CN108373139A - The retracting device and recovery method of sulfur dioxide in a kind of Sucralose chlorination reaction - Google Patents
The retracting device and recovery method of sulfur dioxide in a kind of Sucralose chlorination reaction Download PDFInfo
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- CN108373139A CN108373139A CN201810038349.2A CN201810038349A CN108373139A CN 108373139 A CN108373139 A CN 108373139A CN 201810038349 A CN201810038349 A CN 201810038349A CN 108373139 A CN108373139 A CN 108373139A
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- trichloroethanes
- condenser
- tail gas
- sulfur dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/56—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The present invention relates to a kind of recovery methods of sulfur dioxide in Sucralose chlorination reaction, include the following steps：1. the concentrated sulfuric acid is added into drying tower, the tail gas from gas-liquid separator is removed into moisture, the sulfur dioxide, trichloroethanes tail gas after drying enter first-stage condenser；2. condensate liquid and residual exhaust through first-stage condenser enter trichloroethanes knockout drum, sulfur dioxide, trichloroethanes condensate liquid enter collecting tank, tail gas sulphur dioxide enters secondary condenser；3. sulfur dioxide condensate liquid and tail gas through secondary condenser enter three-level condenser, at 25 DEG C to 30 DEG C, gaseous sulfur dioxide is condensed into liquid and is sent into recycling storage tank three-level condenser temperature.Beneficial effects of the present invention：It being separated by being absorbed hydrogen chloride in tail gas at higher concentration hydrochloric acid, while by trichloroethanes, sulfur dioxide in chlorinated exhaust through tertiary effluent, improving the conversion ratio of product, reducing the consumption of raw material and energy, save every cost consumption to greatest extent.
Description
Technical field
The invention belongs to food additives production fields, are related to a kind of production of Sucralose, and in particular to a kind of trichlorine sugarcane
The retracting device of sulfur dioxide in sugared chlorination reaction further relates to a kind of recycling side of sulfur dioxide in Sucralose chlorination reaction
Method.
Background technology
Key intermediate during sucralose-6-ester is produced as Sucralose, by sucrose-6-ester with chlorinating agent suitable
Under the conditions of chlorination be made.Common chlorinating agent has two classes：One is Vi l s me i e r chlorinating agents, another kind is
Thionyl chloride/pyridine/chlorohydrocarbon ternary chlorine generation.Most domestic Sucralose manufacturing enterprise mostly uses the Vi l s of the first kind
Mei er chlorinating agents are as chlorination raw material.
Sulfur dioxide is will produce out during preparing Vi l s mei er chlorinating agents, domestic technique focuses mostly at present
In the separation of chlorination and chlorinated product, to SO2Processing mostly use lye neutralization method, rarely have to SO2It is recycled
Processing.Patent publication No. is to provide a kind of method of Deep Cooling Method recovering liquid sulfur dioxide, the party in CN106466548A
Method saves a large amount of alkali lye consumptions, will not generate new waste, but finds that there are still problems in producing：1, two level is cold
Trichloroethanes water content is higher in condensing gas after solidifying；2, a small amount of HCl enters first-stage condenser and secondary condenser, is filled to cooling
It sets with compared with strong corrosive；3, the presence of a small amount of HCl not only shortens the service life of cooling device, while also having certain
Security risk.
Invention content
The purpose of the present invention is to solve defect in the prior art, sulfur dioxide in a kind of Sucralose chlorination reaction is provided
Retracting device and recovery method.
