CN210710735U - Device for resolving and separating hydrogen chloride and water from hydrochloric acid - Google Patents
Device for resolving and separating hydrogen chloride and water from hydrochloric acid Download PDFInfo
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- CN210710735U CN210710735U CN201921101887.8U CN201921101887U CN210710735U CN 210710735 U CN210710735 U CN 210710735U CN 201921101887 U CN201921101887 U CN 201921101887U CN 210710735 U CN210710735 U CN 210710735U
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Abstract
A device of analytic separation hydrogen chloride and water in follow hydrochloric acid, belong to the technical field of the analytic production hydrogen chloride of hydrochloric acid, including the analytic system of hydrochloric acid, neutralization system and concentrated system, adopt this device to produce hydrogen chloride, have the advantage that purity is high (purity > 99.9%) and the purity is undulant little, be favorable to hydrochlorination's automatic control, can also utilize the byproduct hydrogen chloride of low concentration in the organochlorine product production process comprehensively, in order to make the high-purity hydrogen chloride gas, in addition, the pressure of the hydrogen chloride of product hydrogen chloride borrowing is carried, thereby save hydrogen chloride's pressurized equipment, equipment investment is economized, the working costs is low, the bad border pollutes fewly.
Description
Technical Field
The invention relates to the technical field of hydrogen chloride production by hydrochloric acid resolution, in particular to a device for separating hydrogen chloride and water from hydrochloric acid by resolution.
Background
At present, the more mature dilute hydrochloric acid desorption process mainly comprises three processes, namely a sulfuric acid extraction and rectification method, a calcium chloride extraction and rectification method and a pressure swing rectification method (a pressure difference method).
A process for extracting and rectifying sulfuric acid features that the sulfuric acid and water are fully dissolved in each other and the boiling point of concentrated sulfuric acid is higher than that of constant-boiling hydrochloric acid, so the water in diluted hydrochloric acid is transferred to concentrated sulfuric acid to obtain relatively diluted sulfuric acid, which is then used to extract hydrogen chloride. However, the concentration of the used concentrated sulfuric acid is high, the boiling point of the sulfuric acid is increased when the sulfuric acid is concentrated to the concentrated sulfuric acid, the method has higher requirements on equipment and large investment, and the evaporated waste water contains hydrogen chloride and can not be discharged up to the standard.
The calcium chloride extractive distillation method is that calcium chloride is added into dilute hydrochloric acid to break the limit of azeotropic point and separate out hydrogen chloride. The method adopts a high tower (packed tower) to carry out mass transfer and heat transfer, the equipment investment is large, a reboiler utilizes the siphon principle, the circulation speed is slow, the heat efficiency is low, calcium chloride material holes are easy to scale, the service life of the equipment is short, the evaporation dehydration is single-effect evaporation, the heat energy utilization is low, the steam consumption is high, the actual value of the HCl concentration in the wastewater is 2-3%, an evaporation device adopts graphite equipment, and the investment is large.
The pressure-variable rectification method is based on the principle that the composition of constant-boiling hydrochloric acid changes with pressure, relative to H2O and HCl, constant boiling hydrochloric acid is always a feature of high boiling point component, thereby achieving the purpose of making H2The purpose of separating O and HCl. The main equipment of the method is a pressurizing tower and a negative pressure tower, the diameter of the negative pressure tower is large, the height of the negative pressure tower is high, and the equipment investment is large; the reflux at the top of the tower causes large steam consumption, namely high operation cost. Due to the circulation of materials between the pressurizing tower and the negative pressure tower, the operation requirement is strict, and the automation level requirement is high.
Disclosure of Invention
The invention provides a device for resolving and separating hydrogen chloride and water from hydrochloric acid, and aims to solve the problems of large investment, high running cost and environmental pollution of the existing equipment and process.
