CN113788457A - Method for separating hydrogen chloride in R134a by using supergravity dry method - Google Patents
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- CN113788457A CN113788457A CN202111239517.2A CN202111239517A CN113788457A CN 113788457 A CN113788457 A CN 113788457A CN 202111239517 A CN202111239517 A CN 202111239517A CN 113788457 A CN113788457 A CN 113788457A
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- 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
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a method for separating hydrogen chloride in R134a by a supergravity dry method, which comprises the following steps: (1) r134a product feed: the R134a product is first separated and pumped into reboiler to the designated liquid level, and then heated and fed into the reboiler at a constant bubble point to maintain the liquid level substantially constant. (2) And (3) supergravity dry separation: adjusting the rotating speed of the supergravity rectifying device until the pressure of the rectifying device reaches the specified pressure, and stabilizing reflux; meanwhile, the condenser is started, and the temperature of the condensed reflux liquid is controlled. (3) Regulating and controlling extraction: after total reflux for a certain time, gradually reducing reflux ratio, sampling and detecting the tower top and the tower bottom, adjusting proper reflux ratio, and continuously extracting. The invention creatively applies the hypergravity rectification technology to the separation of the hydrogen chloride in the R134a product for the first time, can well avoid the generation of fluorine-containing hydrochloric acid, and improves the use value of the byproduct hydrogen chloride. Meanwhile, the equipment is convenient to install, is easier to overhaul and maintain, reduces equipment investment, saves energy, reduces consumption and reduces operation cost.
Description
Technical Field
The invention relates to the field of chemical separation and purification, in particular to a method for separating hydrogen chloride in R134a by a supergravity dry method.
Background
Tetrafluoroethane (R134a) is one of the best performance-price ratio of the substitute of chlorofluorocarbon (ODS) so far, and the synthesis method is mainly characterized in that under the action of a catalyst, trichloroethylene or tetrachloroethane and hydrogen fluoride are subjected to addition and fluorine-chlorine substitution reaction to generate the tetrafluoroethane. Therefore, during the production process, a large amount of hydrogen chloride by-product is produced. In the reaction process, in order to enable the raw material trichloroethylene or tetrachloroethane to completely react, the molar ratio of the hydrogen fluoride to the raw material halogenated hydrocarbon is usually 3-6, or even higher, so that a large amount of hydrogen fluoride gas exists in the R134a product in addition to a large amount of hydrogen chloride gas. In production, although most of the hydrogen fluoride can be removed by condensation, a small portion of the hydrogen fluoride will still be present in the product R134 a.
The separation method of the hydrogen chloride and the R134a mainly comprises a dry separation method and a wet separation method. The wet separation has low pressure, high safety and low equipment requirement; however, because a small part of hydrogen fluoride exists in R134a, additional separation equipment is needed, and after the pressure is released, the product needs to be pressurized and rectified again, so that the energy consumption is high, the application range of the byproduct hydrochloric acid generated by wet separation is relatively small, and the additional value is low. The dry separation method has high pressure and high equipment requirement, the hydrogen fluoride and the product can be separated at one time, no additional separation equipment is needed, pressure release is not needed for separation, the energy consumption is low, the application range of the byproduct hydrogen chloride is wide, and the additional value is relatively high.
The dry separation of the hydrogen chloride is usually carried out by adopting a common pressurization rectification mode, the height of a rectification tower is about 30m generally, and the process of gas-liquid distribution, exchange, mass transfer and balance is realized by the gravity of liquid, so that the separation of the hydrogen chloride and a main product is realized. The method has the phenomena of uneven gas-liquid distribution, easy channeling, wall flow and the like; although this phenomenon can be improved by means of a liquid distributor and a gas distribution device, the problem is not well solved, so that the reflux ratio is increased and the energy consumption of the heat exchange is increased. And because the gas-liquid exchange is carried out in the same pipe, the gas-liquid exchange is easy to be insufficient, so that the pressure difference of the top tower is increased, the problem of flooding is caused, and the separation effect is poor. In addition, the mass transfer mainly depends on a gravity field, and the defects of small mass transfer force, relatively poor mass transfer effect, long balance time and the like exist.