In order to achieve the above object, the technical solution adopted in the present invention is：
The retracting device of sulfur dioxide in a kind of Sucralose chlorination reaction, using following equipment in prior art：Water scrubber, water
Wash tower cycle condenser, water scrubber pump, gas-liquid separator, roots blower, first-stage condenser, secondary condenser, recycling storage tank, screen
Cover pump；
Sucralose tail gas is entered by pipeline from washing tower bottom, is absorbed with the water lotion at the top of water scrubber, water
It washes another outlet of tower bottom water scrubber pump, water scrubber cycle condenser are connected serially at the top of water scrubber by pipeline, water lotion exists
Under water scrubber pumping action, cyclic absorption is participated in after the condensation of water scrubber cycle condenser；Water scrubber absorb after tail gas from washing
Top of tower enters gas-liquid separator by pipeline and is detached, and the separation water that gas-liquid separator comes out returns to water scrubber by pipeline
It uses again, gas-liquid separator top duct is connected with roots blower, by tail gas by sequentially entering first-stage condenser, B-grade condensation
Device；Condensate liquid and residual exhaust in secondary condenser out enter recycling storage tank together；
Characterized by further comprising：
Gas-liquid separator top duct is changed to be connected with the bottom inlet of drying tower by a. drying tower, and dry tower bottom passes through pipe
Road pumps drying tower, recirculation cooler is connected serially at the top of drying tower, and drying tower centre exit passes through pipeline and tail gas storage tank phase
Even, tail gas storage pot bottom is connected to first-stage condenser top entry by roots blower；
B. trichloroethanes knockout drum, first-stage condenser bottom are connected by pipeline with trichloroethanes knockout drum top entry, trichlorine
Ethane separation pot bottom is connected by pipeline with trichloroethanes collecting tank top entry, and trichloroethanes collects pot bottom and passes through trichlorine
Ethane pump is connected to trichloroethanes storage tank, and trichloroethanes knockout drum top exit passes through pipeline and secondary condenser top entry phase
Even, trichloroethanes collecting tank top exit is connected by pipeline with tail gas storage tank top entry；
C. three-level condenser, secondary condenser bottom are connected by pipeline with three-level condenser overhead, three-level condenser overhead and
Bottom is connected by pipeline with recycling storage tank respectively；
The recovery method of sulfur dioxide in a kind of Sucralose chlorination reaction, it is characterised in that include the following steps：
1. the concentrated sulfuric acid is added into drying tower, the concentrated sulfuric acid at drying tower bottom is pumped through drying tower to be conveyed and after recirculation cooler exchanges heat
At the top of into drying tower, the tail gas from gas-liquid separator enters from dry tower bottom to be dried with the concentrated sulfuric acid that tower top gets off
Moisture is removed, control drying tower temperature is at 40 DEG C to 45 DEG C, the tail gas after drying（Sulfur dioxide, trichloroethanes）From drying tower
Portion out enters tail gas storage tank, the tail gas in tail gas storage tank sent under the action of roots blower to primary cycle condenser into
Row condensation；
2. entering trichloroethanes knockout drum together through the condensed condensate liquid of first-stage condenser and residual exhaust, in trichloroethanes point
Natural separation, the condensate liquid after separation are carried out from condensate liquid in tank and residual exhaust（Trichloroethanes）It is collected into trichloroethanes
Tank, the residual exhaust after separation（Sulfur dioxide）It is condensed into secondary condenser；
3. in trichloroethanes collects groove tank, condensate liquid is pumped into trichloroethanes storage tank by trichloroethanes, and gas phase passes through pipeline
Tail gas storage tank is returned to use again；
4. through the condensed condensate liquid of secondary condenser（Sulfur dioxide）And residual exhaust（Sulfur dioxide）It is cold to enter three-level together
Condenser makes the control of three-level condenser temperature at -25 DEG C to -30 DEG C, through three-level condenser to three-level condenser conveying deep cooling brine
After condensation, most of gaseous sulfur dioxide is condensed into liquid, and residual exhaust and condensed sulfur dioxide liquid are sent together
Enter to recycle storage tank.
Beneficial effects of the present invention：By being absorbed hydrogen chloride in tail gas at higher concentration hydrochloric acid byproduct through tertiary effluent
In the process, while sulfur dioxide in chlorinated exhaust being separated and compresses and is cleaned into sulfur dioxide liquid product.Real-time control
The period of reaction, make reaction process is steady, reaction faster more fully；The loss for reducing equipment improves the conversion ratio of product,
Shorten the production cycle；The consumption of raw material and energy is reduced, saves every cost consumption to greatest extent.
Description of the drawings
Fig. 1 is a kind of recovery process flow chart of sulfur dioxide in Sucralose chlorination reaction.
