CN104211563B - A kind of vinyl chloride high-boiling components recovery process and equipment thereof - Google Patents
A kind of vinyl chloride high-boiling components recovery process and equipment thereof Download PDFInfo
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Abstract
The present invention relates to a kind of vinyl chloride high-boiling components recovery process and equipment thereof, described recovery process comprises that the vinyl chloride carrying out successively reclaims, dichloroethanes reclaims and trichloroethanes reclaims, utilize vinyl chloride knockout tower and low two stuffing rectification columns of tower and the auxiliary device thereof of boiling, respectively at the state of normal pressure and pressurization, isolate vinyl chloride gas and highly purified 1,1-dichloroethanes liquid, fully extracts the each several part of vinyl chloride high-boiling components; In airtight system, carry out, can not produce waste residue, waste water, protection of the environment, safe and reliable; Required heating-up temperature is low, utilizes spent hot water and waste hot steam to produce, and consumes energy low, and control point is few, easy and simple to handle. By the raffinate producing in production process is carried out to rectifying, obtain the different material of value, reduce environmental pollution, there is considerable economic benefit.
Description
Technical field
The present invention relates to a kind of recovery process and equipment, be applicable to vinyl chloride high-boiling components, specifically, relate to a kind of vinyl chloride high-boiling components recovery process and equipment thereof, belong to PVC Process Technology field.
Background technology
Produce in polyvinyl chloride process in carbide, acetylene has also produced the higher boiling organic compounds such as dichloroethanes, acetaldehyde, dichloroethylene, trichloro-ethylene, trichloroethanes in reacting in converter with hydrogen chloride and generating vinyl chloride.
Vinyl chloride (being called for short VCM) high-boiling components main component and content: 1,1-dichloroethanes 51%～53%, trans 1,2-dichloroethylene 16%～20%, cis 1,2-dichloroethylene 3%～4%, vinylidene chloride 0.2%～0.6%, trichloro-ethylene 0.3%～0.45%, 1,1,2-trichloroethanes 9%～10%, vinyl chloride 16%～20%.
In this raffinate, contained most of material is all poisonous and hazardous organic substance, and arbitrarily discharge will produce larger pollution to environment. And in this raffinate 1, the content of 1-dichloroethanes is more than 50%, so mainly reclaim 1 in raffinate, 1-dichloroethanes. 1,1-dichloroethanes is a kind of good solvent from purposes, can make the cleaning agent of machinery, electronic component, is also the main component of some binding agents, main, and it is high-efficiency low-toxicity cleaning agent 1,1, the raw material of 1-trichloroethanes.
At present, the recovery of vinyl chloride high-boiling components mainly utilizes vertical sieve tray rectifying column separating chlorine ethylene gas to reclaim, the main problem existing is: vinyl chloride inferior separating effect, remaining a large amount of vinyl chloride in liquid, 1,1 dichloroethanes product purity of institute's extraction is low, high-boiling components inferior separating effect, waste discharge amount is large, and environment is produced to larger pollution.
Summary of the invention
The problem to be solved in the present invention is for above problem, a kind of vinyl chloride high-boiling components recovery process is provided, by adopting the boiling point different principle of different material, high-boiling components is carried out to secondary distillation process, separation obtains vinyl chloride gas raw material and the available dichloroethanes of purity, finally produces a small amount of raffinate, greatly reduces the generation of toxic organics, economize in raw materials, produce considerable economic benefit.
Meanwhile, also provide a kind of VCM high-boiling components reclaimer, described equipment adopts closed-cycle system, can not produce waste residue, waste water, simple to operate, safe and reliable, and good energy-conserving effect.
For addressing the above problem, the technical solution adopted in the present invention is: a kind of vinyl chloride high-boiling components recovery process, is characterized in that: described recovery process comprises that the vinyl chloride carrying out successively reclaims, dichloroethanes reclaims and trichloroethanes reclaims.
