated sulfuric acid obtained after concentration can be added with hydrogen peroxide to remove residual siloxane in the concentrated sulfuric acid, and the concentrated sulfuric acid can be purified.
Drawings
FIG. 1 is a schematic view of a structure of a desorption purification apparatus according to example 1;
FIG. 2 is a schematic view of the structure of an extraction column according to the present invention;
FIG. 3 is a schematic view of the analytical purification apparatus according to example 2;
FIG. 4 is a schematic view of the analytical purification apparatus according to example 3;
FIG. 5 is a schematic view showing the structure of a dilute sulfuric acid concentration apparatus according to example 3.
Detailed Description
the invention will be further described with reference to the following figures and specific examples, but the scope of the invention is not limited thereto.
Example 1
Referring to fig. 1-2, a siloxane-containing dilute hydrochloric acid desorption purification device comprises an extraction tower 1, a hydrogen chloride condenser 2 and a phase separator 3, wherein the top of the extraction tower 1 is provided with a gas outlet 11, the upper part is provided with a concentrated sulfuric acid inlet 12, the lower part is provided with a siloxane-containing dilute hydrochloric acid inlet 13, and the bottom is provided with a dilute sulfuric acid outlet 14; a dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1 is communicated with a liquid inlet of the phase separator 3, and the phase separator 3 is also provided with a dilute sulfuric acid outlet and a siloxane outlet; a gas outlet 11 at the top of the extraction tower 1 is communicated with a gas inlet of a hydrogen chloride condenser 2, and the hydrogen chloride condenser 2 is also provided with a hydrogen chloride discharge port and a condensed water outlet.
The phase separator of the present invention may be commercially available, such as liquid-liquid phase separator PT600-D from Franking, Germany, or liquid-liquid phase separator from Sulsho, Switzerland.
Referring to fig. 2, three layers of fillers 17 are arranged in the extraction tower 1 from top to bottom, a liquid distributor 16 is arranged above each layer of fillers 17, a concentrated sulfuric acid inlet 12 is arranged at the uppermost layer of liquid distributor, and a siloxane-containing dilute hydrochloric acid inlet 13 is arranged at the lowermost layer of liquid distributor.
A dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1 is communicated with a liquid inlet of the phase separator 3 through a second sulfuric acid storage tank 7; a siloxane outlet of the phase separator 3 is communicated with a siloxane storage tank 8; and a dilute sulfuric acid outlet of the phase separator 3 is communicated with a third sulfuric acid storage tank 9.
the analytic purification process of the analytic purification device comprises the following steps:
1. siloxane-containing dilute hydrochloric acid (the mass concentration of siloxane is 0.01-5%, the mass concentration of hydrochloric acid is 3-31%) is input into the extraction tower 1 through a siloxane-containing dilute hydrochloric acid inlet 13, and concentrated sulfuric acid is input into the extraction tower 1 through a concentrated sulfuric acid inlet 12.
2. The dilute hydrochloric acid and the high-concentration sulfuric acid meet in the extraction tower 1, the hydrogen chloride is dissociated from the water, and the hydrogen chloride containing moisture is discharged (can be recycled) through a hydrogen chloride discharge port on the hydrogen chloride condenser 2 after passing through the hydrogen chloride condenser 2; siloxane and water are transferred into sulfuric acid together, and dilute sulfuric acid (the mass concentration is usually 35-65%) is obtained from a dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1;
3. and (4) the dilute sulfuric acid enters a phase separator for phase separation, and the siloxane and the dilute sulfuric acid are separated and respectively recycled.
example 2
referring to fig. 2-3, a siloxane-containing dilute hydrochloric acid desorption purification device comprises an extraction tower 1, a hydrogen chloride condenser 2, a phase separator 3 and a dilute sulfuric acid concentration device 4, wherein the top of the extraction tower 1 is provided with a gas outlet 11, the upper part of the extraction tower is provided with a concentrated sulfuric acid inlet 12, the lower part of the extraction tower is provided with a siloxane-containing dilute hydrochloric acid inlet 13, and the bottom of the extraction tower is provided with a dilute sulfuric acid outlet 14; a dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1 is communicated with a liquid inlet of the phase separator 3, and the phase separator 3 is also provided with a dilute sulfuric acid outlet and a siloxane outlet; a gas outlet 11 at the top of the extraction tower 1 is communicated with a gas inlet of a hydrogen chloride condenser 2, and the hydrogen chloride condenser 2 is also provided with a hydrogen chloride discharge port and a condensed water outlet.
