CN211393845U - Siloxane-containing dilute hydrochloric acid analysis and purification device - Google Patents
Siloxane-containing dilute hydrochloric acid analysis and purification device Download PDFInfo
- Publication number
- CN211393845U CN211393845U CN201921729189.2U CN201921729189U CN211393845U CN 211393845 U CN211393845 U CN 211393845U CN 201921729189 U CN201921729189 U CN 201921729189U CN 211393845 U CN211393845 U CN 211393845U
- Authority
- CN
- China
- Prior art keywords
- sulfuric acid
- condenser
- outlet
- communicated
- inlet
- 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.)
- Active
Links
Images
Landscapes
- Treating Waste Gases (AREA)
Abstract
The utility model relates to a siloxane-containing dilute hydrochloric acid analysis and purification device, which comprises an extraction tower and a hydrogen chloride condenser, 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; 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. The utility model adopts concentrated sulfuric acid to extract dilute hydrochloric acid containing siloxane through the extraction tower, so that hydrogen chloride gas is separated out, and the hydrogen chloride can be recycled; meanwhile, 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.
Description
Technical Field
The utility model relates to a siloxane-containing dilute hydrochloric acid analysis and purification device.
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.
SUMMERY OF THE UTILITY MODEL
In order to overcome the defects existing in the prior art, the utility model provides a siloxane-containing dilute hydrochloric acid analysis and purification device with low cost, small energy consumption, good treatment effect, high reliability and stable operation.
A desorption and purification device of diluted hydrochloric acid containing siloxane comprises an extraction tower and a hydrogen chloride condenser, 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; 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, the device further comprises a phase separator, 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.
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.
Preferably, a circulating sulfuric acid inlet is further 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 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, 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, a dilute sulfuric acid outlet at the bottom of the extraction 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.
Preferably, the device further comprises an oxidation filtering device, wherein the oxidation filtering 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 extraction 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 siloxane outlet of the phase separator is communicated with a siloxane storage tank.
The dilute sulfuric acid concentration device of the utility model can refer to the dilute sulfuric acid vacuum concentration device and the dilute sulfuric acid vacuum concentration method disclosed in the 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 beneficial effects of the utility model reside in that:
1. extracting dilute hydrochloric acid containing siloxane by adopting concentrated sulfuric acid through an extraction tower to separate out hydrogen chloride gas, wherein the hydrogen chloride gas can be recycled; meanwhile, the siloxane is transferred into dilute sulfuric acid, and the siloxane and the sulfuric acid are easy to separate, so that the siloxane and the sulfuric acid can be recycled;
2. by passing through a phase separator, dilute sulfuric acid and most of the siloxane are separated;
3. concentrating the obtained dilute sulfuric acid by a dilute sulfuric acid concentration device to obtain high-concentration concentrated sulfuric acid which can be used as an extracting agent and can also be used for other purposes;
4. the extraction tower with three layers of fillers and a liquid distributor is adopted, so that the liquid mass transfer efficiency is improved;
5. through a fourth sulfuric acid storage tank and a hydrogen peroxide storage tank, the concentrated sulfuric acid obtained after concentration is added with hydrogen peroxide to remove residual siloxane in the concentrated sulfuric acid, so that 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 structural view of the extraction column of 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;
FIG. 6 is a schematic view of the analytical purification apparatus according to example 4.
Detailed Description
The invention will be further described with reference to the accompanying drawings and specific embodiments, 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 utility model can select the mature products on the market, such as the liquid-liquid phase separator PT600-D produced by Germany Franken company, the liquid-liquid phase separator produced by Swiss Sulsho company, etc.
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. diluted hydrochloric acid containing siloxane (the mass concentration of the siloxane is 0.01-5%, and the mass concentration of the hydrochloric acid is 3-31%) is input into the extraction tower 1 through a diluted hydrochloric acid inlet 13 containing siloxane, 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. diluted hydrochloric acid containing siloxane (the mass concentration of the siloxane is 0.01-5 percent, and the mass concentration of the hydrochloric acid is 3-31 percent) is input into the extraction tower 1 through a diluted hydrochloric acid inlet 13 containing siloxane, 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 dilute hydrochloric acid containing siloxane comprises an extraction tower 1, a hydrogen chloride condenser 2, a phase separator 3, a dilute sulfuric acid concentration device 4 and an oxidation filter 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 dilute hydrochloric acid inlet 13 containing siloxane, 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.
Referring to fig. 3, 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 outlet, and liquid outlets of the first condenser and the second condenser are respectively communicated with a 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, a liquid outlet of the two-stage vacuum concentration kettle 42 is sequentially communicated with a 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. diluted hydrochloric acid containing siloxane (the mass concentration of the siloxane is 0.01-5 percent, and the mass concentration of the hydrochloric acid is 3-31 percent) is input into the extraction tower 1 through a diluted hydrochloric acid inlet 13 containing siloxane, 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.
Example 4
Referring to fig. 2 and 6, the analytical purification device for diluted hydrochloric acid containing siloxane comprises an extraction tower 1 and a hydrogen chloride condenser 2, 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 diluted hydrochloric acid inlet 13 containing siloxane, and the bottom is provided with a diluted sulfuric acid outlet 14; 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 a condensed water outlet of the hydrogen chloride condenser 2.