Adopt this technical scheme, by the raffinate producing in production process is reclaimed, obtain the different material of value, reduce environmental pollution, have considerable economic benefit.
A kind of prioritization scheme, described vinyl chloride reclaims and comprises addition step;
In described addition step, vinyl chloride high-boiling components is added to vinyl chloride knockout tower through feed pump, the material in vinyl chloride knockout tower is carried out to Steam Heating.
Another kind of prioritization scheme, described vinyl chloride knockout tower comprises vinyl chloride knockout tower tower reactor, liquid level in vinyl chloride knockout tower tower reactor be controlled at vinyl chloride knockout tower tower reactor height 1/2～1/3 after, steam is passed into vinyl chloride knockout tower tower reactor, material in vinyl chloride knockout tower tower reactor is slowly heated up, heating rate is 30 DEG C/h, controls the temperature of vinyl chloride knockout tower tower reactor at 83 DEG C.
Another prioritization scheme, described vinyl chloride reclaims and comprises rectification step;
In described rectification step by the mass transport after Steam Heating in vinyl chloride knockout tower to vinyl chloride separation column condenser, in the time there is condensate liquid in vinyl chloride separation column condenser, by adjusting quantity of steam, the temperature of controlling vinyl chloride knockout tower tower reactor is 83 DEG C, and the tower top temperature of vinyl chloride knockout tower is 20 DEG C.
Further prioritization scheme, described vinyl chloride reclaims and comprises vinyl chloride extraction step;
While the tower internal pressure of vinyl chloride knockout tower being risen to 0.15MPa in described vinyl chloride extraction step, utilize gas chromatograph to analyze the gas purity of vinyl chloride overhead condenser outlet, when content of vinylchloride reaches 94% when above, extraction vinyl chloride gas.
Adopt technique scheme, separation and recovery of chlorine ethene under atmospheric pressure state in sealing system, can not produce waste residue, waste water, and protection of the environment is safe and reliable; Required heating-up temperature is low, utilizes spent hot water and waste hot steam to produce, and consumes energy low, and control point is few, easy and simple to handle.
A kind of prioritization scheme, described dichloroethanes reclaims and comprises the following steps:
1) feeding:
The mixtures of materials being deposited at the bottom of vinyl chloride knockout tower tower reactor tower after extraction vinyl chloride gas is pressed into the low tower tower reactor of boiling, controls still liquid in the low tower reactor tower reactor of boiling and, at 1/2～1/3 liquid level place, stop feeding;
2) dichloroethanes extraction:
The low material boiling in tower reactor tower reactor is carried out to steam heats, dichloroethanes vapor condensation enters return tank, utilize gas chromatograph to analyze the liquid refluxing in filling with, purity reaches 90%, the contained dichloroethanes purity of the low liquid boiling in tower tower reactor < 50%, in filling with refluxing, 60% of liquid passes back into low boiling in tower, and in the filling that refluxes, 40% of liquid is delivered in dichloroethanes storage tank;
3) dichloroethanes finished product is carried:
After in described dichloroethanes storage tank, liquid level reaches 80%, the liquid in dichloroethanes storage tank is carried.
Adopt this technical scheme, the rectifying of dichloroethanes is separated in closed system to be carried out, and can not produce waste residue, waste water, and protection of the environment is safe and reliable; Required heating-up temperature is low, utilizes spent hot water and waste hot steam to produce, and consumes energy low, and control point is few, easy and simple to handle, and high by the dichloroethanes product purity of rectifying extraction, colourity is good; Separate thoroughly, product quality is high.
Another kind of prioritization scheme, in the low tower tower reactor of boiling after described dichloroethanes is reclaimed, liquid carries out extraction, utilizes differential pressure action that liquid is pressed in trichloroethanes storage tank.
Adopt this technical scheme, effectively the trichloroethanes in separating chlorine ethene high-boiling components, simple to operate.
Another prioritization scheme, described high-boiling components storage tank is communicated with feed pump, and the pressure in feed pump is 3.5 standard atmospheric pressures.