The hypergravity method is proposed by ICI company of UK in 1970, and uses a centrifugal force field to replace a gravity field, and the centrifugal force can reach hundreds to thousands times of the gravity, so the hypergravity method is called as a novel efficient mass transfer separation technology. At present, the method has primary application in the industries of petrifaction, medicine, light industry, environmental protection and the like, and is mainly used for the aspects of solvent recovery, waste gas treatment, rectification separation and the like. The hypergravity rectification technology adopts centrifugal force to replace gravity, so that the contact area between gas and liquid phases and the mass transfer rate can be greatly improved, the pressure drop is small, and the flooding is not easy to happen; the theoretical plate number per unit height can reach 5-10 times of that of a common rectification theoretical plate number, the equipment volume and height are only 1/10-1/5 of the height of a common tower, the investment cost of equipment can be greatly saved, and later maintenance and cleaning are facilitated; meanwhile, due to the large degree of micromixing, high mass transfer efficiency, short gas-liquid equilibrium time and good separation effect, the energy consumption of rectification can be reduced, and the operation cost can be reduced.
Disclosure of Invention
In order to solve the technical problems, the invention creatively applies the hypergravity rectification technology to the separation of the hydrogen chloride in the R134a product for the first time, can well avoid the generation of fluorine-containing hydrochloric acid and improve the use value of the byproduct hydrogen chloride; meanwhile, the equipment is convenient to install, is easier to overhaul and maintain, reduces equipment investment, saves energy, reduces consumption and reduces operation cost.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for separating hydrogen chloride in R134a by a supergravity dry method comprises the following steps:
(1) pumping the R134a product into a reboiler to a designated liquid level, heating to gasify the material and enter a super-gravity separator, and continuously feeding the material into the reboiler at a certain speed to keep the liquid level in the reboiler stable;
(2) adjusting the hypergravity rectifying device, gradually increasing the rotating speed, starting full reflux, keeping the rotating speed stable, gradually heating the reboiler until the pressure of the rectifying device reaches the specified pressure, starting a condenser for condensation, and controlling the condensation reflux temperature;
(3) and (3) starting a reflux pump, gradually reducing the reflux ratio after total reflux is carried out for a certain time, simultaneously sampling at the tower top and the tower kettle, exploring the minimum reflux ratio Rmin, adjusting the reflux ratio and continuously feeding, separating and extracting HCl liquid at the tower top, and continuously extracting an R134a crude product at the tower kettle.
Further, the R134a product is a reaction product including hydrogen fluoride, R133a, hydrogen chloride, R134a, and minor amounts of other impurities.
Preferably, the liquid level in the reboiler is 1/3-2/3, and the temperature of the reboiler is 30-120 ℃;
further, the R134a product in the reboiler is a product obtained by rectifying and separating a gas-phase fluorinated product, the feeding speed is 800-2000 kg/h, and the bubble point is used for feeding;
preferably, the hypergravity rectifying device is a double baffle type hypergravity rectifying device;
furthermore, fin fans are distributed on the baffle plate, the distribution angle of the double-layer fin fans is 30 degrees, and the upper fin fan and the lower fin fan are disturbed in opposite directions;
furthermore, the outer layer of the baffle plate is provided with a gas defoaming distributor which is in a snowflake or other elliptic toothed structure and is in polygonal distribution;
preferably, the supergravity dry separation is a supergravity rectification method, the reflux ratio is statically monitored and adjusted, and the optimal reflux ratio R is determined by adjusting the minimum reflux ratio Rmin, wherein R is 1.1-1.5 Rmin;
preferably, the supergravity rectification method is pressure rectification, the rectification pressure is 0.8-2.0 MPa, and the reflux temperature is-35 to-15 ℃;
furthermore, the temperature in the hypergravity rectification device is controlled to be 20-40 ℃ by adjusting the temperature and reflux quantity of a reboiler in the hypergravity rectification method.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method creatively applies the hypergravity rectification technology to the separation of the hydrogen chloride in the R134a product for the first time, can well avoid the generation of fluorine-containing hydrochloric acid, and improves the use value of the byproduct hydrogen chloride;
(2) according to the invention, the gas is redistributed, so that the influence of gas entrainment on the separation effect can be reduced; meanwhile, the fin fan is added at the baffle plate, so that the gas-liquid contact disturbance is greatly enhanced, and the mass transfer effect is enhanced
(3) The invention has small equipment volume, convenient installation and easier maintenance; the problems of flooding, channeling, wall flow and the like in the traditional rectification can be solved, the mass transfer effect is the magnitude order of the traditional rectification, the separation effect is better, and the energy consumption is lower.
