CN209442638U - A kind of F32 device by-product HCl purification apparatus - Google Patents
A kind of F32 device by-product HCl purification apparatus Download PDFInfo
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- CN209442638U CN209442638U CN201821987147.4U CN201821987147U CN209442638U CN 209442638 U CN209442638 U CN 209442638U CN 201821987147 U CN201821987147 U CN 201821987147U CN 209442638 U CN209442638 U CN 209442638U
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Abstract
The utility model discloses a kind of F32 device by-product HCl purification apparatus, including HCl separative unit, it is adsorbed by drying unit, finished product rectification cell, the HCl separative unit connection is adsorbed by drying unit, is adsorbed by drying unit connection finished product rectification cell；The purification apparatus of the utility model is prevented the fluctuation of upstream production system from having an impact to the charging of HCl separation tower, is stablized output qualified products using the first surge tank；Feed cooler, reactor product cooler can cool down product, the problem that the heat exchange area of elimination product rectifying column condenser and products pot is small, cooling effect is poor；Chlorination hydrogen production tower reboiler heat source is compressor high-temperature gas, not only energy saving, while solving reboiler etching problem；Material is adsorbed using the first absorber, drier, keeps micro heavy metal and fluorine-containing material intercepted, ensure that product purity, added value is high, has accomplished that the efficient circulation of by-product uses, has had great importance.
Description
Technical field
The utility model relates to fine chemistry industry apparatus fields, and in particular to a kind of F32 device by-product HCl purification apparatus.
Background technique
Since resource consumes excessively and increasingly rare, environmental problem is got worse, and restricts expanding economy and society significantly
Whether the progress of meeting, influence of the process of producing product to environment, resource maximally utilize the sustainable development for being related to society.I
State is organic chlorides big producer, generates a large amount of by-product hydrogen chloride, and the total amount of by-product hydrogen chloride is in the situation of cumulative year after year,
The environment and social resources produce to us impacts, when process system is unable to reuse, the most conventional benefit of by-product hydrogen chloride
It is exactly by-product hydrochloric acid with method.Due to hydrochloric acid market, supply exceed demand, utilizes a large amount of by-product chlorinations with the inexpensive way of by-product hydrochloric acid
Hydrogen is outdated, also usually occurs the ring that individual enterprise's sacrificialing environments obtain company interest when by-product hydrochloric acid sale is at burden
Guarantor's problem, therefore, only exploitation recyclable device are recycled hydrogen chloride resource, can just meet resource-conserving, environmentally friendly
The requirement of social development.
F32 fluorination production is to generate F32 and hydrogen chloride under the action of catalyst using HF and R30 as raw material, in raw gas
Complicated component effectively removes these magazines containing many impurity such as R31, R22, R40, moisture, removes oxygen, nitrogen, hydrogen light component,
Finally the product of 99.999% or more extraction is the key that technology in tower.
Summary of the invention
The technical problems to be solved in the utility model is against the above deficiency, mainly to provide a kind of F32 device by-product HCl
Purification apparatus, the equipment include HCl separative unit, are adsorbed by drying unit, finished product rectification cell, and by-product HCl is by the first buffering
Tank enters HCl separation tower, prevents the fluctuation of upstream production system from having an impact to the charging of HCl separation tower, stablizes output
Qualified products；Because HCl separation tower reboiler needs to heat, electric heating rectifying column is transformed, bottom uses reboiler,
Heat source is the condensed water that fluorination reaction generates, and makes full use of thermal energy, reaches energy-efficient purpose；Tower top in finished product rectification cell
The refrigerant of condenser and condenser uses environmental protection refrigerant F32, liquid F32 to be directly entered in condenser, passes through control F32 evaporation
Amount adjusts condensation temperature；Feed cooler, reactor product cooler can cool down product, eliminate product rectifying column condenser and production
The problem that the heat exchange area of product tank is small, cooling effect is poor；Chlorination hydrogen production tower reboiler heat source is compressor high-temperature gas, is utilized
Gas provides heat to chlorination hydrogen production tower reboiler after compression, not only energy saving, while solving reboiler etching problem；Make
Material is adsorbed with the first absorber, drier, keeps micro heavy metal and fluorine-containing material intercepted, ensure that product is pure
Degree.Meanwhile the utility model reduces heat exchange step and improves heat exchange efficiency, reduce other using environmental protection refrigerant F32 as refrigerant
Corrosion of the refrigerating medium to equipment, will not damage ozone layer, and environmental protection is reliable.