In order to solve the technical problems, the invention adopts the following technical scheme:
a device for resolving and separating hydrogen chloride and water from hydrochloric acid comprises a hydrochloric acid resolving system, a neutralizing system and a concentrating system, wherein the hydrochloric acid resolving system comprises a hydrochloric acid preheater, a mixing heater, a separator, a primary cooler, a secondary cooler, a gas-liquid separator, a falling film evaporation separator, a flash evaporation condenser, a resolving system vacuum unit and a resolving system liquid seal tank; the neutralization system comprises a calcium hydroxide storage tank, a spiral metering scale, a mixing pump, a buffer tank, a discharge pump and a filter; the concentration system comprises a first-effect evaporation separator, a second-effect evaporation separator, a calcium chloride circulating pump, an evaporation condenser, a concentration system vacuum unit, a concentration system liquid seal tank and a waste water pump;
the bottom of the hydrochloric acid preheater is added with a hydrochloric acid solution, the middle part of the hydrochloric acid preheater is added with a steam condensate, a top outlet of the hydrochloric acid preheater is connected with a top inlet of the mixing heater, the middle part of the mixing heater is introduced with steam, a bottom outlet of the mixing heater is connected with an inlet of a separator, a top outlet of the separator is connected with a primary cooler, the primary cooler is connected with a secondary cooler, the secondary cooler is connected with a gas-liquid separator, a gas phase of the gas-liquid separator outputs hydrogen chloride gas, a liquid phase of the gas-liquid separator outputs concentrated hydrochloric acid, a bottom outlet of the separator is connected with an inlet of a falling film evaporation separator, the middle part of the falling film evaporation separator is introduced with steam, a gas phase outlet of the flash evaporator is connected with an analytic system;
calcium hydroxide is introduced into an inlet of the calcium hydroxide storage tank, an outlet of the calcium hydroxide storage tank is connected with a spiral metering scale, the spiral metering scale is connected with a mixing pump, the mixing pump is connected with a buffer tank, the buffer tank is connected with a discharging pump, the discharging pump is connected with a filter, the filter is connected with an inlet of a one-effect evaporation separator, and calcium chloride is filtered out;
the utility model discloses a dual-effect evaporation separator, including a dual-effect evaporation separator, a liquid phase outlet of dual-effect evaporation separator is connected with evaporative condenser, evaporative condenser connects concentrated system vacuum unit and concentrated system liquid seal tank, the waste water pump is connected to concentrated system liquid seal tank, the part connects dual-effect evaporation separator, let in steam in the middle part of dual-effect evaporation separator, a dual-effect evaporation separator gas phase outlet of dual-effect evaporation separator.
Preferably, the bottom of the secondary cooler outputs concentrated hydrochloric acid.
Preferably, a hydrochloric acid pump and a flow meter are arranged at a hydrochloric acid solution inlet of the hydrochloric acid preheater.
Compared with the prior art, the invention has the beneficial effects that:
1. equipment investment is saved: because the hydrochloric acid with higher pressure and the calcium chloride with high concentration are fully mixed, a differential mixing structure is arranged in the material pipe of the mixing heater, the hydrochloric acid and the calcium chloride with high concentration are fully mixed, and a large graphite desorption tower and a filler are saved; the hydrogen chloride in the dilute calcium chloride is further reduced by adopting the vacuum falling film evaporation of the dilute calcium chloride solution, the dosage of the calcium hydroxide is reduced for the neutralization process, the neutralized calcium chloride solution becomes alkaline, the requirement on equipment materials can be reduced when the calcium chloride is concentrated, and the equipment investment is saved.
2. The operation cost is low: because the desorption tower is cancelled, the mixed solution of the hydrochloric acid and the calcium chloride enters the separator in an atomization mode, the separator is an empty container, the desorption temperature is 115-125 ℃, and the temperature is 20 ℃ lower than that of the bottom of the desorption tower when the desorption tower operates, so that the energy consumption can be saved; the method for neutralizing the acid-containing calcium chloride is adopted, the concentration of the calcium chloride can adopt two-effect evaporation, the steam is recycled, the steam consumption is greatly reduced, and the core of the invention is also the method for neutralizing the acid-containing calcium chloride; and a reboiler is cancelled, so that the scaling of the equipment can be avoided, the long-term operation of the equipment is ensured, and the updating cost of the equipment is saved. The hydrogen chloride utilization rate is improved by adopting a secondary hydrogen chloride analysis mode (first pressurization analysis and second vacuum analysis), the hydrogen chloride content in the dilute calcium chloride is greatly reduced, the calcium hydroxide dosage is also reduced, and the purchase cost is reduced.