Specific implementation mode
As shown in Figure 1, in a kind of Sucralose chlorination reaction sulfur dioxide retracting device, using following in prior art
Equipment：Water scrubber, water scrubber cycle condenser, water scrubber pump, gas-liquid separator, roots blower, first-stage condenser, B-grade condensation
Device, recycling storage tank, canned motor pump；
Sucralose tail gas is entered by pipeline from washing tower bottom, is absorbed with the water lotion at the top of water scrubber, water
It washes another outlet of tower bottom water scrubber pump, water scrubber cycle condenser are connected serially at the top of water scrubber by pipeline, water lotion exists
Under water scrubber pumping action, cyclic absorption is participated in after the condensation of water scrubber cycle condenser；Water scrubber absorb after tail gas from washing
Top of tower enters gas-liquid separator by pipeline and is detached, and the separation water that gas-liquid separator comes out returns to water scrubber by pipeline
It uses again, the tail gas at the top of gas-liquid separator out sequentially enters first-stage condenser, two by pipeline under the action of roots blower
Grade condenser；Condensate liquid and residual exhaust in secondary condenser out enter recycling storage tank together；
Newly added equipment is as follows：
A. the top exit of drying tower, gas-liquid separator is connected by pipeline with the bottom inlet of drying tower, and dry tower bottom is logical
Piping pumps drying tower, recirculation cooler is connected serially at the top of drying tower, and drying tower centre exit is stored by pipeline and tail gas
Tank is connected, and tail gas storage pot bottom is connected to first-stage condenser top entry by roots blower；
B. trichloroethanes knockout drum, first-stage condenser bottom are connected by pipeline with trichloroethanes knockout drum top entry, trichlorine
Ethane separation pot bottom is connected by pipeline with trichloroethanes collecting tank top entry, and trichloroethanes collects pot bottom and passes through trichlorine
Ethane pump is connected to trichloroethanes storage tank, and trichloroethanes knockout drum top exit passes through pipeline and secondary condenser top entry phase
Even, trichloroethanes collecting tank top exit is connected by pipeline with tail gas storage tank top entry；
C. three-level condenser, secondary condenser bottom are connected by pipeline with three-level condenser overhead, three-level condenser overhead and
Bottom is connected by pipeline with recycling storage tank respectively.
Concrete operation step is as follows：
1. Sucralose tail gas（Hydrogen chloride, sulfur dioxide, trichloroethanes）Water scrubber is first passed around, washes away and carries secretly in gas
HCl, water washing cycles condenser is equipped in water scrubber and its connected water scrubber pumps, and makes in water scrubber washing temperature control 30
DEG C -38 DEG C, as Cl in water scrubber-When >=500ppm, by concentrated water（Hydrochloric acid）It is produced from gas-liquid separator bottom, in gas-liquid separator
Tail gas（Sulfur dioxide, trichloroethanes, Shao Liangshui）It is sent into drying tower；
2. 1500 L of the concentrated sulfuric acid is added to dry tower bottom, drying tower pump is opened, recirculated water is passed through into recirculation cooler, is controlled
Drying tower temperature processed removes a small amount of moisture, tail gas after drying at 40 DEG C -45 DEG C, in drying tower inner exhaust gas through concentrated sulfuric acid drying
（Sulfur dioxide, trichloroethanes）Into tail gas storage tank is entered, the tail gas in subsequent tail gas storage tank is under roots blower effect
It is sent into first-stage condenser and is condensed；
3. being set as -2Kpa when inlet of Roots blower pressure normal operating, start Roots when fan inlet pressure shows+1KPa
Wind turbine, blow in machine outlet valve, and fan inlet negative pressure is set in -2kpa, the tail gas to pressurize through roots blower（Sulfur dioxide, three
Chloroethanes）, it is condensed by the first-stage condenser of deep cooling salt water as medium, is passed through temperature≤- 27 DEG C of deep cooling brine, one
Grade condensator outlet temperature control is at -10 DEG C to -15 DEG C, through the condensed condensate liquid of first-stage condenser（Trichloroethanes）And residue
Tail gas（Sulfur dioxide）It is sent into trichloroethanes knockout drum together, condensate liquid carries out certainly with residual exhaust in trichloroethanes knockout drum
So separation, detaches to obtain condensate liquid（Trichloroethanes）And residual exhaust（Sulfur dioxide）；
4. the separating obtained condensate liquid of step 3（Trichloroethanes）Enter trichloroethanes collecting tank by pipeline, subsequent condensate liquid is logical
It crosses trichloroethanes and is pumped to trichloroethanes storage tank, the gas phase in trichloroethanes collecting tank returns to tail gas storage tank and uses again；
5. by the separating obtained residual exhaust of step 3（Sulfur dioxide）It is sent into secondary condenser to condense again, is passed through temperature≤- 27
DEG C deep cooling brine as refrigerant, control secondary condenser outlet temperature is cold by secondary condenser at -18 DEG C to -22 DEG C
Condensate liquid after solidifying（Sulfur dioxide）It is sent into three-level condenser together with residual exhaust；
6. being passed through the deep cooling brine of temperature≤- 27 DEG C into three-level condenser as refrigerant, three-level condensator outlet is controlled
For temperature at -25 DEG C to -30 DEG C, condensate liquid and residual exhaust in secondary condenser carry out profound level in three-level condenser
Condensation, condensed condensate liquid（Sulfur dioxide）With a small amount of tail gas（Sulfur dioxide）It is sent into recycling storage tank together, recycles storage tank
Gas phase is connected to the fan inlet of big system, liquid SO2It is pumped into sulfur dioxide dashpot through shielding.
