A kind of process for purification of acetylene gas
Technical field
The present invention relates to acetylene technical field of purification, and in particular to a kind of process for purification of acetylene gas.
Background technology
Acetylene is simplest alkynes, and inflammable gas has fierce under liquid and solid-state or under gaseous state and certain pressure
The danger of blast, the factor such as heated, vibrations, electric spark can trigger blast, be insoluble in water, be soluble in acetone, it is current mainly
For welding metal or prepare polyacetylene conductive material or prepare the plastics such as polyvinyl chloride.Acetylene typically leads in the prior art
Cross carbide to prepare, but be due to be mingled with the impurity such as sulphur, arsenic, phosphorus and exothermic heat of reaction in raw material calcium carbide to cause acetylene gas
With foreign gases such as a small amount of hydrogen sulfide, hydrogen phosphide, arsenic hydride, ammonia and vapor in body, the low acetylene gas of purity can shadow
Ring its application and occur the danger such as burning, blast.In the prior art it is general using alkali metal hydroxide, acid, copper sulphate or
Combinations thereof, but impurity-eliminating effect is poor, product purity is low, and copper sulphate is easily generated with foreign gas reaction in use
The many kinds of solids impurity such as copper, copper sulfide, is unfavorable for recycling;Other existing absorption kettle is simple in construction, and gas flow can not
Regulation, the bad control of infiltration rate also causes gas absorption effect poor.
Therefore, these technical problems how to be solved, it has also become those skilled in the art's technical barrier urgently to be resolved hurrily.
The content of the invention
The present invention, there is provided a kind of process for purification of acetylene gas, is solved for the deficiencies in the prior art
The technical problem stated.
To achieve these goals, the present invention provides following technical scheme:A kind of process for purification of acetylene gas, including such as
Lower specific steps:
(1), first iron chloride solid added into mass fraction in 2-5% hydrochloric acid solution, then be diluted with water and obtain certain density
Ferric chloride in aqueous solution, ferric chloride in aqueous solution is added and is internally provided with the reactor of transverse baffle and agitator, then will be anti-
It is -0.1 to -0.6MPa to answer kettle to be evacuated to vacuum;
(2), the acetylene gas crude product containing hydrogen sulfide, hydrogen phosphide, arsenic hydride, ammonia and vapor foreign gas passed through into end
It is provided with air distributor and centre position is provided with the admission line of a ultrasonic gas flowmeter, is passed through fresh configuration
Ferric chloride in aqueous solution in, at a certain temperature reaction a period of time;
(3), by step(2)The gas of middle process preliminary purification has the outlet of No. two ultrasonic gas flowmeters by middle setting
Pipeline is passed through in the concentrated sulfuric acid, finally collects the acetylene gas for drying purifying.
Above-mentioned steps(1)Middle ferric chloride in aqueous solution can effectively absorb hydrogen sulfide, hydrogen phosphide and arsenic hydride foreign gas, solution
Color graduates into light green by brown color, shows that ferric ion is converted into ferrous ion, color transition is substantially, easily first
Step judges impurity content and infiltration rate, and the solid impurity that this method is produced is few, only has simple substance Sulfur releasing substantially, and existing
Copper-bath absorption process is used in technology, color conversion is not obvious, can separate out many kinds of solids impurity such as elemental copper and copper sulfide,
Be inconvenient to recycle;The hydrochloric acid produced in itself is present in solution hydrochloric acid and course of reaction can further absorb ammonia
Deng alkaline gas;In addition when configuring fresh ferric chloride in aqueous solution, in order to prevent that iron chloride hydrolysis from producing precipitation, a small amount of matter is added
Measure the clear that fraction ensures solution for 2-5% dilute hydrochloric acid liquid;As a further improvement on the present invention, the step(1)In
The mass fraction of ferric chloride in aqueous solution is 0.5-1.5%, and concentration is too low, and foreign gas fails to be fully absorbed, and excessive concentration,
Cause to waste.
Above-mentioned steps(1)Middle holding reactor vacuum is -0.1 to -0.6MPa, it is to avoid foreign gas arsenic hydride and oxygen
Generation hypergolic reaction, triggers acetylene explosion phenomenon.
Above-mentioned steps(1)Middle reactor is internally provided with transverse baffle and agitator, and step(2)Middle admission line end
Hold set air distributor, gas is dispersed in micro-bubble form in continuous phase, be for increase gas with
The contact area of liquid and time of contact, good impurity removing effect, product purity are high.
Above-mentioned steps(2)A ultrasonic gas flowmeter and step for middle setting(3)No. two supersonic gas of middle setting
Flowmeter body to charge flow rate and can go out throughput and be monitored respectively, make bubble motion speed suitable, and be directly installed on
On gas pipeline, without injecting pipeline, therefore install convenient, no pressure loss, no leakage pressure risk is particularly suitable for use in vacuum
There is the reactor of particular/special requirement.
As a further improvement on the present invention, the step(2)In reaction temperature be 35-55 DEG C, the reaction time is
0.5-1h, reaction temperature is too high or the reaction time is too short, and foreign gas easily expands spilling liquid level, causes absorptivity low, and
Reaction temperature is too low, and reaction rate is excessively slow, also results in foreign gas and absorbs incomplete;Reaction time is long, inside reactor
Pressure is become larger, it is necessary to increase the anti-pressure ability of pressure relief valve or intensified response kettle to ensure the security of equipment, increase
Cost.
As a further improvement on the present invention, the step(3)The mass fraction of the middle concentrated sulfuric acid is 98%, can be many for a long time
Batch absorbs vapor, and drying effect is obvious.
As a further improvement on the present invention, the transverse baffle inner homogeneous sets cellular gas channel, increases gas
The flow resistance of body, reduces flowing velocity, further contact surface area and time of contact of the increase gas with iron chloride reaction solution.
As a further improvement on the present invention, the admission line runs through transverse baffle from top to bottom, and air distributor is set
Put on the downside of transverse baffle, bubble is run through transverse baffle from bottom to top from reactor bottom, extend the travel of gas, enter
One step increases contact surface area and time of contact of the gas with iron chloride reaction solution.
As a further improvement on the present invention, the step further comprises after the completion of reaction toward adding two in reaction solution
Nitric sulfid, stirs 0.1-0.5h, and processing is separately recovered after refiltering a small amount of metal impurities filter residue of removing, filtrate stratification;On
It is the elemental sulfur generated when abundant dissolved hydrogen sulfide foreign gas is reacted with ferric chloride in aqueous solution to state middle carbon disulfide effect, is easy to
Recycle.
Compared with prior art, the present invention has advantages below:(1), by the way that acetylene raw gas is passed through into chlorination ferrous acid
Property the aqueous solution in, one kettle way removes acid and alkaline gas impurity simultaneously, is easily tentatively judged by reaction solution color change miscellaneous
Matter content and infiltration rate, impurity removal percentage are high, good product purity, up to 98.0% and more than;Analysed during other chemisorbed
Go out single solid, be easy to recycling;(2), by setting transverse baffle, air distributor and in air-flow inside reactor
Ultrasonic gas flowmeter is set on pipeline, gas is dispersed in micro-bubble form in continuous phase, further increase
Contact area and the time of contact of gas and liquid, good impurity removing effect, product purity are high, and gas flow size is convenient controls
System, flowmeter install convenient, no pressure loss, no leakage pressure risk is particularly suitable for use in the reactor for having particular/special requirement to vacuum.
Embodiment
With reference to specific embodiment, the present invention is expanded on further, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention;In addition, it is to be understood that after present disclosure has been read, those skilled in the art can
To be made various changes or modifications to the present invention, these equivalent form of values also fall within appended claims limited range.
Embodiment 1
A kind of process for purification of acetylene gas, is comprised the following specific steps that:
(1), first 0.915Kg iron chloride solid added into 50Kg mass fractions in 2% hydrochloric acid solution, then add 42.5Kg water dilute
The ferric chloride in aqueous solution for obtaining that mass fraction is 1% is released, ferric chloride in aqueous solution is added and is internally provided with transverse baffle and agitator
Reactor in, it is 1000r/min to control mixing speed, and reactor then is evacuated into vacuum for -0.1MPa;The horizontal stroke
Cellular gas channel is uniformly arranged to baffle interior;
(2), will contain hydrogen sulfide, hydrogen phosphide, arsenic hydride, ammonia and vapor foreign gas, initial purity acetylene be 85% gas
Body crude product, is provided with air distributor by end and centre position is provided with the air inlet pipe of a ultrasonic gas flowmeter
In road, the ferric chloride in aqueous solution for being passed through fresh configuration, 1h is reacted at 45 DEG C;The admission line runs through transverse gear from top to bottom
Plate, air distributor is arranged on the downside of transverse baffle;
(3), by step(2)The gas of middle process preliminary purification has the outlet of No. two ultrasonic gas flowmeters by middle setting
Pipeline is passed through in the concentrated sulfuric acid that mass fraction is 98%, finally collects the acetylene gas for drying purifying, and RIKEN is ground using Japan's reason
KEIKI, model SD-1 fixed acetylene detector detection purity acetylene are 98.2%;
(4), after the completion of reaction toward 10g carbon disulfide is added in reaction solution, stir 0.1h, abundant dissolved hydrogen sulfide foreign gas
The elemental sulfur generated when being reacted with ferric chloride in aqueous solution, divides after refiltering a small amount of metal impurities filter residue of removing, filtrate stratification
Do not recycle.
Embodiment 2
A kind of process for purification of acetylene gas, is comprised the following specific steps that:
(1), first 0.915Kg iron chloride solid added into 50Kg mass fractions in 5% hydrochloric acid solution, then add 13.5Kg water dilute
The ferric chloride in aqueous solution for obtaining that mass fraction is 1.5% is released, ferric chloride in aqueous solution is added and is internally provided with transverse baffle and stirring
In the reactor of device, it is 1000r/min to control mixing speed, and reactor then is evacuated into vacuum for -0.6MPa;It is described
Transverse baffle inner homogeneous sets cellular gas channel;
(2), will contain hydrogen sulfide, hydrogen phosphide, arsenic hydride, ammonia and vapor foreign gas, initial purity acetylene be 85% gas
Body crude product, is provided with air distributor by end and centre position is provided with the air inlet pipe of a ultrasonic gas flowmeter
In road, the ferric chloride in aqueous solution for being passed through fresh configuration, 0.5h is reacted at 55 DEG C;The admission line is from top to bottom through laterally
Baffle plate, air distributor is arranged on the downside of transverse baffle;
(3), by step(2)The gas of middle process preliminary purification has the outlet of No. two ultrasonic gas flowmeters by middle setting
Pipeline is passed through in the concentrated sulfuric acid that mass fraction is 98%, finally collects the acetylene gas for drying purifying, and RIKEN is ground using Japan's reason
KEIKI, model SD-1 fixed acetylene detector detection purity acetylene are 98.5%;
(4), after the completion of reaction toward 15g carbon disulfide is added in reaction solution, stir 0.5h, abundant dissolved hydrogen sulfide foreign gas
The elemental sulfur generated when being reacted with ferric chloride in aqueous solution, divides after refiltering a small amount of metal impurities filter residue of removing, filtrate stratification
Do not recycle.
Embodiment 3
A kind of process for purification of acetylene gas, is comprised the following specific steps that:
(1), first 0.915Kg iron chloride solid added into 50Kg mass fractions in 3% hydrochloric acid solution, then add 134.5Kg water dilute
The ferric chloride in aqueous solution for obtaining that mass fraction is 0.5% is released, ferric chloride in aqueous solution is added and is internally provided with transverse baffle and stirring
In the reactor of device, it is 1000r/min to control mixing speed, and reactor then is evacuated into vacuum for -0.3MPa;It is described
Transverse baffle inner homogeneous sets cellular gas channel;
(2), will contain hydrogen sulfide, hydrogen phosphide, arsenic hydride, ammonia and vapor foreign gas, initial purity acetylene be 85% gas
Body crude product, is provided with air distributor by end and centre position is provided with the air inlet pipe of a ultrasonic gas flowmeter
In road, the ferric chloride in aqueous solution for being passed through fresh configuration, 0.8h is reacted at 35 DEG C;The admission line is from top to bottom through laterally
Baffle plate, air distributor is arranged on the downside of transverse baffle;
(3), by step(2)The gas of middle process preliminary purification has the outlet of No. two ultrasonic gas flowmeters by middle setting
Pipeline is passed through in the concentrated sulfuric acid that mass fraction is 98%, finally collects the acetylene gas for drying purifying, and RIKEN is ground using Japan's reason
KEIKI, model SD-1 fixed acetylene detector detection purity acetylene are 98.0%;
(4), after the completion of reaction toward 12g carbon disulfide is added in reaction solution, stir 0.3h, abundant dissolved hydrogen sulfide foreign gas
The elemental sulfur generated when being reacted with ferric chloride in aqueous solution, divides after refiltering a small amount of metal impurities filter residue of removing, filtrate stratification
Do not recycle.