Further prioritization scheme, described recovery process also comprises vinyl chloride high-boiling components composition detection;
Before described vinyl chloride high-boiling components composition detection is arranged on vinyl chloride recovery.
Adopt this technical scheme, effectively detect each constituent and content in vinyl chloride high-boiling components, be more conducive to each constituent to separate recovery.
The present invention also provides a kind of equipment of vinyl chloride high-boiling components recovery process, it is characterized in that: described equipment comprises the high-boiling components storage tank, feed pump, vinyl chloride knockout tower, the low tower that boils, the low tower condenser that boils, return tank, dichloroethanes storage tank and the Loading Pump that are communicated with successively, the low tower that boils is communicated with trichloroethanes storage tank, low boiling is communicated with tail gas condenser between tower condenser and return tank, and the low tower condenser that boils is communicated with the low tower that boils.
Described equipment adopts closed system, can not produce waste residue, waste water, and protection of the environment is safe and reliable; Required heating-up temperature is low, utilizes spent hot water and waste hot steam to produce, and consumes energy low, simple in structure.
The present invention takes above technical scheme, have the following advantages: utilize vinyl chloride knockout tower and low two stuffing rectification columns of tower and the auxiliary device thereof of boiling, respectively at the state of normal pressure and pressurization, isolate vinyl chloride gas and highly purified 1,1-dichloroethanes liquid, fully extracts the each several part of vinyl chloride high-boiling components; In airtight system, carry out, can not produce waste residue, waste water, protection of the environment, safe and reliable; Required heating-up temperature is low, utilizes spent hot water and waste hot steam to produce, and consumes energy low, and control point is few, easy and simple to handle.
1, by the raffinate producing in production process is carried out to rectifying, obtain the different material of value, reduce environmental pollution, have considerable economic benefit.
2, high by the dichloroethanes product purity of rectifying extraction, colourity is good; Separate thoroughly, product quality is high.
3, system adopts sealing and circulating, can not produce waste residue, waste water; Protection of the environment, simple to operate, safe and reliable.
4, the design of rectifying column is through analog computation and experiment, required little energy; Reach maximum energy-saving effect.
Below in conjunction with drawings and Examples, the invention will be further described.
Brief description of the drawings
Accompanying drawing 1 is the structural representation of vinyl chloride knockout tower in the embodiment of the present invention;
Accompanying drawing 2 is structural representations of the low tower that boils in the embodiment of the present invention;
Accompanying drawing 3 is structural representations of technological process in the embodiment of the present invention;
In figure:
1-vinyl chloride knockout tower end socket, 2-vinyl chloride knockout tower tower reactor, 3-vinyl chloride knockout tower heating tube, 4-vinyl chloride knockout tower saddle, 5-vinyl chloride knockout tower tower joint, 6-vinyl chloride knockout tower backflow distributing disc, 7-vinyl chloride separation column condenser, 8-vinyl chloride separation column condenser upper cover; The low tower end socket that boils of 11-, the low tower tower reactor of boiling of 12-, the low tower heating tube that boils of 13-, the low tower saddle that boils of 14-, the low tower feed pipe that boils of 15-, the low Ta Tajie that boils of 16-, the low tower backflow distributing disc that boils of 17-, the low tower return duct that boils of 18-; 101-high-boiling components storage tank, 102-feed pump, 103-vinyl chloride knockout tower charging control valve, 106-vinyl chloride knockout tower, 107-vinyl chloride extraction valve, 108-vinyl chloride knockout tower enters steam control valve, the low tower charging control valve that boils of 109-, 110-is low, and the tower that boils enters steam control valve, the low tower that boils of 112-, the low tower condenser that boils of 113-, 114-tail gas condenser, the 115-filling that refluxes, 116-dichloroethanes storage tank, 117-Loading Pump, 118-trichloroethanes storage tank, 119-dichloroethanes extraction flowmeter, 120-dichloroethanes extraction control valve.
Detailed description of the invention
Embodiment, as shown in Figure 3, a kind of vinyl chloride high-boiling components recovery process and equipment thereof, described recovery process comprises the following steps:
(1) material storing and inspection.
Vinyl chloride high-boiling components is sent in high-boiling components storage tank 101 to main component 1 in inspection vinyl chloride high-boiling components, 1-dichloroethanes, trans 1,2-dichloroethylene, cis 1,2-dichloroethylene, vinylidene chloride, trichloro-ethylene, 1,1, the content of 2-trichloroethanes and vinyl chloride.
Assay, 1, the content of 1-dichloroethanes is 52%, the content of trans 1,2-dichloroethene is 17%, the content of cis 1,2-dichloroethene is 3.5%, the content of vinylidene chloride is 0.7%, the content of trichloro-ethylene is 0.3%, the content of 1,1,2-trichloroethanes is 9%, the content of vinyl chloride is 17.4% and other micro-unknown components.
(2) reinforced.
Vinyl chloride high-boiling components in high-boiling components storage tank 101 is added to vinyl chloride knockout tower 106 through feed pump 102, between described feed pump 102 and vinyl chloride knockout tower 106, be provided with vinyl chloride knockout tower charging control valve 103, vinyl chloride knockout tower charging control valve 103 is for regulating vinyl chloride high-boiling components to enter the speed of vinyl chloride knockout tower 106, pressure in feed pump 102 is adjusted to 3.5 standard atmospheric pressure left and right, by the liquid level in vinyl chloride knockout tower tower reactor 2 be controlled at vinyl chloride knockout tower tower reactor 2 height 1/2～1/3 after, opening vinyl chloride knockout tower enters steam control valve 108 and controls steam flow, vinyl chloride knockout tower tower reactor 2 interior materials are slowly heated up, heating rate is 30 DEG C/h, control the temperature of vinyl chloride knockout tower tower reactor 2 83 DEG C of left and right.
(3) rectifying.
The interior vinyl chloride of vinyl chloride knockout tower 106 and other high-boiling components gas enter in vinyl chloride separation column condenser 7, in the time there is condensate liquid in vinyl chloride separation column condenser 7, by plus-minus quantity of steam, the final temperature of controlling vinyl chloride knockout tower tower reactor 2 is 83 DEG C, and the tower top temperature of vinyl chloride knockout tower 106 is 20 DEG C.
(4) vinyl chloride extraction.
When the tower internal pressure of vinyl chloride knockout tower 106 rises to 0.15MPa, utilize gas chromatograph to analyze the gas purity of vinyl chloride overhead condenser outlet, when content of vinylchloride reaches 94% when above, open vinyl chloride extraction valve 107, extraction vinyl chloride gas; At the bottom of the tower of vinyl chloride knockout tower tower reactor 2, it is the mixture of rest materials.
(5) feeding.
Mixture at the bottom of described vinyl chloride knockout tower tower reactor 2 towers is 1,1-dichloroethanes, cis-dichloroethanes, trichloro-ethylene, 1, and 2-dichloroethanes is flowed out by vinyl chloride knockout tower tower reactor 2; Vinyl chloride knockout tower tower reactor 2 is communicated with the low tower 112 that boils, vinyl chloride knockout tower tower reactor 2 and low boiling are provided with the low tower charging control valve 109 that boils between tower 112, vinyl chloride knockout tower tower reactor 2 and the low differential pressure action boiling between tower 112 by material by low tower charging control valve 109 adjust fluxes that boil, be pressed into the low tower 112 that boils, flow into low boiling in tower tower reactor 12, control the interior still liquid of the low tower tower reactor 12 of boiling at 1/2～1/3 liquid level place, stop feeding.
(6) dichloroethanes extraction.