3. Clean production: because the method of neutralization is adopted, the problem that the hydrogen chloride in the calcium chloride is converted into the calcium chloride is solved, and the separated water can be discharged without the hydrogen chloride. The water can be recycled or treated by a reverse osmosis membrane to produce pure water. The excessive hydrogen chloride can be discharged continuously in the process of neutralization reaction, continuous replacement and updating are carried out, a filter is arranged in the system to filter not only impurities generated by calcium hydroxide reaction, but also other impurities in the system, and the environmental protection problem of calcium chloride solution treatment caused by regular calcium chloride replacement in the process of the desorption tower is avoided.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in the figure: a device for resolving and separating hydrogen chloride and water from hydrochloric acid comprises a hydrochloric acid resolving system, a neutralization system and a concentration system, wherein the hydrochloric acid resolving system comprises a hydrochloric acid preheater 101, a mixing heater 102, a separator 103, a primary cooler 104, a secondary cooler 105, a gas-liquid separator 106, a falling film evaporation separator 107, a flash evaporation condenser 108, a resolving system vacuum unit 109 and a resolving system liquid seal tank 110; the neutralization system comprises a calcium hydroxide storage tank 201, a spiral metering scale 202, a mixing pump 203, a buffer tank 204, a discharge pump 205 and a filter 206; the concentration system comprises a single-effect evaporation separator 301, a double-effect evaporation separator 302, a calcium chloride circulating pump 303, an evaporation condenser 304, a concentration system vacuum unit 305, a concentration system liquid seal tank 306 and a waste water pump 307;
the bottom of the hydrochloric acid preheater 101 is added with a hydrochloric acid solution, a hydrochloric acid pump and a flow meter are arranged at a hydrochloric acid solution inlet of the hydrochloric acid preheater 101, a steam condensate is added at the middle part, a top outlet is connected with a top inlet of the mixing heater 102, steam is introduced into the middle part of the mixing heater 102, a bottom outlet is connected with an inlet of the separator 103, a top outlet of the separator 103 is connected with a first-stage cooler 104, the first-stage cooler 104 is connected with a second-stage cooler 105, the second-stage cooler 105 is connected with a gas-liquid separator 106, a gas phase of the gas-liquid separator 106 outputs hydrogen chloride gas, a liquid phase and a bottom of the second-stage cooler 105 output concentrated hydrochloric acid, a bottom outlet of the separator 103 is connected with an inlet of the falling film evaporation separator 107, steam is introduced into the middle part of the falling film evaporation separator 107, a gas phase, the liquid phase outlet of the falling film evaporation separator 107 is connected with the inlet of the mixing pump 203;
calcium hydroxide is introduced into an inlet of the calcium hydroxide storage tank 201, an outlet of the calcium hydroxide storage tank is connected with the spiral metering scale 202, the spiral metering scale 202 is connected with the mixing pump 203, the mixing pump 203 is connected with the buffer tank 204, the buffer tank 204 is connected with the discharge pump 205, the discharge pump 205 is connected with the filter 206, the filter 206 is connected with an inlet of the one-effect evaporation separator 301, and calcium chloride is filtered out;
the gas-phase outlet of the first-effect evaporation separator 301 is connected with an evaporation condenser 304, the evaporation condenser 304 is connected with a concentration system vacuum unit 305 and a concentration system liquid seal tank 306, the concentration system liquid seal tank 306 is connected with a waste water pump 307, the waste water pump 307 outputs water, the part of the liquid-phase outlet of the first-effect evaporation separator 301 is connected with the concentration system liquid seal tank 306, the part of the liquid-phase outlet of the first-effect evaporation separator is connected with a second-effect evaporation separator 302, steam is introduced into the middle part of the second-effect evaporation separator 302, the gas-phase outlet of the second-effect evaporation separator 302 is connected with the first-effect evaporation separator 301, the liquid-phase outlet of the first-effect.
Example 1:
(1) sending the hydrochloric acid solution into a hydrochloric acid preheater through a hydrochloric acid pump and a flowmeter, introducing steam condensate, preheating to 70 ℃, and then sending into a mixing heater;
(2) feeding hydrochloric acid solution into a mixing heater, fully mixing the hydrochloric acid solution with 55-60% calcium chloride solution from a calcium chloride circulating pump, feeding steam to adjust the temperature to 115 ℃, and feeding the mixture into a separator;
(3) the hydrogen chloride gas analyzed in the separator is discharged from a top outlet and sequentially passes through a primary cooler, a secondary cooler and a gas-liquid separator to enter the next procedure, and concentrated hydrochloric acid in the secondary cooler and the gas-liquid separator is sent to a concentrated hydrochloric acid storage tank; the dilute calcium chloride solution at the bottom of the separator enters a falling film evaporation separator;
(4) the gas phase of the falling film evaporation separator enters a flash evaporation condenser to further remove hydrogen chloride in calcium chloride, the condensed dilute hydrochloric acid solution enters an analysis system liquid seal tank and then is sent into a dilute hydrochloric acid storage tank, the non-condensable gas in the flash evaporation condenser enters an analysis system vacuum unit, the temperature in the falling film evaporation separator is adjusted to be 120 ℃, the liquid phase of the falling film evaporation separator and calcium hydroxide from the calcium hydroxide storage tank are mixed in a mixing pump inlet pump, the PH value is adjusted to be 7, then the mixture enters a buffer tank, the mixture is pressurized by a discharge pump and filtered by a filter, and then the mixture enters a one-effect evaporation separator, and the calcium chloride is filtered by the filter;
(5) the gas phase of the first-effect evaporation separator enters an evaporation condenser for cooling and then enters a liquid seal tank of a concentration system, the gas phase and part of the liquid phase are mixed in the liquid seal tank of the concentration system and then discharged by a waste water pump, the non-condensable gas in the evaporation condenser enters a vacuum unit of the concentration system, and part of the liquid phase of the first-effect evaporation separator enters a second-effect evaporation separator;
(6) the temperature in the two-effect evaporation separator is adjusted to be 120 ℃, the gas phase of the two-effect evaporation separator enters the one-effect evaporation separator, and the liquid phase is sent to the mixing heater through the calcium chloride circulating pump.