In order to solve the above technical problems, the technical solution of the utility model is:
A kind of F32 device by-product HCl purification apparatus, it is characterised in that:
The equipment includes HCl separative unit, is adsorbed by drying unit, finished product rectification cell, the HCl separative unit connection
It is adsorbed by drying unit, it is described to be adsorbed by drying unit connection finished product rectification cell；
The HCl separative unit, including HCl separation tower, HCl separation tower setting feed entrance, gas phase mouth,
Liquid phase mouth and refluxing opening；
The feed entrance and refluxing opening of the HCl separation tower lower end phase with the first surge tank, overhead condenser respectively
Connection；
The gas phase mouth of the HCl separation tower, liquid phase mouth are connected with the lower end of the upper end of reboiler, reboiler respectively.
It is described to be adsorbed by drying unit, including the first absorber and drier；First absorber one end is connected to chlorination
The gas outlet of hydrogen knockout tower, the other end on the other side are connected with drier；
The finished product rectification cell, comprising: the second surge tank, compressor, forecooler, chlorination hydrogen production tower reboiler, chlorine
Change hydrogen rectifying column, reactor product cooler, condenser, products pot, the second absorber；
Second surge tank is connected by compressor with chlorination hydrogen production tower reboiler；
The chlorination hydrogen production tower reboiler is connected with forecooler, hydrogen chloride rectifying column；
The hydrogen chloride rectifying column is provided with feed entrance, gas phase mouth, liquid phase mouth, refluxing opening and kettle liquid outlet；
The feed entrance and refluxing opening of the hydrogen chloride rectifying column are connected with the entrance of forecooler, condenser respectively；
The gas phase mouth of the hydrogen chloride rectifying column, liquid phase mouth respectively with the upper end of chlorination hydrogen production tower reboiler, hydrogen chloride
The lower end of product tower reboiler is connected；
The kettle liquid outlet of the hydrogen chloride rectifying column is connected with the second absorber, the second absorber and reactor product cooler phase
Connection, reactor product cooler are connected with products pot；
Further, the HCl separation tower is packed tower, diameter 800mm, high 35980mm, and material uses Q345R,
Filler is high density wire packing；
The reboiler heat exchange area is 50 ㎡, and 103 heat exchange area of condenser is 80 ㎡.
Further, the hydrogen chloride rectifying column is packed tower, diameter 400mm, high 25789mm.
Further, the first absorber diameter 1600mm, high 4000mm, material use Q345R, adsorbent 3-
5mm active carbon.
Further, the drier, diameter are 1600 mm, and high 4000mm, material is using Q345R, adsorbent 3-
The 5A molecular sieve of 5mm.
Further, the condenser heat exchange area is 20 ㎡, and 109 heat exchange area of forecooler is 30 ㎡, the hydrogen chloride
Product tower reboiler, heat exchange area are 25 ㎡.
Further, the second absorber diameter is 1000 mm, high 3000mm, material 316L, adsorbent 3-5mm
High density mixed adsorbent.
The utility model is described in detail with reference to the accompanying drawings and examples.
Detailed description of the invention
Fig. 1: the utility model device connection schematic diagram；
In figure, the first surge tank -101, HCl separation tower -102, overhead condenser -103, reboiler -104, the first suction
Adnexa -105, drier -106, the second surge tank -107, compressor -108, feed cooler -109, hydrogen chloride rectifying column -
110, chlorination hydrogen production tower reboiler -111, reactor product cooler -112, condenser -113, products pot -114, the second absorber -
115。
Specific embodiment
Following specific embodiments do not limit the utility model convenient for better understanding the utility model.Following embodiments
In experimental method be unless otherwise specified conventional method.Material therefor in following embodiments is unless otherwise specified
Conventional material.Test in following embodiment is respectively provided with unless otherwise specified and repeats to test three times, results are averaged.Below
The present invention will be further described in conjunction with the embodiments.
A kind of embodiment 1: F32 device by-product HCl purification apparatus
It is a kind of F32 device by-product HCl purification apparatus of the invention below, specifically:
The purification apparatus includes: HCl separative unit, is adsorbed by drying unit, finished product rectification cell；
The HCl separative unit connection is adsorbed by drying unit, described to be adsorbed by drying unit connection finished product rectification cell.
The HCl separative unit, including HCl separation tower 102, the HCl separation tower 102 include feed entrance,
Gas phase mouth, liquid phase mouth and refluxing opening；
The feed entrance and refluxing opening of the HCl separation tower 102 respectively with the first surge tank 101 and overhead condenser
103 lower end is connected；HCl separation tower 102 is complete by the difluoromethane contained in gas, fluorochloromethane, HF, methylene chloride
Portion's removal, remaining hydrogen chloride and the boiling point component lower than hydrogen chloride.
The gas phase mouth of the HCl separation tower 102, liquid phase mouth are connected with the top and bottom of reboiler 104 respectively；
The reboiler 104 is connected with the HCl separation tower 102；
The HCl separation tower 102 is packed tower, diameter 800mm, high 35980mm, and material uses Q345R, and filler is
High density wire packing；
104 heat exchange area of reboiler is 50 ㎡, and 103 heat exchange area of condenser is 80 ㎡.
It is described to be adsorbed by drying unit, including the first absorber 105 and drier 106；Described first absorber, 105 one end connects
The gas outlet of HCl separation tower 102 is passed through, the other end on the other side is connected with drier 106；Whereby, uncooled gas
Mutually part can reach the first absorber 105 by pipeline, and drier is entered after the adsorption-edulcoration of the first absorber 105
106 are dried, and obtain product, are adsorbed using the first absorber 105, drier 106 to material, make micro heavy metal
And fluorine-containing material is intercepted, ensure that product purity, purity 99.95%.
First absorber, the 105 diameter 1600mm, high 4000mm, for material using Q345R, adsorbent is 3-5mm activity
Charcoal；
106 diameter of drier is 1600, high 4000mm, and material uses Q345R, and adsorbent is the 5A molecule of 3-5mm
Sieve.
The finished product rectification cell, comprising: the second surge tank 107, compressor 108, forecooler 109, chlorination hydrogen production tower
Reboiler 111, hydrogen chloride rectifying column 110, reactor product cooler 112, condenser 113, products pot 114, the second absorber -115；
Second surge tank 107 is connected with 108 entrance of compressor, increases surge tank before compressor 108, can effectively protect
The pressure of card system is stablized, and the long-acting operation of compressor is protected；Uncooled gas phase exports after the compression of compressor 108 and chlorination
Hydrogen production tower reboiler 111 is connected；111 heat source of product tower reboiler is compressor high-temperature gas, utilizes gas pair after compression
110 rectifying of hydrogen chloride rectifying column provides heat, not only energy saving, while solving the corrosion of chlorination hydrogen production tower reboiler 111
Problem.
The chlorination hydrogen production tower reboiler 111 is connected with forecooler 109 and hydrogen chloride rectifying column 110；
The hydrogen chloride rectifying column 110 is provided with feed entrance, gas phase mouth, liquid phase mouth, refluxing opening and kettle liquid outlet；Chlorination
Hydrogen rectifying column 110 has been accomplished to optimize, energy consumption is few, and energy-saving effect is obvious by stringent design, calculating；
The feed entrance and refluxing opening of the hydrogen chloride rectifying column 110 entrance with forecooler 109 and condenser 113 respectively
It is connected；
The gas phase mouth of the hydrogen chloride rectifying column 110, liquid phase mouth respectively with the upper end of chlorination hydrogen production tower reboiler 111 and
Lower end is connected；
The chlorination hydrogen production tower reboiler 111 is connected with the hydrogen chloride rectifying column 110；
The kettle liquid outlet of the hydrogen chloride rectifying column 110 is connected with the second absorber 115, the second absorber 115 and production
Product cooler 112 is connected, and reactor product cooler 112 is connected with products pot 114.
The hydrogen chloride rectifying column 110 is packed tower, diameter 400mm, high 25789mm, and material uses 316L, and filler is
CX900 wire packing；
113 heat exchange area of condenser is 20 ㎡, and 109 heat exchange area of forecooler is 30 ㎡, 111 heat exchange area of reboiler
For 25 ㎡；
Feed cooler 109, reactor product cooler 112 cool down product, eliminate product rectifying column condenser and product
The heat exchange area of tank is small, the problem of cooling effect difference；
115 diameter of absorber is 1000, high 3000mm, material 316L, and adsorbent is 3-5mm high density mixing and absorption
Agent increases absorber 115, for the trace metal impurities in adsorption production material.
In F32 device by-product HCl purification apparatus of the invention, overhead condenser 103, condenser 113 refrigerant use ring
Refrigerant F32 is protected, liquid F32 is directly entered overhead condenser 103, in condenser 113, adjusts by control F32 evaporation capacity cold
Solidifying temperature.
As shown in Figure 1, a kind of use process of F32 device by-product HCl purification apparatus of the utility model, comprising: cooling,
Separation is adsorbed by drying, rectification working process again, the specific steps are as follows:
Step 1, cooling:
The by-product HCl gas that the raw material that the utility model uses generates for F32 process units, the F32 process units produce
Raw by-product HCl gas enters the first surge tank 101, pressure 1.4MPa by pipeline with the flow velocity of 300m3/h；
Then pass through HCl separation tower 102, the tower pressure interior force of HCl separation tower 102 is 1.38MPa, and it is light to obtain gas phase
Component and heavy constituent material.
The by-product HCl gas that the F32 process units generates includes following components: hydrogen chloride, difluoromethane, fluorine chloromethane
Alkane, HF, methylene chloride, oxygen, nitrogen, hydrogen.
The gas phase light component is chlorination hydrogen production；
The gas phase light component is divided into two parts: condensation liquid phase part and uncooled gas phase；Condense liquid phase and uncooled gas
The ratio of phase is 2:1；
The condensation liquid phase part is condensed by overhead condenser 103, and the liquid obtained after condensation passes through return pipe
It is back in tower, flow velocity is about 320m3/h；
The uncooled gas phase portion enters separation by pipeline and is adsorbed by drying process；
The heavy constituent material flows into tower bottom, and tower bottom mainly contains difluoromethane, fluorochloromethane, HF, methylene chloride；
The heavy constituent material is exchanged heat by reboiler 104 and kettle liquid material in tower, and 10 DEG C of kettle liquid temperature, kettle liquid object
The cold material under gas and tower top stream after material heating swaps；Cold heavy constituent material flows into tower bottom, and tower bottom mainly contains
There are difluoromethane, fluorochloromethane, HF, methylene chloride；
Kettle liquid material in the tower, including difluoromethane, fluorochloromethane, HF, methylene chloride；
The overhead condenser 103, condensation temperature are -23 DEG C；Guarantee tower pressure interior force is 1.38MPa.
104 heat exchange area of reboiler is 50 ㎡, and 103 heat exchange area of condenser is 80 ㎡.
Step 2, separation are adsorbed by drying:
By the first absorber 105, drier 106 after uncooled gas phase extraction, by sampling analysis, by dry
Product purity is 99.95%.
It is former as production can be delivered to trichlorosilane workshop by pipeline for the chlorination hydrogen production of 99.95% or more output
Material.
First absorber 105, diameter 1600mm, high 4000mm, for material using Q345R, adsorbent is 3-5mm activity
Charcoal；
106 diameter of drier is 1600, high 4000mm, and material uses Q345R, and adsorbent is the 5A molecule of 3-5mm
Sieve.