Open the low tower that boils and enter steam control valve 110, for the low material boiling in tower tower reactor 12 heats up, control steam pressure, by the still temperature control of the low tower tower reactor 12 of boiling 64 DEG C of left and right, 50 DEG C of tower top temperatures, dichloroethanes gas phase enters the low tower condenser 113 that boils and carries out condensation, condensate liquid enters to reflux and fills with in 115, in the low tower condenser 113 that boils, uncooled gas enters tail gas condenser 114, carry out deep condensation, low boiling in tower condenser 113 and the condensed condensate liquid inflow of tail gas condenser 114 backflow filling 115, utilize gas chromatograph to analyze the liquid of filling with in 115 that refluxes, purity reaches 90%, the contained dichloroethanes purity of the low liquid boiling in tower tower reactor 12 < 50%, open backflow filling 115 and the low valve boiling between tower 112 liquid 60% in backflow filling 115 is passed back into low boiling in tower 112, 40% is regulated and is entered in dichloroethanes storage tank 116 by dichloroethanes extraction control valve 120, reflux and be provided with dichloroethanes extraction flowmeter 119 between filling 115 and dichloroethanes extraction control valve 120, described dichloroethanes extraction flowmeter 119 is used to indicate flow in pipeline, control flow at 0.3m3/h。
(7) finished product is carried.
After in dichloroethanes storage tank 116, liquid level reaches 80%, carry by Loading Pump 117.
(8) still liquid extraction.
Analyzing trichloroethanes purity in low tower tower reactor 12 liquid that boil through the productions of continuous 5 days is 38.5%, now the low tower 112 that boils continues purification dichloroethanes again, to waste very macro-energy, and therefore the low interior liquid of tower tower reactor 12 that boils is carried out to extraction, utilize differential pressure action that liquid is pressed in trichloroethanes storage tank 118.
Described vinyl chloride high-boiling components reclaimer comprises the high-boiling components storage tank 101, feed pump 102, vinyl chloride knockout tower 106, the low tower 112 that boils, the low tower condenser 113 that boils, return tank 115, dichloroethanes storage tank 116 and the Loading Pump 117 that are communicated with successively, the low tower 112 that boils is communicated with trichloroethanes storage tank 118, low boiling is communicated with tail gas condenser 114 between tower condenser 113 and return tank 115, and the low tower condenser 113 that boils is also communicated with the low tower 112 that boils.
Described high-boiling components storage tank 101 is horizontal tank, and the two ends of high-boiling components storage tank 101 are respectively equipped with end socket, and saddle is established in the bottom of high-boiling components storage tank 101, for fixing high-boiling components storage tank 101.
Described feed pump 102 is centrifugal pump, is made up of impeller, the pump housing, pump shaft, bearing, sealing ring and stuffing-box.
Described tail gas condenser 114 is horizontal pipe bundle condenser, adopts chilled water to carry out cooling, is two-tube-pass, the chilled water that flows in the shell side barrel of tail gas condenser 114, and described tail gas condenser 114 comprises left and right two joint end sockets, middle cylindrical shell, expansion joint; Tail gas condenser 114 inside are provided with four deflection plates, and end socket one side is provided with air inlet and gas outlet, and middle shell ring two ends are provided with leakage fluid dram, and described leakage fluid dram is positioned at the below of tail gas condenser 114; Described chilled water is 7 DEG C of water; Described shell side barrel top is provided with exhaust outlet, and shell side barrel below is provided with discharging hole; Described expansion joint below is provided with discharging hole, and tail gas condenser 114 is connected with two groups of leg seats, and described leg seat is for fixing tail gas condenser 114.