The SO 2 in waste gas content that air is discharged into original technique still has 16% or so, the pungent sour gas of surrounding
Taste is still dense, obtains SO in tail gas in new process after the concentrated sulfuric acid is dried2Content ＞ 99.5%, purity higher；It is cold to increase three-level
System can recycle 3 tons of SO more daily after solidifying2, 1500 yuan per ton by the market price, 1,620,000 yuan of income can be increased every year, imitated
Benefit is significantly considerable.
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form；Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, every content without departing from technical solution of the present invention, according to the technical essence of the invention does above example
Any simple modification, equivalent replacement, equivalence changes and modification, still fall within technical solution of the present invention protection in the range of.
Claims (2)
1. the retracting device of sulfur dioxide in a kind of Sucralose chlorination reaction, including following equipment in prior art：Water scrubber,
Water scrubber cycle condenser, water scrubber pump, gas-liquid separator, roots blower, first-stage condenser, secondary condenser, recycling storage tank,
Canned motor pump；Sucralose tail gas is entered by pipeline from washing tower bottom, is absorbed with the water lotion at the top of water scrubber,
Water scrubber pump, water scrubber cycle condenser are connected serially at the top of water scrubber by another outlet of washing tower bottom by pipeline, water lotion
Under water scrubber pumping action, cyclic absorption is participated in after the condensation of water scrubber cycle condenser；Water scrubber absorb after tail gas from water
It washes top of tower gas-liquid separator is entered by pipeline and detached, the separation water that gas-liquid separator comes out passes through pipeline and returns to washing
Tower is used again, and gas-liquid separator top duct is connected with roots blower, by tail gas by sequentially entering first-stage condenser, B-grade condensation
Device；Condensate liquid and residual exhaust in secondary condenser out enter recycling storage tank together；
Characterized by further comprising：
Gas-liquid separator top duct is changed to be connected with the bottom inlet of drying tower by a. drying tower, and dry tower bottom passes through pipe
Road pumps drying tower, recirculation cooler is connected serially at the top of drying tower, and drying tower centre exit passes through pipeline and tail gas storage tank phase
Even, tail gas storage pot bottom is connected to first-stage condenser top entry by roots blower；
B. trichloroethanes knockout drum, first-stage condenser bottom are connected by pipeline with trichloroethanes knockout drum top entry, trichlorine
Ethane separation pot bottom is connected by pipeline with trichloroethanes collecting tank top entry, and trichloroethanes collects pot bottom and passes through trichlorine
Ethane pump is connected to trichloroethanes storage tank, and trichloroethanes knockout drum top exit passes through pipeline and secondary condenser top entry phase
Even, trichloroethanes collecting tank top exit is connected by pipeline with tail gas storage tank top entry；
C. three-level condenser, secondary condenser bottom are connected by pipeline with three-level condenser overhead, three-level condenser overhead and
Bottom is connected by pipeline with recycling storage tank respectively.
2. it is a kind of using device described in claim 1 to the recovery method of sulfur dioxide in Sucralose chlorination reaction, it is special
Sign is to include the following steps：
A. the concentrated sulfuric acid is added into drying tower, the concentrated sulfuric acid at drying tower bottom is pumped through drying tower to be conveyed and after recirculation cooler exchanges heat
At the top of into drying tower, the tail gas from gas-liquid separator enters from dry tower bottom to be dried with the concentrated sulfuric acid that tower top gets off
Remove moisture, control drying tower temperature at 40 DEG C to 45 DEG C, it is dry after comprising sulfur dioxide, trichloroethanes tail gas from drying
Out enter tail gas storage tank in the middle part of tower, the tail gas in tail gas storage tank send to primary cycle under the action of roots blower and condenses
Device is condensed；
B. enter trichloroethanes knockout drum together through the condensed condensate liquid of first-stage condenser and residual exhaust, in trichloroethanes point
Natural separation is carried out from condensate liquid in tank and residual exhaust, the condensate liquid comprising sulfur dioxide, trichloroethanes after separation enters