Step 3, again rectification working process:
99.9% or more the chlorination hydrogen production that step 2 obtains passes through the second surge tank 107 with the rate of 100Kg/h, via
Compressor 108 compress, compressed pressure be 4.5MPa, 80 DEG C of temperature；
Subsequently into chlorination hydrogen production tower reboiler 111, high-temperature gas heats kettle liquid material in tower, kettle liquid temperature
20℃；
Thermal material rises in tower, and cold material decline in tower, the hydrogen chloride gas after cooling is acted on by forecooler 109, makes
Temperature reduces again, and into hydrogen chloride rectifying column 110, feeding temperature is 18 DEG C, and 110 tower top temperature of hydrogen chloride rectifying column is 10
DEG C, obtain gaseous phase materials；
Gaseous phase materials enter condenser 113, and the condensation temperature of the condenser 113 is 10 DEG C；
Top gaseous phase is back in hydrogen chloride rectifying column 110 after condensation, the tower reactor in the hydrogen chloride rectifying column 110
Material is through analyzing, feed purity 99.9993%.
Uncooled oxygen, nitrogen, hydrogen light component and a small amount of HCl can be discharged into trichlorine by adjusting valve regulation gas output 6Kg/h
Hydrogen silicon manufacturing apparatus is stand-by；
Kettle material in hydrogen chloride rectifying column 110 carries out purification absorption by the second absorber 115, cold using product
But device 112 cools down again, is stored into products pot 114, yield 94Kg/h.
The hydrogen chloride rectifying column 110 is packed tower, diameter 400mm, high 25789mm, and material uses 316L, and filler is
CX900 wire packing.
113 heat exchange area of condenser is 20 ㎡, and 109 heat exchange area of forecooler is 30 ㎡, 111 heat exchange area of reboiler
For 25 ㎡.
Second absorber, 115 diameter is 1000, high 3000mm, material 316L, and adsorbent is the mixing of 3-5mm high density
Adsorbent.
In conclusion the utility model provides a kind of F32 device by-product HCl purification apparatus, which includes HCl separation
Unit is adsorbed by drying unit, finished product rectification cell, and by-product HCl enters HCl separation tower by the first surge tank, prevents upstream
The fluctuation of production system has an impact the charging of HCl separation tower, stablizes output qualified products；Because HCl separation tower boils again
Device needs to heat, and is transformed to electric heating rectifying column, and bottom uses reboiler, and heat source is the condensation that fluorination reaction generates
Water makes full use of thermal energy, reaches energy-efficient purpose；The refrigerant of overhead condenser and condenser is using environmental protection in finished product rectification cell
Refrigerant F32, liquid F32 are directly entered in condenser, adjust condensation temperature by control F32 evaporation capacity；Feed cooler, production
Product cooler can cool down product, and the heat exchange area of elimination product rectifying column condenser and products pot is small, cooling effect is poor
The problem of；Chlorination hydrogen production tower reboiler heat source be compressor high-temperature gas, using gas after compression to chlorination hydrogen production tower again
It boils device and heat is provided, it is not only energy saving, while solving reboiler etching problem；Using the first absorber, drier to material
It is adsorbed, keeps micro heavy metal and fluorine-containing material intercepted, ensure that product purity.
The above is the citing of the utility model preferred forms, wherein the part that do not address in detail is this field
The common knowledge of those of ordinary skill.The protection scope of the utility model is based on the contents of the claims, any to be based on this reality
The equivalent transformation carried out with novel technical inspiration, is also within the protection scope of the utility model.