The analytic purification process of the analytic purification device comprises the following steps:
1. diluted hydrochloric acid containing siloxane (the mass concentration of the siloxane is 0.01-5 percent, and the mass concentration of the hydrochloric acid is 3-31 percent) is input into the extraction tower 1 through a diluted hydrochloric acid inlet 13 containing siloxane, concentrated sulfuric acid is input into the extraction tower 1 through a concentrated sulfuric acid inlet 12, and circulating sulfuric acid 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, and is finally discharged (can be recycled) through a hydrogen chloride discharge port on the hydrogen chloride condenser 2, and condensed water is circulated into the extraction tower 1 through a circulating sulfuric acid inlet 15; the siloxane and the water are transferred into the sulfuric acid together, and the dilute sulfuric acid containing the siloxane is obtained from a dilute sulfuric acid outlet 14 at the bottom of the extraction tower 1.
Claims (10)
1. A siloxane-containing dilute hydrochloric acid desorption purification device is characterized in that: the device comprises an extraction tower and a hydrogen chloride condenser, 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; 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.
2. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 1, characterized in that: the device also comprises a phase separator, wherein 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.
3. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 1 or 2, characterized in that: the extraction tower is internally provided with three layers of fillers from top to bottom, a liquid distributor is arranged above each layer of filler, 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.
4. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 3, characterized in that: 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.
5. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 4, 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.
6. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 2, 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.
7. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 6, 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.
8. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 7, characterized in that: and a dilute sulfuric acid outlet at the bottom of the extraction 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.
9. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 6, characterized in that: the device further comprises an oxidation filtering device, the oxidation filtering 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 extraction 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.
10. The apparatus for the analytical purification of dilute hydrochloric acid containing siloxane according to claim 2, characterized in that: and the siloxane outlet of the phase separator is communicated with a siloxane storage tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921729189.2U CN211393845U (en) | 2019-10-15 | 2019-10-15 | Siloxane-containing dilute hydrochloric acid analysis and purification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921729189.2U CN211393845U (en) | 2019-10-15 | 2019-10-15 | Siloxane-containing dilute hydrochloric acid analysis and purification device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211393845U true CN211393845U (en) | 2020-09-01 |
Family
ID=72210138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921729189.2U Active CN211393845U (en) | 2019-10-15 | 2019-10-15 | Siloxane-containing dilute hydrochloric acid analysis and purification device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211393845U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110562923A (en) * | 2019-10-15 | 2019-12-13 | 杭州东日节能技术有限公司 | Analytical purification process and analytical purification device for diluted hydrochloric acid containing siloxane |
| CN112456450A (en) * | 2020-10-15 | 2021-03-09 | 浙江迪邦化工有限公司 | System and method for resource utilization of waste sulfuric acid containing organic matters |
-
2019
- 2019-10-15 CN CN201921729189.2U patent/CN211393845U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110562923A (en) * | 2019-10-15 | 2019-12-13 | 杭州东日节能技术有限公司 | Analytical purification process and analytical purification device for diluted hydrochloric acid containing siloxane |
| CN110562923B (en) * | 2019-10-15 | 2023-10-13 | 杭州东日节能技术有限公司 | Analysis and purification process and analysis and purification device for dilute hydrochloric acid containing siloxane |
| CN112456450A (en) * | 2020-10-15 | 2021-03-09 | 浙江迪邦化工有限公司 | System and method for resource utilization of waste sulfuric acid containing organic matters |
| CN112456450B (en) * | 2020-10-15 | 2022-02-18 | 浙江迪邦化工有限公司 | System and method for resource utilization of waste sulfuric acid containing organic matters |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110562923B (en) | Analysis and purification process and analysis and purification device for dilute hydrochloric acid containing siloxane | |
| CN110642229A (en) | Mixed analysis purification process and mixed analysis purification device for siloxane-containing hydrochloric acid and organic matter-containing sulfuric acid | |
| CN211393845U (en) | Siloxane-containing dilute hydrochloric acid analysis and purification device | |
| CN102145251B (en) | Dechloridation device and process in chlorinated paraffin production process | |
| CN100525874C (en) | Six-column differential-pressure distillation device for extra edible alcohol and process therefor | |
| CN102153449B (en) | Continuous refining separation device and method for coal gasification crude phenol | |
| CN106866368A (en) | Alcoholic gas field sewage methanol recovery device and technique based on air- extraction and vacuum membrane distillation method | |
| CN106430789A (en) | Technology for preparing boiler water from process condensate | |
| CN211393846U (en) | Siloxane-containing hydrochloric acid and organic matter-containing sulfuric acid mixing, analyzing and purifying device | |
| CN113247862A (en) | High-purity electronic-grade hydrogen chloride production device and process | |
| CN110734045B (en) | Method for removing siloxane from concentrated sulfuric acid containing siloxane | |
| CN208182895U (en) | A kind of tetrahydrofuran fractional order reaction separator | |
| CN104108686B (en) | Pressure-relief discharge, absorption, treatment and recycling method in production process of thionyl chloride | |
| CN201949806U (en) | Dechlorination device in process of producing chlorinated paraffin | |
| CN206328320U (en) | A kind of high purity caprolactam refining plant | |
| CN201537408U (en) | Purification treatment tower for producing hydrogen with natural gas | |
| CN101440102B (en) | Method for processing methyl monomer synthesized washing slurry | |
| CN204973822U (en) | A many functional response cauldron for epoxy plasticizer production | |
| CN209619032U (en) | A kind of oil-removing iron-removing apparatus of sulfuric acid process alkylation system | |
| CN207793117U (en) | A kind of improved refining of crude phenol system | |
| CN201952379U (en) | Continuous refining and separating device of gasified crude phenol | |
| CN112759608A (en) | Equipment and process for removing metal impurities in octamethylcyclotetrasiloxane | |
| CN218901388U (en) | Purification system for chlorosilane hydrolysis byproduct hydrogen chloride | |
| CN110964053A (en) | Device and method for purifying trimethylsilyl trifluoromethanesulfonate | |
| CN220861410U (en) | Methyl chloride synthesis system without byproduct hydrochloric acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |