CN209475934U

CN209475934U - A kind of apparatus system of carbide acetylene purification

Info

Publication number: CN209475934U
Application number: CN201920085289.XU
Authority: CN
Inventors: 刘丽; 张礼树; 刘昕; 何秀容; 张剑锋
Original assignee: Sichuan Tianyi Science and Technology Co Ltd
Current assignee: Southwest Research and Desigin Institute of Chemical Industry; Haohua Chemical Science and Technology Corp Ltd
Priority date: 2019-01-18
Filing date: 2019-01-18
Publication date: 2019-10-11
Anticipated expiration: 2029-01-18

Abstract

The utility model belongs to the purification treatment technology field of calcium carbide acetylene, more particularly to a kind of apparatus system of carbide acetylene purification, it is characterized by: being equipped with desulfurizer, absorber, cooler, unstripped gas input pipe, product gas efferent duct and vacuum pump, unstripped gas input pipe is connect with the absorber of desulfurizer and alternating temperature pressure-swing absorption apparatus, vacuum pump both ends are connect with cooler, cooler one end is connect with sequencing valve, and one end is connect with regeneration off gases pipeline；Vacuum pump and cooler are located at below absorber；Product gas efferent duct is connect with absorber top；It is connected between all devices by pipeline；Wherein the working condition of alternating temperature potential device absorber and gas trend are controlled by sequencing valve.To H in the thick acetylene gas of calcium carbide in the utility model₂S impurity can be removed to 0.005% or less, PH₃Equal impurity can be removed to 0.003% such as the following, be stripped of aldehyde alcohol ketone impurity；And process flow is simple, high degree of automation, operating cost is low.

Description

A kind of apparatus system of carbide acetylene purification

Technical field

The utility model belong to calcium carbide acetylene purification treatment technology field more particularly to a kind of carbide acetylene purification Apparatus system.

Background technique

The main source of acetylene is natural gas pyrolysis acetylene and calcium carbide legal system acetylene, since natural gas resource is deficient, by Its preparing ethyne by cracking it is at high cost, therefore the technique of calcium carbide legal system acetylene become acetylene production mainstream, but calcium carbide produce second Alkynes, whether side reaction is more in process of production for dry method or wet process, produces more foreign gas, such as H₂S、PH₃, aldehyde, The impurity such as alcohol, ketone and higher alkyne.H₂S、PH₃It is easy to react with the synthetic catalyst of vinyl acetate, catalyst activity is caused to subtract Less or completely lose poisoning；The polymerization reaction meeting blocking catalyst hole of higher alkyne, makes catalyst activity reduction while influencing Vinyl acetate quality；Water will increase the side reaction of synthesis, generates the substances such as acetaldehyde, influences product quality.It is therefore desirable to electricity The thick acetylene of stone carries out purified treatment, removes these objectionable impurities, aldehyde, alcohol, ketone are slightly smaller to synthetic reaction harm, but can reduce acetylene Purity.

The main method of purification acetylene is sodium hypochlorite oxidization, concentrated sulfuric acid absorption process and alternating temperature pressure swing adsorption method at present. Sodium-hypochlorite process is that the oxidations of impurities such as hydrogen sulfide, hydrogen phosphide in thick acetylene are become acidic materials, and further processing removes, But the reducing impurities such as hydrogen sulfide, hydrogen phosphide are only eliminated with the sodium hypochlorite method of purification, higher alkyne class impurity cannot be removed； And the sodium hypochlorite method of purification is easy to happen explosion, brings security risk.Concentrated sulfuric acid absorption process is to utilize the concentrated sulfuric acid and higher alkyne At 20 DEG C~30 DEG C of temperature, pressure carries out absorbing reaction under conditions of being slightly above atmospheric pressure.During absorbing reaction, ethylene Ethyl-acetylene, H₂S and PH₃It is removed, acetylene has a small amount of loss.The shortcomings that concentrated sulfuric acid absorption process is that the concentrated sulfuric acid has corrosivity, right Its pipeline passed through and pump are corroded, and pipe leakage is caused；It needs to consume a large amount of concentrated sulfuric acid in absorption process, so that operation Higher cost, while the discharge of Waste Sulfuric Acid causes serious environmental pollution.Pressure and temperature varying adsorption cleaning method is physisorphtion, fortune At low cost, the non-environmental-pollution of row, Patent No. ZL01128864.7 remove C3+ or more hydrocarbon impurities and are returned from acetylene gaseous mixture The method for receiving acetylene essentially describes the removing of the purification to the middle-and-high-ranking alkynes hydrocarbon impurities of acetylene, is not directed to H₂O、H₂S and PH₃It is de- It removes.There are respective shortcomings for three kinds of methods of existing purification acetylene now.

Utility model content

In order to solve the above technical problems, the utility model provides a kind of apparatus system of carbide acetylene purification, removing electricity Impurity in stone acetylene, to H in the thick acetylene gas of calcium carbide₂S impurity can be removed to 0.005% or less, PH₃Equal impurity can be removed to 0.003% or less, the alkyne impurities such as vinylacetylene are removed to 0.003% hereinafter, H respectively₂O is removed to 0.05% hereinafter, same When be stripped of aldehyde alcohol ketone impurity；And process flow is simple, high degree of automation, operating cost is low.

Solve the apparatus system of one of the utility model of above technical problem carbide acetylene purification, including sequencing valve And pipeline, it is characterised in that: it is equipped with adsorbing mechanism, cooler, unstripped gas input pipe, product gas efferent duct and vacuum pump, they Alternating temperature pressure-swing absorption apparatus is constituted, unstripped gas input pipe is connect by sequencing valve with absorber, and vacuum pump both ends and cooler connect It connects, cooler one end is connect with sequencing valve, and one end is connect with regeneration off gases pipeline；Vacuum pump and cooler are located under absorber Side；Product gas efferent duct is connect with absorber top；It is connected between all devices by pipeline；Wherein alternating temperature pressure-swing absorption apparatus Working condition and the gas trend of absorber are controlled by sequencing valve.

The adsorbing mechanism forms one by 3 or 3 or more absorbers and continuously runs system, adsorbers parallel connection； It is additionally provided with regeneration steam input pipe and cold blowing gas input pipe, regeneration steam input pipe and cold blowing gas input pipe and product gas efferent duct It is arranged in parallel, and is connect respectively with absorber top.

Adsorbent is filled in the absorber.Adsorbent be carbon absorbent and alumina adsorbant, have enrich it is big-and-middle Pore structure.

The partial size of the adsorbent are as follows: 2~4mm of carbon absorbent, 3~5mm of aluminium oxide.

The absorber is equipped with insulating layer, and insulating layer is located at absorber outer wall.

Described device system is additionally provided with desulfurizer, and desulfurizer one end connects unstripped gas input pipe, and one end and alternating temperature become Press adsorbent equipment connection.

The desulfurizer is desulfurizing tower, can be 1 or 2.

Unstripped gas described in the utility model is the carbide acetylene gas in calcium carbide production acetylene.

3 or 3 or more absorbers compositions one are included at least in pressure and temperature varying adsorbent equipment and continuously run system, are adsorbed Adsorbent is filled in absorber in device, each absorber successively rinses through absorption, pressure drop, heating in one cycle, is cold It blows, evacuate and pressure rises step, the acetylene gas of pressure-drop steps discharge is sent into pressure and rises step.

Regeneration is overheated steam with thermal medium in heating rinsing step；Cold blowing medium is nitrogen or other in cold blowing step Gas without high-carbon component, wherein oxygen < 0.5%.

Sulphur impurity in desulfurizer removing carbide acetylene in the utility model, including H₂S and organic sulfur；Alternating temperature pressure-variable adsorption Device carries out deep purifying to acetylene gas, the residual impurity including hydrogen phosphide is removed, such as water, aldehyde alcohol ketone, hydrogen phosphide, ethylene The impurity such as ethyl-acetylene.Dry desulfurization device is using sulphur impurity in desulfurizing agent removing carbide acetylene.

Specific step is as follows for each absorber process in alternating temperature potential device absorber in the utility model:

(1) it adsorbs:

What the feeding by the unstripped gas of 0.10MPa~0.15MPaA pressure after dry desulfurization from bottom to top had regenerated It is adsorbed in absorber, adsorbent is to PH in device layer₃, a small amount of H₂S, the impurity such as water and vinylacetylene are adsorbed, purification The discharge from the top of device layer of gas afterwards.When impurity concentration reaches required concentration when absorber outlet, it can be considered that the absorber has reached Saturation state stops the thick acetylene of raw material and enters, stops absorption.

(2) pressure drop:

Pressure is reduced to the absorber for completing adsorption step, recycles acetylene in absorber.

(3) heating is rinsed:

By regeneration gas overheated steam and unstripped gas air-flow back through device layer, make the impurity being adsorbed with regeneration air stream Device layer out, adsorbent are regenerated.

(4) cold blowing:

Heating continues after stopping with cold regeneration gas such as nitrogen or other gas (oxygen < without high alkynes component 0.5%).It is rinsed cooling.

(5) it evacuates:

Use evacuation mode by N in device layer the absorber of cold blowing to environment temperature₂Or other regeneration without high alkynes Gas (oxygen < 0.5%) extracts adsorbent layer out.

(6) pressure liter:

The absorber evacuated is completed, rises to absorber device layer close to adsorptive pressure with acetylene, preparation is adsorbed next time.

Each absorber will undergo identical step, mutually stagger in timing, to guarantee that separation process is carried out continuously.

The utility model removes impurity in carbide acetylene, to H in the thick acetylene gas of calcium carbide₂S impurity can be removed to 0.005% with Under, PH₃Equal impurity can be removed to the alkyne impurities such as 0.003% or less, vinylacetylene and be removed to 0.003% respectively hereinafter, H₂O 0.05% is removed to hereinafter, H₂S≤0.005%, while being stripped of aldehyde alcohol ketone impurity；And process flow is simple, the degree of automation Height, operating cost are low.

Detailed description of the invention

With reference to the accompanying drawing and specific embodiment does more detailed description to the utility model:

Fig. 1 is the purification calcium carbide acetylene unit schematic diagram of test 1 in the utility model

Fig. 2 is the purification calcium carbide acetylene unit schematic diagram of test 2 in the utility model

Fig. 3 is the purification calcium carbide acetylene unit schematic diagram of test 3 in the utility model

Wherein, it is identified in figure are as follows: 1. desulfurizers, 2. absorbers, 3. vacuum pumps, 4. coolers, 5. sequencing valves, 6. pipes Road, 7. unstripped gas input pipes, 8. product gas efferent ducts, 9. regeneration steam input pipes, 10. insulating layers, 11. cold blowing gas input pipes

Specific embodiment

The utility model is further described With reference to embodiment:

Embodiment 1

A kind of apparatus system of carbide acetylene purification, is equipped with sequencing valve, pipeline, adsorbing mechanism, cooler, unstripped gas input Pipe, product gas efferent duct and vacuum pump, they constitute alternating temperature pressure-swing absorption apparatus, and unstripped gas input pipe passes through sequencing valve and absorption Device connection, vacuum pump both ends are connect with cooler, and cooler one end is connect with sequencing valve, and one end is connect with regeneration off gases pipeline； Vacuum pump and cooler are located at below absorber；Product gas efferent duct is connect with absorber top；Pass through pipe between all devices Road connection；Wherein the working condition of absorber and gas trend are controlled by sequencing valve.

Adsorbing mechanism forms one by 3 or 3 or more absorbers and continuously runs system, is equipped with absorber in device, inhales Adnexa is connected in parallel, and adsorbent is filled in absorber；It is additionally provided with regeneration steam input pipe and cold blowing gas input pipe, regeneration steam is defeated Enter pipe and cold blowing gas input pipe to be arranged in parallel with product gas efferent duct, and is connect respectively with absorber top.Extraneous steam passes through Regeneration steam input pipe enters absorber, and cold blowing gas (including nitrogen, nitrogen are one of which) enters by cold blowing gas input pipe Absorber.

Absorber bottom end is connect with cooler and vacuum pump.The partial size of adsorbent are as follows: carbon absorbent 2 or 4mm, aluminium oxide 3 or 5mm.

The feed end of each absorber of alternating temperature pressure-swing absorption apparatus connects acetylene original by sequencing valve in the utility model Expect gas input pipe, product end connects product gas efferent duct by sequencing valve, and regeneration steam passes through regeneration steam input pipe and program-controlled Valve connection enters absorber to be regenerated, and regeneration exhaust steam exports after sequencing valve, and regeneration is defeated by regeneration cold blowing gas with cold blowing gas Enter pipe to be connected with sequencing valve into cold blowing absorber, regenerates cold blowing exhaust gas and exported after sequencing valve and cooler.

Embodiment 5

A kind of apparatus system of carbide acetylene purification, be equipped with desulfurizer, sequencing valve, pipeline, adsorbing mechanism, cooler, Unstripped gas input pipe, product gas efferent duct and vacuum pump, desulfurizer one end are connect with unstripped gas input pipe, one end and adsorption machine Structure connection；Vacuum pump both ends are connect with cooler, and cooler one end is connect with sequencing valve, and one end is connect with regeneration off gases pipeline； Vacuum pump and cooler are located at below absorber；Product gas efferent duct is connect with absorber top；Pass through pipe between all devices Road connection；Wherein the working condition of adsorbing mechanism and gas trend are controlled by sequencing valve；The desulfurizer is desulfurizing tower, can be 1 or 2.

Adsorbing mechanism forms one by 3 or 3 or more absorbers and continuously runs system, is equipped with absorber in device, inhales Adnexa is connected in parallel, and adsorbent is filled in absorber；It is additionally provided with regeneration steam input pipe and cold blowing gas input pipe, regeneration steam is defeated Enter pipe and cold blowing gas input pipe to be arranged in parallel with product gas efferent duct, and is connect respectively with absorber top.Extraneous steam passes through Regeneration steam input pipe enters absorber, and cold blowing gas enters absorber by cold blowing gas input pipe.

Absorber bottom end is connect with cooler and vacuum pump.Each absorber is equipped with insulating layer.The partial size of adsorbent are as follows: Carbon absorbent 3mm, aluminium oxide 4mm.

The feed end of each absorber of alternating temperature pressure-swing absorption apparatus described in the utility model connects second by sequencing valve Alkynes unstripped gas input pipe, product end connect product gas efferent duct by sequencing valve, regeneration with steam by regeneration steam input pipe and Sequencing valve connection enters absorber to be regenerated, and regeneration exhaust steam exports after sequencing valve, and regeneration passes through regeneration cold blowing with cold blowing gas Gas input pipe is connected with sequencing valve into cold blowing absorber, is regenerated cold blowing exhaust gas and is exported after sequencing valve and cooler.

The steam of heating goes out apparatus system from regenerated steam port, and the exhaust gas of cold blowing step is after cooling from regeneration off gases The pipeline discharger of mouth evacuates exhaust gas and is also discharged from the pipeline of regenerated port.

Wherein, specific step is as follows for each absorber process in embodiment:

(1) it adsorbs:

The absorption that feeding by the unstripped gas of 0.10MPa~0.15MPaA pressure after desulfurization from bottom to top has regenerated It is adsorbed in device, adsorbent is to PH in device layer₃, a small amount of H₂S, the impurity such as water and vinylacetylene are adsorbed, purified Gas discharge from the top of device layer.When impurity concentration reaches required concentration when absorber outlet, it can be considered that the absorber has reached saturation State stops the thick acetylene of raw material and enters, stops absorption.

(2) pressure drop:

(3) heating is rinsed:

(4) cold blowing:

(5) it evacuates:

(6) pressure liter:

The absorber evacuated is completed, rises to absorber device layer close to adsorption pressure with the acetylene of depressurization step and product acetylene Power, preparation are adsorbed next time.

Each absorber will undergo identical step, only mutually stagger in timing, with guarantee separation process continuously into Row.

Test 1

Purify 2000Nm³The composition of/h carbide acetylene gas is as shown in table 1.Purification device schematic process flow diagram is shown in Fig. 1.

Pressure 0.15MPaA, 40 DEG C of temperature of carbide acetylene enter back into first after desulfurization by 3 absorbers (A, B, C) A series of adsorption cleaning system constituted with process control valves.

In adsorption cleaning system, any moment always has 1 absorber to be in adsorption cleaning step, is passed through by arrival end Raw material acetylene gas obtains product acetylene gas in outlet end, wherein S≤0.002%, PH₃≤ 0.003%, H₂O≤0.05%, C₄H₄≦ 0.003%.

Every absorber successively undergoes absorption (A), inverse put (D), heating to rinse (H), cold blowing (C), evacuation in different time (V) and boosting (ER) etc. 6 steps.The superheated steam of 0.6MPaG enters absorber from absorber outlet end, heats to it Regeneration, outflow steam can utilize the laggard torch pipe network of heat with other gas converting heats, and liquid is into wastewater disposal basin.Steam is added with nitrogen Absorber after heat is complete carries out purge, and entrained steam in absorber is purged out absorber and cooling absorber is to room temperature, Prepare absorption next time.

The composition (v%) of 1 carbide acetylene of table

O₂	N₂	CH₄	CO₂	Aldehyde ketone	C₄H₄	H₂S	PH₃	Organic sulfur	C₂H₂
										0.03	0.2	0.02	0.03	0.008	0.04	0.005	0.05	0.028	It is remaining

Test 2

Purify 7000Nm³The composition of/h carbide acetylene gas is as shown in table 2.Purification device schematic process flow diagram is shown in Fig. 2.

Pressure 0.15MPaA, 40 DEG C of temperature of carbide acetylene enter by 5 absorbers (A, B, C, D, E) and a series of programs The adsorption cleaning system that control valve is constituted.

In adsorption cleaning system, any moment always has 3 absorbers to be in adsorption cleaning step, is passed through by arrival end Raw material acetylene gas obtains product acetylene gas in outlet end, wherein H₂S≤0.001%, PH₃≤ 0.003%, H₂O≤0.05%, C₄H₄ ≤ 0.001%.

Every absorber successively undergoes absorption (A), inverse put (D), heating to rinse (H), cold blowing (C), evacuation in different time (V) and boosting (ER) etc. 6 steps.The superheated steam of 1.0MPaG enters absorber from absorber outlet end, heats to it Regeneration, outflow steam can utilize the laggard torch pipe network of heat with other gas converting heats, and liquid is into wastewater disposal basin.With groups such as nitrogen methane Absorber after the gaseous mixture divided has heated steam carries out purge, and entrained steam in absorber is purged out absorber simultaneously Cooling absorber prepares absorption next time to room temperature.

The composition (v%) of 2 carbide acetylene of table

O₂	N²	CH₄	CO₂	Aldehyde alcohol ketone	C₄H₄	H₂S	PH3	C₂H₂
									0.01	0.15	0.03	0.04	0.0007	0.005	0.002	0.07	It is remaining

Test 3

Purify 9000Nm³The composition of/h carbide acetylene gas is as shown in table 3, and purification device schematic process flow diagram is shown in Fig. 3.