Claims (7)
1. a kind of F32 device by-product HCl purification apparatus, it is characterised in that:
The equipment includes HCl separative unit, is adsorbed by drying unit, finished product rectification cell, the HCl separative unit connection absorption
Drying unit, it is described to be adsorbed by drying unit connection finished product rectification cell；
Feed entrance, gas phase mouth, liquid phase is arranged in the HCl separative unit, including HCl separation tower, the HCl separation tower
Mouth and refluxing opening；
The feed entrance and refluxing opening of the HCl separation tower are connected with the lower end of the first surge tank, overhead condenser respectively
It is logical；
The gas phase mouth of the HCl separation tower, liquid phase mouth are connected with the lower end of the upper end of reboiler, reboiler respectively；
It is described to be adsorbed by drying unit, including the first absorber and drier；First absorber one end is connected to hydrogen chloride point
Gas outlet from tower, the other end on the other side are connected with drier；
The finished product rectification cell, comprising: the second surge tank, compressor, forecooler, chlorination hydrogen production tower reboiler, hydrogen chloride
Rectifying column, reactor product cooler, condenser, products pot, the second absorber；
Second surge tank is connected by compressor with chlorination hydrogen production tower reboiler；
The chlorination hydrogen production tower reboiler is connected with forecooler, hydrogen chloride rectifying column；
The hydrogen chloride rectifying column is provided with feed entrance, gas phase mouth, liquid phase mouth, refluxing opening and kettle liquid outlet；
The feed entrance and refluxing opening of the hydrogen chloride rectifying column are connected with the entrance of forecooler, condenser respectively；
The gas phase mouth of the hydrogen chloride rectifying column, liquid phase mouth respectively with the upper end of chlorination hydrogen production tower reboiler, chlorination hydrogen production
The lower end of tower reboiler is connected；
The kettle liquid outlet of the hydrogen chloride rectifying column is connected with the second absorber, and the second absorber is connected with reactor product cooler
Logical, reactor product cooler is connected with products pot.
2. a kind of F32 device by-product HCl purification apparatus according to claim 1, it is characterised in that:
The HCl separation tower is packed tower, and diameter 800mm, high 35980mm, for material using Q345R, filler is high density silk
Net filler；
The reboiler heat exchange area is 50 ㎡, and condenser (103) heat exchange area is 80 ㎡.
3. a kind of F32 device by-product HCl purification apparatus according to claim 1, it is characterised in that:
The hydrogen chloride rectifying column is packed tower, diameter 400mm, high 25789mm.
4. a kind of F32 device by-product HCl purification apparatus according to claim 1, it is characterised in that:
The first absorber diameter 1600mm, high 4000mm, material use Q345R, and adsorbent is 3-5mm active carbon.
5. a kind of F32 device by-product HCl purification apparatus according to claim 1, it is characterised in that:
The drier, diameter are 1600 mm, and high 4000mm, for material using Q345R, adsorbent is the 5A molecular sieve of 3-5mm.
6. a kind of F32 device by-product HCl purification apparatus according to claim 1, it is characterised in that:
The condenser heat exchange area is 20 ㎡, and forecooler (109) heat exchange area is 30 ㎡, and the chlorination hydrogen production tower boils again
Device, heat exchange area are 25 ㎡.
7. a kind of F32 device by-product HCl purification apparatus according to claim 1, it is characterised in that:
The second absorber diameter is 1000 mm, high 3000mm, material 316L, and adsorbent is 3-5mm high density mixing and absorption
Agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201821987147.4U CN209442638U (en) | 2018-11-29 | 2018-11-29 | A kind of F32 device by-product HCl purification apparatus |
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| CN201821987147.4U CN209442638U (en) | 2018-11-29 | 2018-11-29 | A kind of F32 device by-product HCl purification apparatus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113499741A (en) * | 2021-08-10 | 2021-10-15 | 聊城氟尔新材料科技有限公司 | Difluoromethane reaction gas separation device and method and application thereof |
| CN115646125A (en) * | 2022-11-08 | 2023-01-31 | 瑞燃(上海)环境工程技术有限公司 | System and method for purifying and recycling high-concentration hydrogen chloride tail gas |
-
2018
- 2018-11-29 CN CN201821987147.4U patent/CN209442638U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113499741A (en) * | 2021-08-10 | 2021-10-15 | 聊城氟尔新材料科技有限公司 | Difluoromethane reaction gas separation device and method and application thereof |
| CN115646125A (en) * | 2022-11-08 | 2023-01-31 | 瑞燃(上海)环境工程技术有限公司 | System and method for purifying and recycling high-concentration hydrogen chloride tail gas |
| CN115646125B (en) * | 2022-11-08 | 2023-10-31 | 瑞燃(上海)环境工程技术有限公司 | System and method for purifying and recycling high-concentration hydrogen chloride tail gas |
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