The described low tower condenser 113 that boils is for the horizontal pipe bundle condenser that tilts, and the cylindrical shell of the low tower condenser 113 that boils and tubulation are 8 ° with respect to angle of inclination, placed side, adopt recirculated water to carry out cooling, are two-tube-pass, flow circuit water in shell side barrel; The described low tower condenser 113 that boils comprises left and right two end sockets, cylindrical shell; Low tower condenser 113 inside of boiling are provided with six deflection plates, and end socket one side is provided with air inlet and gas outlet, and cylindrical shell two ends are provided with leakage fluid dram, and described leakage fluid dram is positioned at low tower condenser 113 belows of boiling; Described shell side barrel top is provided with exhaust outlet, and shell side barrel below is provided with discharging hole; Described expansion joint below is provided with discharging hole; The low tower condenser 113 that boils is connected with two groups of leg seats, and described leg seat is for the fixing low tower condenser 113 that boils.
Described return tank 115 is horizontal tank, and the two ends of return tank 115 are respectively equipped with end socket, and the bottom of return tank 115 is provided with saddle, for fixing return tank 115.
Described trichloroethanes storage tank 118 is horizontal tank, and the two ends of trichloroethanes storage tank 118 are respectively equipped with end socket, and the bottom of trichloroethanes storage tank 118 is provided with saddle, for fixing trichloroethanes storage tank 118.
Described dichloroethanes storage tank 116 is vertical tank, and the two ends of dichloroethanes storage tank 116 are respectively equipped with end socket, and the bottom of dichloroethanes storage tank 116 is provided with skirt, for fixing dichloroethanes storage tank 116.
As shown in Figure 1, described vinyl chloride knockout tower 106 comprises vinyl chloride knockout tower tower reactor 2, vinyl chloride knockout tower tower joint 5, vinyl chloride separation column condenser 7, described vinyl chloride knockout tower tower reactor 2 diameters are 1500mm, the two ends of vinyl chloride knockout tower tower reactor 2 are equipped with vinyl chloride knockout tower end socket 1, vinyl chloride knockout tower tower reactor 2 is provided with vinyl chloride knockout tower heating tube 3, vinyl chloride knockout tower heating tube 3 is U-shaped, in vinyl chloride knockout tower heating tube 3, passing into steam heats to material in still, described vinyl chloride knockout tower tower joint 5 is provided with eight joints, every joint length is 1500mm, with bolts between every joint, described every joint vinyl chloride knockout tower tower saves 5 bottoms and is provided with catch tray, on catch tray, place packing support screen, support screen upper strata paving one deck stainless (steel) wire, load respectively Pall ring filler, calculate and fill in 80% ratio according to test data, the first segment of described vinyl chloride knockout tower tower joint 5 is provided with vinyl chloride knockout tower backflow distributing disc 6, described vinyl chloride knockout tower backflow distributing disc 6 comprises riser, downspout and distributing disc base, described riser is DN100 seamless carbon steel tube, described downspout is DN20 seamless pipe, and described distributing disc base diameter is 490mm, the 7th tower joint of vinyl chloride knockout tower tower joint 5 is provided with charge pipe and gos deep in tower, described vinyl chloride separation overhead condenser 7 is positioned at the first tower joint top of vinyl chloride knockout tower tower joint 5, is tubular heat exchanger, inside establishes five deflection plates.
As shown in Figure 2, the described low tower 112 that boils comprises the low tower tower reactor 12 of boiling, the low tower tower joint 16 that boils, described low tower tower reactor 12 diameters that boil are 1500mm, low two ends of boiling tower tower reactor 12 are equipped with the low tower end socket 11 that boils, in the low tower tower reactor 12 of boiling, be provided with the low tower heating tube 13 that boils, the low tower heating tube 13 that boils is U-shaped, in the low tower heating tube 13 that boils, passing into steam heats to the low interior material of tower tower reactor 12 that boils, the described low tower tower joint 16 that boils is provided with six joints, every joint length is 1500mm, with bolts between every joint, the low tower tower that boils of described every joint saves 16 bottoms and is provided with catch tray, on catch tray, place packing support screen, support screen upper strata paving one deck stainless (steel) wire, load respectively Pall ring filler, calculate and fill in 80% ratio according to test data, the described low first segment that boils tower tower joint 16 is provided with the low tower backflow distributing disc 17 that boils, the described low tower backflow distributing disc 17 that boils comprises riser, downspout and distributing disc base, described riser is DN100 seamless carbon steel tube, described downspout is DN20 seamless pipe, and described distributing disc base diameter is 490mm, the 5th tower joint of the low tower tower joint 16 that boils is provided with charge pipe and gos deep in tower.