Pressure 0.15MPaA, 40 DEG C of temperature of carbide acetylene first pass around enter after desulfurization by 6 absorbers (A, B, C, D, E, F) and a series of process control valves constitute adsorption cleaning system.

In adsorption cleaning system, any moment always has 4 absorbers to be in adsorption cleaning step, is passed through by arrival end Raw material acetylene gas obtains product acetylene gas in outlet end, wherein H2S≤0.001%, PH3≤0.003%, H2O≤0.05%, C4H4≤0.003%.

Every absorber successively undergoes absorption (A), inverse put (D), heating to rinse (H), cold blowing (C), evacuation in different time (V) and boosting (ER) etc. 6 steps.The superheated steam of 0.3MPaG enters absorber from absorber outlet end, heats to it Regeneration, outflow steam can utilize the laggard torch pipe network of heat with other gas converting heats, and liquid is into wastewater disposal basin.Steam is added with nitrogen Absorber after heat is complete carries out purge, and entrained steam in absorber is purged out absorber and cooling absorber is to room temperature, Prepare absorption next time.

The composition (v%) of 3 carbide acetylene of table

O₂	N₂	CH₄	CO₂	Aldehyde alcohol	C₄H₄	H₂S	PH₃	C₂H₂
									0.01	0.12	0.01	0.04	0.001	0.005	0.006	0.06	It is remaining

The advantages of basic principles and main features and the utility model of the utility model have been shown and described above, on It states and only illustrates the principles of the present invention described in embodiment and specification, do not departing from the spirit and scope of the utility model Under the premise of, the utility model also has various changes and improvements, these changes and improvements fall within claimed reality With in novel range.The range of the requires of the utility model protection is defined by the appending claims and its equivalent thereof.

Claims

1. a kind of apparatus system of carbide acetylene purification, including sequencing valve and pipeline, it is characterised in that: be equipped with adsorbing mechanism, cold But device, unstripped gas input pipe, product gas efferent duct and vacuum pump, they constitute alternating temperature pressure-swing absorption apparatus, unstripped gas input pipe Connect with alternating temperature pressure-swing absorption apparatus, vacuum pump both ends are connect with cooler, and cooler one end is connect with sequencing valve, one end with again Raw exhaust piping connection；Vacuum pump and cooler are located at below absorber；Product gas efferent duct is connect with absorber top；It is all It is connected between absorber by pipeline；Wherein the working condition of alternating temperature pressure-swing absorption apparatus absorber and gas trend are by sequencing valve Control.

2. a kind of apparatus system of carbide acetylene purification according to claim 1, it is characterised in that: the adsorbing mechanism by 3 or 3 or more absorbers form one and continuously run system, adsorbers parallel connection；Be additionally provided with regeneration steam input pipe and Cold blowing gas input pipe, regeneration steam input pipe and cold blowing gas input pipe are arranged in parallel with product gas efferent duct, and respectively with absorption The connection of device top.

3. a kind of apparatus system of carbide acetylene purification according to claim 2, it is characterised in that: filled in the absorber Fill out adsorbent.

4. a kind of apparatus system of carbide acetylene purification according to claim 3, it is characterised in that: the grain of the adsorbent Diameter are as follows: 2 ~ 4mm of carbon absorbent, 3 ~ 5mm of aluminium oxide.

5. a kind of apparatus system of carbide acetylene purification according to claim 1, it is characterised in that: set on the absorber There is insulating layer.

6. a kind of apparatus system of carbide acetylene purification according to any one of claims 1-5, it is characterised in that: described Apparatus system is additionally provided with desulfurizer, and desulfurizer one end is connect by unstripped gas input pipe with unstripped gas, one end and adsorption machine Structure connection.

7. a kind of apparatus system of carbide acetylene purification according to claim 6, it is characterised in that: the desulfurizer is Desulfurizing tower.