Referring to fig. 2, three layers of fillers 17 are arranged in the extraction tower 1 from top to bottom, a liquid distributor 16 is arranged above each layer of fillers 17, a concentrated sulfuric acid inlet 12 is arranged at the uppermost layer of liquid distributor, and a siloxane-containing dilute hydrochloric acid inlet 13 is arranged at the lowermost layer of liquid distributor; and a circulating sulfuric acid inlet 15 is also arranged at the liquid distribution layer of the middle layer, and the circulating sulfuric acid inlet 15 is communicated with the first sulfuric acid storage tank 5 and the condensed water outlet of the hydrogen chloride condenser 2. The first sulfuric acid storage tank 5 is used for storing concentrated sulfuric acid containing organic matters.
the hydrogen chloride condenser 2 comprises a first condenser 21 and a second condenser 22, a gas outlet 11 at the top of the extraction tower 1 is communicated with a gas inlet of the first condenser 21, a gas outlet of the first condenser 21 is communicated with a gas inlet of the second condenser 22, the second condenser 22 is provided with a hydrogen chloride discharge port, and liquid outlets of the first condenser and the second condenser are respectively communicated with the circulating sulfuric acid inlet 15.
A dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1 is communicated with a liquid inlet of the phase separator 3 through a second sulfuric acid storage tank 7; a siloxane outlet of the phase separator 3 is communicated with a siloxane storage tank 8; and a dilute sulfuric acid outlet of the phase separator 3 is communicated with a third sulfuric acid storage tank 9.
The analytic purification process of the analytic purification device comprises the following steps:
1. Siloxane-containing dilute hydrochloric acid (the mass concentration of siloxane is 0.01-5%, the mass concentration of hydrochloric acid is 3-31%) is input into the extraction tower 1 through a siloxane-containing dilute hydrochloric acid inlet 13, concentrated sulfuric acid is input into the extraction tower 1 through a concentrated sulfuric acid inlet 12, and concentrated sulfuric acid containing organic matters in a first sulfuric acid storage tank 5 is input into the extraction tower 1 through a circulating sulfuric acid inlet 15.
2. The dilute hydrochloric acid and the high-concentration sulfuric acid (comprising concentrated sulfuric acid input at two positions in the step 1) meet in an extraction tower 1, hydrogen chloride is dissociated from water and separated out, the hydrogen chloride containing water passes through a hydrogen chloride condenser 2 to be subjected to two-stage condensation, and finally is discharged (can be recycled) through a hydrogen chloride discharge port on the hydrogen chloride condenser 2; siloxane and water are transferred into sulfuric acid together, and dilute sulfuric acid is obtained from a dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1;
3. After the dilute sulfuric acid passes through the phase separator, siloxane is separated from the dilute sulfuric acid, and the siloxane and the dilute sulfuric acid are respectively recycled.
example 3
Referring to fig. 2, 4 and 5, the analytical purification device for siloxane-containing dilute hydrochloric acid comprises an extraction tower 1, a hydrogen chloride condenser 2, a phase separator 3, a dilute sulfuric acid concentration device 4 and an oxidation filtration device 500, wherein the top of the extraction tower 1 is provided with a gas outlet 11, the upper part is provided with a concentrated sulfuric acid inlet 12, the lower part is provided with a siloxane-containing dilute hydrochloric acid inlet 13, and the bottom is provided with a dilute sulfuric acid outlet 14; a dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1 is communicated with a liquid inlet of the phase separator 3, and the phase separator 3 is also provided with a dilute sulfuric acid outlet and a siloxane outlet; a gas outlet 11 at the top of the extraction tower 1 is communicated with a gas inlet of a hydrogen chloride condenser 2, and the hydrogen chloride condenser 2 is also provided with a hydrogen chloride discharge port and a condensed water outlet.