Describe as an example of the Economic and Efficiency Analysis that produces after annual 4000 tons of vinyl chloride high-boiling components rectification and purification example:
To reclaim purity be 98% vinyl chloride: 4000t/a × 15% × 5000 yuan/ten thousand yuan of t=300;
Wherein: detecting vinyl-chloride-containing in high-boiling components is 18%, considers that a small amount of remnants get 15% and estimate, wherein vinyl chloride price per ton is 5000 yuan.
Reclaim dichloroethanes (50%): 4000t/a × 50% × 2000 yuan/ten thousand yuan of t=400;
Wherein: detecting in high-boiling components is 52% containing dichloroethanes, considers that a small amount of remnants get 50% and estimate, wherein vinyl chloride price per ton is 2000 yuan.
Add up to and reclaim and can produce: the income of 3,00+,400 ten thousand=7,000,000.
Finally it should be noted that: the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although the present invention is had been described in detail with reference to previous embodiment, for a person skilled in the art, its technical scheme that still can record previous embodiment is modified, or part technical characterictic is wherein equal to replacement. Within the spirit and principles in the present invention all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a vinyl chloride high-boiling components recovery process, is characterized in that: described recovery process comprises that the vinyl chloride carrying out successively reclaims, dichloroethanes reclaims and trichloroethanes reclaims;
Described vinyl chloride reclaims and comprises addition step, rectification step and vinyl chloride extraction step;
In described addition step, the liquid level in vinyl chloride knockout tower tower reactor (2) is controlled at vinyl chloride knockout tower tower reactor (2) height 1/2～1/3 after, steam is passed into vinyl chloride knockout tower tower reactor (2), the interior material of vinyl chloride knockout tower tower reactor (2) is slowly heated up, heating rate is 30 DEG C/h, controls the temperature of vinyl chloride knockout tower tower reactor (2) at 83 DEG C;
While the tower internal pressure of vinyl chloride knockout tower (106) being risen to 0.15MPa in described vinyl chloride extraction step, utilize gas chromatograph to analyze the gas purity of vinyl chloride overhead condenser (7) outlet, when content of vinylchloride reaches 94% when above, extraction vinyl chloride gas;
Described dichloroethanes reclaims and comprises dichloroethanes extraction step;
In described dichloroethanes extraction step, the material in the low tower reactor tower reactor (12) of boiling being carried out to steam heats, dichloroethanes vapor condensation enters return tank (115), utilize gas chromatograph to analyze the liquid of filling with in (115) that refluxes, purity reaches 90%, the low contained dichloroethanes purity of the liquid < 50% boiling in tower tower reactor (12), 60% of the middle liquid of filling (115) that will reflux passes back in the low tower that boils (112), and in the filling (115) that refluxes, 40% of liquid is delivered in dichloroethanes storage tank (116);
In described trichloroethanes recycling step, utilize differential pressure action that liquid is pressed in trichloroethanes storage tank (118).
2. a kind of vinyl chloride high-boiling components recovery process as claimed in claim 1, it is characterized in that: in described addition step, vinyl chloride high-boiling components is added to vinyl chloride knockout tower (106) through feed pump (102), the material in vinyl chloride knockout tower (106) is carried out to Steam Heating.
3. a kind of vinyl chloride high-boiling components recovery process as claimed in claim 1, it is characterized in that: in described rectification step by the mass transport after Steam Heating in vinyl chloride knockout tower (106) to vinyl chloride separation column condenser (7), in the time there is condensate liquid in vinyl chloride separation column condenser (7), by adjusting quantity of steam, the temperature of controlling vinyl chloride knockout tower tower reactor (2) is 83 DEG C, and the tower top temperature of vinyl chloride knockout tower (106) is 20 DEG C.