Trichloroethanes collecting tank, the residual exhaust sulfur dioxide after separation enter secondary condenser and are condensed；
C. in trichloroethanes collects groove tank, condensate liquid is pumped into trichloroethanes storage tank by trichloroethanes, and gas phase passes through pipeline
Tail gas storage tank is returned to use again；
D. enter three-level condenser together through the condensed sulfur dioxide condensate liquid of secondary condenser and remaining SO 2 tail gas,
Make the control of three-level condenser temperature at -25 DEG C to -30 DEG C to three-level condenser conveying deep cooling brine, is condensed through three-level condenser
Afterwards, most of gaseous sulfur dioxide is condensed into liquid, and residual exhaust and condensed sulfur dioxide liquid are sent into back together
Store up slot.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810038349.2A CN108373139A (en) | 2018-01-13 | 2018-01-13 | The retracting device and recovery method of sulfur dioxide in a kind of Sucralose chlorination reaction |
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| CN201810038349.2A CN108373139A (en) | 2018-01-13 | 2018-01-13 | The retracting device and recovery method of sulfur dioxide in a kind of Sucralose chlorination reaction |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205573A (en) * | 2018-07-23 | 2019-01-15 | 江苏焕鑫新材料股份有限公司 | A kind of acyl chloride reaction tail gas, which efficiently separates, utilizes technique |
| CN109503314A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of Sucralose produces the recovery method of trichloroethanes in tail gas |
| CN109574791A (en) * | 2018-12-10 | 2019-04-05 | 安徽金禾实业股份有限公司 | The recovery method of trichloroethanes in a kind of Sucralose tail gas |
| CN110368785A (en) * | 2019-01-30 | 2019-10-25 | 山东康宝生化科技有限公司 | A method of it solves to generate carbon black and air excess during Sucralose tail gas separation |
| CN110721493A (en) * | 2019-11-19 | 2020-01-24 | 安徽金禾实业股份有限公司 | Method for separating trichloroethane from crude sulfur dioxide |
| CN112742179A (en) * | 2020-12-11 | 2021-05-04 | 安徽金禾实业股份有限公司 | Method for treating chlorination tail gas in sucralose production |
| CN112933880A (en) * | 2021-02-04 | 2021-06-11 | 济源市恒通高新材料有限公司 | Sulfur dioxide recovery process and device for terephthaloyl chloride production tail gas |
| CN113391026A (en) * | 2021-06-11 | 2021-09-14 | 北京华澳维科技有限公司 | Rapid distillation method and detection method for sulfur dioxide |
| CN114225650A (en) * | 2021-11-23 | 2022-03-25 | 安徽金禾实业股份有限公司 | Sucralose chlorination high-temperature tail gas treatment device and method |
| CN115849308A (en) * | 2022-11-17 | 2023-03-28 | 安徽金禾实业股份有限公司 | Byproduct SO in sucralose production 2 Of (2) |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205573A (en) * | 2018-07-23 | 2019-01-15 | 江苏焕鑫新材料股份有限公司 | A kind of acyl chloride reaction tail gas, which efficiently separates, utilizes technique |
| CN109503314B (en) * | 2018-12-10 | 2021-10-22 | 安徽金禾实业股份有限公司 | Method for recovering trichloroethane in tail gas in sucralose production |
| CN109503314A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of Sucralose produces the recovery method of trichloroethanes in tail gas |
| CN109574791A (en) * | 2018-12-10 | 2019-04-05 | 安徽金禾实业股份有限公司 | The recovery method of trichloroethanes in a kind of Sucralose tail gas |
| CN110368785A (en) * | 2019-01-30 | 2019-10-25 | 山东康宝生化科技有限公司 | A method of it solves to generate carbon black and air excess during Sucralose tail gas separation |
| CN110368785B (en) * | 2019-01-30 | 2021-07-30 | 山东康宝生化科技有限公司 | Method for solving problems of carbon black generation and excessive air generation in sucralose tail gas separation process |
| CN110721493A (en) * | 2019-11-19 | 2020-01-24 | 安徽金禾实业股份有限公司 | Method for separating trichloroethane from crude sulfur dioxide |
| CN112742179A (en) * | 2020-12-11 | 2021-05-04 | 安徽金禾实业股份有限公司 | Method for treating chlorination tail gas in sucralose production |
| CN112933880A (en) * | 2021-02-04 | 2021-06-11 | 济源市恒通高新材料有限公司 | Sulfur dioxide recovery process and device for terephthaloyl chloride production tail gas |
| CN113391026A (en) * | 2021-06-11 | 2021-09-14 | 北京华澳维科技有限公司 | Rapid distillation method and detection method for sulfur dioxide |
| CN113391026B (en) * | 2021-06-11 | 2023-08-15 | 北京华澳维科技有限公司 | Sulfur dioxide rapid distillation method and detection method |
| CN114225650A (en) * | 2021-11-23 | 2022-03-25 | 安徽金禾实业股份有限公司 | Sucralose chlorination high-temperature tail gas treatment device and method |
| CN115849308A (en) * | 2022-11-17 | 2023-03-28 | 安徽金禾实业股份有限公司 | Byproduct SO in sucralose production 2 Of (2) |
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Application publication date: 20180807 |
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