Referring to fig. 2, three layers of fillers 17 are arranged in the extraction tower 1 from top to bottom, a liquid distributor 16 is arranged above each layer of fillers 17, a concentrated sulfuric acid inlet 12 is arranged at the uppermost layer of liquid distributor, and a siloxane-containing dilute hydrochloric acid inlet 13 is arranged at the lowermost layer of liquid distributor; and a circulating sulfuric acid inlet 15 is also arranged at the liquid distribution layer of the middle layer, and the circulating sulfuric acid inlet 15 is communicated with the first sulfuric acid storage tank 5 and the condensed water outlet of the hydrogen chloride condenser 2. The first sulfuric acid storage tank 5 is used for storing concentrated sulfuric acid containing organic matters.
Referring to fig. 5, the dilute sulfuric acid concentration device 4 includes a first-stage vacuum concentration kettle 41 and a second-stage vacuum concentration kettle 42, the dilute sulfuric acid outlet of the phase separator 3 is communicated with the liquid inlet of the first-stage vacuum concentration kettle 41, the liquid outlet of the first-stage vacuum concentration kettle 41 is communicated with the liquid inlet of the second-stage vacuum concentration kettle 42, and the liquid outlet of the second-stage vacuum concentration kettle 42 is communicated with the concentrated sulfuric acid inlet 12 of the extraction tower 1.
The first-order vacuum concentration kettle be equipped with first-order heater 43 and first-order condenser 45, first-order heater 43 adopts 0.6 ~ 1.0Mpa low pressure saturated steam as the heat source, the gas inlet of first-order condenser 45 communicates the gas outlet of first-order vacuum concentration kettle 41, the gas outlet intercommunication vacuum of first-order condenser 45, the liquid outlet intercommunication condensate water storage tank 6 of first-order condenser 45.
The second-stage vacuum concentration kettle 42 is provided with a second-stage heater 44 and a second-stage condenser 46, the second-stage heater 44 adopts 1.0-2.0 Mpa medium-pressure saturated steam as a heat source, a gas inlet of the second-stage condenser 46 is communicated with a gas outlet of the second-stage vacuum concentration kettle 42, a gas outlet of the second-stage condenser 46 is communicated with vacuum, and a liquid outlet of the second-stage condenser 46 is communicated with the condensed water storage tank 6.
The hydrogen chloride condenser 2 comprises a first condenser 21 and a second condenser 22, a gas outlet 11 at the top of the extraction tower 1 is communicated with a gas inlet of the first condenser 21, a gas outlet of the first condenser 21 is communicated with a gas inlet of the second condenser 22, the second condenser 22 is provided with a hydrogen chloride discharge port, and liquid outlets of the first condenser and the second condenser are respectively communicated with the circulating sulfuric acid inlet 15.
A dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1 is communicated with a liquid inlet of the phase separator 3 through a second sulfuric acid storage tank 7; a siloxane outlet of the phase separator 3 is communicated with a siloxane storage tank 8; the dilute sulphuric acid outlet of the phase separator 3 is communicated with the liquid inlet of the first-stage vacuum concentration kettle 41 through a third sulphuric acid storage tank 9.
Referring to fig. 4, the oxidation filtering apparatus 500 includes a cooler 50, a fourth sulfuric acid storage tank 51, a filter 52, a fifth sulfuric acid storage tank 53 and a hydrogen peroxide storage tank 54, the liquid outlet of the two-stage vacuum concentration kettle 42 is sequentially communicated with the concentrated sulfuric acid inlet 12 of the extraction tower 1 through the cooler 50, the fourth sulfuric acid storage tank 51, the filter 52 and the fifth sulfuric acid storage tank 53, and the fourth sulfuric acid storage tank 51 is further communicated with the hydrogen peroxide storage tank 54.
The analytic purification process of the analytic purification device comprises the following steps:
1. Siloxane-containing dilute hydrochloric acid (the mass concentration of siloxane is 0.01-5%, the mass concentration of hydrochloric acid is 3-31%) is input into the extraction tower 1 through a siloxane-containing dilute hydrochloric acid inlet 13, concentrated sulfuric acid is input into the extraction tower 1 through a concentrated sulfuric acid inlet 12, and concentrated sulfuric acid containing organic matters in a first sulfuric acid storage tank 5 is input into the extraction tower 1 through a circulating sulfuric acid inlet 15.