Drawings
FIG. 1 is a schematic diagram of a device for separating hydrogen chloride by a supergravity dry method in the form of R134 a;
reference numerals: 1. reboiler, 2, intake pipe, 3, air inlet, 4, flange, 5, gas distribution hole, 6, quiet book, 7, wing fan, 8, backward flow liquid distributor, 9, backward flow feed liquor pipe, 10, gland, 11, gas outlet, 12, outlet duct, 13, move book, 14, pivot, 15, liquid outlet, 16, drain pipe, 17, condenser, 18, receiving tank, 19, stand-by pump, 20, reflux pump.
Detailed Description
In order to enhance the understanding of the present invention, the present invention will be further described with reference to the following specific examples.
Examples
A method for separating hydrogen chloride in R134a by a supergravity dry method,
the method comprises the following steps:
(1) pumping the R134a product into a reboiler to a designated liquid level, heating to gasify the material and enter a super-gravity separator, and continuously feeding the material into the reboiler at a certain speed to keep the liquid level in the reboiler stable;
(2) adjusting the hypergravity rectifying device, gradually increasing the rotating speed, starting full reflux, keeping the rotating speed stable, gradually heating the reboiler until the pressure of the rectifying device reaches the specified pressure, starting a condenser for condensation, and controlling the condensation reflux temperature;
(3) and (3) starting a reflux pump, gradually reducing the reflux ratio after total reflux is carried out for a certain time, simultaneously sampling at the tower top and the tower kettle, exploring the minimum reflux ratio Rmin, adjusting the reflux ratio and continuously feeding, separating and extracting HCl liquid at the tower top, and continuously extracting an R134a crude product at the tower kettle.
The device for separating hydrogen chloride by using the R134a supergravity dry method is shown in figure 1, and sequentially comprises a reboiler 1, an air inlet pipe 2, an air inlet 3, a flange 4, a gas distribution hole 5, a static folding disc 6, a wing fan 7, a reflux liquid distributor 8, a reflux liquid inlet pipe 9, a gland 10, an air outlet 11, an air outlet pipe 12, a dynamic folding disc 13, a rotating shaft 14, a liquid outlet 15, a liquid outlet pipe 16, a condenser 17, a receiving tank 18, a standby pump 19 and a reflux pump 20.
In the embodiment, the gas phase fluorination reaction product is primarily cooled to 0-15 ℃, and then the hydrogen fluoride and the intermediate product R133a are separated by pressure rectification under the pressure of 1.0-2.2 MPa. Pumping the separated R134a product into a reboiler, wherein the R134a product mainly comprises the following components: hydrogen chloride, R134a, small amounts of R133a, hydrogen fluoride and other impurities; the R134a product is fed as a bubble point material, when the liquid level in a reboiler reaches 1/2, the material is heated to be gasified, and the temperature in the reboiler is 40-100 ℃; meanwhile, feeding continuously, wherein the feeding flow is 1000-2000 kg/h;
starting a hypergravity rectifying device after the material begins to be heated, wherein the diameter height of the hypergravity rectifying device is 1100 x 2300mm, the diameter height of a rotor is 850mm, the power is 11Kw, and the maximum rotating speed is 1000 r/min; gradually increasing the rotating speed, wherein the initial rotating speed is set to be 0-200 r/min; meanwhile, a condensing device is started, R22 is used as a coolant, and the condensing temperature is-35 to-15 ℃. And starting a reflux pump until the liquid level of the receiving tank is about 1/3, fully refluxing until the pressure is stably increased to 0.9-2.0 MPa, and setting the rotating speed of the supergravity rectifying device to 600-800 r/mim after the pressure is stable to stabilize the reflux. After the total reflux is carried out for 0.5h, the reflux ratio R is adjusted to 10, the material is stably discharged, the extraction speed of the receiving tank and the extraction speed of the reboiler are consistent with the feeding speed, and the liquid level of the receiving tank and the liquid level of the reboiler are controlled to be basically kept unchanged. Taking an HCl discharging sample, detecting the discharging sample by referring to GB/T24469-. Adjusting the reflux ratio R to be 2, and continuously discharging at 800-1500 kg/h, wherein the specific indexes are shown in table one. Taking a crude product R134a discharged material sample at the bottom of the reboiler, and detecting according to GB/T18826-2016 standard, wherein the sample is Cl-％≤0.3％(w) continuously extracting at 500-1000 kg/h, wherein the specific indexes are shown in the second table.