Example 2:
(1) sending the hydrochloric acid solution into a hydrochloric acid preheater through a hydrochloric acid pump and a flowmeter, introducing steam condensate, preheating to 80 ℃, and then sending into a mixing heater;
(2) feeding hydrochloric acid solution into a mixing heater, fully mixing the hydrochloric acid solution with 55-60% calcium chloride solution from a calcium chloride circulating pump, feeding steam to adjust the temperature to 125 ℃, and feeding the mixture into a separator;
(3) the hydrogen chloride gas analyzed in the separator is discharged from a top outlet and sequentially passes through a primary cooler, a secondary cooler and a gas-liquid separator to enter the next procedure, and concentrated hydrochloric acid in the secondary cooler and the gas-liquid separator is sent to a concentrated hydrochloric acid storage tank; the dilute calcium chloride solution at the bottom of the separator enters a falling film evaporation separator;
(4) the gas phase of the falling film evaporation separator enters a flash evaporation condenser to further remove hydrogen chloride in calcium chloride, the condensed dilute hydrochloric acid solution enters an analysis system liquid seal tank and then is sent into a dilute hydrochloric acid storage tank, the non-condensable gas in the flash evaporation condenser enters an analysis system vacuum unit, the temperature in the falling film evaporation separator is adjusted to be 130 ℃, the liquid phase of the falling film evaporation separator and calcium hydroxide from the calcium hydroxide storage tank are pumped and mixed at the inlet of a mixing pump, the pH value is adjusted to be 7.5, then the mixture enters a buffer tank, the mixture is pressurized by a discharge pump and filtered by a filter, and then the mixture enters a one-effect evaporation separator, and the calcium chloride is filtered by the filter;
(5) the gas phase of the first-effect evaporation separator enters an evaporation condenser for cooling and then enters a liquid seal tank of a concentration system, the gas phase and part of the liquid phase are mixed in the liquid seal tank of the concentration system and then discharged by a waste water pump, the non-condensable gas in the evaporation condenser enters a vacuum unit of the concentration system, and part of the liquid phase of the first-effect evaporation separator enters a second-effect evaporation separator;
(6) the temperature in the double-effect evaporation separator is adjusted to 130 ℃, the gas phase of the double-effect evaporation separator enters the single-effect evaporation separator, and the liquid phase is sent to the mixing heater through the calcium chloride circulating pump.
Example 3:
(1) sending the hydrochloric acid solution into a hydrochloric acid preheater through a hydrochloric acid pump and a flowmeter, introducing steam condensate, preheating to 75 ℃, and then sending into a mixing heater;
(2) feeding hydrochloric acid solution into a mixing heater, fully mixing the hydrochloric acid solution with 55-60% calcium chloride solution from a calcium chloride circulating pump, feeding steam to adjust the temperature to 120 ℃, and feeding the mixture into a separator;
(3) the hydrogen chloride gas analyzed in the separator is discharged from a top outlet and sequentially passes through a primary cooler, a secondary cooler and a gas-liquid separator to enter the next procedure, and concentrated hydrochloric acid in the secondary cooler and the gas-liquid separator is sent to a concentrated hydrochloric acid storage tank; the dilute calcium chloride solution at the bottom of the separator enters a falling film evaporation separator;
(4) the gas phase of the falling film evaporation separator enters a flash evaporation condenser to further remove hydrogen chloride in calcium chloride, the condensed dilute hydrochloric acid solution enters an analysis system liquid seal tank and then is sent into a dilute hydrochloric acid storage tank, the non-condensable gas in the flash evaporation condenser enters an analysis system vacuum unit, the temperature in the falling film evaporation separator is adjusted to be 125 ℃, the liquid phase of the falling film evaporation separator and calcium hydroxide from the calcium hydroxide storage tank are pumped and mixed at an inlet of a mixing pump, the pH value is adjusted to be 7.2 and then enter a buffer tank, the mixture is pressurized by a discharge pump and filtered by a filter and then enters a one-effect evaporation separator, and the calcium chloride is filtered by the filter;
(5) the gas phase of the first-effect evaporation separator enters an evaporation condenser for cooling and then enters a liquid seal tank of a concentration system, the gas phase and part of the liquid phase are mixed in the liquid seal tank of the concentration system and then discharged by a waste water pump, the non-condensable gas in the evaporation condenser enters a vacuum unit of the concentration system, and part of the liquid phase of the first-effect evaporation separator enters a second-effect evaporation separator;
(6) the temperature in the two-effect evaporation separator is adjusted to 125 ℃, the gas phase of the two-effect evaporation separator enters the one-effect evaporation separator, and the liquid phase is sent to the mixing heater through the calcium chloride circulating pump.