2. the dilute hydrochloric acid meets high-concentration sulfuric acid (comprising concentrated sulfuric acid input at two positions in the step 1) in an extraction tower 1, hydrogen chloride is dissociated from water and separated out, the hydrogen chloride containing water passes through a hydrogen chloride condenser 2 to be subjected to two-stage condensation, and is finally discharged (can be recycled) through a hydrogen chloride discharge port on the hydrogen chloride condenser 2, and condensed water circularly enters the extraction tower 1 through a circulating sulfuric acid inlet 15; siloxane and water are transferred into sulfuric acid together, and dilute sulfuric acid is obtained from a dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1;
3. Dilute sulfuric acid enters a phase separator 3, siloxane is separated from the dilute sulfuric acid, the siloxane enters a siloxane storage tank 8, and the dilute sulfuric acid enters a third sulfuric acid storage tank 9;
4. the dilute sulfuric acid obtained by separation in the phase separator 3 enters a dilute sulfuric acid concentration device, and is subjected to vacuum concentration in a first-stage vacuum concentration kettle 41 and a second-stage vacuum concentration kettle 42 in sequence to obtain concentrated sulfuric acid (usually 80-97%) with the mass concentration of more than 80%. The waste water obtained by the dilute sulfuric acid concentration device enters a condensed water storage tank 6, can be recycled and can also be subjected to centralized treatment and discharge.
5. And inputting the concentrated sulfuric acid and hydrogen peroxide into a fourth sulfuric acid storage tank 51 together for oxidation reaction, wherein the adding amount of the hydrogen peroxide in the hydrogen peroxide accounts for 0.03-20% of the mass of the concentrated sulfuric acid, and removing residual siloxane in the concentrated sulfuric acid. The produced white carbon black is filtered off by a filter 52. The treated concentrated sulfuric acid enters the extraction tower 1 through a fifth sulfuric acid storage tank 53 and a concentrated sulfuric acid inlet 12 to perform the circulating extraction operation.
Claims (13)
1. A process for the analytical purification of dilute hydrochloric acid containing siloxane, characterized in that it comprises the following steps:
(1) Extracting dilute hydrochloric acid containing siloxane by adopting concentrated sulfuric acid to separate out hydrogen chloride gas, and transferring the siloxane into dilute sulfuric acid;
(2) The diluted sulfuric acid containing siloxane is subjected to phase separation to obtain siloxane and diluted sulfuric acid.
2. the process according to claim 1, characterized in that: in the diluted siloxane-containing hydrochloric acid obtained in the step (1), the mass concentration of siloxane is 0.01-5%, and the mass concentration of hydrochloric acid is 3-31%.
3. The process according to claim 1, characterized in that: the concentrated sulfuric acid is organic matter-containing concentrated sulfuric acid.
4. the process according to claim 1, wherein the process comprises the steps of: further comprising the step (3): and (3) concentrating the dilute sulfuric acid to obtain concentrated sulfuric acid, and returning the concentrated sulfuric acid to the step (1) for extraction.
5. The process according to claim 4, characterized in that: and (3) carrying out vacuum concentration on the dilute sulfuric acid obtained in the step (2) to obtain concentrated sulfuric acid with the mass concentration of more than 80%.
6. The process according to claim 4 or 5, characterized in that: adding hydrogen peroxide into the concentrated sulfuric acid, wherein the adding amount of the hydrogen peroxide in the concentrated sulfuric acid accounts for 0.03-20% of the mass of the concentrated sulfuric acid, oxidizing siloxane in the hydrogen peroxide into white carbon black, filtering to remove the white carbon black, and returning the concentrated sulfuric acid to the step (1) for use.