Table one example content of HCl sample separated by supergravity rectification
TABLE II example reboiler bottom effluent sample content
Comparative example
The comparative example differs from the examples in that the comparative example is a distillation in a conventional distillation column with a diameter and height of 1000 x
30000mm, feeding at 10000mm position in the tower, with reflux ratio R of 3.5, respectively taking the top of the tower and the bottom of the tower to discharge, and detecting, the results are shown in Table three and Table four.
Content of HCl sample separated by using epi-III hypergravity rectification
Table four reboiler tower still discharge sample content
Through comparison between the embodiment and the comparative example, it can be known that under the same conditions, the height of the hypergravity dry separation HCl tower is less than 1/10 of the height of the common rectifying tower, and if the height of the base is calculated, the height is only about 1/10 of the height of the common rectifying tower, so that the construction and installation cost is greatly saved, and the subsequent maintenance and repair operation is more convenient. The reflux ratio is relatively small, which can save about 40% of energy compared with the common rectification; as the motor load is increased compared with the ordinary rectification, the total energy consumption of the hypergravity rectification can be reduced by about 20-30% compared with the ordinary rectification.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the invention has been described in detail with reference to the foregoing illustrative embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for separating hydrogen chloride in R134a by a supergravity dry method is characterized by comprising the following steps:
(1) pumping the R134a product into a reboiler to a designated liquid level, heating to gasify the material and enter a super-gravity separator, and continuously feeding the material into the reboiler at a certain speed to keep the liquid level in the reboiler stable;
(2) adjusting the hypergravity rectifying device, gradually increasing the rotating speed, starting full reflux, keeping the rotating speed stable, gradually heating the reboiler until the pressure of the rectifying device reaches the specified pressure, starting a condenser for condensation, and controlling the condensation reflux temperature;
(3) and (3) starting a reflux pump, gradually reducing the reflux ratio after total reflux is carried out for a certain time, simultaneously sampling at the tower top and the tower kettle, exploring the minimum reflux ratio Rmin, adjusting the reflux ratio and continuously feeding, separating and extracting HCl liquid at the tower top, and continuously extracting an R134a crude product at the tower kettle.
2. The method for the dry separation of hydrogen chloride in R134a by the supergravity method as claimed in claim 1, wherein the R134a product is a reaction product comprising hydrogen fluoride, R133a, hydrogen chloride, R134a and small amounts of other impurities.
3. The method for the dry separation of hydrogen chloride in R134a by the hypergravity as claimed in claim 1, wherein the liquid level in the reboiler is 1/3-2/3, and the temperature in the reboiler is 30-120 ℃.
4. The method for separating hydrogen chloride in R134a by the high-gravity dry method according to claim 3, wherein the R134a product in the reboiler is a product obtained by rectifying and separating a gas-phase fluorinated product, and the feeding speed is 800-2000 kg/h and the bubble point is the bubble point.
5. The method for separating hydrogen chloride in R134a by the dry method through the hypergravity as claimed in claim 1, wherein the dry method through the hypergravity is a hypergravity rectification method, the reflux ratio is statically monitored and adjusted, and the optimal proportion R of reflux is determined by adjusting the minimum reflux ratio Rmin, wherein R is 1.1-1.5 Rmin.
6. The method for separating the hydrogen chloride in the R134a by the supergravity dry method according to claim 5, wherein the supergravity rectification method is pressure rectification, the rectification pressure is 0.8-2.0 MPa, and the reflux temperature is-35 to-15 ℃.
7. The method for separating hydrogen chloride in R134a by the supergravity dry method according to claim 5, wherein the temperature in the supergravity rectifying device is controlled to be 20-40 ℃ by adjusting the temperature of a reboiler and the reflux amount in the supergravity rectifying method.
8. The method for separating the hydrogen chloride in the R134a by the supergravity dry method according to claim 1, wherein the supergravity dry separation device is a double baffle type supergravity rectification device.
9. The method for separating the hydrogen chloride in the R134a by the dry method through the hypergravity as claimed in claim 8, wherein the baffle plates are distributed with fins, the distribution angle of the double-layer fins is 30 degrees, and the upper and lower layer fins are disturbed in the opposite direction.
10. The method for the dry separation of hydrogen chloride in R134a by the hypergravity method as claimed in claim 8, wherein the outer layer of the baffle is designed with a gas demister distributor which is in the shape of snowflake or other elliptic toothed structures and takes a polygonal distribution.
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