The hydrogen chloride obtained by analysis in the step (3) of the method has the advantages of high purity (purity is more than 99.9%) and small purity fluctuation, and is beneficial to automatic control of hydrochlorination.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. The device for resolving and separating hydrogen chloride and water from hydrochloric acid comprises a hydrochloric acid resolving system, a neutralizing system and a concentrating system, and is characterized in that: the hydrochloric acid analysis system comprises a hydrochloric acid preheater, a mixing heater, a separator, a primary cooler, a secondary cooler, a gas-liquid separator, a falling film evaporation separator, a flash evaporation condenser, an analysis system vacuum unit and an analysis system liquid seal tank; the neutralization system comprises a calcium hydroxide storage tank, a spiral metering scale, a mixing pump, a buffer tank, a discharge pump and a filter; the concentration system comprises a first-effect evaporation separator, a second-effect evaporation separator, a calcium chloride circulating pump, an evaporation condenser, a concentration system vacuum unit, a concentration system liquid seal tank and a waste water pump;
the bottom of the hydrochloric acid preheater is added with a hydrochloric acid solution, the middle part of the hydrochloric acid preheater is added with a steam condensate, a top outlet of the hydrochloric acid preheater is connected with a top inlet of the mixing heater, the middle part of the mixing heater is introduced with steam, a bottom outlet of the mixing heater is connected with an inlet of a separator, a top outlet of the separator is connected with a primary cooler, the primary cooler is connected with a secondary cooler, the secondary cooler is connected with a gas-liquid separator, a gas phase of the gas-liquid separator outputs hydrogen chloride gas, a liquid phase of the gas-liquid separator outputs concentrated hydrochloric acid, a bottom outlet of the separator is connected with an inlet of a falling film evaporation separator, the middle part of the falling film evaporation separator is introduced with steam, a gas phase outlet of the flash evaporator is connected with an analytic system;
calcium hydroxide is introduced into an inlet of the calcium hydroxide storage tank, an outlet of the calcium hydroxide storage tank is connected with a spiral metering scale, the spiral metering scale is connected with a mixing pump, the mixing pump is connected with a buffer tank, the buffer tank is connected with a discharging pump, the discharging pump is connected with a filter, the filter is connected with an inlet of a one-effect evaporation separator, and calcium chloride is filtered out;
the utility model discloses a dual-effect evaporation separator, including a dual-effect evaporation separator, a liquid phase outlet of dual-effect evaporation separator is connected with evaporative condenser, evaporative condenser connects concentrated system vacuum unit and concentrated system liquid seal tank, the waste water pump is connected to concentrated system liquid seal tank, the part connects dual-effect evaporation separator, let in steam in the middle part of dual-effect evaporation separator, a dual-effect evaporation separator gas phase outlet of dual-effect evaporation separator.
2. The apparatus according to claim 1, wherein the apparatus comprises: the bottom of the secondary cooler outputs concentrated hydrochloric acid.
3. The apparatus according to claim 1, wherein the apparatus comprises: and a hydrochloric acid pump and a flow meter are arranged at a hydrochloric acid solution inlet of the hydrochloric acid preheater.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110510579A (en) * | 2019-07-15 | 2019-11-29 | 杭州众立化工科技有限公司 | A kind of device and technique parsing separating hydrogen chloride and water from hydrochloric acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110510579A (en) * | 2019-07-15 | 2019-11-29 | 杭州众立化工科技有限公司 | A kind of device and technique parsing separating hydrogen chloride and water from hydrochloric acid |
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