4. a kind of vinyl chloride high-boiling components recovery process as claimed in claim 1, is characterized in that: described dichloroethanes reclaims and also comprises feeding step:
The mixtures of materials being deposited at the bottom of vinyl chloride knockout tower tower reactor (2) tower after extraction vinyl chloride gas is pressed into the low tower tower reactor (12) of boiling, controls the low interior still liquid of tower reactor tower reactor (12) that boils at 1/2～1/3 liquid level place, stop feeding.
5. a kind of vinyl chloride high-boiling components recovery process as claimed in claim 1, is characterized in that: described dichloroethanes reclaims and also comprises dichloroethanes finished product supplying step:
After in described dichloroethanes storage tank (116), liquid level reaches 80%, the liquid in dichloroethanes storage tank (116) is carried.
6. a kind of vinyl chloride high-boiling components recovery process as claimed in claim 1, is characterized in that: the low interior liquid of tower tower reactor (12) that boils after described dichloroethanes is reclaimed carries out extraction, utilizes differential pressure action that liquid is pressed in trichloroethanes storage tank (118).
7. a kind of vinyl chloride high-boiling components recovery process as claimed in claim 2, is characterized in that: in described vinyl chloride recycling step, the pressure in feed pump (102) is 3.5 standard atmospheric pressures.
8. a kind of vinyl chloride high-boiling components recovery process as claimed in claim 1, is characterized in that: described recovery process also comprises vinyl chloride high-boiling components composition detection;
Before described vinyl chloride high-boiling components composition detection is arranged on vinyl chloride recovery.
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| CN104474730B (en) * | 2014-11-20 | 2016-09-21 | 新疆中泰化学股份有限公司 | High-boiling components special VCM rectification segregation apparatus and separation method |
| CN107235823B (en) * | 2017-06-27 | 2021-11-16 | 山东新龙科技股份有限公司 | Process and equipment for recovering and refining calcium carbide VCM high-boiling residues |
| CN112079686A (en) * | 2019-06-12 | 2020-12-15 | 北京先锋创新科技发展有限公司 | Vinyl chloride high-boiling-point substance rectification recovery process |
| CN111056916B (en) * | 2019-12-12 | 2023-08-25 | 连州市润邦生物科技有限公司 | High boiling point waste treatment method in chloroethylene production |
| CN111689833A (en) * | 2020-07-03 | 2020-09-22 | 安徽华塑股份有限公司 | VCM high-boiling-point substance purification device and purification method |
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| CN102267865B (en) * | 2011-05-30 | 2014-03-12 | 新疆天业（集团）有限公司 | Method for purifying dichloroethane from vinyl chloride rectification residual liquid |
| CN102863314A (en) * | 2011-07-06 | 2013-01-09 | 北京先锋创新科技发展有限公司 | Refining method for vinyl chloride in production of polrvinyl chloride |
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Inventor after: Han Wei Inventor after: PAERHATI MAIMAITIYIMING Inventor after: Zhao Yonglu Inventor after: Yang Xiuling Inventor after: Lv Xiaokai Inventor after: Fan Qingpei Inventor after: Wang Yanbo Inventor after: Wang Shigang Inventor before: Miao Naifen Inventor before: Yang Xiuling Inventor before: Cao Hongsheng Inventor before: Zhang Jiliang Inventor before: Wang Jiyan |
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Effective date of registration: 20160411 Address after: 830026 the Xinjiang Uygur Autonomous Region Urumqi Yangcheng Lake Economic and Technological Development Zone, Road No. 39 Applicant after: Xinjiang Zhongtai Chemical Co., Ltd. Address before: 262709 Shandong city in Weifang Province, Shouguang City, Wang Xinlong Industrial Park Industrial Company West Road PVC Applicant before: Shandong Xinlong Technology Co., Ltd. |