7. a siloxane-containing dilute hydrochloric acid desorption purification device is characterized in that: the device comprises an extraction tower, a hydrogen chloride condenser and a phase separator, wherein the top of the extraction tower is provided with a gas outlet, the upper part of the extraction tower is provided with a concentrated sulfuric acid inlet, the lower part of the extraction tower is provided with a diluted hydrochloric acid inlet containing siloxane, and the bottom of the extraction tower is provided with a diluted sulfuric acid outlet; a dilute sulfuric acid outlet at the bottom of the extraction tower is communicated with a liquid inlet of the phase separator, the phase separator is also provided with a dilute sulfuric acid outlet and a siloxane outlet, and the siloxane outlet is communicated with a siloxane storage tank; the gas outlet at the top of the extraction tower is communicated with the gas inlet of a hydrogen chloride condenser, and the hydrogen chloride condenser is also provided with a hydrogen chloride outlet and a condensed water outlet.
8. The analytical purification device for dilute hydrochloric acid containing siloxane according to claim 7, characterized in that: three layers of fillers are arranged in the extraction tower from top to bottom, a liquid distributor is arranged above each layer of fillers, a concentrated sulfuric acid inlet is arranged at the uppermost layer of liquid distributor, and a siloxane-containing dilute hydrochloric acid inlet is arranged at the lowermost layer of liquid distributor; and a circulating sulfuric acid inlet is also arranged at the liquid distribution layer of the middle layer and is communicated with the first sulfuric acid storage tank and the condensed water outlet of the hydrogen chloride condenser.
9. the analytical purification device for dilute hydrochloric acid containing siloxane according to claim 7, characterized in that: the device also comprises a dilute sulfuric acid concentration device, wherein the dilute sulfuric acid concentration device comprises a primary vacuum concentration kettle and a secondary vacuum concentration kettle, a dilute sulfuric acid outlet of the phase separator is communicated with a liquid inlet of the primary vacuum concentration kettle, a liquid outlet of the primary vacuum concentration kettle is communicated with a liquid inlet of the secondary vacuum concentration kettle, and a liquid outlet of the secondary vacuum concentration kettle is communicated with a concentrated sulfuric acid inlet of the extraction tower.
10. The analytical purification device for dilute hydrochloric acid containing siloxane according to claim 9, characterized in that:
The primary vacuum concentration kettle is provided with a primary heater and a primary condenser, the primary heater adopts 0.6-2.0 Mpa saturated steam as a heat source, a gas inlet of the primary condenser is communicated with a gas outlet of the primary vacuum concentration kettle, a gas outlet of the primary condenser is communicated with vacuum, and a liquid outlet of the primary condenser is communicated with a condensed water storage tank;
The second-stage vacuum concentration kettle is provided with a second-stage heater and a second-stage condenser, the second-stage heater adopts 1.0-2.0 Mpa saturated steam as a heat source, a gas inlet of the second-stage condenser is communicated with a gas outlet of the second-stage vacuum concentration kettle, a gas outlet of the second-stage condenser is communicated with vacuum, and a liquid outlet of the second-stage condenser is communicated with a condensed water storage tank.
11. The analytical purification device for dilute hydrochloric acid containing siloxane according to claim 9, characterized in that: the device further comprises an oxidation and filtration device, the oxidation and filtration device comprises a cooler, a fourth sulfuric acid storage tank, a filter, a fifth sulfuric acid storage tank and a hydrogen peroxide storage tank, a liquid outlet of the second-stage vacuum concentration kettle is communicated with a concentrated sulfuric acid inlet of the desorption tower through the cooler, the fourth sulfuric acid storage tank, the filter and the fifth sulfuric acid storage tank in sequence, and the fourth sulfuric acid storage tank is communicated with the hydrogen peroxide storage tank.
12. the analytical purification device for dilute hydrochloric acid containing siloxane according to claim 8, characterized in that: the hydrogen chloride condenser comprises a first condenser and a second condenser, a gas outlet at the top of the extraction tower is communicated with a gas inlet of the first condenser, a gas outlet of the first condenser is communicated with a gas inlet of the second condenser, the second condenser is provided with a hydrogen chloride discharge port, and liquid outlets of the first condenser and the second condenser are respectively communicated with a circulating sulfuric acid inlet.
13. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 10, characterized in that: and a dilute sulfuric acid outlet at the bottom of the desorption tower is communicated with a liquid inlet of the phase separator through a second sulfuric acid storage tank, and a dilute sulfuric acid outlet of the phase separator is communicated with a liquid inlet of the first-stage vacuum concentration kettle through a third sulfuric acid storage tank.
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